Quality Assurance Program Plan

Quality Assurance Program Plan for Analytical Testing Laboratories Performing Analyses of Finished Medical
Marijuana Products and Marijuana-Infused Products in Massachusetts
Title: Quality Assurance Program Plan for Analytical Testing Laboratories

Performing Analyses of Finished Medical
The Protocol contains the following sections:
TABLE OF CONTENTS
1.0 SCOPE AND APPLICATION ....................................................................................... 5
2.0 PROBLEM STATEMENT ............................................................................................ 5
3.0 DECISION RULE......................................................................................................... 6
4.0 MONITORING REQUIREMENTS ................................................................................ 6
5.0 QUALITY MANAGEMENT SYSTEM ..........................................................................11
5.1 Laboratory Quality Assurance Manual ........................................................................11
5.2 General Requirements and Responsibilities for Laboratory Staff ................................11
5.2.1 Laboratory Staff ...................................................................................................11
5.2.2 Laboratory Management ......................................................................................12
5.2.3 Laboratory Quality Officer ....................................................................................12
5.2.4 Deputies and Points of Contact ............................................................................13
5.3 Personnel Experience, Training and Qualifications .....................................................14
5.3.1 Management Responsibility .................................................................................14
5.3.2 Training Goals .....................................................................................................15
5.3.3 Contracted Personnel ..........................................................................................16
5.3.4 Job Descriptions ..................................................................................................16
5.4 Standard Operating Procedures (SOPs) .....................................................................16
5.5 Laboratory Logbooks ..................................................................................................18
5.6 Instrument Data and Records .....................................................................................18
5.7 Electronic Logging ......................................................................................................19
5.8 Maintenance Logs.......................................................................................................19
5.9 Requests, Tenders, and Contracts..............................................................................19
5.10 Storage of Data...........................................................................................................20
5.11 Software Control .........................................................................................................20
5.11.1 In-House Software Tools .....................................................................................20
5.11.2 In-House Developed Software and Tools .............................................................21
6.0 Proper, Legal and Ethical Actions and Data Integrity Reporting - Policies, Training, and
Procedures .................................................................................................................21
6.1.1 Data Integrity Requirements ................................................................................22
6.1.2 Manual Integration Procedures ............................................................................23
7.0 PROCEDURE GUIDANCE ON SAMPLE HANDLING AND STORAGE .....................24
7.1 Sample Receipt and Sample Custody Requirements ..................................................24
7.1.1 Sample Temperature Measurement .....................................................................25
7.1.2 Chain-of-Custody Verification ..............................................................................26
7.1.3 Sample Storage ...................................................................................................26
7.1.4 Communicating Sample Receipt Issues ...............................................................26
7.1.5 Holding Times ......................................................................................................27
7.1.6 Subsampling and Homogenization.......................................................................27
8.0 DATA QUALITY INDICATORS ...................................................................................28
8.1 Precision .....................................................................................................................28
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8.2 Accuracy .....................................................................................................................28

8.3 Representativeness ....................................................................................................28
8.4 Comparability ..............................................................................................................28
8.5 Sensitivity ...................................................................................................................29
9.0 Validation of Methods .................................................................................................29
9.1 References: ICH Q2 (R1), USP <1225>, ISO/IEC 17025:2005, and FDA OAR ...........29
9.2 Validation Guidance for Quantitative Chemical Analyses ............................................31
9.2.1 System Suitability ................................................................................................31
9.2.2 Determination of the Limit of Detection (LOD) ......................................................31
9.2.3 Limit of Quantitation (LOQ) ..................................................................................35
9.2.4 Linear Range .......................................................................................................36
9.2.5 Accuracy ..............................................................................................................37
9.2.6 Precision (USP, ICH and ISO 17025) ..................................................................37
9.2.7 Selectivity/Specificity............................................................................................38
9.3 Validation Requirements for Demonstrating Selectivity in Chromatographic Chemical
Analysis ......................................................................................................................38
9.3.1 Retention Times...................................................................................................40
9.3.2 Peak Resolution...................................................................................................40
9.3.3 Peak Symmetry (Tailing Factor, T) .......................................................................40
9.3.4 Peak Purity (HPLC-UV Methods Only) .................................................................41
9.4 Validation Guidance for Microbiological Analyses .......................................................42
9.4.1 Environmental Control Samples ...........................................................................44
9.4.2 Negative Controls ................................................................................................44
9.4.3 Positive Culture Controls .....................................................................................44
9.4.4 Precision ..............................................................................................................45
9.4.5 Specificity ............................................................................................................45
9.4.6 Assay Ruggedness ..............................................................................................46
9.4.7 Re-Validation .......................................................................................................46
10.0 Quality Control Samples and Procedures ...................................................................46
10.1 General .......................................................................................................................46
10.2 Batch Quality Control Samples ...................................................................................48
10.2.1 Establishing Control Limits ...................................................................................48
10.2.2 QC Sample Data Review .....................................................................................49
10.2.3 QC Sample Documentation and Review ..............................................................50
10.3 Equipment ..................................................................................................................51
10.3.1 Testing, Inspection, Maintenance and Calibration of Support Equipment .............51
10.3.2 Testing, Inspection, Maintenance and Calibration of Analytical Equipment ..........52
10.3.3 Testing, Inspection, Maintenance and Calibration of Microbiological Equipment
and Support Equipment .......................................................................................55
10.4 Water for Analysis .......................................................................................................56
10.5 Preventative measures ...............................................................................................57
10.6 Lock Out and Tag Out Procedures..............................................................................57
11.0 Quality Assurance Activities........................................................................................57
11.1 Preventative Actions ...................................................................................................58
11.2 Complaints ..................................................................................................................58
11.3 Identifying and Recording Non-Conformances ............................................................59
11.4 Informal Corrective Actions .........................................................................................61
11.5 Performing Formal Corrective Action ..........................................................................61
11.5.1 Root Cause Analysis............................................................................................61
11.5.2 Assignment of Corrective Actions ........................................................................62
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11.5.3 Monitoring of Corrective Actions ..........................................................................62

11.6 Internal Audits .............................................................................................................62
11.7 External Oversight ......................................................................................................63
11.7.1 Confidential Business Information (CBI) Considerations ......................................63
11.7.2 Corrective Actions for Internal Audits and External Oversight ..............................64
11.8 Proficiency Test Samples............................................................................................64
11.8.1 PT Sample Handling, Analysis and Reporting ......................................................64
11.9 Management Review ..................................................................................................66
11.9.1 Management Review Topics ................................................................................66
11.10 Data Review, Verification, Validation and Reconciliation with DQOs ...........................67
11.11 Treatment of Out-of-Specification (OOS) results .........................................................69
12.0 REPORTING OF RESULTS .......................................................................................69
12.1 Significant Figures ......................................................................................................69
12.2 Reporting Results Obtained from Subcontractors .......................................................70
12.3 Reporting Not-Detected and Low-Level Results ..........................................................70
12.4 Amendments to Reports .............................................................................................70
12.5 MDPH-specific Reporting Requirements .....................................................................70
12.5.1 Report Template ..................................................................................................71
13.0 REFERENCES ...........................................................................................................80
Tables:
Table 1 Monitoring Requirements of Finished Plant Material for Massachusetts Registered
Medical Marijuana Dispensaries ............................................................................... 7
Table 2 Monitoring Requirements of Marijuana Resin and Concentrates for Massachusetts
Registered Medical Marijuana Dispensaries ............................................................. 8
Table 3 Monitoring Requirements of Marijuana Infused Products (MIPs) for Massachusetts
Registered Medical Marijuana Dispensaries ............................................................. 9
Table 4 Monitoring Requirements of Environmental Media and Water Sources for
Massachusetts Registered Medical Marijuana Dispensaries Product.......................10
Table 5 American Society for Testing and Materials Reagent Grade Water Specifications
ASTM D1193-06 (2011) ...........................................................................................57
Table 6 American Society for Testing and Materials ASTM D1193-06 (2011) ......................57
Table 7 Production Stage Classification for Medical Marijuana Products .............................74
Table 8 Microbiological Contaminant Analysis Symbol .........................................................77
Table 9 Pathogenic Bacteria Contaminant Analysis Symbol ................................................78
Appendix A Data Quality Objective (DQO) Tables .................................................................. A-1

Appendix B Data Review Instructions and Checklists.............................................................. B-1
Appendix C Report Template .................................................................................................. C-1
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Acronym Definition
AHP American Herbal Pharmacopeia
ASTM American Society for Testing and Materials
BAM FDA Bacteriological Analytical Manual
CBI Confidential Business Information
CCB Continuing Calibration Blank
CCV Continuing Calibration Verifications
cGMP Current Good Manufacturing Practices
COC Chain-of-Custody
DAD Diode Array Detection
DOC Demonstration of Capability
DOT Department of Transportation
DQI Data Quality Indicators
DQO Data Quality Objectives
EDD Electronic Data Deliverables
EPA United States Environmental Protection Agency
FDA United States Food and Drug Administration
ICH International Conference for Harmonization
IR Infrared
ISO International Organization for Standardization
LCL Lower Control Limit
LCS Laboratory Control Sample
LIMS Laboratory Information Management System
LOD Limit of Detection
LOQ The Limit of Quantitation
LWL Lower Warning Limit
LOD Limit of Detection
MDPH Massachusetts Department of Public Health
MIP Marijuana Infused Products
MMP Medical Marijuana Products
NIST National Institute of Standards and Technology
OOS Out-of-Specification
PE Performance Evaluation
POC Point-of-Contact
PT Proficiency Testing
QA Quality Assurance
QAPP Quality Assurance Program Plan
QC Quality Control
QMS Quality Management System
RMD Registered Marijuana Dispensary
RPD Relative Percent Difference
RSD Relative Standard Deviation
SAP Sampling and Analysis Plan
SOP Standard Operating Procedures
TNI The NELAC Institute
UCL Upper Control Limit
USP United States Pharmacopeia
VTSR Validated Time of Sample Receipt
WHO World Health Organization
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1.0 SCOPE AND APPLICATION
This document serves as sub-regulatory guidance for all laboratories performing testing for the
Massachusetts Department of Public Health (MDPH) Medical Use of Marijuana Program in
order to provide data of known and appropriate quality when conducting the MDPH Protocol for
Sampling and Analysis of Finished Medical Marijuana Products and Marijuana-Infused Products
for Massachusetts Registered Medical Marijuana Dispensaries, and the Protocol for Sampling
and Analysis of Environmental Media for Massachusetts Registered Medical Marijuana
Dispensaries, with related Exhibits 4 through 7. The practices that are described in this Quality
Assurance Program Plan (QAPP) are based upon the applicable guidance and regulations in 21
CFR Part 211, Subpart I (Current Good Manufacturing Practices [cGMP] for Finished
Pharmaceutical Products, Laboratory Controls), relevant United States Pharmacopeia (USP)
general chapters and methods, the International Conference for Harmonization (ICH)
Guidelines, and the international standard requirements of ISO/IEC 17025:2005, The 2009 EL
TNI (The NELAC Institute) Standard, Standard American Herbal Pharmacopeia (AHP), United
States Food and Drug Administration (FDA) methods and guidance from relevant reference
methods listed in the Appendix A Table 01 (Method Reference Table).
This document provides guidance on general procedures for laboratory operations including, for
example, method validation, quality control (QC) sample analysis, and data review, reporting of
results, as they relate to method compliance, laboratory systems, and overall good laboratory
practices. In general, the document describes acceptable approaches for meeting the
requirements of the existing MDPH protocols, incorporating best practices to the extent
necessary for acceptable data. This document provides guidance within which the laboratories
are to implement technical procedures to produce an objective account of reliable sample
handling and analysis from the time of receipt of the sample, to the time analysis. Guidance is
also provided for data reduction, data review, and final reporting of results. This document is
meant to provide the Good Laboratory Practices for laboratory operations described in the
attestation required by MDPH in the medical marijuana license application:
“I, on behalf of the laboratory, attest that the laboratory will use Good Laboratory
Practices for laboratory operations consistent with DPH guidance described in the
Quality Assurance Program Plan for Analytical Testing Laboratories Performing
Analyses of Finished Medical Marijuana Products and Marijuana-Infused Products
in Massachusetts.”
In order to outline the required Good Practices more clearly in

this document, they are presented in italics. As compliance can Required Good
be shown in a number of ways depending on the laboratory’s Laboratory Practices
processes, additional guidance on possible implementation
approaches and suggestions for more robust compliance than are presented in italics
the minimum is displayed in grey boxes. These grey boxes are in this document.
not meant to be requirements and are only provided as
assistance to the laboratories in their compliance efforts.
2.0 PROBLEM STATEMENT
A set of minimum standards for laboratory performance is required to assure that data
submitted from the analysis of medical marijuana products and related matrices is of known and
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appropriate quality. Within laboratory quality management systems such as ISO/IEC

17025:2005 and ISO-based standards such as the TNI Standard, USP, ICH and cGMP, critical
references are made to client needs and specifications, and to the required level of confidence
or method performance for the application of the testing method. Those requirements, including
how method performance is to be validated, documented and communicated, and how the data
are to be reported have not, prior to the issuance of this QAPP, been clearly defined.
3.0 DECISION RULE
Materials subject to analysis under the MDPH Protocol for Sampling and Analysis of Finished
Medical Marijuana Products and Marijuana-Infused Products for Massachusetts Registered
Medical Marijuana Dispensaries (MMJ_PR_3.0_020516) are to be analyzed using the current
version of the MDPH protocols listed below:
 Exhibit 4. Analysis Requirements and Recommended Limits for Metals in Finished

Medical Marijuana Products
 Exhibit 5. Minimum Analysis Requirements for Residues of Pesticides and Plant Growth
Regulators Commonly Used in Cannabis Cultivation
 Exhibit 6. Analysis Requirements for Microbiological Contaminants and Mycotoxins in
Medical Marijuana Products
 Exhibit 7 (a). Concentration Limits for Residual Solvents
 Exhibit 7 (b). Concentration Limits for Residual Levels of Propane, n-Butane, or
Iso-Butane, as Revised, November 23, 2016.
Direction, on which materials are to be subjected to given protocol sections (Exhibits), is

provided in Exhibit 8 (b). Laboratory Testing Flowchart.
The response to laboratory results is described and defined in Exhibit 8 (a). Actions in
Response to Laboratory Analytical Results. The first decision point in the workflow depicted in
Exhibit 8 (a) is the determination of whether the analytical results are valid with respect to the
requirements. This is determined by evaluation of the validation and verification indicators and
data quality indicators identified in this document.
4.0 MONITORING REQUIREMENTS
The protocols for the analysis of marijuana and marijuana products have requirements
applicable to the different product types for contaminants as well as for the potency value of
cannabinoids. These requirements are summarized by product type on Tables 1-4 with the
established action limits prescribed in Exhibits 4-7 of the MDPH Protocol for Sampling and
Analysis of Finished Medical Marijuana Products and Marijuana-Infused Products for
Massachusetts Registered Medical Marijuana Dispensaries (MMJ_PR_3.0_020516). The data
quality objectives are outlined in Appendix A and the specific requirements for the analysis by
technology are described in Section 10.3 of this document.

Table 1 Monitoring Requirements of Finished Plant Material for Massachusetts

Registered Medical Marijuana Dispensaries
Product Type Analyte Class Analyte(s) Action Limit Comment

1
Finished Plant Pesticides Exhibit 5 List 10 ppb or 5% of MDPH Protocol
Material (all) (MDPH Protocol and any EPA established MMJ_PR_3.0_020516,
MMJ_PR_3.0_0 additional tolerance of Section 7.3
20516, pesticides residue
Exhibit 5) analyzed
2 3
Finished Plant Metals As, Cd, Pb, As: 1500 /200 If passes limits for Exhibit 4(b)
Material (Final (MDPH Protocol Hg (total) µg/kg for ingestion only but not Exhibit
2 3
Point of Sale) MMJ_PR_3.0_0 Cd: 500 /200 4(a) for all uses then refer to
20516, µg/kg protocol Section 7.2 for labeling
2 3
Exhibit 4) Pb: 1000 /500 requirements
µg/kg
Hg (total):
2 3
1500 /200
µg/kg
5
Bacteriological Aerobic Plate < 10 CFU/g
contaminants Count
4
(MDPH Protocol Total Yeast < 10 CFU/g
MMJ_PR_3.0_0 and Mold
3
20516, Total Coliform < 10 CFU/g
Exhibit 6) and E. Coli
3
Bile Tolerant < 10 CFU/g
Gram-
Negative
Pathogenic E. Not Detected in
Coli and 1g
Salmonella
4
Mycotoxins < 20 µg of any
mycotoxin per
kg material
9
Cannabinoid Δ THC, CBD, N/A
Profile THCa, CBDa (Report Results)
1
Pesticide compound as referenced in MMJ_PR_3.0_020516, Exhibit 5: bifenazate, bifenthrin, cyfluthrin,
etoxazole, imazalil, imidacloprid, myclobutanil, spiromesifen, trifloxystrobin
2
MMJ_PR_3.0_020516 Exhibit 4b – Ingestion Only
3
MMJ_PR_3.0_020516 Exhibit 4a – All Use
4
Mycotoxins is defined in the MDPH protocols as the sum of aflatoxin B1 (AFB1), B2 (AFB2), G1 (AFG1)
and G2 (AFG2)

Table 2 Monitoring Requirements of Marijuana Resin and Concentrates for

Massachusetts Registered Medical Marijuana Dispensaries
Product Analyte Class Analyte Action Comment

Type Limit
Marijuana Solvents Exhibit 7(a) Exhibit 7(a)
Resin and (MDPH Protocol and 7(b) and 7(b)
Concentrates MMJ_PR_3.0_020516,
5
(All) Exhibit 7) Butane 12 mg/kg
Metals As, Cd, Pb, As: If passes limits for Exhibit
6 7
(MDPH Protocol Hg (total) 1500 /200 4(b) for ingestion only but
MMJ_PR_3.0_020516, µg/kg not Exhibit 4(a) for all uses
Exhibit 4) Cd: then refer to protocol
2 3
500 /200 Section 7.2 for labeling
µg/kg requirements
Pb:
2 3
1000 /500
µg/kg
Hg (total):
2 3
1500 /200
µg/kg
5
Marijuana Bacteriological Aerobic < 10 CFU/g
Resin and contaminants Plate Count
4
Concentrates (MDPH Protocol Total Yeast < 10 CFU/g
(Final Point of MMJ_PR_3.0_020516, and Mold
3
Sale) Exhibit 6) Total < 10 CFU/g
Coliform and
E. Coli
3
Gram-
Negative
Pathogenic Not
E. Coli and Detected in
Salmonella 1g
1
Mycotoxins < 20 µg of
any
mycotoxin
per kg
material
9
Cannabinoid Profile Δ THC, N/A
CBD, (Report
THCa, CBDa Results)
5
Circulation letter: DHCQ 16-11-663, November 23, 2016. Analysis Requirements for Residual Solvents
in Cannabis Oil.
6
7

Table 3 Monitoring Requirements of Marijuana Infused Products (MIPs) for

Massachusetts Registered Medical Marijuana Dispensaries
Product Type Analyte Class Analyte Action Limit Comment

5
MIPS (all) Bacteriological Aerobic Plate < 10 CFU/g
contaminants Count
4
3
3
Gram-
Negative
Coli and 1g
Salmonella
8
mycotoxin per
kg material
9
Cannabinoid Δ THC, CBD, N/A
Profile THCa, CBDa (Report Results)
8
and G2 (AFG2)

Table 4 Monitoring Requirements of Environmental Media and Water

Sources for Massachusetts Registered Medical Marijuana Dispensaries
Product
Product Type Analyte Class Analyte Action Limit Comment

9
Soil and Growth Pesticides Exhibit 5 and 10 ppb or 5% of Protocol Section 7.3
Media, Water (MDPH Protocol any additional EPA established
Sources MMJ_PR_3.0_0 pesticides tolerance of
20516, analyzed residue
Exhibit 5)
10 11
Metals As, Cd, Pb, As: 1500 /200 If passes limits for Exhibit 4(b)
(MDPH Protocol Hg (total) µg/kg for ingestion only but not Exhibit
2 3
MMJ_PR_3.0_0 Cd: 500 /200 4(a) for all uses then refer to
20516, µg/kg protocol Section 7.2 for labeling
2 3
Exhibit 4) Pb: 1000 /500 requirements
µg/kg
Hg (total):
2 3
1500 /200
µg/kg
5
Water Sources Bacteriological Aerobic Plate < 10 CFU/g
contaminants Count
4
3
3
Gram-
Negative
Coli and 1g
Salmonella
12
mycotoxin per
kg material
9
Pesticide compound as referenced in MMJ_PR_3.0_020516, Exhibit 5: bifenazate, bifenthrin, cyfluthrin,
etoxazole, imazalil, imidacloprid, myclobutanil, spiromesifen, trifloxystrobin
10
11
12
and G2 (AFG2)

5.0 QUALITY MANAGEMENT SYSTEM
The laboratory shall establish and maintain a quality management system based on the
required elements contained in this section and the requirements set forth in the most current
version of MDPH protocols and ISO/IEC 17025. The quality management system is to be
appropriate for the type, range, and volume of medical marijuana testing activities undertaken
by the laboratory. The elements of the QC system shall be documented in the laboratory’s
Quality Assurance Manual (QAM).
5.1 Laboratory Quality Assurance Manual
The Laboratory Quality Assurance Manual (QAM) and related quality documentation shall
present the laboratory’s quality management system (QMS) with the requirements contained
in clause 4 of ISO 17025 and additional requirements addressing the guidance in this
document and laboratory supplemental quality procedures that support the goal of
continuous improvement.
A Laboratory QAM should address all elements that relate to the ISO 17025 Clause 4
requirements and any other activities that support compliance to these requirements;
however, it does not need to contain all of the detail of each of these activities. For the ease
of document revisions and approvals, the QAM may reference independent SOPs that
contain the detailed procedures. In this way, one part of the lab QMS can be revised without
necessitating a change to the entire manual.
The Quality Assurance Manual shall include the following information on the title page:
document title, the laboratory’s complete name and address, the name of the Quality
Assurance Officer (however named), the identification of all major organizational units that
are to be covered by the Laboratory Quality Assurance Manual, and the effective date of the
version.
The most current ISO 17025 and this document are to be referenced for guidance when
establishing a laboratory quality management system and preparing the Laboratory Quality
Assurance Manual.
5.2 General Requirements and Responsibilities for Laboratory Staff
5.2.1 Laboratory Staff
Laboratory staff members are responsible for the following activities:
 Performing procedures in accordance with the SOPs, project-specific

requirements, and policies set forth by the laboratory management. In this
context, the requirements of this QAPP are referred to as project-specific
requirements.
 Understanding and implementing the QA/QC requirements that pertain to their

organizational/technical function.

 Each technical staff member is to have a combination of experience, education,

and training to demonstrate adequately a specific knowledge and understanding
of his/her individual responsibilities and a general knowledge of laboratory
operations, test methods, QA/QC procedures, and records management.
5.2.2 Laboratory Management
The laboratory management is responsible for the following activities:
 Appointing of a technical manager that has appropriate education and experience to

have the ultimate responsibility over all decisions in the laboratory pertaining to
technical issues, however defined by the laboratory, such as method development,
staff technical training, stop and start work authorization, equipment maintenance and
monitoring and evaluation of client requests pertaining to laboratory technical
capabilities.
 Assuring that the laboratory has sufficient personnel with the appropriate education,
training, technical knowledge, and experience to perform their assigned functions.
 Assuring that the laboratory has appropriate, secure, well-maintained facilities and
equipment for the safe, successful conduct of analysis.
 Defining the minimum level of qualification, experience, and skills necessary for all
positions in the laboratory. In addition to education and/or experience, basic
laboratory skills such as using a balance, pipetting, and performing quantitative
techniques are to be considered.
 Assuring that all technical laboratory staff members have demonstrated capability in
the activities for which they are responsible. Such initial and ongoing demonstrations
are to be documented in personnel training files.
 Assuring that all technical laboratory staff members understand, have access to, and
conduct work in accordance with specific requirements provided by the Registered
Marijuana Dispensary (RMD) and those requirements established in the MDPH
protocols.
 Ensuring that thorough and accurate documentation of all analytical and operational
activities of the laboratory is conducted and maintained.
 Providing supervision or providing for supervision of all personnel employed by the

laboratory.
 Safety training and maintenance of safety records.
5.2.3 Laboratory Quality Officer
The laboratory shall appoint a staff member at management level as Laboratory Quality
Officer and this person’s duties shall be separate from production activities that may
apply undue pressures to the decisions regarding compliance and data quality. This

Quality Officer shall have the responsibilities listed in ISO 17025:2005 Section 4.1.5 and
authority in decisions where production and quality are in conflict.
In small laboratories, it may be necessary for one person to hold both technical manager
and quality officer authorities and responsibilities. If this is the case, it should be clear in
laboratory procedures which position holds ultimate responsibility and authority for
decisions that relate to quality, technical, operational concerns. It is important that the
QMS provides for the person to have direct access to the highest level of management.
5.2.4 Deputies and Points of Contact
The laboratory management, however defined in the laboratory procedures, is to appoint

deputies with the appropriate qualifications in the event of an extended absence of
longer than one week. The responsibility for the technical data and quality decisions is to
be clearly outline in the position descriptions to show authority when conflicts between
production and quality arise.
The laboratory is to designate a single point of contact (POC) and an alternate to act as
the primary RMD contact responsible for timely identification and resolution of any and
all issues. The POC is responsible for the following activities:
 Returning any phone calls initiated by the RMD or its designated consultant to
the laboratory in a timely manner (i.e., within 1-2 hours) on a normal business
day if the POC (or alternate) is not available at the initiation of the phone call.
 Initiating frequent communications with appropriate RMD personnel or the

designated consultant during project activities that involve sampling and analysis.
Note: If the POC shall be unavailable for more than 3-business days, the RMD
and/or its designated consultants are to be notified. In this notification, the
laboratory is to provide contact information for the appropriate alternate contact.
 Providing prompt verbal, text, or e-mail communication of any nonconformance

observed during sample receipt to appropriate RMD personnel or the RMD’s
designated consultant as soon as possible but always within 24 hours (preferably
3 hours, beginning with the normal business day immediately following for
problems noted during second shifts or weekends) of discovery. Problems may
include, but are not limited to, broken bottles, errors, or ambiguities in paperwork,
insufficient sample volume/weight, preservation checks outside of acceptance
criteria, and elevated receipt and/or storage temperature. Nonconformance upon
sample receipt that does not meet the laboratory sample acceptance policy is to
result in the rejection of samples if the condition does not meet the criteria in
Appendix A, Table 02.
 When sample receipt issues are discovered after hours, impacting samples with
short holding times (< 24 hours remaining), the laboratory is to contact the RMD
as soon as possible following discovery with follow-up during normal business
hours.

 The POC is responsible for day-to-day activities associated with the

management of the various analytical activities. These duties include scheduling
analyses, oversight, and assignment of any activities related to client services.
 The laboratory is responsible for identifying associated QC failures that require

decisions pertaining to resampling, repreparation, reanalysis, and report
amendments and keeping records supporting the decisions.
 In the event that the laboratory becomes aware of any changes in local, state or
federal regulations, state certification, analytical methodology, sampling
regulation, Department of Transportation (DOT) regulations, or any other
information that may affect the RMD sampling and/or analytical programs, the
POC is to confirm the request for analysis with the RMD as soon as practical.
5.3 Personnel Experience, Training and Qualifications
All sample analyses described in the MDPH protocols and governed by this QAPP are to be
conducted by a laboratory that is either:
 Accredited to International Organization for Standardization (ISO) 17025 by a third

party accrediting body such as A2LA or ANAB, or PJLA; or
 Certified, registered, or accredited by an organization approved by the MDPH.
Further requirements concerning the eligibility and responsibilities of analytical

laboratories are provided in 105 CMR 725.105(C)(2). In addition to the regulatory
qualifications and requirements referenced above, the laboratory is to have a
demonstrated ability to perform the specific analytical methods required and to
provide complete records and a robust quality assurance system.
5.3.1 Management Responsibility
Laboratory management is to ensure the competence of all who operate specific

equipment, perform tests and/or calibrations, evaluate results, and review and
approve client reports. Appropriate supervision shall be provided to staff that are
undergoing training. Personnel performing specific tasks are to be qualified based
on appropriate education, training, experience, and/or demonstrated skills as
required.
The laboratory management is to authorize specific personnel to perform particular

types of sampling, testing, and/or equipment calibration, issue test reports, review,
and interpret data, and to operate particular types of equipment. The laboratory is to
maintain records of the relevant authorization(s), competence, educational and
professional qualifications, training, skills, and experience of all technical personnel,
including contracted personnel. This information is to be readily available and
include the date on which authorization and/or competence is confirmed.
The laboratory management is responsible for the following personnel training

activities:

 Assuring that the training of each member of the technical staff is maintained
up-to-date (ongoing).
- Records are to be on file demonstrating that each employee has read,

understand, and is using the latest version of the applicable SOPs and the
laboratory’s in-house quality documentation that relates to his/her job
responsibilities.
- Training courses or workshops on specific equipment, analytical

techniques, or laboratory procedures are to be documented.
- Training courses in ethical and legal responsibilities, including the

potential disciplinary actions and penalties for improper, unethical, or
illegal actions are to be documented.
- Analyst training shall be considered up-to-date if his/her training file

contains certifications that he/she has read and understands the most
recent version of the test method (the approved method or standard
operating procedure) and associated supporting procedural and guidance
documents; documentation of continued proficiency for all parameters
performed is to be demonstrated by at least one of the following once per
year:
- Records of at least four separately prepared, separately analyzed, non-

consecutive laboratory control samples with acceptable levels of precision
and accuracy. This is required for all initial demonstrations of capability.
After initial demonstration of capability, acceptable analysis of an ISO
17043 proficiency test sample or four passing laboratory control sample
(LCS) samples from routine analyses are valid as an ongoing
demonstration of capability.
- The laboratory’s training procedures are to define clearly when an analyst

is able to independently perform analyses and report data. There is to be
a clear record of the completion of initial training and approval to work
independently in the area of training.
- An authorized technical staff member is to oversee work of a technical

staff member in training and both staff members are to be identified in the
analysis record to show that training was occurring.
5.3.2 Training Goals
Laboratory management is to communicate and establish goals with respect to

education, training, and skills of the laboratory personnel. The laboratory is to have
a procedure for identifying ongoing training needs and providing training of
personnel. The training program is to be relevant to the present and anticipated
tasks of the laboratory. The effectiveness of the training actions taken is to be
evaluated and recorded as approved for the training to be considered complete.

5.3.3 Contracted Personnel
The laboratory is to use personnel who are employed by, or under contract to, the
laboratory. Regardless of the type of employment contract, the personnel are to
adhere to the requirements in the laboratory quality management system and the
guidance provided herein.
5.3.4 Job Descriptions
The laboratory is to maintain current job descriptions for managerial, technical, and
key support personnel involved in testing, data reduction and review and approval of
reports.
The following elements are needed in job descriptions:
 Responsibilities with respect to performing tests;

 Responsibilities with respect to the planning of testing and review of results;
 Responsibilities for reporting, review and approval of client reports;
 Responsibilities for performing method modification and method development
and validation of new methods;
 Expertise and experience required;
 Qualifications and training needed to fulfill the responsibilities; and
 Managerial duties.
5.4 Standard Operating Procedures (SOPs)
Standard Operating Procedures (SOPs) shall be developed by the laboratory for every
activity performed during standard laboratory operation. This includes quality
procedures, technical procedures, and any activities that support those activities
including software, administrative, and calculation procedures. These procedures shall
contain enough detail to perform the methods and shall be consistent with the current
activities relevant to that SOP. In the instance where the procedures do not reflect
current activities, they shall be revised according to a laboratory document control
procedure, and this revision is to be tracked within the document for historical review
purposes. SOPs detailing the laboratory’s procedures are to be maintained under a
formal document control system that includes a unique identification system and the
retrieval/accounting of all outdated versions. SOPs are to be reviewed and updated
when there is a change in the method, activity, or material such that the SOP is
consistent with the method and laboratory procedures. A documented (including signoff)
review of all SOPs is required at a frequency required by the laboratory’s accreditation
standards or own procedures. Laboratory SOPs are to be stored in a manner that
provides protection from catastrophic loss (such as a fire).
The quality assurance (QA) department is to have a formal system for the distribution,
tracking, and archiving of SOPs, logbooks, electronic logs, notebooks, and any other
controlled documents. Periodic (monthly or quarterly, depending on usage) documented
supervisory or peer review is to be performed on all logbooks and electronic logs utilized
throughout the laboratory. The laboratory shall keep each SOP at the laboratory

premises and ensure that each SOP is accessible to laboratory employees during
operating hours. The laboratory shall make each SOP, as well as any other SOPs
associated with the licensee’s ISO/IEC 17025 certificate of accreditation available for
inspection upon request by MDPH.
5.4.1.1 Components of Analytical SOPs
References: ISO/IEC 17025:2005; The current adopted version and approved

revision of the EL TNI Standard
Following the validation of a given method, generate analytical SOPs that shall be
reviewed and approved by laboratory management. Critical sections of information
to include in the analytical SOPs are listed below. It is important that the information
in these sections be consistent with the method validation performed.
The following topics (where applicable) should be considered when determining
critical components necessary for technical SOP:
 Clear Identification of the Method Name/Title;
 Scope and Application including applicable analytes and matrices;
 Method sensitivity statement and demonstration;
 Potential interferences with the analysis, if any;
 Measurement uncertainty (quantitative methods only);
 Description of type of item to be tested;
 Parameters or quantities and ranges to be determined;
 Apparatus, supplies, and equipment, including technical performance
requirements and instrument operation parameters;
 Reference standards and reference materials required, including
reagents;
 Instrument calibration procedures and acceptance criteria;
 Types, frequency, acceptance criteria and corrective actions for QC
samples and calibration standards;
 Procedure for the preparation of test samples, QC samples, calibration
standards, solutions, reagents and reference material preparation,
including the following:
o Sample identification and labeling requirements;
o Sample Collection (specific to analytical methods used)
o Sample Handling, Transport and Storage;
o Sample Preservation;
o Hold Time;
o Sample homogenization and subsampling
o Sample Preparation and Clean-up;
 Procedure for analyzing analytical batch samples;
 Data to be recorded, method of data analysis, primary and peer review,
and data reporting/presentation requirements;
 The method of recording observations and results;
 Calculations performed;
 Environmental conditions required and any stabilization period needed;
 Waste management and waste disposal;
 References, and
 Health and safety precautions.

5.5 Laboratory Logbooks
All laboratory records are to be maintained in an organized manner. Logbooks

themselves are to be uniquely identified and included in the laboratory document control
system. Corrections to hardcopy records are to be made using a single strike-through
and are to be initialed and dated by the individual making the correction. All
corrections/changes/updates made to records in the laboratory information management
system (LIMS) are to include an appropriate comment and be traceable via audit trail.
All data recorded in logbooks, notebooks, and LIMS are to undergo routine periodic
(e.g., monthly) documented supervisory review.
5.6 Instrument Data and Records
All instrument use (including rinses and diagnostic checks) is to be included in an

analysis logbook or an electronic log. The data representing all such use is to be
retained and archived in an organized manner whether reportable or not. The laboratory
shall process instrument software chromatograms and data in a manner that allow for
the historical reconstruction of the analysis. Instrument software is to track changes and
chromatography changes with an audit trail and the laboratory shall have procedures for
tracking changes in all other analytical records.
The records of the analysis that shall be retained include, but are not limited to:
 Preparation records,
 Instrument conditions,
 Instrument method,
 Tunes,
 Check standards,
 Calibration records for each analyte (including a summary of any dropped points
or change in reporting range),
 Instrument sequence,
 Chromatograms,
 Before and after records of manual integrations and any analyte deletion that
includes a reason for the professional judgement decision,
 QC sample calculations,
 Dilutions and re-analysis samples of samples,
 Carryover reviews, and
 Data review.
Analytical sequence logs (manually or electronically generated) are to contain every

analysis/injection, regardless of the nature of the analysis/injection (i.e., reportable, non-
reportable, or troubleshooting). Overwriting files is strictly prohibited. All QC
components, including those samples from failed or unreported runs are to be
maintained as part of laboratory records, as they shall be considered for use in
laboratory control charts to generate limits unless determined to be a statistical outlier or
result of an assignable cause.
Electronic files are not to be overwritten under any circumstance; documented training of
staff on this issue is to be provided. Laboratory staff is to be trained to record actions

taken in the logbooks or electronic logs when any standard, tune, or QC sample initially
fails and is repeated, such that the situation and action are fully documented and can be
understood after-the-fact based on independent review of any logbook or electronic log.
5.7 Electronic Logging
Electronic logs are to be replicated to a separate medium (e.g., server, drive, or hard
medium) daily at a minimum (more frequently is preferred). Electronic logs are to have a
functional audit trail enabled and in use at all times. At a minimum, the audit trail
function is to retain and retrieve the initial values in each field, updated values, the date,
time, and operator identification for each update. Changes to analytical and compliance
parameters are to be associated with a documented reason for the change, recorded by
the identified operator.
Examples of analytical and compliance parameters include peak/signal intensity, peak

area, normalizing parameters, time of analysis, response factors, weight and volume
values, units, and dilution factors.
5.8 Maintenance Logs
Maintenance logs are to include records of all maintenance performed on an instrument

(e.g., routine maintenance and external repairs) such that the maintenance performed
can be historically traced (problem, solution, outcome format) with records documenting
when instrument returned to control. It is recommended that the laboratory supplement
the descriptions of problems, troubleshooting steps, and solutions with chromatograms
or data showing the instrument response at each step. The author and date of entry are
to be included for all log entries. All instrument maintenance logbooks are to include the
serial number(s) or permanently tagged identifier for the instrument and the associated
peripherals such that the logbook is unambiguously associated with the instrument and
the associated peripherals.
5.9 Requests, Tenders, and Contracts
The laboratory is to determine whether the client is submitting samples for regulatory
reporting. This is to be determined and recorded before sample receipt and log in
through the request for analysis, chain of custody records and documented
conversations with the client. This designation is to be included in project information
and effectively communicated to laboratory staff who shall be involved in sample
handling, analysis and reporting to ensure that the applicable ISO requirements, relevant
guidance contained herein and the regulatory requirements are considered and applied
to the samples at every point of the process.
If samples are not designated as regulatory, the sample report is to clearly state whether
the analyses performed met the requirements of the regulatory analysis and
accreditation to inform the Registered Marijuana Dispensary (RMD) and MDPH of the
state of compliance to regulation if the data is to be reported to MDPH for any reason. If
the analysis was not designated as regulatory and the client had specific requests that
depart from ISO 17025 standard requirements, MDPH requirements, or documented
laboratory procedures, these departures are to be clearly stated and the client report

narrative shall contain the language “this data is to be used for informational purposes
only.”
Data qualified as “Informational Purposes Only” when the sample was analyzed for
purposes other than MPDH compliance reporting leaves a question as to whether the
analysis was also performed to meet all of the requirements of the ISO accredited
scope. In any event, where the requirements of the ISO accredited scope are not met,
data should be separately qualified with language such as “Was not analyzed under ISO
Scope of Accreditation” regardless of whether or not the samples are used for MDPH
compliance.
5.10 Storage of Data
All data, instrument output (inclusive of electronic media), logbooks, electronic logs,
reports, hardcopy and electronic copy of all data packages delivered, and applicable
peripheral documentation, including, but not limited to, financial documents and invoices
generated by each laboratory are to be stored in an organized, categorized, inventoried
fashion for five (5) years after completion of the RMD request. At the RMD and/or
MDPH’s request, any and all data are to be submitted to the MDPH and/or RMD or their
designated consultant/authorized representative upon request. Overwriting or disposal
of any electronic media prior to this expiration period is strictly prohibited. All electronic
and hardcopy data are to be stored in an easily accessible, climate-controlled
environment. The laboratory is to exercise “best practices” in terms of frequent,
redundant electronic backup procedures on proper long-term storage media and/or to
remote servers to ensure that all raw data representing RMD sample analyses shall be
maintained for the 5-year storage period. Electronic data are to be stored in a secure,
limited access area with redundant copies stored in fireproof vaults and/or stored at an
off-site facility. After the 5-year storage period, the laboratory is to contact the RMD to
determine if data is to be properly disposed of, maintained for an extended period, or
shipped to the RMD for storage. No data is to be disposed of without contacting the
RMD for approval.
5.11 Software Control
Maintain an approved procedure for verifying the proper functioning of software

implementations and measures to prevent loss of data integrity. This is to include
documented procedures for data storage, back-up, archiving, and retrieval. This is also
to include a set of procedures for capturing the unique identifier for a given QC sample
(e.g., check standard, method blank, etc.) allowing for traceability back to the actual
documentation supporting the preparation of that sample.
5.11.1 In-House Software Tools
For in-house developed software tools such as spreadsheet formulae and macros,
instrument upload files, and worksheets for calculations as well as any in-house
developed databases, document the verification of proper functionality and security
of each version and identify the version used to generate results. Implement
databases with audit trails, registering each edit, the editor, date and time of edit.

Electronic records are to be protected by locking formula cells, locking worksheets

upon completion of the analysis day, using locked and controlled templates as a
source instead of a previous record, employing a unique identification system for
files, and identifying personnel who create electronic records. Any changes to
locked areas of macros, worksheets, and databases are to contain the initial record,
the changed record, and the authorization and reason for change.
For original software, developed by, or under the direction of the laboratory, a
lifecycle approach is to be incorporated into the validation procedure. Major steps of
the lifecycle approach are listed below.
5.11.2 In-House Developed Software and Tools
For in-house developed software and tools, the laboratory is encouraged to establish
a software lifecycle. For each piece of software, the software lifecycle should be
defined by establishing the activities to assure quality and evidence of validation.
This lifecycle is to include the following elements:
 Requirements – Intended performance and use of the software. Generate a
functional requirement document.
 Design
 Source Code – create the source code needed for desired software
functionality
 Test Plan – Develop a plan of the parameters and acceptance criteria to
verifies proper software operation.
 Install – install the software onto the hardware
 Traceability – Generate reports and supporting documentation that maps the
requirements of the Test Plan to the test actual results. This includes
displaying the tested version number of the software on the output from the
software.
Electronic uploads from software or to software that has not been validated by a
known and reputable manufacturer are to be reviewed completely as though it were
a manual transcription.
6.0 PROPER, LEGAL AND ETHICAL ACTIONS AND DATA INTEGRITY REPORTING -
POLICIES, TRAINING, AND PROCEDURES
The laboratory shall have a process/procedure in place for educating and training personnel.
Data integrity and ethics procedures in the laboratory include training, signed, and dated
integrity documentation for all laboratory employees, periodic monitoring of data integrity, and
documented data integrity procedures. Section managers uphold the spirit and intent by
supporting integrity procedures, by enforcing data integrity procedures and ensuring staff
participate in annual data integrity training.
Data integrity training is to be provided for all employees initially upon hire and annually
thereafter. Attendance at an initial data integrity training (part of new employee orientation) and
the annual refresher training are to be recorded with a signature attendance sheet. The data
integrity training is to cover the difference between fraud and other data integrity issues defining
intent and the correct documentation of errors immediately upon discovery.

A one-on-one session held between a new hire and the laboratory quality assurance manager
accomplished within the first four (4) weeks of employment, preferably sooner, can be a major
step assuring the employee has received needed initiation to quality system requirements.
Discussion regarding the critical aspect of the role data integrity has with respect to the success
of the laboratory cannot be understated. In addition to covering the systems by which to report
suspected ethical violations, covering such basics as the importance of support equipment
documentation, what constitutes a controlled document, policies regarding the treatment of raw
data with respect to data obliteration/line-outs, are all basic examples that lead the new hire on
the path that ultimately benefits both the lab and the staff member in the short and long term.
Specific integrity procedures for analyses involving chromatography (IC, GC, GCMS, HPLC,
etc.) require the understanding and implementation of MDPH’s Manual Integration Procedures
(Section 6.1.2). Training on these procedures is to be provided to all staff that performs
chromatographic analyses.
When contracted technical or support personnel are used laboratory management is

responsible for ensuring that, they are trained to the laboratory’s quality management system
and data integrity procedures, competent to perform the assigned tasks, and appropriately
supervised.
Employees shall report all violations to laboratory management or quality assurance. Failure to
report an integrity violation is an act of condoning the activity and is seen by MDPH as
equivalent to having actually committed the violation.
The mechanism for confidential reporting of ethics and data integrity issues is to contain (1)
unrestricted access to laboratory management or QA officers, (2) an assurance that personnel
shall not fear repercussion for reporting instances of ethics and data integrity breaches, and (3)
anonymous reporting.
Laboratories can comply with the anonymous reporting structure in simple ways such as
suggestion boxes or with intranet entry pages or a common “Data Integrity Report” email
address that is accessible by all personnel. It should be noted to the staff during training that
anonymous reporting may hinder the efforts to fully investigate the report.
Any potential data integrity issue is to be handled confidentially, to the extent possible, until a
follow-up evaluation, full investigation, or other appropriate actions have been completed and
the issues clarified. Inappropriate activities are documented, including disciplinary actions,
corrective actions, and notifications of clients, if applicable. These documents are to be
maintained according to the laboratory’s records retention schedule.
Data integrity procedures are to be reviewed as part of the annual internal audit and periodically
monitored through in-depth data review of audit trails or records review.
6.1.1 Data Integrity Requirements
The laboratory is to be committed to ensuring the integrity of data, incorporating the

highest appropriate standard of quality in all analytical programs.

 Personnel shall not condone any accidental or intentional reporting of deceptive or

misleading data. If laboratory management requests personnel to engage in an
activity that compromises data integrity, they have the right to refuse compliance
with the request and to appeal the action through the QA officer.
 Laboratory management shall not instruct subordinates to perform any practices
that would violate this policy, nor shall laboratory management discourage,
intimidate, or inhibit a staff member who may choose to appeal instruction under
this agreement and shall not retaliate against those who do so.
 All work assigned to personnel shall be performed in compliance with the MDPH
protocols, MDPH QAPP, laboratory QA manual and SOPs. It is the responsibility
of staff to be aware of and compliant with current policies and procedure
requirements for assigned duties.
 Personnel shall only report results or data that match the actual results observed or
measured.
 Personnel shall not intentionally falsify any data in any manner. Data shall not be
modified unless the modification is technically justified through a measurable
analytical process approved by the QA officer. All such modifications shall be
clearly documented.
 Recording of dates, times, and initials on data shall accurately reflect who and
when the procedure was performed.
 Personnel shall not intentionally make false statements to, or seek to otherwise
deceive data users, agency representatives, or auditors.
 Personnel shall not, through intentional acts of omission, commission, erasure, or
destruction improperly report measurements, standard results, data, test results, or
analytical conclusions.
 Personnel shall not destroy, or overwrite records of analyses or original
observations. This includes, electronic files and instrument sequences, analytical
reports, original recording of observations, etc.
 Personnel are required to understand, through training and review of quality
systems documents, that any infractions of the laboratory data integrity procedures
shall result in a detailed investigation that could lead to very serious consequences
such as immediate termination, or civil/criminal prosecution.
6.1.2 Manual Integration Procedures
Manual Integration is the process performed by the data user when the automatic
integration performed by the system is in error. It is to be used when there is a
misidentification or lack of identification of peaks due to retention time shifts, or when the
software does not properly integrate split peaks, co-eluting peaks, peaks affected by
baseline noise, negative baselines, rising or falling baselines, and excessive peak tailing.
If manual integration is necessary, the analyst is to save the original file in paper or
electronic format, record the reason for the integration, the analyst initials, and the date,
and save the final file. All of these are to be available for review. This includes
situations where an analyst has determined that the software has incorrectly identified a
peak and has changed the identification to a non-detect.
All samples, standards, and QC samples are to be integrated in the same manner.
Manual integrations shall never be performed in an attempt to meet acceptance criteria.

Any deviations from manual integration procedures that occur during data processing
are to be documented in the final report. The SOPs are to include at least two levels of
data review (primary and peer review) on each chromatogram in the analytical run that
includes checks for improper software integration and consistent manual integration.
Manual integration may be necessary and appropriate when a slight shift in

chromatographic retention times results in undetected peaks or false positive
identification of compounds. Manual integration may also be necessary and appropriate
when:
 Peak splitting resulting in the entire peak area not being integrated.
 Integration of closely eluting peaks or indistinguishable groups of peaks with
the same quantitation signal, are integrated together as one peak.
 Baseline interference caused by highly contaminated samples, effect the
integration of target and analytes.
 The target peak does not begin or end at baseline, but begins or ends on
another peak or valley.
Examples of unacceptable manual integrations are peak shaving, peak enhancement,

changing peak height, and shifting retention time windows without justification.
7.0 PROCEDURE GUIDANCE ON SAMPLE HANDLING AND STORAGE

Following established procedures for sample management is important in maintaining data
quality. Strict custody procedures are necessary to maintain the integrity of the medical
marijuana product samples. The subsections below detail the components of the sample
handling and tracking system and address sample identification, packaging, shipping, and
documentation
7.1 Sample Receipt and Sample Custody Requirements
The primary objective of sample custody procedures is to create an accurate written record
that can be used to trace the possession and handling of all samples from collection, to
shipment to the laboratory, to analysis, and to their final disposal. Documentation of proper
custody by following Chain-of-Custody (COC) procedures is essential to establish sample
integrity and validity of analytical results. COC procedures also serve to minimize loss or
misidentification of samples and unauthorized tampering of collected samples. Properly
filled out COC records are to be part of the laboratory sample acceptance policy. If
contracted couriers are used, the couriers are to be aware of the custody procedures to
properly receive and relinquish custody.
The integrity of samples after receipt by the laboratory is to be maintained through proper
handling/storage procedures and preparation/analysis within applicable holding times. The
laboratory is to refer to the specific method and regulation for applicable holding times.
Documentation of appropriate sample handling/storage, and preparation/analytical
procedures is to be maintained by the laboratory.

Laboratory custody of samples begins when samples are received by the laboratory. The
laboratory is to have procedures in place to maintain the custody, security, and integrity of
samples.
At a minimum, the Sample Custodian shall sign and record the date and time of sample
receipt on the COC. The validated time of sample receipt (VTSR) is the time the samples
are received at the laboratory from the RMD personnel or representative, or private courier;
it is not the time the samples are opened or logged in at the laboratory. The laboratory is to
have documented procedures for receipt of samples outside normal hours of operation.
Sample custody procedures are to be implemented to ensure that samples are not
tampered with from the time of sample collection through time of transport to the
independent testing laboratory. Custody of the samples by a given person is defined by:
 Physical possession of the samples (i.e., carrying or holding the samples),

 Having the samples within clear view after having possession, or
 Having physical possession and leaving them in a secure location so that they
cannot be tampered with. In addition, when samples are secured in a restricted
area accessible only to authorized personnel, they shall be deemed to be in the
custody of such authorized personnel.
Sample custody documentation includes both laboratory notebooks and COC forms.
Samples shall be accompanied by a properly completed COC form. The sample
identifiers shall be listed on the COC form. When transferring the possession of samples,
the individuals relinquishing and receiving shall sign, date, and note the time on the COC
form. This record documents transfer of custody of samples from the sampler to another
person, to the laboratory, and to any subcontracted laboratory.
7.1.1 Sample Temperature Measurement
Samples requiring thermal preservation are not to be allowed to reach temperatures

> 6.0°C during sample receipt/login procedures (prior to being placed in laboratory cold
storage). Sample receipt temperatures are to be recorded on the COC or sample
receipt form to the nearest 0.1°C using a thermometer or other appropriate temperature
measurement device that is calibrated at least annually against a National Institute of
Standards and Technology (NIST)-certified thermometer (see Section 10.3.1 for
thermometer calibration requirements). The unique identifier for the thermometer or
other device is to be recorded
Temperatures shall be taken using the temperature blank provided with the laboratory
bottle shipment; if the temperature blank is broken, missing, or frozen, the temperatures
of other sample bottles may be taken by non-invasive methods (e.g., uniquely identified,
NIST-calibrated infrared [IR] gun). If temperatures are measured on sample bottles, this
is to be noted in sample receipt documentation and on the COC. The IR thermometer is
to be checked daily (or weekly at a minimum) when in use against a NIST-calibrated
thermometer in the sample storage area. IR thermometer procedures are to contain
consistent use between laboratory staff such as representative placement of bottle
checked, type of bottle (glass, plastic, etc.) checked and distance from bottle and
whether or not to include label of bottle according to manufacturer instruction. The
laboratory procedures are to be specific as to whether a temperature blank or single IR

sample temperature failure indicates exceedance for the entire cooler or if individual
sample temperatures shall be taken to assess compliance.
The laboratory is to maintain a record of samples that are received at temperatures

outside of acceptance criterion (e.g., ≥ 6.0°C). (Please see the section below entitled,
Communicating Sample Receipt Issues)
7.1.2 Chain-of-Custody Verification
Following sample temperature measurement, the Sample Custodian shall examine the
sample containers received and note any damage to sample containers/media. Sample
container labels shall be compared to the COC Form, and any discrepancies (e.g.,
sample identification, preservation, sample matrix, requested analyses, etc.) shall be
noted. Discrepancies between the samples received and the field COC Form are to be
communicated to the RMD or its designee, who shall provide directions on how to
proceed.
7.1.3 Sample Storage
The laboratory is to maintain sample storage refrigerators at ≤ 6.0°C and sample storage
freezers at < -10°C. The laboratory is to have adequate cold storage units to maintain
temperature preservation as required by the requested analytical method. When sample
storage cooler and freezer temperatures are outside of the acceptance range, the
laboratory is to document corrective action, and any samples stored in the affected units
shall be immediately moved to a cold storage unit within criterion and the impact on data
quality is to be assessed and recorded. Samples are to be stored separately from
performance evaluation (PE) samples, standards, spiking solutions, prepared reagents,
and sample extracts or refrigerator blanks are to be run to assess contamination.
7.1.4 Communicating Sample Receipt Issues
Any issues noted during sample receipt that may adversely impact data quality
(including, but not limited to, loss of sample volume, samples with temperatures > 6.0°C;
improper chemical preservation of samples; or documentation discrepancies) shall be
communicated to the RMD or its designated consultant was soon as practical (via phone
log or e-mail based on project personnel requirements) so that proper corrective action
can be taken; documentation of this communication is to be preserved with the project
records. If the sample receipt criteria are not met, the samples are to be rejected and the
RMD is to be informed immediately of the need to resample.
All samples placed “on hold” because of sample receipt issues is to be stored in
accordance with sample temperature preservation requirements (e.g., in sample
refrigerators or freezers) until the issues have been resolved. When an issue requiring
notification is discovered after normal business hours (i.e., between 0800 and 1700
Eastern Standard Time, Monday through Friday), the laboratory is to provide prompt
verbal, text, or e-mail notification to the RMD or its designee. The laboratory is to
maintain documentation detailing any sample receipt issues and the resolution directed
by the RMD or its designee in the project files.

7.1.5 Holding Times
Holding times shall be as specified in the tables presented in Appendix A, which are
based on the most current MDPH protocols, USP monograph or general chapter, AHP,
United States Environmental Protection Agency (EPA), and other MDPH-approved
methods unless a shorter holding time is specifically requested by the RMD or the
MDPH.
Holding time begins upon sample collection (the date/time the sample is collected as
documented on the COC). The samples are to be in good condition and are to be
received by the laboratory generally within 1-calendar day of sampling unless different
arrangements have been made in advance with the laboratory. For shipments to be
received by the laboratory after normal business hours (Monday-Friday, 0800-1700
hours), prior arrangements shall be made so that laboratory personnel are available to
receive the samples. Samples with holding times of < 48 hours are to have
documentation of the time they were set up for the short hold-time analysis. For all
sample shipments, the primary laboratory contact, for the dispensary shipping the
samples, is to notify all applicable laboratory personnel of the expected sample delivery
so that laboratory personnel can prepare to receive the samples.
The laboratory is to adhere to the required holding times for the initial sample
preparation/analyses. If samples are received with a significant portion of the holding
time expired and the laboratory is concerned about meeting holding time requirements,
RMD, or its designee is to be notified immediately upon sample receipt. If subsequent
analysis/extraction becomes necessary due to method or technical requirements or
failing QC, the laboratory is to make every effort to analyze these dilutions/re-extractions
/reanalyses within the method holding time specified in Appendix A.
7.1.6 Subsampling and Homogenization
Samples received by the laboratory are to be homogenized in full before subsampling for
analysis or subcontracting takes place. The laboratory is to maintain procedures for
homogenization and subsampling that include instructions on all matrices and how to
handle samples that cannot be homogenized.
Homogenization and subsampling equipment and procedures are to be validated by

laboratory-defined procedures that demonstrate the effectiveness of homogenization
and subsampling through precision indicators (e.g., homogenization duplicates) and the
effectiveness of the equipment cleaning through evaluation of blanks associated with the
equipment.
A homogenization duplicate and a homogenization blank are to be assigned separately

for flower and extract sample batches at defined intervals. The homogenization blank
shall be randomly placed in the batch as to check all of the homogenization equipment
for possible carryover rather than using a dedicated homogenization apparatus for the
blank each time it is requested.

8.0 DATA QUALITY INDICATORS
Data Quality Objectives (DQOs) are listed below in Appendix A, Tables 03-09. Whenever
possible, these objectives were set with the reference methods listed in the MDPH protocols.
When additional information was needed for marijuana-specific, technology-specific, or analyte-
specific objectives, other ancillary methods were utilized. Primary reference methods and
ancillary reference methods used to develop data quality objectives for the required analytes are
contained in Appendix A, Table 01. If the laboratory employs methods other than those listed in
Appendix A, Table 01, they shall be validated using the guidance in Section 9.0 of this
document. Table 02 of Appendix A contains the sample handling, receipt, and storage
requirements that are to be followed to ensure sample integrity for the required analyses.
In order to assist in decision-making and to meet DQOs, measurement performance criteria

have been established for the data that shall be generated under the guidance of this QAPP
and have been determined by matrix, analytical group, and analyte. Measurement performance
criteria are evaluated in relation to the five data quality indicators (DQIs) of: precision,
accuracy/bias, representativeness, comparability, and sensitivity. The DQIs used in this QAPP
are defined below in Sections 8.1 – 8.5. The DQOs are listed in the tables presented in
Appendix A.
8.1 Precision
Precision is a measure of the agreement of independent sample results obtained under the
same specified conditions. The goal is to maintain a level of analytical precision consistent
with the objectives of the sampling activities. Checks for analytical precision are to include
the analysis of matrix spike and matrix spike duplicates, laboratory duplicates and medical
marijuana product sample duplicates.
8.2 Accuracy
Accuracy is a measure of how close a measured result is to the true value. When applied to
test results, accuracy includes a combination of random and systematic error. When applied
to a test procedure, accuracy refers to a combination of trueness and precision. Analytical
accuracy is to be monitored through initial and continuing calibration of instruments and the
accuracy of the analytical data is to be assessed by the analysis of reference standards,
matrix spikes, blank spikes, rinse blanks, and surrogate standards.
8.3 Representativeness
Representativeness is the degree to which data accurately and precisely represent medical
marijuana product quality, and is dependent on sampling and analytical variability and the
variability of the product. The use of the prescribed laboratory analytical methods with
associated holding times, preservation requirements, homogenization, subsampling,
laboratory duplicates and DQOs are intended to provide representative data.
8.4 Comparability
Comparability is the degree of confidence with which one data set can be compared to
another. Comparability between product data collected over time is to be maintained
through consistent use of the analytical methodologies set forth in this QAPP, using

established quality assurance/quality control (QA/QC) procedures, and through utilization of

appropriately trained personnel.
8.5 Sensitivity
Sensitivity is a quantitative measurement to determine if the independent testing laboratory’s

procedures/methodologies and their associated Limit of Detection (LOD) can satisfy the
requirements, objectives and action limits established in the MDPH protocols. LOD studies
are required and are to be updated by the independent testing laboratory annually. The
current LODs for the independent testing laboratory are to be maintained in a controlled
document.
The Limit of Quantitation (LOQ) is the minimum concentration of an analyte that can be
routinely identified and quantified above the LOD by a laboratory with satisfactory accuracy
and precision meeting the method requirements set forth in Appendix A of this document.
Sensitivity can be measured either by performing an LOD study or by calculating the percent
recovery of the analytes at the LOQ level. In the event that data are to be reported in a
range below the LOQ, LOD studies are to be performed as described in this QAPP.
9.0 VALIDATION OF METHODS
9.1 References: ICH Q2 (R1), USP <1225>, ISO/IEC 17025:2005, and FDA OAR
Each independent testing laboratory is to implement an approved procedure for method

validation for both quantitative chemical analyses and microbiological analyses. The
objective of validation of an analytical procedure is to demonstrate that it is suitable for its
intended purpose.
The objective of the analytical procedure is to be clearly understood and defined in a

reviewed and approved validation protocol prior to performing the actual method validation.
The validation protocol shall govern the validation characteristics that need to be evaluated.
The validation protocol and eventually, the analytical standard operating procedure (SOP),
are to document clearly the manner in which the method is performed. It is to describe in
detail the steps necessary to perform the analytical test, which includes (where applicable)
but is not limited to: sample preparation, the equipment, reference standards and reagents
used, preparation of reagents and buffers, equipment use and operation, instrument
calibration, QC sample preparation and analysis frequency, QC sample acceptance criteria
and corrective actions, calculations used.
The independent testing laboratory is to validate all methods prior to sample analysis,
including laboratory-designed or developed methods, commercially developed methods
used outside their intended scope and methods that have been modified, in order to confirm
that the methods are fit for the intended use.
Specifically, method validation is required for the following:
 A new or original method;

 Expansion of the scope of an existing method to include additional analytes;
 Expansion of the scope of an existing method to include additional matrix types;

 Changes in the intended use of an existing method (e.g., screening vs. confirmatory);
and
 Modifications to a method that may alter its performance specifications (e.g.,
modifications that could significantly affect the precision and accuracy, changes to
the fundamental science of an existing method, significant changes to reagents,
apparatus, instrumental parameters, sample preparation and/or extraction, or
modification of a method’s range beyond validated levels).
The validation is to be as extensive as is necessary to meet the needs of the given

application or field of application.
An example of a method that needs further validation would be Cannabinoid analysis. In

this validation, it is important to demonstrate the ability to measure the major cannabinoids
at multiple concentration ranges on the HPLC. In addition, selectivity may need to be further
demonstrated pertaining to identification by providing confirmatory identification as a
validation component using technologies such as NMR.
The independent testing laboratory is to record the results obtained, the procedure used for
the validation, and a statement as to whether the method is fit for the intended use. Each
method shall be validated appropriately before use. The documentation maintained from
the development and validation of new test methods is to contain at least the following
information:
 Clear Identification of the Method Title;

 Scope and Application;
 Description of type of item to be tested;
 Parameters or quantities and ranges to be determined;
 Apparatus and equipment, including technical performance requirements and
instrument operation parameters;
 Reference standards and reference materials required;
 Environmental conditions required and any stabilization period needed;
Typical validation characteristics, at a minimum, are to contain precision and accuracy

studies and a demonstration of the quantitation limit to obtain an estimation of uncertainty.
Characteristics to be evaluated, whenever practicable, are listed below and are described in
the subsequent sections in further detail:
 Accuracy
o Spike Recovery
 Precision
o Repeatability/Reproducibility
o Intermediate Precision
 Sensitivity
 Specificity
 Limit of Detection
 Limit of Quantitation
 Linearity
 Range
 Robustness

 Confirmation of Identity
When changes are made in the validated method, the influences of such changes are to be
documented and, if appropriate, a new validation is to be carried out. The range and
accuracy of the values obtainable from validated methods (e.g. the uncertainty of the
results, detection limit, selectivity of the method, linearity, limit of repeatability and/or
reproducibility, robustness against external influences and/or cross-sensitivity against
interference from the matrix of the sample/test object), as assessed for the intended use, is
to be relevant to the customers' needs.
9.2 Validation Guidance for Quantitative Chemical Analyses
For quantitative chemical analysis methods, validation is typically comprised of the

following elements. Specific criteria for meeting the data quality objectives of this QAPP
are presented in Appendix A of this document.
9.2.1 System Suitability
It is good practice to perform system suitability tests that are based on the concept
that the equipment, electronics, analytical operations and samples to be analyzed
constitute an integral system that can be evaluated as such. System suitability test
parameters to be established for a particular procedure depend on the type of
procedure being validated. These requirements typically include:
 injection repeatability,
 peak resolution,
 relative retention times for liquid chromatography analyses
9.2.2 Determination of the Limit of Detection (LOD)
The following method shall be performed if results are to be reported below the LOQ.
The independent testing laboratory is to develop a procedure for the determination of
a LOD for each analytical method for which the analyte can be spiked into a
reference matrix. The general steps required for the procedure are described below:
When determining the LOD, prepare an adequate number of spikes of known
amounts of analyte near, but above the instrument detection limit that are taken
through the entire analytical method, including sample preparation (e.g., digestion,
extraction, derivatizations, cleanups). From the variation in these measures, use the
student t statistic to establish the upper confidence limit at p ≥ 0.99 for n-1 degrees of
freedom. Compare this to a similar set of independent testing laboratory method
blanks, applying the same statistic. Use the higher of the two calculated LOD
values. Validate the LOD value by analyzing a suitable number of samples known to
be near or prepared at the detection limit and perform a statistical evaluation on the
associated results in order to determine the LOD value. Draft, review, and issue a
written set of procedures detailing the procedures for the determination and
verification of the LOD. Provide documented training to the procedures.
Note: The LOD determination method accepted for compliance with this QAPP is
based on the procedure for determining the Method Detection Limit presented in 40
CFR 136 Appendix B.

9.2.2.1 Estimate the Initial LOD using one of the following:
 The mean plus three times the standard deviation of a set of method blanks.
 The concentration value that corresponds to an instrument signal/noise ratio
in the range of 3:1 to 2.5:1. This is performed preferably without smoothing
of the analytical signal, but if smoothing is applied, it shall be the same
smoothing method as is used for all sample and quality control sample
analysis.
 The concentration equivalent of three times the standard deviation of
replicate instrumental measurements of spiked blanks.
 That region of the standard curve where there is a significant change in
sensitivity, i.e., a break in the slope of the standard curve.
 Instrumental limitations.
 Previously determined LOD obtained using the same instrument conditions.
It is recognized that the experience of the analyst is important to this process.

However, the analyst is to include some or all of the above considerations in the
initial estimate of the LOD.
9.2.2.2 Determine the Initial LOD
1. Select a spiking level, typically 2 – 10 times the estimated LOD in the section
above
2. Process a minimum of seven spiked blank samples and seven method blank
samples through all steps of the method, including any sample preservation.
Both preparation and analysis of these samples are to include at least three
batches on three separate days’ results in the method-reporting units.
a. If there are multiple instruments that shall be assigned the same LOD,
then the samples are to be distributed across all of the instruments.
b. A minimum of two spiked samples and two method blank samples

prepared and analyzed on different days is required for each instrument.
c. Evaluate the spiking level: If any result for any individual analyte from the
spiked blank samples does not meet the method qualitative identification
criteria 2 or does not provide a numerical result greater than zero then
repeat the spikes at a higher concentration.
3. Make all computations according to the defined method with final results in
the method-reporting units.
a. Calculate the sample standard deviation (S) of the replicate spiked blank
measurements and the sample standard deviation of the replicate method
blank measurements from all instruments.
b. Compute the LODs (LOD based on spiked blanks) as follows:
𝐿𝑂𝐷𝑠 = 𝑡(𝑛−1, 1−𝛼=0.99) 𝑆

Where:
LODs = the Limit of Detection

t(n-1, 1-α = 0.99) = the students t value appropriate for a 99% confidence level
13
and a standard deviation estimate with n-1 degrees of freedom..
S = sample standard deviation of the replicate spiked blank sample
analyses.
c. Compute the LODb (LOD based on method blanks) as follows:
i. If none of the method blanks give numerical results3 for an individual

analyte, the LODb does not apply.
ii. If some (but not all) of the method blanks for an individual analyte
give numerical results, set the LODb equal to the highest method
blank result.
iii. If all of the method blanks for an individual analyte give numerical
results, calculate the LODb as:
𝐿𝑂𝐷𝑏 = 𝑋 + 𝑡(𝑛−1,1−𝛼=0.99) 𝑆𝑏
Where:
LODb = the LOD based on method blanks
𝑋= mean method blank
t(n-1, 1-α = 0.99) = the students t value appropriate for a 99% confidence level
and a standard deviation estimate with n-1 degrees of freedom.
Sb = sample standard deviation of the replicate blank sample analyses.
4. Set the greater of LODs or LODb as the initial LOD.
For qualitative measurements, determine the concentration threshold below

which specificity becomes unreliable.
9.2.2.3 Ongoing LOD Data Collection
 During any quarter in which samples are being analyzed, prepare, and
analyze a minimum of two spiked samples on each instrument, in separate
preparation batches, using the same spiking concentration level that was
used to determine the LOD initially per the instructions in Section 9.2.2.2.
 Ensure that at least seven spiked samples and seven method blanks are
completed for the annual verification that is described below in Section
9.2.2.2. If only one instrument is in use for a given method, then a minimum
of seven spikes are still required, but they may be drawn from the last two
years of data collection.
13
NIST/SEMATECH. 2013. E-Handbook of Statistical Methods.
http://itl.nist.gov/div898/handbook/eda/section3/eda3672.htm

9.2.2.4 Requirements for Re-determining the LOD
 Annually, at a minimum, the independent testing laboratory is to re-evaluate the

spiking level used to determine the initial LOD. If more than 5% of the spiked
samples analyzed, as part of the ongoing LOD data collection described in
Section 9.2.2.2, do not return positive numerical results that meet all method
qualitative identification criteria, then the spiking level shall be increased and the
initial LOD
re-determined following the procedure in Section 9.2.2.2.
 If the method is altered in a way that can be reasonably expected to change

its sensitivity, then re-determine the initial LOD according to Section 9.2.2.2
and restart the ongoing data collection described in Section 9.2.2.2.14
 If a new instrument is added to a group of instruments whose data are being

pooled to create a single LOD, analyze a minimum of two spiked replicates
and two method blank replicates on the new instrument. If both method blank
results are below the existing LOD, then the existing LODb is validated.
Combine the new spiked sample results to the existing spiked sample results
and recalculate the LODs as described in Section 9.2.2. If the recalculated
LODs is within 0.5 to 2.0 times the existing LODs, and fewer than 3% of the
method blank results (for the individual analyte) have numerical results above
the existing LODs, then the existing LODs is validated and may optionally be
left unchanged. If either of these two conditions is not met, then calculate a
new LOD following the instructions in Section 9.2.2.
9.2.2.5 Annual Verification of LOD
 Annually, at a minimum, the independent testing laboratory is to re-calculate

the LOD from the collected spiked samples and method blank results using
the equations in Section 9.2.2.2
 When recalculating the LOD the independent testing laboratory is to include
the ongoing data generated within the last twelve months which meet the
following criteria for inclusion into the LOD calculation:
o Data with the same spiking level used to determine the LOD previously.
Only documented instances of gross failures (e.g., instrument
malfunctions, mislabeled samples, cracked vials, formal statistical outlier
testing) may be excluded from the calculations.
o If outliers are removed, then the rationale for removal of specific outliers
shall be tracked by matrix type, documented, and maintained by the
independent testing laboratory with the results of the initial LOD
determination.
o If the independent testing laboratory believes the sensitivity of the method
has changed significantly, then the most recent data available may be
used, as long as compliance with the requirement for at least seven
14
A numerical result includes both positive and negative results, including results below the current LOD.
Results do not include any value where a chromatographic peak is not present.

replicates in three separate batches on three separate days has been met
(see Section 9.2.2).
o If the method has been altered in a way that can be reasonably expected
to change its sensitivity then use only data collected after the change.
o Include the initial LOD spiked samples, if the data were generated within
12 months.
o Only use data associated with acceptable calibrations and acceptable
batch QC.
o Include all routine data, with the exception of batches that are rejected
and the associated samples reanalyzed.
o Ideally, use all method blank results from the last 12 months for the LODb
calculation. The independent testing laboratory has the option to use only
the last six months of method blank data or the fifty most recent method
blanks, whichever criteria yields the greater number of method blanks.
 The verified LOD is the greater of the LODs or LODb. If the verified LOD is
within 0.5 to 2.0 times the existing LOD and fewer than 3% of the method
blank, results (for the individual analyte) have numerical results above the
existing LOD then the existing LOD may optionally be left unchanged.
Otherwise, adjust the LOD to the new verification LOD.
Note: The range of 0.5 to 2.0 approximates the 95th percentile confidence interval
for the initial LOD determination with six degrees of freedom.
9.2.3 Limit of Quantitation (LOQ)
The LOQ is to be determined for each analysis, using a documented standard

procedure developed by the independent testing laboratory. The general steps
required for the independent testing laboratory LOQ procedure are described below:
Determine the LOQ by preparing spikes of known amounts of analyte near the
minimum level at which the analyte can be quantified with acceptable accuracy and
precision. Experience and theory (e.g. Horwitz) holds that this is generally several
multiples (e.g. three times) higher than the LOD (two times at a minimum). Take the
LOQ spikes through the sample preparation steps of the method. Validate the LOQ
value by analyzing a suitable number of samples (three spiked samples at a
minimum) known to be near or prepared at the LOQ and evaluate the associated
results in order to determine whether the results meet the DQOs for precision and
percent recovery. It is required that the value also be supported by a calibration
point at or below the LOQ for any given method and that method blanks be held to
½ the LOQ or less. On a periodic frequency, check samples that are taken through
all method procedural steps are to be analyzed at the LOQ level in order to verify the
method’s accuracy near the LOQ value. Draft, review, and issue a written set of
procedures detailing the procedures for the determination and verification of the
LOQ. Provide documented training to the procedures.
9.2.3.1 Ongoing Verification of the LOQ
On a periodic frequency, check samples that are taken through all method
procedural steps are to be analyzed at the LOQ level in order to verify the method’s

accuracy near the LOQ value. The independent testing laboratory is to draft, review,
and issue a written set of procedures detailing the procedures for the determination
and verification of the LOQ. The default DQO for ongoing validation are to match
those specified in the DQO Tables presented in Appendix A or independent testing
laboratory generated limits specific to LOQ verification can be established.
9.2.4 Linear Range
For quantitative measurements determine the linear calibration range if a standard curve
is to be used or determine the target calibration standard and linearity if only a one
calibration point is to be used.
As a general rule for a calibration curve, the mid-point is set at the target level
(concentration) for quantitation of the analyte. Ideally, for the determination of
contaminants in medical marijuana products (MMPs) and marijuana infused products
(MIPs) the target LOQ is to be set at the contamination limits for each contaminant
compound, where practical and achievable, as required by the MDPH Protocol for
Sampling and Analysis of Finished Medical Marijuana Products and Marijuana-Infused
Products for Massachusetts Registered Medical Marijuana Dispensaries, Protocol for
Sampling and Analysis of Environmental Media for Massachusetts Registered Medical
Marijuana Dispensaries.
For the establishment of linearity for chromatographic methods (i.e. GC and HPLC), the
analysis of a minimum of five concentrations of analyte is recommended, with the low
calibration standard being set at or below the LOQ. The coefficient of determination (r2)
for a calibration curve shall be ≥ 0.990.
The coefficient of determination (r2), y-intercept, slope of the regression line and residual
sum of squares are to be submitted as part of the validation results when determining
the linear range of the method. A plot of the data is to be included. In addition, an
analysis of the deviation of the actual data points from the regression line may also be
helpful for evaluating linearity. Weighted linear calibrations using a 1/x2 weighting factor
are encouraged if the relative error is thereby reduced at the critical concentration level.
For residual solvent analysis by gas chromatography and pesticide analysis by

LC/MS/MS, higher order linear calibration models (e.g., quadratic or cubic) may be used
if performed frequently or verified throughout the range on an ongoing basis. Non-
standard calibration fits for a specific analyte cannot be applied to arbitrarily to force a
passing calibration. If an analyte shows to conform to a curve fit on a regular basis, the
decision to change the calibration model is to be recorded along with justification such
as change of column or decreased instrument performance.
In the event that support equipment calibration is limited to a single calibration point, the
zero-point of the curve may be forced (i.e. set) to zero. If a multipoint calibration curve is
analyzed, the intercept is not to be forced through zero, however the impact of a non-
zero intercept may be diminished by use of a weighted calibration model.
The range of the method is typically derived from the linearity studies by confirming that
the analytical procedure provides an acceptable degree of linearity, accuracy, and

precision when applied to samples containing known amounts of analyte within or at the
extremes of the specified range of the analytical procedure.
The exact requirements for linearity are specified in the QAPP DQO Tables presented in
Appendix A.
9.2.5 Accuracy
For quantitative measurements, prepare and analyze spiked blanks in solvent or matrix
samples with known concentration of analyte. Determine the accuracy of the method
across the range of the method by utilizing at least three different concentration levels:
low, middle, and high. Where the low concentration is the limit of quantitation and the
high concentration is the highest concentration of the linear range. For the
determination of accuracy a minimum of 9 determinations (e.g., 3 concentrations /3
replicates each of the total analytical procedure). These samples are carried through the
complete sample preparation procedure.
Matrix effects can also be assessed with these samples. Accuracy is to be reported as a
percent recovery of the analyte that is calculated from the results.
The default DQOs for accuracy are specified in the TSM DQO Tables presented in
Appendix A.
9.2.6 Precision (USP, ICH and ISO 17025)
When determining the precision of the method, there are three primary elements:
repeatability, reproducibility, and intermediate precision.
Repeatability can be assessed using the same procedure that was recommended for the
determination of accuracy in the preceding section (e.g., three concentrations /three
replicates each). An alternative approach to determining repeatability would be a
minimum of six determinations at a mid-level concentration or the target concentration
for the method.
Reproducibility can be determined by participating in an interlaboratory study (e.g., PE

study, etc.). The objective of reproducibility is to verify that the method shall provide the
same results in different laboratories. Laboratories are expected to participate in
interlaboratory studies that are become commercially available.
Intermediate precision expresses the variation of a given method within the same
laboratory. The extent to which intermediate precision is to be established depends on
the circumstances under which the procedure is intended to be used. Intermediate
precision is determined by comparing the results of a method run within a single
laboratory over a number of days. A method’s intermediate precision may reflect
discrepancies in results obtained from the following:
 different analysts
 inconsistent working practice
 different instruments
 standards and reagents from different suppliers

 columns, reagents and media from different batches

 a combination of the parameters listed above
Precision shall be reported as the standard deviation or relative standard deviation

(coefficient of variation). The confidence interval for which this precision is determined is
to be reported for each type of precision investigated. The default DQOs are to match
those specified in the DQO Tables presented in Appendix A or those developed in
accordance with the independent testing laboratory’s technical procedure may be used
in place the default DQOs. Where independent testing laboratory limits have been
established, they are, at a minimum, to be used to identify trending and out of control
events in order to inform continual improvement efforts. Repeatability shall be
determined to be adequate so that reliable achievement of the method specific DQOs in
Appendix A tables shall be supported.
9.2.7 Selectivity/Specificity
Evaluate potential interferences for each analyte under a given set of method conditions.
For the evaluation of spectral, physical, or chemical interferences analyze a sample
containing various suspected interferences in the presence of the measure. Spectral
interference may be observed when an overlap of a spectral line from another element
or background contribution occurs. Physical interference may occur from effects
associated with sample transport processes on instruments. Chemical interferences are
characterized by compound formation, ionization, or vaporization effects. Additional
interference may occur from the contribution of signal from previous sample preparations
which contaminate (or carry-over) into the next sample being tested.
Suitable identification tests are to be able to discriminate between compounds of closely

related structures that are likely to be present (e.g., cannabinoid profiles in the presence
of terpenoids, flavonoids, and alkaloids). The discrimination of a procedure may be
confirmed by obtaining positive results (perhaps by comparison with a known reference
material) from samples containing the analyte, coupled with negative results from
samples that do not contain the analyte. In addition, the identification test may be
applied to materials structurally similar to or closely related to the analyte to confirm that
a positive response is not obtained. The choice of such potentially interfering materials
is to be based on sound scientific judgement with a consideration of the interferences
that could occur.
9.3 Validation Requirements for Demonstrating Selectivity in Chromatographic

Chemical Analysis
For chromatographic procedures, representative chromatograms are to be used to

demonstrate selectivity and individual components are to be appropriately and qualitatively
identified and labelled. Critical separations in chromatography are to be investigated at an
appropriate level. For critical separations, selectivity can be demonstrated by the resolution
of the two components, which elute closest to each other. Co-elution of peaks is to be
monitored by monitoring retention times, applying peak symmetry criteria, and analyzing
HPLC-UV peaks for peak purity using a diode-array detector (DAD).

Specific QC elements as they relate to chromatographic analyses are discussed below and
a QC table summarizing those elements that are to be demonstrated when chromatographic
methods are performed is presented in Appendix A.

9.3.1 Retention Times
For chromatographic methods, all of the target analytes shall be retained on the column
at a retention time that results in a minimum retention/capacity factor (k’) 15 of > 2 and
shall be resolved apart from any observed peaks and meet the peak identification
requirements listed below shall be met.
For all initial calibration levels, the retention times for each target analyte shall be within
± 3 seconds of the midpoint standard for each target analyte. For CCV standards, the
retention time of the CCV should not differ by > ± 6 seconds (0.2 minutes) or ± 0.04
relative retention time (RRT) units when internal standards are used, from the retention
time established by the middle standard of the initial calibration. In MS methods, all
internal standards retention times in the sample should not differ by > ± 6 seconds (0.2
minutes) or ± 0.04 RRT units (if applicable) from the retention time established by the
associated CCV standard. For all target analytes reported in RMD samples and other
method QC samples the retention time of the target analyte in the sample should not
differ by ± 6 seconds (0.2 minutes) or ± 0.04 RRT units (if applicable) from the retention
time established by the associated CCV standard. When retention time window criteria
are not met, samples shall be reanalyzed within a new calibration or CCV to meet the
retention time window criteria.
9.3.2 Peak Resolution
For chromatographic peak resolution, a minimum acceptance criterion of ≤ 30% valley

(that the valley between two adjacent peaks are not to exceed 30% of the peak height of
the shorter peak) is required to provide for closely eluting compounds to be adequately
resolved from each other. If resolution is determined to be insufficient, the independent
testing laboratory shall modify method conditions where applicable in order to resolve
co-eluting peaks from one another. Applicable components of validation of the modified
method shall be completed successfully prior to sample analysis during method
validation is described in Section 9.1.
9.3.3 Peak Symmetry (Tailing Factor, T)
The accuracy of quantitation decreases with increase in peak tailing because of the
difficulties encountered during peak integration when determining where/when the peak
ends. As a result, the calculation of the area under the peak becomes less accurate.
For all chromatographic peaks, the tailing factor is required to be ≤ 2, when calculated
using the following calculation:
𝑇 = 𝑊0.05 /2𝑓
Where W0.05 is the width of the peak at 5% height and f is the distance from the peak
maximum to the leading edge of the peak, the distance being measured at a point 5% of
the peak height from the baseline. See example in figure below.
15
k’ = (Rt – t0)/t0; where: t0 is the column void volume (min) and Rt is the target analyte retention time
(min).

Figure 1. Determination of Tailing Factor on an Asymmetrical Peak

[Reference: USP Chapter 621]
The independent testing laboratory is required to capture peak tailing for all
chromatographic methods, where applicable. The independent testing laboratory is to
provide the calculation used for determining peak tailing factor when requested by
MDPH.
9.3.4 Peak Purity (HPLC-UV Methods Only)
Certain considerations are to be made when using instruments capable of calculating

peak purity at multiple wavelengths, however named in the software, to determine the
presence of co-eluting peaks in chromatographic methods. The HPLC method used the
software settings and the parameters that independent testing laboratory selects within
the peak purity software menu shall have an effect on the results that are obtained. The
independent testing laboratory shall not use peak purity software to analyze peak, which
elute at or near the column void volume.
The correct detector sample rate, signal wavelength, and bandwidths need to have been
selected and used (e.g., reference wavelength is to be turned OFF). Two spectral
reference points are to be selected and placed at times before and after the peak of
interest in clear baseline areas where no other peaks or spectra are seen. Select a
minimum of seven spectra from the sample peak for comparison.
For all chromatographic peaks detected in HPLC-UV analyses, a DAD detector is to be

used and the peak purity is to be monitored. When peaks have met the qualitative
identification requirements presented in Section 9.1, and peak purity is calculated and no
differences in the spectra are seen then the spectra are considered to be similar or
homogeneous and no further action is required. When there is a difference between
peak spectra and/or obvious co-elution during a chromatographic analysis and the peak
resolution and/or tailing factor criteria established above are not met, then the
independent testing laboratory is to modify method conditions in order to separate the
two compounds from one another if detected during method development or validation.
If the peak purity factor is below independent testing laboratory specifications for any
sample, the RMD shall be contacted and the result shall be qualified if included in the
report.

It is important to note that the absence of any spectral differences across a peak is not
an indication of and should never be equated to actual chemical purity, as compounds
similar to the target analyte may have similar absorbance profiles, the relative
concentration of actual impurities may not be high enough to detect, the peaks are not
resolved sufficiently (peak purity requires some resolution), or the compounds/impurities
may not absorb light at the wavelengths scanned. To determine chemical purity, the
sample may be analyzed using different analytical techniques such as liquid
chromatography coupled with mass spectrometry (LC-MS), infrared spectroscopy (IR),
nuclear magnetic resonance spectroscopy (NMR), or other wet chemistry techniques.
Peak purity, as determined with DAD is used to help with the method development
process and is used as an indication that a peak may not be composed of a single
compound.
9.4 Validation Guidance for Microbiological Analyses
This section establishes method validation criteria for performing single-laboratory validation
of methods that were developed to detect, identify, and quantify microbial analytes. This
section applies when validating the performance of plate-count methods (e.g., Petrifilm™,
pour plates, spread plates, etc.), commercially-available microbiological diagnostic kits or
automated instruments whose performance parameters were fully validated in multi-
laboratory collaborative studies and evaluated by an independent accrediting body (e.g.
AOAC, AFNOR, etc.) or validated by the USP, FDA, EPA or WHO.

Such applicable areas of methods development and evaluation include, but are not
limited to, the following:
 Qualitative microbiological methods (i.e., detection assays)

 Quantitative microbiological methods (i.e., real-time polymerase chain reaction
[PCR])
 Organism specific methods:
o Bacteriological pathogens:
 Salmonella spp.
 Pathogenic Escherichia coli
 Aspergillus
 Phenotypic Methods:
o Biochemical characterization for identification
o Antibiotic resistance traits for identification
o Antigenic characterization for identification
 Genetic Based Methods:
o Nucleic acid isolation/concentration/purification
o Polymerase Chain Reaction
 Conventional
 Real-time
 Reverse transcription
o Sequencing:
 Whole genome
 Selective sequencing
 Single nucleotide polymorphism (SNP) analysis
o Strain-typing applications
 Immunological Methods:
o Antibody capture
o ELISA
o Flow cytometry
 Plate-count methods (e.g., Petrifilm™, pour plates, spread plates, etc.);
 Commercially-available microbiological diagnostic kits or automated instruments
whose performance parameters were fully validated in multi-laboratory
collaborative studies and evaluated by an independent accrediting body (e.g.
AOAC, AFNOR, etc.) or validated by the USP, US FDA, US EPA or WHO.
Validation is the confirmation by examination and the provision of objective evidence that
the particular requirements for a specific intended use are fulfilled. The independent testing
laboratory shall validate non-standard methods, laboratory-designed/developed methods,
standard methods used outside their intended scope, and amplifications and modifications
of standard methods to confirm that the methods are fit for the intended use. Validation of
microbiological methods is performed to demonstrate with adequate confidence that the
results obtained by the in-house developed method are comparable to or exceed the
precision and accuracy obtained relative to a validated reference method using a pre-
determined statistical criteria contained in an approved validation protocol. When
performing method verification, the independent testing laboratory is to confirm that the
method can detect, identify, and quantitate an analyte while meeting the performance
specifications established during method validation. The independent testing laboratory

shall record the results obtained, the procedure used for the validation, and a statement as
to whether the method is fit for the intended use.
Each independent testing laboratory shall perform an in-house validation for the “first use” of
such methods per the requirements prescribed in the subsequent sections below. For
subsequent use(s) of the method, independent testing laboratory control samples are to be
prepared for each lot of media and/or lot of diagnostic kits used to re-verify the method. For
microbiological methods, typical validation would be comprised of the following elements:
9.4.1 Environmental Control Samples
Controls for environmental conditions are to be used to assess biological sterility of the
ambient independent testing laboratory environment. Acceptable environmental QC
samples are to exhibit minimal total growth and growth of the target organisms are to be
< LOD to demonstrate control. These controls are to be analyzed with each preparation
batch (as defined in Section 1.1), and at a weekly frequency unless client samples are
not analyzed for that method within the week. Environmental condition controls include,
at a minimum, air settling plates and/or petri dishes utilizing every medium utilized in the
method being evaluated. These controls are to be located in the immediate environment
(e.g. hood, benchtop, instrument area, etc.) of client samples during sample set-up,
enrichment, incubation, and analysis. The controls are to be left exposed to the sample
environment from the start of the method (i.e. client sample set-up of the first sample)
through the recording of the final raw result when the independent testing laboratory
procedures indicate the associated client sample analysis is complete.
9.4.2 Negative Controls
Prepare and analyze negative culture controls with each preparation batch of samples
as defined in Section 1.1 to assess contamination associated with sterile technique and
test sample handling and transport. Negative controls can be sterile dilution buffer (for
non-selective media) or an organism for which growth is not supported by the selective
medium; e.g., atypical or no growth. These controls are to be of a matrix similar to the
batch of associated samples (when available) that is free of contamination and is
processed simultaneously with and under the same conditions as samples through all
steps of the analytical procedures and in which no contamination is present at
concentrations that impact the analytical results for sample analyses.
For validation studies, six replicates of the sterile matrix (non-selective media) or six
replicates of non-target organisms (selective media) are to be prepared, tested, and
confirmed by the method. The default acceptance criterion for negative controls are <1
CFU/g of matrix being tested. If the independent testing laboratory negative control(s)
fail to meet acceptance criteria, then the associated samples that were prepared in the
independent testing laboratory since the last acceptable independent testing laboratory
blank are considered suspect and reanalyzed.
9.4.3 Positive Culture Controls
The independent testing laboratory shall prepare and analyze positive culture controls in
order to assess and demonstrate method accuracy. A positive culture control shall
exhibit positive growth or exhibit expected characteristics to assure the system is

working. For example, turbidity in a tube filled with enrichment broth showing growth or
a characteristic physical (phenotypic) colony for the bacterial culture showing a positive
test result.
For validation studies, six replicates are to be prepared in the inoculated matrix, tested,
and confirmed by the method. The default acceptance criterion for accuracy, reported
as percent recovery of the spiked amount, is 80-120%.
9.4.4 Precision
Sample duplicates are not required but are recommended for microbiological sample
analyses. When the precision is expressed as relative percent difference (RPD)
between duplicate samples, the RPD is to be ≤ 20% unless otherwise specified in the
QAPP or by a control limit determined in accordance with the technical procedure. For
results expressed as Most Probable Number (MPN), both results should be within the
95% confidence interval (if available) for at least one of the results.
Six replicates each are to be prepared in the inoculated matrix, tested, and confirmed by
the method. When samples are not analyzed in duplicate, control can be demonstrated
by maintaining false positives or false negatives at a rate of ≤ 5%.
9.4.5 Specificity
Evaluate potential interferences for each analyte under a given set of method conditions.
For the evaluation of microbial interferences, analyze a sample containing various
suspected interferences in the presence of the measure.
 All growth and recovery media shall be checked to assure that the target
organism(s) respond in an acceptable and predictable manner.
 To ensure that analysis results are accurate, target organism identity shall be
verified as specified in the method (e.g., by use of the completed test) or by use
of secondary verification tests.
 In order to ensure identity and traceability, reference cultures used for positive
and negative controls shall be obtained under an ISO Guide 34 accreditation.
Microorganisms may be single-use preparations or exist as cultures that are
maintained. Cultures that are maintained shall be verified for their intended use
(e.g., acceptable purity, stability, and viability of the organism) using documented
procedures and acceptance criteria.
 Reference cultures may be revived (if freeze-dried) or transferred from slants and
sub-cultured one time, in order to provide stock reference material. The
reference material shall be preserved by a technique that maintains the
characteristics of the strain/organism. Characterized reference materials shall be
used to prepare working standards for routine work. If reference materials have
been thawed, they shall not be refrozen and re-used.

 Working standards shall not be sequentially cultured more than five times and
shall not be sub-cultured to replace the original stock reference material.
9.4.6 Assay Ruggedness
Demonstrate the ruggedness of the assay by adjusting critical parameters such as

incubation time, incubation temperature and waiting time before incubation.
9.4.7 Re-Validation
When the testing procedure is modified from the existing SOP/protocol in such a way
that does not meet the criteria in Section 9.0, the independent testing laboratory is to
demonstrate that the modifications do not adversely affect the precision and accuracy of
the method. If the results are acceptable then re-validation of the test method is not
necessary. However, if the accuracy and precision of the method is not acceptable
following a modification to the method then validation is to be performed using the new
conditions, prior to sample analysis.
10.0 QUALITY CONTROL SAMPLES AND PROCEDURES
The independent testing laboratory is to implement an approved procedure defining warning

limits, control limits, analysis frequency, acceptance criteria, and corrective actions for QC
samples or for calibrations in the SOPs for metals, cannabinoid profile, pesticides, residual
solvents, mycotoxins, and microbiological methods.
10.1 General
QC includes all technical activities that measure the characteristics and performance of a
MDPH approved independent testing laboratory process or procedure against defined
standards. The MDPH QAPP and associated technical procedures are to provide those
standards and procedures for identifying those standards. In order to monitor and control
data quality, independent testing laboratories are to apply MDPH-provided guidance in
addition to approved methods and good laboratory practices to define QC samples and
establish performance indicators. Such indicators include instrument- or protocol-related
parameters that are routinely monitored in order to evaluate the independent testing
laboratory’s performance and to provide information needed for estimating measurement
uncertainty (i.e., precision, bias, etc.). QC samples are used to demonstrate control over the
analytical process and are to be tracked by appropriate personnel. If the QC sample control
limits are exceeded, independent testing laboratory management is to be informed and
corrective action is to be initiated.
The independent testing laboratory is to define method QC sample preparation, warning

limits, control limits, sample analysis frequency, acceptance criteria, and corrective actions
for QC samples or for calibrations in each analytical SOP. In the absence of method-
specified limits, apply a defined procedure for determining warning limits and control limits,
involving outlier testing, and statistical process control principles.
Within each written SOP/protocol, establish the following QC procedures in order to monitor
method performance and QC:

 Positive and negative controls, chemical or microbiological as applicable to the test

type, to monitor tests such as blanks, matrix spikes, etc.;
 Tests to define the variability and/or repeatability of the independent testing
laboratory results such as replicates;
 Measures to assure the accuracy of the method including calibration and/or
continuing calibrations, use of certified reference materials, proficiency test samples,
or other measures;
 Measures to evaluate method capability, such as Limit of Detection and limit of
quantitation or range of applicability such as linearity;
 Selection of appropriate formulae to reduce raw data to final results such as
regression analysis, comparison to internal/external standard calculations, and
statistical analyses;
 Selection and use of reagents and standards of appropriate quality;
 Measures to assure the selectivity of the test for its intended purpose; and
 Measures to assure constant and consistent test conditions (both instrumental and
environmental) where required by the method such as temperature, humidity, light or
specific instrument conditions.
Method performance is typically monitored by evaluating certain QC samples along with

each batch of samples under study. A batch is defined as samples prepared and/or
analyzed together with the same process and personnel, using the same lot(s) of reagents.
A preparation batch is composed of 1-20 sample(s) of the same quality systems matrix,
meeting the above-mentioned criteria and with a maximum time between the start of
processing of the first and last sample in the batch to be 24 hours. An analytical batch is
composed of prepared samples (extracts, digestates, or concentrates) which are analyzed
together as a group. An analytical batch can include prepared samples originating from
various quality management system matrices and can exceed 20 samples. The QC
samples included in each batch measure performance characteristics of the entire process
on an ongoing basis.
When preparing QC samples, any piece of equipment that comes in contact with the product
under analysis (e.g. forceps, syringes, scalpels, scissors, swabs, pipettes, membranes, or
other special items that may be required by a specific test, etc.) along with any
manipulations performed by the analysts, are to be controlled and tested throughout each
analysis. Thus, all equipment, fluids, and culture media used to prepare quality control
samples shall be handled in a manner that duplicates, as closely as possible, the
manipulations of the actual sample being analyzed.
For microbiological assays, all materials used as laboratory controls are to be sterilized by
the independent testing laboratory. However, the method of sterilization need not be the
same as that used for the product sample, but shall render the material sterile. When
products are tested by direct inoculation (e.g. non-filterable materials, insoluble solids, etc.)
the independent testing laboratory shall use uncontaminated products for laboratory controls
that are similar in size, shape, and texture as the product being tested. As part of daily
verification of method performance,

10.2 Batch Quality Control Samples
The default set of batch QC samples are as follows:
 Laboratory/Method blanks (Negative Controls): A sample of a matrix similar to the

batch of associated samples (when available) that is free from the analytes of
interest and is processed simultaneously with and under the same conditions as
samples through all steps of the analytical procedures (e.g., homogenization,
subsampling, digestion, extraction, cleanup and analysis), and in which no target
analytes or interferences are present at concentrations that impact the analytical
results for sample analyses.
 Laboratory Control Samples: A spiked sample for chemistry or positive culture

control for microbiology analyses that is generally used to establish intra-laboratory
or analyst specific precision and bias or to assess the performance of all or a portion
of the measurement system.
 Matrix Spike (spiked sample or fortified sample): A sample prepared, taken through
all sample preparation and analytical steps of the procedure unless otherwise noted
in a referenced method, by adding a known amount of target analyte to a specified
amount of sample for which an independent test result of target analyte
concentration is available. Matrix spikes are used, for example, to determine the
effect of the matrix on a method's recovery efficiency.
 Laboratory Duplicates/Matrix Spike Duplicates: Two aliquots of the sample used to

assess precision of the analytical process.
The independent testing laboratory should determine, based on the objectives and confines
of the method, whether laboratory duplicates or matrix spike duplicates will make a more
useful comment on precision. If the target analytes are assumed to be mostly non-detect,
as in a contaminant analysis, it is prudent to choose the Matrix Spike Duplicates so that
actual numbers are compared. If the target analytes are expected to present in
concentrations above the method LOQ, a laboratory duplicate is very useful, especially in
the case of an investigation of a data request or an evaluation of whether re-analysis is
necessary.
The QC samples listed above are in addition to required instrument-specific checks such as
calibrations and Calibration Verification Samples: (Calibration check standards analyzed
periodically in the analytical batch for quantitative analyses), instrument blanks and
interference checks.
10.2.1 Establishing Control Limits
The default advisory limits for accuracy (Appendix A) are to be used until such time as
20 or more data points are obtained under a set procedure. After that time, the data are
to be examined for statistical outliers, or failures from a known, assignable cause. Both
types of values are to be removed from the data set, and then summary statistics are to
be calculated to determine mean and standard deviation for the purpose of setting
warning and control limits. The independent testing laboratory is to use these

laboratory-developed control limits, unless they exceed the limits in the DQO tables, in
which case the DQO limits are to be applied.
The upper and lower warning limits (UWL, LWL) are to be set at 2 σ from the mean and
the upper and lower control limits (UCL, LCL) are to be set at 3 σ from the mean.
For example, when a QC sample data point is outside of ± 3σ this is considered a rare
event, which indicates that there is only a 0.3% chance that this was caused by the
normal laboratory process. Since this data was outside of the warning limits, the data
would typically be rejected and an investigation shall typically be conducted. The
investigation is a planned action to correct the problem and to prevent the reporting of
incorrect results. Sometimes the investigation shall reveal a recording or computational
mistake that can be revised to obtain the correct value. If the investigation reveals an
assignable cause, i.e. deterioration of reagents, improperly prepared reagents,
inadequate storage of reagents or standards, then the analysis is to be repeated. When
outliers are found, all analytical results for that analytical batch are inspected to ensure
that erroneous results are not reported.
Additional detail should be provided in the independent testing laboratory’s technical

procedures for establishing and updating normality testing, skewness correction, proper
exclusion of for-cause outliers and statistical outliers.
10.2.2 QC Sample Data Review
Implement an approved procedure for review of data supporting reported sample results
and associated QC data. This is to include an independent review of data supporting
sample results and associated QC data.
Data that is determined to be a statistical outlier shall be flagged as such and is

excluded from the data set before statistical calculations are made. Control limits
calculated from data sets containing outliers are not valid.
Each suspected outlier is evaluated and rejected if found to be unrepresentative, or to

have a high probability of being unrepresentative. Rejection for a reason is referred to
as rejection for assignable cause.
An outlier is a data point that is different from the main data pattern, and/or is not
representative of the data set. Outliers are extreme cases of one variable, or a
combination of variables, which have a strong influence on the calculation or statistics.
The primary protections against obtaining or using an outlier are awareness during all
operations and visual inspection of data before performing statistical analyses. Formal
outlier testing or assignable causes shall be the only basis for point exclusion.
Control charts are typically used for detecting shifts of the monitored variable than charts
based on individual observations. The chart shall disclose trends and shifts from
assignable causes that can be corrected. A trend shall show a tendency or movement in
a particular direction. If a series of consecutive data points move steadily either upward
or downward, a trend is indicated. If a series of consecutive data points fall either above
or below the centerline, a shift is indicated. When a trend or shift is detected, it is
annotated as such on the chart and reviewed to the extent possible to identify if a

significant concern is indicated regarding the QC sample results and overall method
performance. If the review indicates a significant concern, a corrective action is initiated
to determine the cause.
The following rules should be considered when conducting trend analysis:

1. A data point is greater than three standard deviations from the mean.
2. Nine points in a row are all on the same side of the mean.
3. Six points in a row are all either increasing or decreasing.
4. Fourteen points in a row alternating up and down.
5. Two out of the last three points are greater than two standard deviations away
from the mean on the same side.
6. Four out of the last four points are greater than one standard deviation from the
mean on the same side.
7. Fifteen points in a row are less than one standard deviation from the mean on
either side.
8. Eight points in a row are greater than one standard deviation from the mean on
either side.
10.2.3 QC Sample Documentation and Review
Implement the following QC procedures:

 Document an unbroken chain of QC procedures tracing the final preparation to the
initial lot of materials (e.g., equipment, standards and reagents);
 Identify QC samples that are prepared and analyzed with a given sample analysis
sequence in the instrument software for an analytical sequence and/or on the work
instruction sheets;
 Document a review of independent testing laboratory notebooks at a specified
frequency.
The independent testing laboratory shall, upon request, provide all supporting data and
information to demonstrate that the laboratory is in compliance with these requirements.
This information may include, but is not limited to the following:
 Data verifying the training of the analyst performing the analyses;

 Data pertaining to the sample preparation and cleanup that is material to the
sample result and associated quality control sample results.
 Data verifying that the analytical system was properly calibrated and in control at
the time of analysis, including:
o Calibration and verification method and frequency,

o Source of standards,
o Concentrations of standards,
o Response factors,
o Instrument linear ranges,
o Check standards,
o Control limits,
o Logbooks,
o SOPs,

o Sample preparation records,

o LOQ verifications, and
o LOD studies
10.3 Equipment
10.3.1 Testing, Inspection, Maintenance and Calibration of Support Equipment
All quantitative apparatus used as part of sample preparation (including, but not limited
to, thermometers, micropipettes, microsyringes, auto dispensers, balances, and weights)
are to undergo frequent, documented calibration/tuning checks inclusive of meeting a
reasonable acceptance criterion (e.g., ± 2% of the true value for volumetrics) and
documented corrective action when acceptance criteria are not met. Certification
information (cleanliness and volume precision) for all quantitative apparatus are to be
maintained with complete traceability. All volumetric labware shall be Class A.
Disposable labware used for volumetric measurements shall be demonstrated on a
production lot basis to have accuracy and precision meeting Class A specifications.
Extracts for the analysis of organic compounds are to be stored in the same type of vials
(amber or clear) as the associated standards and at the appropriate storage
temperatures. Sample preparation is to be fully documented and inclusive of sample
preparation conditions (e.g., digestion, extraction, cleanup, etc.) and documentation that
allows traceability of analytical data back to all prepared and purchased reagents,
acids/solvents, filters, digestion tubes, and reference solutions, and their certificates of
analysis or statements of purity (e.g., lot numbers of solvents and acids recorded in
preparation logs). Wherever practicable, support equipment is to be labeled with a
unique ID and a calibration expiration date. If an expiration date of calibration cannot be
directly labeled, it is the responsibility of the staff member who utilizes that piece of
equipment to ensure it remains in calibration.
10.3.1.1 Thermometer Calibration
Thermometers or other appropriate temperature measurement devices are to be

calibrated at least annually against a NIST-certified thermometer. All thermometers
are to be labeled with a unique identification number, the date of calibration, the date
that the next calibration is required, and the correction factor (even if “0.0°C”). The
independent testing laboratory NIST-certified thermometer is to be re-certified at a
minimum of every 3 years. Recorded temperatures are to include the identifier for
the thermometer used, the actual thermometer measurement and corrected
thermometer measurement.
10.3.1.2 Balance Calibration and Verification
Balances and weights shall be checked by an ISO 17025 accredited outside vendor
on an annual basis, and inspection stickers are to be available for examination.
Logbooks and electronic logs are to contain the unique IDs of the balance and the
weights, the acceptance criteria and are to include periodic documented peer or
supervisory review. The review period for this review is to be at least quarterly.
If the independent testing laboratory wishes to verify the linearity of the balances on
a daily basis in addition to bracketing the use range then include a protocol for

testing a minimum of three weights for linearity checks, and include additional
weights needed to bracket the current use range. When performing balance
verification use ASTM Class 1 weights (or equivalent). Incorporate the acceptance
criteria listed in the DQO tables in Appendix A
Laboratory top-loading balances shall be capable of 0.1-gram accuracy for sampling.

Analytical balances shall be capable of accuracy to 0.001 mg. All balances and their
records shall be inspected at minimum by an accredited vendor performing
calibration and certification in compliance with ISO/IEC 17025. The independent
testing laboratory QA department is accountable for verifying a label is placed on
each calibrated balance and that a calibration certificate is obtained.
10.3.2 Testing, Inspection, Maintenance and Calibration of Analytical Equipment
10.3.2.1 HPLC (UV-Vis or DAD)
Note: Additional details on the following requirements appear in Appendix A.
Instrument stability and performance are to be monitored on an ongoing basis to

determine if there are conditions that affected the data quality of client samples. The
independent testing laboratory is to, as part of the data review record, document this
evaluation for each analytical batch. If it is determined from this evaluation that the
data quality was possibly affected, it shall be documented in the client report
narrative.
This is achieved by evaluating baselines, chromatographic peak shape, retention

times, interferences, or reduced sensitivity on each analysis of standards, samples,
dilutions, and QC samples.
Evaluation in chromatography methods includes the monitoring of surrogates that

closely match the behavior of the target analyte. If the lab deems there is an
appropriate mix of surrogates for the target analytes or there are suggested
surrogates listed in accepted reference methods for chromatography analysis of the
target analytes in marijuana matrices, it is recommended the independent testing
laboratory use these surrogates to monitor extraction efficiency and instrument
performance to the criteria found in Appendix A, Table 6.
10.3.2.2 ICP-MS
The ICP-MS method validation is to include a Linear Dynamic Range study that
exceeds the daily working linear range to determine the initial instrument linearity.
This range is to be verified annually or as need to identify any possible degradation
of the instrument components that would affect data quality. Interelement correction
factors shall be measured and updated at least semi-annually. Interelement and
isobaric interferences shall by monitored daily and collision cell or reaction cell
technology shall be used to suppress such interferences.

A minimum of four measures of intensity are to be used and averaged in determining

signal intensity. Downward trending of the individual measures is to be used in
assessing whether carryover is affecting the measurement.
Internal Standards are available and required when analyzing for metals in marijuana
matrices.
10.3.2.3 GC-FID
Instrument stability and performance are to be monitored on an ongoing basis to

narrative. If large differences are noted between two columns or between GC/FID
and GC/MS analysis, GC/MS analysis shall be used to report the result of the target
analyte
This is achieved by evaluating baselines, chromatographic peak shape,

interferences, or reduced sensitivity on each analysis of standards, samples,
dilutions, and QC samples.
Gas chromatography requires confirmation of result on a column of different polarity

or an MS detector. When sample results are confirmed using two dissimilar columns
or with two dissimilar detectors, the agreement between the quantitative results
should be evaluated after the identification has been confirmed. Large differences in
the numerical results from the two analyses may be indicative of positive
interferences with the higher of the results, which could result from poor separation
of target analytes, or the presence of a non-target compound.
Evaluation in chromatography methods includes the monitoring of surrogates that

closely match the behavior of the target analyte. If the lab deems there is an
appropriate mix of surrogates for the target analytes or there are suggested
surrogates listed in accepted reference methods for chromatography analysis of the
target analytes in marijuana matrices, it is recommended the independent testing
laboratory use these surrogates to monitor extraction efficiency and instrument
performance to the criteria found in Appendix A, Table 03b.
10.3.2.4 GC-MS
Instrument stability and performance is to be monitored on an ongoing basis to

narrative.

Due to the nature of mass spectrometry, if the lab deems that there is an appropriate
mix of internal standards is available or there are lists of internal standards listed in
an accepted reference method for MS detection in the analysis of the target analytes
in marijuana matrices, the independent testing laboratory is to utilize these internal
standards to monitor instrument performance to the criteria found in Appendix A,
Table 3a.
Monitoring instrument stability and performance is achieved by evaluating baselines,

chromatographic peak shape, interferences, or reduced sensitivity on each analysis
of standards, samples, dilutions, and QC samples. Evaluation in chromatography
methods includes the monitoring of surrogates that closely match the behavior of the
target analyte. If the lab deems there is an appropriate mix of surrogates for the
target analytes or there are suggested surrogates listed in accepted reference
methods for chromatography analysis of the target analytes in marijuana matrices, it
is recommended the independent testing laboratory use these surrogates to monitor
extraction efficiency and instrument performance to the criteria found in Appendix A,
Table 3a.
10.3.2.5 LC-MS-MS
Instrument stability and performance is to be monitored on an ongoing basis to

narrative.
Due to the nature of mass spectrometry, if the lab deems that there is an appropriate
mix of internal standards is available or there are lists of internal standards listed in
an accepted reference method for MS detection in the analysis of the target analytes
in marijuana matrices, the independent testing laboratory is to utilize these internal
standards to monitor instrument performance to the criteria found in Appendix A,
Table 4.
Monitoring instrument stability and performance is achieved by evaluating baselines,

chromatographic peak shape, interferences, or reduced sensitivity on each analysis
of standards, samples, dilutions, and QC samples. Evaluation in chromatography
methods includes the monitoring of surrogates that closely match the behavior of the
target analyte. If the lab deems there is an appropriate mix of surrogates for the
target analytes or there are suggested surrogates listed in accepted reference
methods for chromatography analysis of the target analytes in marijuana matrices, it
is recommended the independent testing laboratory use these surrogates to monitor
extraction efficiency and instrument performance to the criteria found in Appendix A,
Table 4.

10.3.3 Testing, Inspection, Maintenance and Calibration of Microbiological

Equipment and Support Equipment
10.3.3.1 PCR/Fluorescence Systems
QC samples included in the instrument procedure provide feedback on the

functioning of PCR/Fluorescence instrumentation. The microbiology procedures in
the laboratory shall include record keeping that traces each QC check in Appendix A,
Table 09 to a result.
10.3.3.2 Temperature Measuring Devices
Temperature measuring devices such as liquid-in-glass thermometers,

thermocouples, and platinum resistance thermometers used in incubators,
autoclaves and other equipment used during microbiological analyses shall have the
appropriate graduation and quality to meet specification(s) in the method. These
devices shall be verified to national or international standards for temperature.
Verification shall be done at least annually.
10.3.3.3 Incubators
Temperature of the incubator should be verified twice a day when in use, with the
time of each verification separated by at least four hours. If temperature windows
are exceeded, catalog contents of incubator and re-prepare. If there is not enough
sample mass to reanalyze, qualify the results on the client report.
The surfaces within the incubator that come into direct contact with sample plates or
films (i.e. trays or racks) should be cleaned using a lint free cloth and disinfectant
after each use, or daily at a minimum. The remaining surfaces and other
components of the incubator should be cleaned with a lint-free cloth and disinfectant
on a weekly basis.
10.3.3.4 Autoclaves
The performance of each autoclave is to be initially evaluated by establishing its

functional properties and performance, for example heat distribution characteristics
with respect to typical uses. Demonstration of sterilization temperature is to be
provided by use of a continuous temperature-recording device or by use of a
maximum registering thermometer with every cycle. At least once during each
month that the autoclave is used, appropriate biological indicators shall be used to
determine effective sterilization. The selected biological indicator shall be effective at
the sterilization temperature and time needed to sterilize lactose-based media.
Temperature sensitive tape shall be used with the contents of each autoclave run to
indicate that the autoclave contents have been processed. Autoclave maintenance
(either internally or by service contract) shall be performed annually and shall include
a pressure check and verification of the temperature device performance. The
autoclave mechanical timing device shall be verified quarterly against a stopwatch
and the actual time elapsed documented.

Records of autoclave operations shall be maintained for every cycle. Records shall
include: date, contents, maximum temperature reached, pressure, time in
sterilization mode, total run time (may be recorded as time in and time out) and
analyst’s initials.
10.3.3.5 UV Instruments used for Sterilization
UV instruments, used for sanitization, shall be tested quarterly for effectiveness with
an appropriate UV light meter, by plate count agar spread plates or other methods
providing equivalent results such as UVCide® strips. If the output is less than 70% of
original for light tests or if count reduction is less than 99% for a plate containing 200
to 300 organisms, the bulbs of the UV instrument are to be replaced.
10.3.3.6 Labware
The independent testing laboratory shall have a documented procedure for washing
labware used for microbiological analysis, if applicable. Detergents designed for
independent testing laboratory use shall be used. Glassware shall be made of
borosilicate or other non-corrosive material, free of chips and cracks, and shall have
readable measurement marks. Washed labware shall be tested at least once daily,
each day of washing, for possible acid or alkaline residue by testing at least one
piece of labware with a suitable pH indicator such as bromothymol blue. Records of
testing of washed labware shall be maintained.
10.4 Water for Analysis
Water specifications have been described by ASTM (American Society for Testing and
Materials) D1193, ASTM D5196, ISO 3696, and USP <1231> Water for Pharmaceutical
Purposes. Historically waters of the highest purities have often been described as “Type I”
to designate ultrapure waters, and Type II, Type III or Type IV to designate lower grades
(Table 5).
Resistivity and conductivity are concepts to be familiar with when it comes to water purity.
Resistivity is the tendency of water without ions to resist conducting electricity. The unit of
measure is megaohm-centimeter (MΩ-cm), and varies with temperature. The theoretical
maximum is 18.2 to 18.3 MΩ-cm at 25°C. The higher the ionic content, the lower the resistivity
and conversely, the lower the ionic content, the higher the resistivity.
Conductivity is the tendency of water that contains ions to conduct electricity. The unit of
measure is the Siemen(S), microsiemens/centimeter (μS/cm) or micro-ohms/cm. Conductivity
increases with temperature so values are reported as compensated at 25 °C whereas
resistivity is the inverse of conductivity and is expressed in 18.2 MΩ-cm @ 25 °C.
The ASTM establishes specifications for Types I, II, III, and IV reagent grade water (D1193-06-
2011) as shown on Table 5. The water quality is further classified as Type A, Type B, or Type
C depending on the applicable bacteriological and endotoxin quality (Table 6). ASTM D1193-
06 Type I water (or equivalent) is to be used for all chemical analyses performed under the
guidance provided in this QAPP.

The conductivity of the deionizing water systems shall be monitored and recorded in a log or
logbook on each working day. Additionally, the cell constant of each resistivity meter shall be
checked on an annual basis. Proper indication of corrective actions shall be recorded as
comments in the logbook when the resistivity does not meet the lower acceptance limits.
For ongoing checks of water used for microbiological analyses the criteria for Type I water and
those presented on Table 6 should be met. Additionally, for microbiological analyses, the
established DQO criteria for specific pathogens in dilution water and buffers presented within
the DQO Tables presented on Tables 8 and 9 of Appendix A, should be established per lot or
batch of water or buffer used.
Table 5 American Society for Testing and Materials Reagent Grade Water
Specifications ASTM D1193-06 (2011)
Parameter Type I Type II Type III Type IV
Resistivity, min. MΩ-cm (@ 25°C) 18.0 1.0 4.0 0.2
pH, SU (@ 25°C) NA NA NA 5 to 8
TOC, max. (µg/L) 50 50 200 NS
Sodium, max. (µg/L) 1 5 10 50
Chloride, max. (µg/L) 1 5 10 50
Total Silica, max. (µg/L) 3 3 500 NA
Table 6 American Society for Testing and Materials ASTM D1193-06 (2011)
Parameter Type A Type B Type C
Bacteria, max. (CFU/100 mL) 1 10 1000
Endotoxin (EU/mL) < 0.03 0.25 NA
10.5 Preventative measures
Specific procedures for maintaining a sterile workspace and preventing cross-contamination

are to be written in to each SOP as appropriate for the target organisms. Floors and work
surfaces shall be non-absorbent and easy to clean and disinfect. Work surfaces shall be
adequately sealed. Laboratories shall provide sufficient storage space, and shall be clean
and free from dust accumulation. Plants, food, and drink are prohibited from the laboratory
work area.
10.6 Lock Out and Tag Out Procedures
If any piece of laboratory equipment is not functioning properly, proper tag out or lock out
procedures are to be followed according to established written procedures. No piece of
equipment that is properly locked out or tagged out is to be used for analytical purposes.
11.0 QUALITY ASSURANCE ACTIVITIES
Several assessment and oversight activities are to be conducted in order to prevent and correct
non-conformities and other quality management system issues. These include preventative
actions; identifying and tracking non-conformities; implementing and monitoring informal and
formal corrective actions, internal auditing and external oversight; performance testing;
performing root cause analysis; management review. The following sections provide details on
implementing good practice for these activities.

11.1 Preventative Actions
Preventative actions and corrective actions are often thought to be synonymous. Although
they can be handled with the same process preventative action by definition occurs prior to
non-conformity. Preventative action often occurs informally by independent testing
laboratory staff involved with the quality management system. If an independent testing
laboratory can foresee an event or a process at risk, the laboratory management often takes
action to avert the potential loss of control and avert disruption to operations.
Preventative actions applied may include training on upcoming new methods, hiring back-
ups, and training them before employee turnover, maintenance on an instrument that is
known to decline in performance during a certain timeframe etc.
This practice is to be recorded to show the effectiveness of client feedback, management

review, and staff engagement in the independent testing laboratory quality management
system. The concern of potential nonconformance and supporting information can be
entered into the same tracking and use the same forms as corrective action with an
examination of potential nonconformance based on the observed possible root cause.
All employees are to be trained in recording potential causes of nonconformance, whether in

a separate tracking system or in the same system as the Corrective Action Tracking System
and these are to be discussed at management review meetings.
An effective procedure to involve staff in the recognition of causes at the root of

nonconformances requires setting aside roughly 10 minutes of regularly conducted
department meetings to allow the quality manager to address nonconformances and client
complaints. Developing this communication between the QA department and individual
departments, explaining the importance to the continual improvement of independent testing
laboratory operations and procedures, explaining the importance of tracking the corrective
and preventative actions as a tool that is both a best practice and a certification requirement
all serve to meet data integrity requirements. Feedback at such meetings of successful
corrective actions taken as a result of nonconformances and preventative actions succeed
in bolstering the quality assurance procedures in place.
11.2 Complaints
The independent testing laboratory is to demonstrate a commitment to continuous

improvement and service to the client in all of its documentation of communication with
clients.
The independent testing laboratory shall have a detailed definition of a client compliant in its
procedures and these procedures shall apply to all staff of the independent testing
laboratory in order to capture complaints regardless of the method through which they are
received. The independent testing laboratory shall track all complaints for evaluation during
the Management Review and shall outline in the procedures which types of complaints are
to be elevated to the proper independent testing laboratory personnel member in order to be
included in the formal Corrective Action system. The types of complaints that shall be
elevated to require formal corrective action include, but are not limited to:

 Data/report amendments,
 Non-Conformance affecting data quality,
 Non-Conformance to lab procedures,
 Non-Conformance to MDPH Protocols and QAPP
 Sampling Non-Conformance,
 Request for Raw Data pertaining to report that is unavailable,
 Requests for Re-Runs not met, and
 Re-Sampling and Re-analysis results differ.
The independent testing laboratory personnel that are responsible for investigation of any
corrective actions are to have documented training on root cause analysis. Laboratory
investigation records are to include an assigned corrective action that follows from the root
cause analysis and are to include records of follow-up on the corrective action to ensure
effectiveness. Follow-up records are to include date of follow-up, person performing the
follow-up, records reviewed, and an evaluation of whether the corrective action, and
therefore the root cause analysis, was sound enough to correct the problem and prevent
recurrence.
It is helpful to define clearly complaints that need to be recorded in order to track client
feedback that pertains to quality. These procedures should be required in the training plans
of all staff as the staff members who most often receive complaints, such as sample receipt
personnel, are sometimes unaware that it is necessary to record these and have them
investigated.
11.3 Identifying and Recording Non-Conformances
The independent testing laboratory is to have procedures describing the process by which
non-conformances are identified and recorded and the formal Corrective Action process is
to be used if these nonconformances are defined in the laboratory procedures as requiring
formal Corrective Action.
All employees are to be trained to identify non-conformance and to document the

occurrence according to independent testing laboratory procedure. When nonconformance
is detected or suspected within independent testing laboratory operations, the laboratory
management is notified and is to evaluate the situation and proceed in accordance with the
laboratory procedure for nonconformances. An evaluation of the significance of the
nonconformance is to be made by authorized individuals within the independent testing
laboratory management.
A nonconformance is a result, condition, or action that falls outside procedural or quality

management system requirements.
Nonconformance may consist of any of the following:

 Nonconforming Laboratory Analyses:
o Invalid test results;
o Incomplete test reports;
o Incorrect equipment information;
o Incorrect data reduction and calculation of sample results;

o Late test reports;

o Deviation from laboratory standard operating procedures;
o Other
 Deviations from laboratory quality management system policies and procedures (e.g.,
Quality Manual, SOPs);
 Analytical and/or general equipment issues;
 Software issues;
 Third-party Vendor services or products that do not meet the requirements of the
laboratory quality management system
o Reagents or standards which are expired or do not meet laboratory
specifications;
o Nonconforming service (i.e. contract laboratory analysis);
o Damaged materials or client samples; and
o Other.
 Client error:
o Incomplete or failure to provide comprehensive testing specifications
o Inappropriately preserved, transported or documented materials or samples;
 Other as applicable.
A major nonconformance is a situation that affects critical laboratory processes and

operations and requires immediate attention and action, a situation that may cause
significant impact to data quality or utility. A minor nonconformance is a situation that
affects laboratory operations and could become a major nonconformance if it recurs
frequently. With frequent recurrence, it becomes a threat to the laboratory operations or is a
situation that may cause changes to laboratory environments if not controlled. Minor
nonconformances are to be tracked to ensure they are random and not systemic.
Each identified nonconformance requires prompt action and may require additional action,
including the suspension of a particular independent testing laboratory process until an
investigation can be performed. The quality manager (or designee) has the authority and
responsibility to lead the investigation of a nonconformance, to determine root cause and to
identify the corrective action needed.
When a nonconformance is recognized as major nonconformance, an investigation is to be

initiated by the independent testing laboratory as described in Section 11.5.1. When a
nonconformance is recognized as a minor nonconformance the independent testing
laboratory shall determine whether an investigation is to be initiated and whether formal
corrective action is warranted. Each identified nonconformance is to be recorded by the
independent testing laboratory and the record is to indicate the nature of the
nonconformance and the action taken.
The RMD is to be notified when analytical testing requests do not have sufficient information
regarding testing specifications or when sample receipt issues are encountered.
Nonconforming or out-of-specification (OOS) samples are to be identified, segregated and
quarantined (whenever possible) to a designated hold area.
Nonconformance reports shall be analyzed for trends during the management review
meetings and a determination shall be made as to whether an investigation and/or additional
action(s) are required.

11.4 Informal Corrective Actions
Informal Corrective actions are comprised of activities defined in the procedures in response
to minor, nonsystematic non-conformances, which can be corrected in order to avoid data
impact but do not require the full process of formal corrective action.
The independent testing laboratory may choose to perform informal corrective action when a
nonconformance is identified but does not impact the client data or the effectiveness of the
laboratory quality management system in a significant manner provided that the departure
from procedure is random and does not consistently recur. These are to be defined in the
independent testing laboratory SOPs with simple corrective actions assigned and they shall
be tracked to identify any patterns or reoccurrence which would indicate they required
formal corrective action. Informal corrective actions are to be reviewed, approved, recorded,
and reviewed by appropriate personnel designated in the associated procedures.
Departures that can be handled with informal corrective action include but are not limited to
single QC failures, instrument performance that exceeds warning limits, a missed entry in a
support record such as a balance verification and other events that are due to human error
but upon investigation are found to not impact the sample or data integrity.
11.5 Performing Formal Corrective Action
Formal Corrective Actions are comprised of activities designed to address quality

management system failure. Formal corrective action shall be performed for the following
events:
 External audit findings (Client or regulatory);

 Internal audit findings;
 Management review findings;
 Recurring technical analysis departures such as calibration failures, qc failures,
decreased instrument performance, and missed components in primary or secondary
data review;
 Proficiency test failures;
 Client complaints pertaining to issues other than administrative or unavoidable
circumstances;
 Recurring sample rejection due to laboratory container shipment errors;
 Records that cause breaks in traceability;
 Data recalls or amended reports;
 Failure to maintain schedules effectively for document review, internal audits,
demonstrations of capability, or training.
11.5.1 Root Cause Analysis
The procedure for corrective action shall start with an investigation to determine the root
cause(s) of the problem. Root cause analysis is the key and sometimes the most
difficult part in the corrective action procedure. Staff that are designated and authorized
to investigate major nonconformances are to be provided documented root cause
analysis training. Investigation and root cause analysis records are to be kept including

data packages that identify the nonconformance so that corrective action effectiveness
can be monitored on an ongoing basis.
Often the root cause is not obvious and thus a careful analysis of all potential causes of
the problem is required. Potential causes could include customer requirement training,
consumables, or equipment and its calibration. It is recommended that root cause
analysis be performed by two methods or two individuals to examine several possible
causes. If the root cause is not clear, an individual not involved in the day-to-day
operation under study can be a valuable addition to the team.
11.5.2 Assignment of Corrective Actions
Corrective action is the action taken to eliminate the causes of an existing non-
conformity, defect, or other undesirable situation in order to prevent recurrence. The
independent testing laboratory is to select, document and implement corrective actions
in a timely manner. The corrective actions selected by the independent testing
laboratory are to be congruent with the result of the root cause analysis, the address the
problem and prevention of problem recurrence. The degree of corrective action is to be
appropriate to the magnitude and the risk of the problem. The independent testing
laboratory is to set a goal date for the completion of the corrective action and identify in
the records the individuals responsible for implementation and the components to be
tracked to ensure effectiveness.
11.5.3 Monitoring of Corrective Actions
The independent testing laboratory is to monitor the results to ensure that the corrective
actions taken have been effective. The independent testing laboratory is to assign an
appropriate goal date for the completion of the corrective actions upon implementation.
The independent testing laboratory is to record the follow-up activities and records of
effectiveness over an appropriate time period. Closed corrective actions are to be
included as a detailed component in the next internal audit. If the departure was severe
enough, the corrective action is not to be considered closed until an internal audit of the
affected parts of the system has been performed. (ISO/IEC 17025:2005 Section 4.11.5)
11.6 Internal Audits
Annually, the independent testing laboratory is to prepare a schedule of internal audits to be

performed during the year. These audits verify compliance with the requirements of the
MDPH protocols, and the requirements of the laboratory QMS, including analytical methods,
SOPs, the Quality Manual, ethics policies, data integrity, other laboratory policies, and the
ISO 17025 Standard. These audits are to be performed by trained and qualified personnel
who are, wherever resources permit, independent of the activity to be audited. While the
Quality Manager is responsible for scheduling of the Internal Audit, it is recommended that
Supervisors and Staff are included in this process in order to promote ownership and
engagement in the laboratory’s activities.
In addition to the scheduled internal audits, it may sometimes be necessary to conduct

special audits as a follow-up to corrective actions, PT results, complaints, regulatory audits
or alleged data integrity issues. These audits address specific issues.

The area audited, the audit findings, and corrective actions are to be recorded. Audit results
are to be reviewed after completion to assure that corrective actions were implemented and
effective. Records are to be kept pertaining to the scheduling of internal audits, the timely
completion of audit activities, the number of findings arising from audit activities, and the
timely resolution of the corrective actions implemented as a result of audit activities. These
metrics are to be included in the Management Review meeting(s).
While the ISO 17025 requirement is for the entire Internal Audit to be completed annually, it
is often scheduled in a staggered manner to avoid the bottleneck of such a large
undertaking. In addition, although the standard states that the auditor must be “independent
of the activity performed”, this does not preclude supervisors and backups auditing
analytical work that is performed by the primary analyst within the same department or by
the same methodology as the auditor performs. There are other schemes that should be
considered in order to engage all independent testing laboratory staff further in the internal
audit activities and resulting corrective actions. This assignment of audits can actually
encourage cooperation and consistency throughout the department or technology.
11.7 External Oversight
Laboratories performing analysis of medical marijuana products for regulatory reporting to

MDPH shall participate in the accreditation activities of the ISO accreditation body (AB),
including compliance to the requirements addressing client or RMD audits, and monitoring,
auditing, and on-going examination as required by MDPH. Laboratories are to make staff
and records available to the RMD, MDPH, and the ISO AB upon request for audits, desk
reviews, and investigation of complaints at all times. The laboratories are to be prepared for
these activities by maintaining a clear and organized records management system and
procedures to compile data in simplified formats.
The MDPH program may employ a variety of methods to assess the ongoing quality
produced by laboratories. These activities may be conducted to address events such as
complaints, product failures, or recalls, the potential for litigation, and rule changes or
implementations. They shall also address on-going efforts of MDPH such as gathering data
and information for education, reporting, research, or standardization with other state health
programs.
Deliverables that may be requested by MDPH may include independent testing laboratory
SOPs, full data packages, including all QC and raw data associated with samples, requests
for specific reports or electronic data deliverables (EDD) formats that compile data differently
than a standard client report. MDPH or its agents may conduct unannounced onsite
inspections. These activities may result in suggestions by MDPH of opportunities for
improvement and are encouraged to maintain open dialogues and participate in cooperative
efforts outside of the scope of the activities defined here.
11.7.1 Confidential Business Information (CBI) Considerations
During on-site audits, on-site auditors may come into possession of information claimed
as business confidential. A business confidentiality claim is defined as “a claim or
allegation that business information is entitled to confidential treatment for reasons of

business confidentiality or a request for a determination that such information is entitled

to such treatment.”
When information is claimed as business confidential, the independent testing laboratory

is to place on (or attach to) the information at the time it is submitted to the auditor, a
cover sheet, stamped or typed legend or other suitable form of notice, employing
language such as “trade secret”, “proprietary”, “business confidential” or “company
confidential”. Confidential portions of documents otherwise non-confidential shall be
clearly identified. CBI may be redacted or edited to eliminate references to client identity
by the responsible independent testing laboratory official at the time of removal from the
laboratory. However, sample identifiers or other components necessary to the nature of
the review, may not be obscured from the information. Alternate numbering systems
and crosswalks may be employed if sample identifiers jeopardize the client confidential
information.
11.7.2 Corrective Actions for Internal Audits and External Oversight
The independent testing laboratory is identify who is responsible for initiating corrective
action where a nonconformance is found that could reccur (beyond expected random
QC failures) or where there is doubt about the compliance of the independent testing
laboratory to its own policies and procedures. In addition, the independent testing
laboratory shall identify the personnel responsible for monitoring and recording the
corrective action
Internal or external audit findings are responded to within the time frame agreed to at the
time of the audit. The response may include action plans that could not be completed
within the response time frame. A completion date is established by independent testing
laboratory management for each action item and included in the response.
Audit findings that cast doubt on the effectiveness of the independent testing laboratory
operation to produce data of known and documented quality or that question the
correctness or validity of sample results shall be investigated. Corrective action
procedures above are to be followed. The RMD is to be notified in writing if the
investigation shows the independent testing laboratory results have been negatively
affected and the MDPH testing requirements have not been met. The RMD is to be
notified as soon as practical after the independent testing laboratory discovers the issue.
Independent testing laboratory management shall ensure that this notification is carried
out within the specified time frame.
11.8 Proficiency Test Samples
11.8.1 PT Sample Handling, Analysis and Reporting
Proficiency Testing (PT) samples are a pillar of ISO accreditation in that they are meant
to demonstrate the independent testing laboratory’s ability to report accredited analysis
data of unknown client samples within a defined accuracy window. They are samples
spiked with known concentration levels of target analytes prepared by a third-party
organization accredited to ISO 17043.

At a minimum, the independent testing laboratory is to complete the requirements of

their accrediting body, which includes one successful PT for each method and matrix
included in Massachusetts regulation, if available, prior to reporting samples for
compliance and one additional PT for each method and matrix combination annually.
Although a double-blind PT is not currently available, the independent testing laboratory

is to make every effort to treat the PT according to their procedures. Also, in order to
make an effective statement as to the independent testing laboratory’s capability of
accurately analyzing an unknown client sample, the independent testing laboratory shall
not treat the PT sample in any way that differs from the handling of a client sample. This
is demonstrated by the records relating to the PT sample from sample receipt through to
reporting.
This includes the following instructions but can also include any handling of the PT that
would give the independent testing laboratory additional assurance of the result that
would not be available for client samples.
To demonstrate independent testing laboratory proficiency, PT samples are to be treated

as and analyzed with typical samples in the normal production process where possible,
including the same sample log-in procedures analysts, maintenance triggers,
preparation, calibration, QC and acceptance criteria, sequence of analytical steps,
number of replicates, data analysis, manual integrations, identification, and confirmation
procedures. PT samples are not analyzed multiple times unless routine samples are
analyzed multiple times. When PT samples present data analysis challenges such as
high concentrations or coelutions, those challenges are to be addressed as they would
with a client sample.
The type, composition, concentration, and frequency of QC samples analyzed with the
PT samples are the same as with typical samples.
Whenever possible, the PT sample is to be prepared and analyzed with other samples to
avoid having a QC set unique to the PT. The PT cannot be chosen for spiking or
duplication within a batch consistently, but if there are no other samples in-house for the
analysis, the required QC for a batch is to be performed.
Prior to the closing date of a study, independent testing laboratory personnel are not to:
 Subcontract analysis of a PT sample to another laboratory that is to be reported for

accreditation purposes.
 Knowingly receive and analyze a PT for another laboratory that is to be reported.
 Communicate with an individual from another laboratory concerning the analysis of
the PT sample.
 Attempt to find out the assigned value of a PT from the PT Provider.
 Perform maintenance or calibration on an instrument when the data quality
samples or instrument performance data would not normally necessitate such
actions.
 Provide additional verification, validation, or review.
 Analyze the sample in multiple batches, on multiple instruments, or by multiple
analysts.

11.9 Management Review
Independent testing laboratory management is to review the laboratory quality management

system (QMS) and technical operations annually, and may perform these reviews on a more
frequent basis at the discretion of the laboratory management.
All employees are to be trained in entering potential causes of nonconformance and these
are to be discussed at regular intervals and summarized at management review meetings.
The effectiveness of the participation and documentation of nonconformances shall be
evaluated along with the effectiveness of the corrective actions that were implemented.
Management review is intended as a resource for help in other areas of the quality
management system but is not a substitute for performing internal audits.
It is recommended that the independent testing laboratory management meet more
frequently and review sections of the quality management system and technical operations
on a rotating basis to cover all sections within a year. A process by which more frequent
section review with respect to the quality management system can be achieved with
success and acceptance from independent testing laboratory operations should involve the
QAM and independent testing laboratory director/manager scheduling and performing
department specific quarterly meetings. It is beneficial that these meetings discuss the
successes of completing corrective actions, encouraging the continual feedback from staff
regarding department operations and throughput, successful response to any audit findings
and client complaints, and any ideas to improving overall processes and procedures.
11.9.1 Management Review Topics
The following are to be reviewed to ensure their suitability and effectiveness:
 The suitability of policies and procedures;

 Reports from managerial and supervisory personnel;
 The outcome of recent internal audits;
 Prior, ongoing and aging corrective and preventive actions;
 Effectiveness of previous corrective and preventive actions taken;
 Changes in external and internal conditions relevant to the quality management
system;
 Assessments by external bodies;
 The results of interlaboratory comparisons or proficiency tests;
 Changes in the volume and type of the work;
 Customer feedback;
 Complaints;
 Recommendations for improvement; and
 Other relevant factors, such as QC activities, resources, and staff training.
Findings from management reviews and the actions that arise are to be recorded.
Independent testing laboratory management is to verify that the actions are discharged
within an appropriate and agreed upon timeline. If needed, a corrective or preventive
action shall be initiated for identified action items examined during the management
review. The laboratory is to follow their corrective or preventative action items until they

are declared closed and informal (i.e., the results of the investigation are implemented
and follow-up has been completed).
11.10 Data Review, Verification, Validation and Reconciliation with DQOs
The independent testing laboratory shall have procedures that include two levels of full data
review of every component of the analysis. The primary review is typically performed by the
analyst and the secondary review by someone trained in the independent testing laboratory
quality management system and, if possible, with a demonstration of capability (DOC) in the
analysis. If the independent testing laboratory staff is limited, the second level of review is
to be performed by someone who has demonstrated technical knowledge of the analysis
according to the independent testing laboratory training procedures.
The independent testing laboratory training standard operating procedure, (and/or the data
review procedure should such exist), should state qualification procedures needed for
adequate secondary review of data from a primary analyst. Basic training requirements as
documentation of a read/understood of the SOP, a knowledge of the instrumentation used to
produce the result, and established competency in the quality assessment of data are
minimum requirements an independent testing laboratory establishes in order to obtain the
required integrity of the result reported.
The following elements are required when reviewing data in addition to any elements
contained in the reference methods, laboratory SOPs, and relevant state and federal
regulation:
 Technical data review records are to contain associated preparation and batch IDs
and references to controlled versions of the SOPs used in preparing and analyzing
the samples.
 Chemistry analyses review is to include a review of all required data elements such
as sample prep conditions, chromatograms, identification of peaks, manual
integrations, calibration criteria, QC samples, sample preservation and hold times,
reporting ranges, and data upload or transcription.
 Microbiology analysis review is to include a review of the method requirements such

as incubator temperature ranges and minimum times of incubation, and acceptability
of the criteria contained in the DQO tables.
 Review of microbiological data shall also include the times of analysis, the
temperatures of the support equipment and a periodic review of the physical count
(as marked on a plate or re-counted from a saved plate) against the written record.
 For microbiological data, regardless of schedule, all QC checks such as air checks,
media checks, dilution water checks, equipment-cleaning checks and any other
checks pertinent to the analysis are to be traceable to results and are to be treated
as bracketing checks if a failure occurs.
For all analyses, periodic review of support equipment calibration and verification records,
standard and reagent preparation records, and sample receipt records are to be performed.

This review is to be performed on a frequency defined by independent testing laboratory

management, based on the amount of data the independent testing laboratory is prepared
to recall and reissue and the amount of clients they are willing to notify based on the
timeframe.
It is recommended that the reviews happen frequently enough to notify clients of any
possible error before it is too late to re-sample and re-analyze the batch before it is sold by
the client.
The independent testing laboratory is to have procedures for a full review by the quality
assurance manager (or designee) of a minimum of 10% of client sample events from sample
receipt to sample reporting.
The independent testing laboratory is to have procedures that outline verification of data in
cases where the analytical result may be in doubt due to historical inconsistency, possible
contamination, or carryover, and other possible causes of inaccuracy as identified by the
professional judgement of competent personnel and procedural triggers based on the
evaluation of quality control sample results and other DQIs.
 Carryover procedures are to be developed and are to identify steps in the analysis that
contain risk of carryover of target analytes to the subsequent samples and provide
detail on verification that sample detections are not caused by contamination from other
sources during primary and secondary data review. They are to include the reanalysis
of samples following a sample of unknown matrix that have significant detections at
levels determined by the independent testing laboratory based on observed carryover
per analyte in the method development stages. If a sample has detections above this
concentration, the independent testing laboratory shall re-analyze any samples
following any samples with significant detections in the same target analytes. If the
independent testing laboratory places instrument blanks before or after QC samples,
the carryover procedures shall match the concentration of those samples. These
evaluations shall be documented. Samples associated with visual detections in blanks
or rinses, even if values are below the LOQ are to be considered for reanalysis if the
same target analytes are detected.
In the event that the instrument can be programmed to add additional rinse times when a
certain concentration is reached, the method shall apply to both QC and samples and the
samples are to be evaluated as above for carryover if the rinse is extended
 Verification of sample results that fall close to the action limits shall be performed. A
sample is considered close to the action limit if the result exceeds the precision
criteria for the method.
 If sample verification is performed and the results do not agree with the initial
analysis and there is not an assignable cause, such as a misinjection, the sample
shall be evaluated a third time. A favorable sample result, whether from an initial run
or a verification run cannot be arbitrarily chosen and verification shall include at a
minimum, a third confirmation analysis.

 Data verification is performed by assessing the combined data quality indicators

such as results of the data review and the review of support documentation as well
as an understanding of expected data results such as the expected cannabinoid
amounts in known matrices. Data validation is performed on an ongoing basis by the
independent testing laboratory staff as defined in these procedures to ensure that the
reported result meets the criteria of the independent testing laboratory and is of
known and appropriate quality according to the independent testing laboratory’s
quality management system and the relevant standards and regulations.
11.11 Treatment of Out-of-Specification (OOS) results
The independent testing laboratory is to implement an approved procedure for investigating

OOS test results, including RMD samples that fail to meet current MDPH Protocol limits for
regulated contaminants and QC sample failures.
The procedure(s) are to detail the circumstances, criteria, and documentation required to
conduct and complete an investigation of OOS results. The independent testing laboratory
is to provide documented training to the procedures. Include in the procedure the
assessment of independent testing laboratory practices associated with the OOS result and
include details for retesting samples. The specifications for whether to retest are to be
based on the objectives of the testing and clearly defined decision rules.
The independent testing laboratory is to specify the maximum number of retests to be

performed on a sample in advance in the written SOP. The number may vary depending
upon the variability of the particular test method employed, but shall be based on
scientifically sound principles. In the predetermined retesting procedure, the independent
testing laboratory is to determine a point at which the additional testing ends and the batch
of product are statistically evaluated. In addition, the independent testing laboratory is to
develop a corrective action procedure for the review of unsatisfactory data.
The independent testing laboratory is to establish criteria with instructions for reporting of
results in this procedure. In the case of a clearly identified laboratory error, the retest results
would substitute for the original test result. The independent testing laboratory is to retain all
original data and record an explanation of the error. The records shall include the initials of
all personnel involved in the review or the investigation, date, a discussion of the error and
supervisory comments. If no laboratory or calculation errors are identified in the first
analysis, there is no scientific basis for invalidating initial OOS results in favor of passing
retest results. All test results, both passing and suspect, are to be reported and the report
shall contain all of the information necessary for the client or regulatory authority to interpret
the result and understand the related factors of uncertainty.
12.0 REPORTING OF RESULTS
12.1 Significant Figures
Unless directed otherwise in writing by MDPH or its designated consultant, or unless

conflicting state or regulatory agency requirements exist, analytical results for chemical
analyses are to be reported as if three digits were significant. For analyses with regulatory
action limits, the independent testing laboratory shall report in the state tracking system with

the amount of significant figures in the action limit with one additional significant figures, if
achievable based by the method. For plate counts, round results to two significant figures.
Application of significant figures is not to result in decimal places added to any value as it
approaches a method LOQ/reporting limit (RL). In the event that a discrepancy exists
between the guidelines provided above and project-specific requirements, the RMD and/or
MDPH are to be contacted for resolution.
12.2 Reporting Results Obtained from Subcontractors
When the test report contains results of tests performed by subcontractors, these results are
to be clearly identified. The subcontractor is to report the results in compliance with the
requirements of RMD, ISO 17025 and relevant state and federal regulation. The
independent testing laboratory is responsible for the results of the subcontractor, and is to
have procedures detailing the review of the subcontractor results for conformance and
known data quality.
The independent testing laboratory may reproduce these reports in full within the laboratory
official report. This is recommended as it is easy to identify the subcontracted laboratory,
the subcontracted results. In addition, the primary laboratory takes responsibility for the
subcontracted laboratory results as it pertains to data review and reports. If the report is
reproduced in full, this mitigates the risk of transcription errors, LOQ differences, and
missing narratives.
12.3 Reporting Not-Detected and Low-Level Results
Generally, results that are not detected above the LOQ are to be reported as “<” followed by
the numerical value of the sample-specific LOQ. The sample specific LOQ value is the
default LOQ value determined in accordance with this QAPP, adjusted for any variations in
sample size analyzed and final volume of the extract or digestate (i.e., dilution factor).
Results below the LOQ may only be reported if authorized in writing by MDPH. Results
below the LOD are never to be reported. For guidance on the determination of LOD and
LOQ, refer to Sections 9.2.2 and 9.2.3 of this document.
12.4 Amendments to Reports
Material amendments to a report after issue shall be made only in the form of a further
document, or data transfer, which includes the statement:
“Supplement to Test Report number...[or as otherwise identified]”, or an equivalent form of

wording. Such amendments are to meet all the requirements of ISO 17025:2005E. When it
is necessary to issue a complete new report, the report is to be uniquely identified and is to
contain a reference to the original report that it replaces.
12.5 MDPH-specific Reporting Requirements
The results of each test, or series of tests carried out by all laboratories performing analyses
for the MDPH Medical Marijuana Program are to be reported accurately, clearly,
unambiguously and objectively, and in accordance with any specific instructions in the
MDPH Protocol for Sampling and Analysis of Finished Medical Marijuana Products and

Marijuana-Infused Products for Massachusetts Registered Medical Marijuana Dispensaries

(Section 8.0), Protocol for Sampling and Analysis of Environmental Media for Massachusetts
Registered Medical Marijuana Dispensaries, as well as ISO/IEC 17025:2005(E), Section
5.10.
Specific operational requirements from the MDPH Protocols and ISO 17025 standard with
regard to results reporting are combined and summarized below.
The accurate reporting of results is an important aspect of gathering information in a way

that is consistent and appropriate for the assessment of the quality of medical marijuana
products. The MDPH may require data to be reported in certain formats that are not
specified in this QAPP, with specific compounds and quantitation or limits of detection for
reporting. Without written permission provided by the MDPH, data are not to be reported as
a quantitative estimate below the method LOQs.
Data may only be reported as quantitative estimates or with data qualifiers if a QC sample
failure occurs during reanalysis after the corrective actions described in Appendix A, Tables
03-09 have been implemented and documented. Only the following QC sample failures
may result in the reporting of qualified data:
 Contamination observed in the method blank at concentration levels that exceed the
criteria listed in Appendix A, Tables 03-08 for chemical analyses.
 The recovery of target analytes in the LCS/LCSD or MS/MSD fail to meet the criteria
established in Appendix A, Tables 03-08 for chemical analyses.
 The recovery of surrogate and/or internal standard compounds fails to meet the
criteria established in Appendix A, Tables 03-08 for chemical analyses.
 Water bath and/or incubator temperature exceeds temperature window during
microbial analysis and insufficient sample exists to repeat analysis.
 Ambient air checks fail to meet acceptance criteria for microbial analyses as
prescribed on Table 09, Appendix A.
 QC sample (e.g. laboratory duplicates, negative controls, positive controls, etc.)
failures during microbial analyses as prescribed on
 Table 09, Appendix A, but insufficient sample is available to repeat analysis.
Data are not to be reported with instrument calibration and/or continuing calibration failures.
The corrective actions described in Appendix A, Tables 03-09 shall be followed if the
instrument calibration or continuing calibration check fails. Data are not to be reported with
sample receipt, holding time or other documented sampling issues that may affect sample
integrity as described in Appendix A, Table 02.
When reporting qualified results, the qualifier (e.g., J, *, etc.) shall be presented immediately
adjacent to the reported result and/or as a footnote reference and an explanation of the
qualifier shall be included within the client report. If a QC sample fails then the corrective
actions presented in the DQO tables presented in Appendix A are to be followed.
12.5.1 Report Template
Each independent testing laboratory is to enter results into the MDPH standardized
results report template presented in Appendix C. This reporting template is intended to

eliminate reporting differences between laboratories, while capturing comprehensive and

complete laboratory records across all laboratories within the MDPH Medical Marijuana
testing program. The template offers a common ISO/IEC 17025 compliant reporting
format that shall be used to unify and standardize the information and tools being
provided to patients and providers of healthcare.
The template contains two major sections: (1) a cover page, which contains information
about the sample being tested and the lab authorization of the reported results, and (2)
the analytical results of the sample testing. Many fields in the template display notes
when selected that provide instruction for data entry. Some fields are restricted to a list
of options; this is portrayed in the template using drop-down lists. Fields with data
restrictions and fields that apply to particular types of samples are noted within the data
dictionary. As the template is refined, some fields may be optional or even removed if
deemed non-essential. The report template includes the following sections to document
the information described below:
COVER PAGE
The cover page contains fields that are included within several different “boxes” or sections.
Box A: Report Heading
Box A contains basic descriptive information about the independent testing laboratory report.
A1. Lab Name: Name of the independent testing laboratory issuing the report.
A2. Lab Address: Address and other contact information of the independent testing laboratory.
A3. Lab Sample ID: Sample identification number assigned by the independent testing
laboratory. Each lab report should contain information about one sample, and the sample ID
number should be unique from all other reports from that laboratory (except for revised versions
of previously submitted reports).
A4. Report Title: Title of the report.
A5. Revision number (if necessary): To be included if report is a revision of previously submitted
report.
A6. Report Date: Date on which the laboratory report is finalized and submitted/published
(mm/dd/yy).
BOX B: RMD Info
Box B includes information about the client transaction.
B1. RMD Name (List - unrestricted): Name of the Registered Marijuana Dispensary (RMD) that
submitted the sample, using a 2-5 letter code associated with that RMD.
B2. RMD Address: Address and other contact information of the RMD, specifically the
cultivation/production location from which the sample was collected and shipped.

B3. Manifest/COC Number: Identifier of the Manifest or Chain-of-Custody form used when
sample was relinquished to the independent testing laboratory.
B4. Date Received: Date the sample was delivered to the independent testing laboratory.
BOX C. Sample Identification
Box C contains the various RMD identifiers relevant to the sample. Identifiers are assigned by
the RMD following the guidelines in Section 5.0 of Protocol for Sampling and Analysis of
Finished Medical Marijuana Products and Marijuana-Infused Products for Massachusetts
Registered Medical Marijuana Dispensaries (henceforth referred to as “MDPH Protocols”).
C1. RMD Sample ID: Sample identifier assigned by the RMD. An RMD sample ID is unique to
each sampling event. An RMD Sample ID may be associated with one or more laboratory
reports, as the sample could be split after collection and sent to multiple labs for testing, or
could be re-tested. Multiple RMD sample IDs may be associated with one Batch ID if the
production batch was sampled on multiple distinct occasions.
C2. Batch ID: Unique alphanumeric ID of the production batch from which the sample was
collected. Production batch is defined in Section 5.0 of the MDPH Protocols as:
“Production Batch means a batch of finished plant material, cannabis resin, cannabis
concentrate, or MIP made at the same time, using the same methods, equipment, and
ingredients. The RMD shall assign and record a unique, sequential alphanumeric identifier to
each production batch for the purpose of production tracking, product labeling, and product
recalls. All production batches shall be traceable to one or more marijuana cultivation
batch(es).”
C3. Parent Batch ID: The production or cultivation batch ID(s) of the parent product used in the
production of the sample. For resin and concentrate samples, the parent batch ID shall be the
batch ID(s) of the flower/plant material used to produce the resin or concentrate. For MIP
samples, the parent batch ID shall be the batch ID(s) of the concentrate/oil used to produce the
MIP. For flower samples, the parent batch ID shall be the ID of the cultivation batch(es) that
produced the finished plant material.
BOX D: Picture of Sample
D. Sample Picture: Picture of delivered sample prior to laboratory analyses.
BOX E: Sample Properties
Box E describes physical properties of the delivered sample.
E1. Sample Size: Weight or volume of the sample upon receipt. Must be reported in weight or
volume units, such as grams or milliliters; “number of units” is not permitted for this field (see
E2).
E2. Number of servings/units: The number of “servings” or units present in the submitted
sample. This field is required for marijuana-infused-product samples only.

E3. Matrix (list): Sample matrix. The field is limited to a list of the matrix categories described in
Section 5.3 of the MDPH Protocols (Liquid; Plant Material or Friable Solid; Solid or Semi-Solid)
and an option for “other,” which should be specified in adjoining cell.
E4. Sample Condition: The condition of the sample upon receipt. This includes any notable
observations (e.g., presence of moisture).
E5. Re-test: Indicate if the laboratory report represents a re-test of an RMD sample (i.e., Yes or
No).
E6. Remediated Sample: Indicate if the RMD sample comes from a remediated batch (i.e., Yes
or No). If “Yes” is selected, a description of the batch remediation should be provided.
BOX F: Product Characterization
Box F includes several fields used for characterizing the tested product.
F1. Production Stage (list - restricted): Stage of medical marijuana production from which
sample was collected and includes: (1) Plant Material; (2) Cannabis Resins and Concentrates;
and (3) Marijuana-Infused Product (MIP). All products must be placed into one of the three
categories because the production stage determines the contaminant tests required for the
sample (see Exhibit 8b of the MDPH Protocols).
F2. Product Class (list): Second tier of product categorization. Each production stage
classification (F1) is divided into one or more product class categories, as displayed on Table 7
below.
Table 7 Production Stage Classification for Medical Marijuana Products

Production Stage Product Class
Finished Plant Material Flower
Cannabis Resin & Concentrates Oil
Resin
Shatter
Wax
Marijuana-Infused Product (MIP) Edible (Food, Drink, Capsule)
Suppository
Tincture
Topical
Other
F3. Product Type: Description of the product type. Examples of a product type description
include: plant material (e.g., flower); cannabis resin and concentrates (e.g., kief, bubble hash,
rosin, wax, shatter, vape oil, RSO, etc.); MIPs (edibles) (e.g., beverage, capsule, brownie, bar,
cookie, gummy, lozenge, nugget, etc.); and MIPs (non-edibles) (e.g., tincture, spray, lotion,
patch, suppository, etc.).
F4. Retail Name: Retail name of the finished product. The retail name is included primarily to
provide supplemental descriptive information, and to help understand how products are being
presented to patients. Some product sample may not be intended for sale (e.g., oil intended to
be used in the production of a MIP) and therefore this field may be left blank. Include in the

specify field the species of flower (e.g., C. sativa, C. indica, hybrid), as well as the cultivar or
strain name (e.g., Bruce Banner).
F5. Grow Material: For flower samples only; the type of grow material used during the cultivation
of the marijuana plant from which the finished plant material was harvested from.
F6. Intended Route of Consumption: The consumption method intended for the product, as
determined by the RMD. This field lists options “all uses” and “ingestion only,” as well as
options for inhalation and various absorption pathways (i.e., dermal, sublingual, rectal), and
includes an “other” option with an opportunity to specify additional consumption routes.
F7. Extraction Solvent: The type of solvent used for cannabinoid extraction in the production of
the sample. Solvent types commonly used for cannabinoid extraction include: Hydrocarbons,
which includes n-Butane, iso-butane, and Propane; CO2 (supercritical fluid); alcohols, which
includes ethanol; and lipids, which includes butter and vegetable oils.
BOX G. Test Types Run
This field includes a checkbox indicating which tests were performed on the sample. Each
option in the check box corresponds to an individual subsection in the analytical results section
of the template. The test types included in the checkbox represent all required tests for product
samples, as outlined in Section 7.0 of Protocol for Sampling and Analysis of Finished Medical
Marijuana Products and Marijuana-Infused Products for Massachusetts Registered Medical
Marijuana Dispensaries, with an additional option to describe Terpene Profile.
BOX H: Authorization
Box H provides the independent testing laboratory’s interpretations of the laboratory results and
authorization of the report.
H1. Case Narrative, Laboratory Notes, and Statement: Write-up of case narrative including data
interpretations. Any accreditations of certifications the laboratory wishes to report, any
additional notes from the laboratory on the sample analysis, and any statements (i.e., “results
relate only to the samples tested,” “report may not be reproduced except in its entirety,” etc.) are
to be included in this field.
H2. Product Approval: Check box indicating interpretation of the results. Enter an "X" in a box
to denote whether the product may be dispensed for all uses, may be dispensed as an ingestion
only product, or may not be dispensed, based on the interpretation of the laboratory analyses as
compared to the MDPH standard limits.
H3. Authorization signature: Signature from the independent testing laboratory authorizing the
report and certifying the results.
ANALYTICAL RESULTS
The analytical results section is split into subsections representing each possible type of test
that may be reported by the independent testing laboratory. Tests that are not run may be left
blank. Each section includes the following general information in addition to the analytical
results-specific sections:

Lab Sample ID: Sample identification number assigned by the independent testing laboratory.
Each laboratory report should contain information about one sample, and the sample ID number
should be unique from all other reports from that laboratory (except for revised versions of
previously submitted reports); also reported in A3.
Analysis Date: Date(s) when the analysis was performed.
Analytical Method: The analytical method used (e.g., GC-MS/MS, GC-FID, HPLC-MS/MS,
HPLC-UV-Vis, ELISA, MPN with cultured enrichments, etc.).
Lab SOP #: Laboratory-specific standard operating procedure (SOP) used for sample
preparation and all analyses (i.e., cannabinoid profile, heavy metals, microbiological
contaminants, pathogenic bacteria, mycotoxins, residual solvents, pesticides, and terpene
profile).
Analyst: Initials of the independent testing laboratory analyst who performed the analysis.
Narrative: Written narrative summary of the analysis, including relevant instrumentation and
standard methods.
Test ID: Unique identifier given to each specific test run (i.e., cannabinoid profile, heavy metals,
microbiological contaminants, pathogenic bacteria, mycotoxins, residual solvents, pesticides,
terpene profile).
TABLE I. CANNABINOID PROFILE
Analyte: MDPH requires that products are tested for, at minimum, Δ9-THC, THCa, CBD, and
CBDa. The cannabinoid profile table includes several rows without a defined analyte for the
independent testing laboratory to enter additional cannabinoids that are tested beyond those
that are required.
Result (Concentration): The measured concentration for each cannabinoid. Percentage dry
weight (%wt) is the preferred unit of measurement, though any mass(cannabinoid)-to-
mass(sample) can be used.
Result (“Dose” weight): Optional field – may be used for MIP samples. The calculated amount
of cannabinoid in a single serving of a MIP. Requested units are mg/serving.
LOD: Limit of Detection.
LOQ: Limit of Quantitation.
TABLE J. HEAVY METALS ANALYSIS
Analyte: MDPH requires that heavy metal testing of MMJ product samples includes testing of
Arsenic (inorganic) (As), Cadmium (Cd), Lead (Pb), and total Mercury (Hg).
Result (Concentration): The measured concentration for each analyte. Results are to be
reported in parts-per-billion (ppb) units (or the equivalent μg/kg).

Limits (All Uses): The MDPH standard limit of each analyte for products intended for all uses.
Limit Test (All Uses): Pass/Fail field for the “all uses” standard limits.
Limits (Ingestion Only): The MDPH standard limit of each analyte for products intended for
ingestion only.
Limit Test (Ingestion Only): Pass/Fail field for the ingestion only standard limits.
TABLE K. MICROBIOLOGICAL CONTAMINANTS TEST
Analyte Symbol: Symbol for analyte test as described below on Table 8.
Test Analysis: Name of the analyte test as described below on Table 8.
Table 8 Microbiological Contaminant Analysis Symbol

Analyte Symbol Test Analysis
AC Total Viable Aerobic Bacteria
YM Total Yeast & Mold
CC Total Coliforms
EB Total Bile-Tolerant Gram Negative Bacteria
Result: Reported result of the microbial test analysis.
Unit: Unit of measurement associated with the reported result.
Standard Limits: The MDPH standard limit of each analyte. The standard limits differ based on
product characteristics (see Exhibit 6 of the MDPH Protocols), and shall have to be selected
and entered into the table by the independent testing laboratory.
Limit Test: Sample pass/fail for the analyte standard limit test.
TABLE L. PATHOGENIC BACTERIA SCREEN
Analyte Symbol: Symbol for analyte test as described below on Table 9.
Test Analysis: Name of the analyte test as described above on Table 9.

Table 9 Pathogenic Bacteria Contaminant Analysis Symbol

Analyte Symbol Test Analysis
ECPT E. coli (O157)
SPT Salmonella
Result: Reported result of the pathogen screen. As these analyses are usually indicator tests,
result shall be “positive” or “negative,” rather than a quantitative result.
Unit: Unit of measurement associated with the reported result.
Standard Limits: The MDPH standard limit of each analyte.
TABLE M. MYCOTOXIN TEST
Analyte Symbol: Symbol for analyte test.
Test Analysis: Name of the analyte test.
Result (Concentration): The measured concentration for each analyte. A cell in the table
heading can be used to report the unit of measurement of the reported results. Parts-per-billion
(ppb) units are preferred.
Standard Limits: The MDPH standard limit for total mycotoxins.
TABLE N. RESIDUAL SOLVENTS TEST
Analyte: Analyte tested
heading can be used to report the unit of measurement of the reported results. Parts-per-million
(ppm) units are preferred. When hydrocarbon analysis are reported, a “Total Hydrocarbons” row
should be included which sums the results of n-butane, iso-butane, and propane. The total
hydrocarbons value is to be evaluated against the 12 ppm standard limit.
Standard Limits: The MDPH standard limit for residual solvent parameters.

TABLE O. PESTICIDE SCREEN
Analyte: Analyte tested
heading can be used to report the unit of measurement of the reported results. Parts-per-billion
(ppb) units are preferred.
Standard Limits: The MDPH standard limit for pesticides
Method QA/QC Test: Due to ongoing method development and validation for pesticides testing
at the analytical laboratories, analytical tests have occasionally failed laboratory QA/QC tests for
particular pesticides. Including this field in the results table shall enable the reviewer to make a
quick determination on the reliability of the reported result.
TABLE P. TERPENE PROFILE
Analyte: Analyte tested.
CAS Number: CAS Number of the analyte being tested.
Result (Concentration): The measured concentration for each analyte. Percent weight (wt%)
units are preferred.

13.0 REFERENCES
ASTM D6299-17. 2017. “Standard Practice for Applying Statistical Quality Assurance
Techniques to Evaluate Analytical Measurement System Performance.” American Society for
Testing and Material International.
ASTM E882. 2016. “Standard Guide for Accountability and Quality Control in the Chemical
Analysis Laboratory.” American Society for Testing and Material International.
ICH. 2005. “Validation of Analytical Procedures: Text and Methodology, Q2 (R1).” ICH
Harmonised Tripartite Guideline of The International Conference for Harmonization of Technical
Requirements for Registration of Pharmaceuticals for Human Use, November, 2015.
ISO/IEC 17025. 2005. General Requirements for the Competence of Testing and Calibration
Laboratories. International Organization for Standardization/International Electrotechnical
Commission.
ISO/IEC 12119. 1994. Information Technology – Software Packages – Quality Requirements

and Testing. International Organization for Standardization/International Electrotechnical
Commission.
ISO/IEC 12207. 1995 “Information Technology – Software Lifecycle Processes.” International

Organization for Standardization and the International Electrotechnical Commission.
MDPH 2016. “Protocol for Sampling and Analysis of Finished Medical Marijuana Products and
Marijuana-Infused Products for Massachusetts Registered Medical Marijuana Dispensaries.” The
Commonwealth of Massachusetts Executive Office of Health and Human Services Department of
Public Health Bureau of Health Care Safety and Quality Medical Use of Marijuana Program,
Massachusetts Department of Public Health, February 5, 2016.
MDPH. 2015. “Protocol for Sampling and Analysis of Environmental Media for Massachusetts
Registered Medical Marijuana Dispensaries.” The Commonwealth of Massachusetts Executive
Office of Health and Human Services Department of Public Health Bureau of Health Care Safety
and Quality Medical Use of Marijuana Program, Massachusetts Department of Public Health, May
7, 2015.
Montgomery, Douglas C. 2005. Introduction to Statistical Quality Control (5 ed.), Hoboken, New
Jersey: John Wiley & Sons, ISBN 9780471656319, OCLC 56729567
National Environmental Laboratory Accreditation Conference. 2009 and 2016. Quality Systems
General Requirements.
United States Pharmacopeia. 2015. General Chapter <61> Microbial Enumeration Tests.
United States Pharmacopeia. 2015. General Chapter <561> Articles of Botanical Origin.
United States Pharmacopeia. 2015. General Chapter <621> Chromatography.
United States Pharmacopeia. 2015. General Chapter <736> Mass Spectrometry

United States Pharmacopeia. 2015. General Chapter <1225> Validation of Compendial

Procedures.
US FDA and OFVM. 2015. “Guidelines for the Validation of Analytical Methods for the Detection
of Microbial Pathogens in Foods and Feeds, 2nd Edition. US Food and Drug Administration,
Office of Foods and Veterinary Medicine. April, 2015. Available at:
http://www.fda.gov/ScienceResearch/FieldScience/ucm273423.htm
Western Electric Company. 1956. Statistical Quality Control handbook (1 ed.), Indianapolis,
Indiana: Western Electric Co., p. v, OCLC 33858387.
US EPA 2185. 1995. “Good Automated Laboratory Practices Principles And Guidance To
Regulations For Ensuring Data Integrity In Automated Laboratory Operations With
Implementation Guidance 1995 Edition,” U.S. Environmental Protection Agency, August 10,
1995.
US FDA. 2011. “General Principals of Software Validation; Final Guidance for Industry and FDA
Staff.” U.S. Food and Drug Administration, January 11, 2002
21 CFR 211. 2016. Subpart I -- Laboratory Controls. Title 21 – Food and Drugs. Chapter 1 –
Food and Drug Administration, Department of Health and Human Services, Subchapter C –
Drugs: General. Part 211 Current Good Manufacturing Practices (cGMP) for Finished
Pharmaceuticals, Code of Federal Regulations, April 1, 2016.
40 CFR, Part 136. 2016. Guidelines Establishing Test Procedures for the Analysis of Pollutants.
Edition July, 1, 2016.

Appendix A
Data Quality Objective (DQO) Tables
Version 5.0 May 15, 2018 Page A-1

Quality Assurance Program Plan for Analytical Testing Laboratories Performing Analyses of Finished Medical Marijuana Products and Marijuana-
Infused Products in Massachusetts
Appendix A - Table 01
Method Reference Table
Analysis Technology Primary Reference(s) Ancillary Reference(s) Comment
Residual Solvents GC/MS  USP <467>  EPA 8260C* *Consulted for additional
Residual Solvents GC-MS and Headspace
 USP <621> specific objectives and
Chromatography details on quantitation
 USP <736> Mass
Spectrometry
Residual Solvents GC/FID  USP <467>  EPA 8000D* *Consulted for additional
Residual  EPA 8015D chromatography
Solvents confirmation
 USP <621> requirements
Chromatography
 USP <736> Mass
Spectrometry
Pesticides LC/MS/MS  AHP (2013) *The AHP does not

 EPA 1694* discuss methodology for
the most current limits of
pesticides set by MDPH.
EPA 1694 was consulted
for LC/MS/MS specific
objectives of
contaminants
Metals ICP/MS  USP <233>  EPA 6020A* *Consulted for additional

 USP <232> ICP-MS specific
 USP <2232> objectives
Cannabinoids HPLC (UV-Vis or DAD)  AHP (2013)  EPA 548.1* *Consulted for additional
 UNODC (2009) HPLC specific objectives

Method Reference Table
Analysis Technology Primary Reference(s) Ancillary Reference(s) Comment
% Moisture Gravimetric  USP <921>
 ASTM Method
D2216 – 98
Microbiology Plates and Films  AHP (2013) 1. BAM

1. Viable Aerobic  FDA Bacteriological Chapter 3
Bacteria Analytical Manual Aerobic Plate Count
2. Total Yeast and (BAM) 2. BAM Chapter 18,
Mold  USP <62> 3. BAM Chapter 4
3. Total Coliforms 4. USP <62>
4. Bile-tolerant
Gram-negative
Bacteria
Microbiology PCR, ELISA  AHP (2013) 1. BAM Chapter 4a

1. Pathogenic E.coli  USP <561> 2. BAM Chapter 5
2. Salmonella  FDA BAM 3. BAM Chapter 18
3. Mycotoxins
Sample Handling and Sample Collection  USP <561>

Storage  EPA 8000D
 FDA BAM

MDPH Sample Handling and Receipt Requirements
Quality Control Requirements
Item Requirement Acceptance Condition Corrective Action

Sample Sample vessels/media shall be appropriate for Sample containers that are one-use only shall be Samples associated with a contaminated
Containers the type analytical parameters for which the lot tested to show the level of target analytes are blank may not be re-prepared and re-
bottle type is to be used for collection. < ½ LOQ. analyzed. Samples shall be resampled and
reanalyzed. The contamination (including a
Pesticides, solvents, and cannabinoids analyses There shall be an SOP outlining the validation of list of affected samples) shall be
require amber glass containers with PTFE-lined bottle lots and the cleaning of any sample documented and formal corrective action
lids and metals analyses may come from the containers that are used more than once. shall be performed.
amber glass containers if only the target
analytes are being analyzed. This SOP shall contain a validation of the Trip blanks, field blanks, rinse blanks, and
cleaning procedure that includes an equipment equipment blanks shall not be reanalyzed
If other metals besides those required in the blank analyzed at least monthly for the target solely for the purpose of reporting “not-
protocols are analyzed or metals speciation is to analytes to validate the on-going acceptability of detected” results. Blanks may only be
be performed, a representative sample shall be the cleaning procedure. Results from these reanalyzed if there is a valid technical
contained in high density polyethylene samples shall be < ½ LOQ for each relevant reason for reanalysis (e.g., injection failure
containers. target analyte. or QC failure)
Sample vessel/media and preservative lot Records of frequency of sample container If the validation of cleaning procedure
numbers shall be recorded for each outgoing cleaning shall be maintained and available for analysis has hits > ½ LOQ, the samples
bottleware shipment to maintain traceability. inspection. bracketed by the failed study that were
placed in that batch of containers shall be
catalogued as affected by contamination,
resampling, repreparation, and reanalysis of
the samples shall be performed.


Sample Size Sufficient sample vessels shall be provided for The laboratory verifies that the mass required for The samplers shall be advised that the
the collection of the required increments if they each analysis, including QC samples and sample mass is insufficient. The
are to be composited at the laboratory. validation procedures contained in its sample determination on whether additional sample
acceptance policy. collection is needed or would be compliant
The protocols indicate the number of increments may only be made with concurrence from
that shall be taken for analysis. These amounts MDPH.
are to be received by the laboratory regardless
of the particular analytes to be tested.
The representative sample shall provide enough

mass for all relevant laboratory analyses and
required QC as defined in the laboratory sample
receipt policy. Sufficient sample mass for
reanalysis and duplicate analyses is to be
considered in determining the minimum sample
mass required.
Holding Time The amount of time from sample collection to Microbiology parameters – 48 hours (if micro Samples received outside of the holding
sample preparation and analysis shall be limited DQOs are not met a second analysis may be time shall be rejected by the laboratory for
based on the known stability of the analytes in a performed within 96 hours of sample collection) the appropriate analyses and resampled.
given matrix.
Metals parameters – 14 days (if Mercury is not If some analyses are within hold time, the
analyzed, 6 months) laboratory shall confirm with the client that
they want these analyzed or if the entire
Pesticides – 7 days to extraction, 40 days from suite of analyses shall be resampled.
extraction to analysis
Residual Solvents – 7 days
Cannabinoids – 7 days to extraction, 7 days from

extraction to analysis


Preservative Temperature preservation between 0°C < 6.0°C The laboratory shall document a received The RMD shall be held responsible for any
and Storage is required for all analyses. If Mercury is not to temperature of 0°C - ≤ 6.0°C for all samples resampling/reanalysis resulting from
be analyzed, metals samples collected unless sampled same day. If sampled same samples not shipped and stored at
separately do not require temperature day, the temperature and evidence of cooling appropriate temperatures.
preservation. shall be documented upon receipt.
Samples that were not sampled same-day
that are received by the laboratory out of
temperature shall be rejected by the
laboratory and resampled.
Samples that arrive the same day of

sampling without evidence of cooling shall
be rejected by the laboratory and
resampled.
Trip Blanks/ Trip blanks, field blanks, rinse blanks, and Target compounds/analytes shall not be present Samples associated with a contaminated
Field Blanks/ equipment blanks are recommended to be at concentrations > ½ LOQ. blank shall not be reprepared and
Rinse Blanks/ included with each sampling event and strongly reanalyzed. The contamination (including a
Equipment recommended for sampling events that include All blanks shall meet QC criteria (e.g., list of affected samples) shall be
Blanks residual solvent analysis to ensure that surrogates, internal standards). documented in the client report.
contamination was not introduced at the
sampling site or by the sampling equipment. Trip blanks, field blanks, rinse blanks, and
The laboratory shall prepare blanks the same equipment blanks shall not be reanalyzed
day as the sampling event or of the preparation solely for the purpose of reporting “not-
of sample containers (not days or weeks in detected” results. Blanks may only be
advance). reanalyzed if there is a valid technical
reason for reanalysis (e.g., injection failure
Ultra-pure, deionized/distilled water shall be or QC failure).
provided for use when field personnel collect
field, rinse, or equipment blanks.


Sample The laboratory shall have in its procedures and The laboratory has delivered the current sample The laboratory shall contact the client if
Documentation available to all sample collectors and couriers a acceptance criteria, shipping requirements, blank there are questions on the sample
sample acceptance policy that includes the sample labels, and COC forms that meet MDPH documentation. The client conversation
requirements contained in this table. sampling protocol requirements. shall be documented by the laboratory. If
the client does not have the information
Sample container labels and COC forms shall required for the sample, the sample shall be
include the following information at a minimum: rejected and resampled.
site location, sample date and time, initials of
sampler, licensee number, batch number,
location within facility, increment location within
batch, sample number, analytical method, and
preservative.
The laboratory shall provide enough blank
labels and containers to allow for the maximum
amount of samples that may be collected from
the site.
Sample The lab shall receive a request for analysis. The laboratory shall include the applicable If the RMD does not have an official
Documentation This can be a standalone document or in the request for analysis, COC, sampling records, sampling and analysis plan and the COC is
form of a COC or a sampling and analysis plan and/or SAP in the final report. unclear, the laboratory shall confirm a
(SAP). request for analysis with the RMD. If the
request for the analysis is for standard
The lab shall receive a sampling field record compliance testing as confirmed by the
that has the information required in the sampling RMD and the sample field records have
protocols such as the location and mass of enough information to confirm the required
increments that were combined in the field from sampling from the protocols was performed,
the RMD. the laboratory should note the lack of
documentation and the confirmation with
the RMD in the report narrative.


Chain-of- All bottleware shipments shall be documented The laboratory shall place sample containers in When tampering with bottleware shipments
Custody under COC procedures. appropriate custody-sealed sample coolers for is evident, the client and MDPH shall be
outgoing shipment. notified immediately for instructions on how
to proceed.
The laboratory shall have custody procedures
consistent with state regulation and that define
custody as it pertains to times when the sample
is not in immediate sight of the person who holds
custody.
Custody seals, locked coolers and containers,

locked vehicles, and other precautions shall be
discussed in the custody procedures if not
explicitly stated in the state regulation.

Appendix A - Table 03a

MDPH Residual Solvents by GC/MS
Quality Control Item Frequency Acceptance Criteria Corrective Action

GC/MS Tuning Every 12 hours. Ensure correct mass assignment. Retune instrument. Do not proceed with
Ion abundances shall meet the instrument calibration until tune criteria are met.
manufacturer tuning criteria.
2
Initial Calibration Each time the instrument is set A calibration curve shall be generated with all If the calibration curve is R ≤ 0.990, perform
up and when calibration target compounds and surrogate compounds if corrective action and recalibrate the
2
verification criteria are not met. used with an R ≥ 0.990. instrument.
A minimum of five calibration For all initial calibration levels, the retention When retention -time -window -criteria are
standards is required for first times shall be within ± 3 seconds of the not met, samples shall be reanalyzed within
order linear (at least six midpoint standard. a new calibration or CCV to meet the
standards are required for higher retention time window criteria.
order calibration).
The low-level calibration
standard shall be at or below the
LOQ.
Weighting should be utilized to

minimize Relative Standard
Error (RSE) at the protocol
action limit.
Initial Calibration A second-source calibration Recovery of all target compounds and Correct system and reanalyze ICV.
Verification (ICV) verification standard, when surrogates should be 70-130%. If second ICV fails, recalibrate system.
commercially available, shall be
analyzed after every initial
calibration within the same tune
as the initial calibration



Continuing Calibration Initially, after each set of 10 Recovery of all target compounds and Correct system and reanalyze CCV.
Verification (CCV) sample analyses, and at the end surrogates should be 70-130%. If second CCV fails, recalibrate system and
of each sequence. reanalyze all samples since last successful
Retention time of the CCV should not differ by CCV.
The final CCV shall be prepared  6 seconds or 0.04 RRT units from the
at the same time as the other retention time established by the middle
standards in order to assess the standard of the initial calibration.
stability of the light gasses.
Internal Standards If used, the IS shall be added to Area counts of the internal standard peaks Reanalyze affected samples at dilution to
every standard, sample, and QC shall be 50-150% of the internal standard area check for matrix interference. If internal
sample. observed in the associated CCV. standard still fails, perform corrective action,
recalibrate the instrument, and reanalyze
For all samples and QC The RT of the internal standard shall not vary sample.
samples, sample internal more than  6 seconds from the RT or 0.04
standard area counts and RTs RRT units of the internal standards observed in
shall be compared to the internal associated CCV standard.
standard area counts and RTs of
the associated CCV standard.
CCV internal standard area
counts and RTs shall be
compared to the area counts
and RTs of the ICV standard.
Method Blank One per preparation batch of up All target compounds for which there is a If positive results for contaminant compounds
to 20 samples. detection in associated samples, ≤½ the LOQ are not observed in the associated samples,
or < 10% of associated positive sample results record the failure in the client narrative. If
(whichever is higher). positive results for contaminant compounds
are observed in the associated samples, re-
prepare and reanalyze associated samples.



Surrogate Recovery If used, added to all calibration All surrogates shall meet laboratory-generated Check instrument performance. Correct the
standards, blanks, samples, and acceptance limits and fall within the retention problem and reanalyze the sample if a
QC samples. time windows. problem is identified. If the problem is
suspected to be matrix interference, dilute
and reanalyze the samples.
If surrogate recovery criteria are met upon

reanalysis, report the reanalysis results.
If the observed retention time of a surrogate

is outside of the established retention time
window, corrective action shall be performed
and the affected samples and QC shall be
reanalyzed.
Laboratory Control One LCS per preparation batch % Recoveries within laboratory-generated Reanalyze LCS to confirm results.
Sample (LCS) of up to 20 samples. limits. Laboratory generated acceptance If LCS results are outside of acceptance
criteria recovery windows cannot be set at criteria upon reanalysis, re-prepare the
≤ 15% at the low end and cannot be set at preparation batch and reanalyze samples. If
≥ 150% at the high end. the LCS results are still outside of
acceptance criteria, recalibrate and
reanalyze associated project samples.
If high recoveries are observed and “not-

detected” results are reported for the
associated samples, reanalysis is not
necessary. Record the failure in the client
report narrative.



Matrix Spike/Matrix One per matrix per preparation % Recoveries and RPDs within laboratory- Reprepare or reanalyze the affected sample
Spike Duplicate batch of up to 20 samples. generated limits. Laboratory generated (s) at a dilution or with additional cleanups to
(MS/MSD) acceptance criteria recovery windows cannot examine matrix affects.
All requested target compounds be set at ≤ 15% at the low end and cannot be
shall be included in the spiking set at ≥ 150% at the high end. Laboratory If LCS results meet acceptance criteria and
solution. generated limits for precision cannot exceed the MS/MSD still exceed criteria, note the
%RPD ≤ 40% nonconformance in the client report narrative
with information on matrix interference if
apparent in the reanalysis at a dilution.
Medical Marijuana or Duplicate of a sample taken at a %RPD ≤ 30% until enough points are collected If the field duplicate exceeds precision
MIP Field Duplicate frequency of once per medical for laboratory generated acceptance limits to criteria, RMD shall be informed and the batch
marijuana or marijuana-infused be statistically derived. Laboratory generated shall be resampled and reanalyzed. If the
product batch. limits for precision cannot exceed %RPD field duplicate exceeds precision criteria
≤ 40% upon resampling and reanalysis, the
laboratory shall note this on the report.
Qualitative/ Each target analyte. The instrument level of all target compounds Dilute the sample to bring the target
Quantitative Issues shall be below the upper calibration level. compound level within the instrument
calibration range.

Appendix A - Table 03b

MDPH Residual Solvents by GC-FID

2
Initial Calibration Each time the instrument is set A calibration curve shall be generated with all If the calibration curve is R ≤ 0.990, perform
up and when calibration target compounds and surrogate compounds if corrective action and recalibrate the
2
verification criteria are not met. used with an R ≥ 0.990. instrument.
A minimum of five calibration For all initial calibration levels, the retention When retention time window criteria are not
standards is required for first times shall be within ± 3 seconds of the met, samples shall be reanalyzed within a
order linear (at least six midpoint standard. new calibration or CCV to meet the retention
standards are required for higher time window criteria.
order calibration).
The low-level calibration

standard shall be at or below the
LOQ.
Weighting should be utilized to

minimize Relative Standard
Error (RSE) at the protocol
action limit.
Initial Calibration A second-source calibration Recovery of all target compounds and Correct system and reanalyze ICV.
Verification (ICV) verification standard, when surrogates should be 70-130%. If second ICV fails, recalibrate system.
commercially available, shall be
analyzed after every initial
calibration within the same tune
as the initial calibration



Continuing Calibration Initially, after each set of 10 Recovery of all target compounds and Correct system and reanalyze CCV.
Verification (CCV) sample analyses, and at the end surrogates should be 70-130%. If second CCV fails, recalibrate system and
of each sequence. reanalyze all samples since last successful
Retention time of the CCV should not differ by CCV.
The final CCV shall be prepared  6 seconds from the retention time
at the same time as the other established by the middle standard of the initial
standards in order to assess the calibration.
stability of the light gasses.
Retention Time (RT) Each analyte within each sample Retention time of each analyte should not differ 1.) Reject the identification of the analyte.
Window analysis. by > 3 seconds of the retention time 2.) Apply analyst judgement on the basis of
established for that analytes in the last CCV chromatographic data to make the
analyzed. identification with confirmation and
concurrence from a second analyst.
Method Blank One per preparation batch of up All target compounds for which there is a If positive results for contaminant compounds
to 20 samples. detection in associated samples, ≤½ the LOQ are not observed in the associated samples,
or < 10% of associated positive sample results record the failure in the client narrative. If
(whichever is higher). positive results for contaminant compounds
are observed in the associated samples, re-



Surrogate Recovery If used, added to all calibration All surrogates shall meet laboratory-generated Check instrument performance. Correct the
standards, blanks, samples, and acceptance limits and fall within the retention problem and reanalyze the sample if a
QC samples. time windows. problem is identified. If the problem is
suspected to be matrix interference, dilute
and reanalyze the samples.

If the observed retention time of a surrogate

is outside of the established retention time
reanalyzed.
Laboratory Control One LCS per preparation batch % Recoveries within laboratory-generated Reanalyze LCS to confirm results.
Sample (LCS) of up to 20 samples. limits. Laboratory generated acceptance If LCS results are outside of acceptance
criteria recovery windows cannot be set at criteria upon reanalysis, re-prepare the
≤ 15% at the low end and cannot be set at preparation batch and reanalyze samples. If
≥ 150% at the high end. the LCS results are still outside of
acceptance criteria, recalibrate and

report narrative.



Matrix Spike/Matrix One per matrix per preparation % Recoveries and RPDs within laboratory- Reprepare or reanalyze the affected sample
Spike Duplicate batch of up to 20 samples. generated limits. Laboratory generated (s) at a dilution or with additional cleanups to
(MS/MSD) acceptance criteria recovery windows cannot examine matrix affects.
All requested target compounds be set at ≤ 15% at the low end and cannot be
shall be included in the spiking set at ≥ 150% at the high end. Laboratory If LCS results meet acceptance criteria and
solution. generated limits for precision cannot exceed the MS/MSD still exceed criteria, note the
%RPD ≤ 40% nonconformance in the client report narrative
Confirmation Tentative identification of an All confirmation techniques: QC requirements If a peak is not confirmed, the sample is
analyte occurs when a peak (listed on Tables 3a and 3b) shall pass on both reported as < LOQ on the client report.
from a sample extract falls within initial and confirmation analyses.
the daily retention time window. If QC such as an LCS, surrogate, or method
Confirmation techniques include If two dissimilar columns are used for blank fails high on a column but all of the hits
analysis using a second column confirmation, the results shall be confirmed are ND, the results may be reported with a
with dissimilar stationary phase, with an RPD ≤ 40%. note in the client report narrative.
GC/MS, or by other recognized
confirmation techniques. If the QC does not pass on a column or the
RPD > 40%, and the analyte is detected, the
sample shall be reprepared and reanalyzed.
Dilution or additional cleanups are

recommended if chromatographic
interference is noted.
If QC on one or both columns fails upon

reanalysis or if the two columns again
produce an RPD > 40%, the analyte
detection shall be confirmed using a
recognized confirmatory technique.



Qualitative/ Each target analyte. The instrument level of all target compounds Dilute the sample to bring the target
Quantitative Issues shall be below the upper calibration level. compound level within the instrument
Professional judgement of highly calibration range.
experienced individuals is If there is obvious interference on the primary
required for a dual-column column, the secondary column may be chosen If secondary column is used for reporting and
analysis. There are some as the primary reporting column as long as the primary column is used for confirmation, this
situations where the quantitative secondary column still confirms the detected shall be noted in the client narrative.
result may be reported off the peaks both qualitatively (retention time) and
secondary column. quantitatively (QC passes and RPD < 40%).

MDPH Pesticides by LC-MS/MS
Mass Calibration and Annually and upon any major Mass calibrate to ensure accurate If optimization shifts, perform troubleshooting
Optimization maintenance or procedural changes assignments of mass to charge ratios corrective action as noted in maintenance
(m/z). Optimize to best mass assignment, procedures and record in maintenance log until
retention time, transition ion assignment, optimization is achieved.
and ratio abundance of transition ions for
each target analyte.
2
Initial calibration Each time the instrument is set up and A calibration curve shall be generated If the calibration curve is R ≤ 0.990, perform
when calibration verification criteria are with all target compounds and surrogate corrective action and recalibrate the
2
not met. compounds if used with an R ≥ 0.990. instrument.
A minimum of five calibration standards For all initial calibration levels, the When retention time window criteria are not
is required for first order linear (at least retention times shall be within ± 3 met, samples shall be reanalyzed within a new
six standards are required for higher seconds of the midpoint standard. calibration or CCV to meet the retention time
order calibration). window criteria.
The low-level calibration standard shall

be at or below the LOQ.
Weighting should be utilized to minimize

Relative Standard Error (RSE) at the
protocol action limit.
Initial Calibration A second-source calibration verification Recovery of all target compounds and Correct system and reanalyze ICV.
Verification (ICV) standard, when commercially available, surrogates should be 70-130%.
shall be analyzed after every initial If second ICV fails, recalibrate system.
calibration within the same tune as the
initial calibration

Continuing Calibration Initially, after each set of 10 sample Recovery of all target compounds and Correct system and reanalyze CCV.
Verification analyses, and at the end of each surrogates should be 70-130%. If second CCV fails, recalibrate system and
sequence. reanalyze all samples since last successful
Retention time of the CCV should not CCV.
The final CCV shall be prepared at the differ  6 seconds from the retention time
same time as the other standards in or 0.04 RRT units established by the
order to assess the stability of the light middle standard of the initial calibration.
gasses.
Internal standards When used, Internal Standards are Internal standards shall meet laboratory Reanalyze affected samples at dilution to
added to all blanks, standards, QC generated limits of a minimum of 30 check for matrix interference. If internal
samples, and samples. samples Express the assessment as a standard still fails, perform corrective action,
percent recovery interval of ± two recalibrate the instrument, and reanalyze
Sample internal standard area counts standard deviations. sample.
and RTs shall be compared to the
internal standard area counts and RTs of  6 seconds from the retention time or
the associated CCV standard. CCV 0.04 RRT units established by the
internal standard area counts and RTs associated continuing calibration
shall be compared to the area counts standard.
and RTs of the ICV standard.
Method Blank One per preparation batch of up to 20 All target compounds for which there is a If positive results for contaminant compounds
samples. detection in associated samples, ≤ ½ the are not observed in the associated samples,
LOQ or < 10% of associated positive record the failure in the client narrative. If
sample results (whichever is higher). positive results for contaminant compounds are
observed in the associated samples, re-

Laboratory Control One LCS per preparation batch of up to % Recoveries within laboratory-generated Reanalyze LCS to confirm results.
Sample (LCS) 20 samples. limits. Laboratory generated acceptance If LCS results are outside of acceptance criteria
criteria recovery windows cannot be set at upon reanalysis, re-prepare the preparation
≤ 15% at the low end and cannot be set at batch and reanalyze samples. If the LCS
≥ 150% at the high end. results are still outside of acceptance criteria,
recalibrate and reanalyze associated project
samples.

report narrative.
Matrix Spike/Matrix Spike One per matrix per preparation batch of % Recoveries and RPDs within Reprepare or reanalyze the affected sample (s)
Duplicate up to 20 samples. laboratory-generated limits. Laboratory at a dilution or with additional cleanups to
generated acceptance criteria recovery examine matrix affects.
All requested target compounds shall be windows cannot be set at ≤ 15% at the
included in the spiking solution. low end and cannot be set at ≥ 150% at If LCS results meet acceptance criteria and the
the high end. Laboratory generated limits MS/MSD still exceed criteria, note the
for precision cannot exceed %RPD ≤ 40% nonconformance in the client report narrative
Qualitative/Quantitative Each target analyte. The instrument level of all target Dilute the sample to bring the target compound
Issues compounds shall be below the upper level within the instrument calibration range.
calibration level.

Surrogate Compounds If used, added to all calibration All surrogates shall meet laboratory- Check instrument performance. Correct the
standards, blanks, samples, and QC generated acceptance limits. problem and reanalyze the sample if a problem
samples. is identified. If the problem is suspected to be
matrix interference, dilute and reanalyze the
samples.

If the observed retention time of a surrogate is

outside of the established retention time
reanalyzed.

MDPH Metals by ICP/MS
Tune and Optimization Daily, before analysis. According to instrument manufacturer Perform instrument maintenance and reanalyze
specifications. tune solution until criteria are met.
Initial Calibration Daily. The laboratory may draw a The correlation coefficient (r) for a Any single standard may be rerun once, however
calibration curve using a four-point four-point calibration curve shall be repeated failure requires that the standards be
curve and a blank with the lowest non- ≥ 0.995. reprepared and the instrument calibration shall be
zero standard being at or below 0.5 of rerun.
the Target analyte action limit and the
top standard being at or above 1.5 of
the Target analyte action limit).
Initial Calibration Each time the instrument is calibrated. ICV is within 90-110% of the true Reanalyze ICV or ICB once, if ICV or ICB is still
Verification/Blanks Immediately after instrument value. out, terminate analysis, correct problem, and
(ICV/ICB) calibration, the ICV and ICB are recalibrate instrument.
analyzed. ICB All targets < ½ the LOQ.
Linear Dynamic Range LDR may be > the standard solution at LDR standard shall be within 10% of Reprepare and reanalyze once. If LDR standard
determination 1.5 target analyte action limit. LDR true value. is still out, the full linear dynamic range
shall be determined initially for each determination shall be rerun.
target analyte and whenever major
instrument maintenance is performed.

Continuing Calibration After a passing ICV and ICB, the CCV is within 90-110% recovery. Reanalyze CCV or CCB. If CCV or CCB is still
Verifications/Continuing CCV/CCB shall be analyzed initially, out, terminate analysis, correct problem, and
Calibration Blank after each set of 10 sample analyses, CCB contains all target compounds for recalibrate instrument. Reanalyze all analytical
(CCV/CCB) and at the end of each sequence. which there is a detection in samples since the last compliant CCV/CCB.
associated samples, ≤ ½ the LOQ or
< 10% of associated positive sample For CCB failures, if positive results for
results (whichever is higher). contaminant compounds are not observed in the
associated samples, record the failure in the client
narrative. If positive results for contaminant
compounds are observed in the associated
samples, re-prepare and reanalyze associated
samples.
Method Blank One per preparation batch of up to 20 All target compounds for which there If positive results for contaminant compounds are
samples. is a detection in associated samples, not observed in the associated samples, record
≤ ½ the LOQ or < 10% of associated the failure in the client narrative. If positive results
positive sample results (whichever is for contaminant compounds are observed in the
higher). associated samples, re-prepare and reanalyze
associated samples.
Laboratory Control Sample One LCS per digestion batch of up to 80-120% recovery Reanalyze LCS to confirm results.
(LCS) 20 samples. If LCS results are outside of acceptance criteria
. upon reanalysis, re-prepare the preparation batch
and reanalyze samples. If the LCS results are
still outside of acceptance criteria, recalibrate and
If high recoveries are observed and “not-detected”

results are reported for the associated samples,
reanalysis is not necessary. Record the failure in
the client report narrative.

Matrix Spike/Matrix Spike One LCS per digestion batch of up to 80-120% recovery. RPD  20%. Reprepare or reanalyze the affected sample (s) at
Duplicate 20 samples. a dilution to examine matrix affects.
(MS/MSD; If LCS results meet acceptance criteria and the
pre-digestion) MS/MSD still exceed criteria, note the
nonconformance in the client report narrative with
information on matrix interference if apparent in
the reanalysis at a dilution.
Internal Standards (ISs) All internal standards for analysis used The internal standard intensity If the exceedance is in a CCV or CCB, the
for reporting are evaluated against the recovery shall be within 70% to 125% analysis should be stopped and the instrument
mid-level standard of the initial of the corresponding internal standard recalibrated.
calibration. in the mid-level standard of the initial
calibration. If the exceedance is only observed in field sample
analysis, matrix effect is indicated and the
affected samples should be diluted 5×
(successively) until the IS(s) pass criteria and the
reason for the dilution should be noted in the
client report narrative.
Qualitative/ Each target analyte. The instrument level of all target Dilute the sample to bring the target compound
Quantitative Issues compounds shall be below the upper level within the instrument calibration range.
calibration level.

Cannabinoids by HPLC

2
Initial Calibration Each time the instrument is set up and The calibration curve shall have a If the calibration curve is R ≤ 0.990, perform
correlation coefficient R  0.990
2
when calibration verification standard corrective action and recalibrate the instrument.
acceptance criteria are not met.
For all initial calibration levels, the When retention time window criteria are not met,
A minimum of five calibration standards is retention times shall be within ± 3 samples shall be reanalyzed within a new
required for first order linear (at least six seconds of the midpoint standard. calibration or CCV to meet the retention time
standards are required for higher order window criteria.
calibration).
The low-level calibration standard shall be
at or below the LOQ.
Weighting should be utilized to minimize

Relative Standard Error (RSE) at the
protocol action limit.
Initial Calibration A second-source calibration verification Recovery of all target compounds and Correct system and reanalyze ICV. If second ICV
Verification (ICV) standard shall be analyzed after every initial surrogates should be 70-130%. fails, recalibrate system.
calibration.
Continuing Calibration Initially, after each set of 10 sample Recovery of all target compounds and Correct system and reanalyze CCV.
Verification (CCV) analyses, and at the end of each sequence. surrogates should be 70-130%. If second CCV fails, recalibrate system and
reanalyze all samples since last successful CCV.
Retention time of the CCV should not
differ by  6 seconds from the
retention time or 0.04 RRT units the
established by the middle standard of
the initial calibration.


Laboratory Control The surrogate in the method blank shall Surrogate recoveries should be within Reanalyze LCS to confirm results.
Sample (LCS) serve as the LCS unless an approved laboratory-generated limits. If LCS results are outside of acceptance criteria
reference material of appropriate upon reanalysis, re-prepare the preparation batch
concentration is available. % Recoveries within 70-130% when and reanalyze samples. If the LCS results are
the LCS is prepared from an approved still outside of acceptance criteria, recalibrate and
When an approved reference material of reference material. reanalyze associated project samples.
appropriate concentration is available,
prepare one LCS from that material per
preparation batch of up to 20 samples. If high recoveries are observed and “not-
detected” results are reported for the associated
samples, reanalysis is not necessary but the
failure shall be noted in the client report narrative.
Matrix Spike The Matrix Spike is required if there is an % Recoveries within laboratory Reprepare or reanalyze the affected sample (s) at
approved reference material of appropriate generated limits. Laboratory a dilution or with additional cleanups to examine
concentration to fall within calibration range generated acceptance criteria matrix affects.
after extraction available under an ISO recovery windows cannot be set at
Guide 34 accreditation available. One per ≤ 15% at the low end and cannot be If LCS results meet acceptance criteria and the
preparation batch of up to 20 samples. set at ≥ 150% at the high end. MS/MSD still exceed criteria, note the
All requested target compounds shall be nonconformance in the client report narrative with
included in the spiking solution. information on matrix interference if apparent in
the reanalysis at a dilution.


Matrix Sample Duplicate One per extraction batch per matrix per ≤ 20% RPD Reprepare and reanalyze the affected sample
concentration level  20 samples per day. with an LCS and an LCS duplicate to show that
Shall undergo all sample preparative the precision of the analysis is still within criteria.
procedures. If sample results still exceed criteria and
LCS/LCS duplicate were within laboratory
generated precision criteria, note the
nonconformance in the client report narrative as
possible matrix interference or non-uniform
product.
Retention Time (RT) Each analyte within each sample analysis. Retention time of each analyte should 3.) Reject the identification of the analyte.
Window not differ by > 3 seconds of the 4.) Apply analyst judgement on the basis of
retention time established for that chromatographic data to make the
analytes in the last CCV analyzed. identification with confirmation and
concurrence from a second analyst.
Surrogate If used, added to all calibration standards, All surrogates shall meet laboratory- Check instrument performance. Correct the
blanks, samples, and QC samples. generated acceptance limits and fall problem and reanalyze the sample if a problem is
within the retention time windows. identified. If the problem is suspected to be
matrix interference, dilute and reanalyze the
samples.

If the observed retention time of a surrogate is

outside of the established retention time window,
corrective action shall be performed and the
affected samples and QC shall be reanalyzed.


Qualitative/ Each target analyte. The instrument level of all target Dilute the sample to bring the target compound
Quantitative Issues compounds shall be below the upper level within the instrument calibration range.
calibration level.

MDPH % Moisture by Gravimetric Analysis

Balance Calibration and Calibration annually under ISO ± 0.1% of certified mass for Balances outside of the acceptance criteria shall be taken
Verification 17025 calibration. Verified weights out of service and serviced by a technician. Balances shall
daily, prior to sample analysis. > 1.0 g. not be used until the acceptance criteria can be met.
Weight range shall bracket the ± 0.2% of certified mass for
measured sample weights and weights
their tared containers. < 1.0 g.
Preparation Blank One per preparation batch up Blanks ≤ 0.01 g Reanalyze all associated samples displaying positive
to 20 samples. results ≤ 10 the blank level.
Corrective action is not required if sample concentration is

> 10 the blank level.
Laboratory Duplicate One per 10 analyses. ≤ 20% RPD Flag data and report unacceptable precision as a qualifier
for all associated results that are required to be reported in
dry weight.
Constant Weight Each Sample The laboratory shall perform two If a constant weight is not reached, the laboratory shall
measurements between heating to repeat the heating and measuring procedural steps until a
ensure that a constant weight has constant weight is achieved. If a continuous loss of weight
been established. These two is occurring, it is possible that the laboratory is losing
masses shall agree within analytes that are volatile at the oven temperature and the
± 0.2%. laboratory should consider other methods or lower
temperatures that allow for loss of water but not the
constituent analytes of the product.
Notes:
- Method-specific requirements supersede the QC requirements in this table. The more stringent of the method requirements and
requirements provided herein shall be followed.
- Sample weights shall be bracketed by the balance calibration range.

MDPH % Moisture by Gravimetric Analysis

MDPH Microbiology by Plates and Films
Media Every lot, before use Negative Control < 1 CFU/g Reject Lot. Check other variables such as
1. APC positive and negative controls and media
2. Yeast and Mold with fresh lot of media. Catalog any
3. Total Coliforms affected samples and reanalyze.
4. Bile-tolerant Gram-negative
Bacteria
Plates/Bottles/Films Every lot, before use Negative Control < 1 CFU/g Reject Lot. Check other variables such as
1. APC positive and negative controls and media
2. Yeast and Mold with new plates/bottles/films. Catalog any
3. Total Coliforms affected samples and reanalyze.
4. Bile-tolerant Gram-negative
Bacteria
Dilution Water or Buffer Every lot, before use or Meet all ongoing criteria Reject lot of water. If system is in-house,
 All methods where dilutions monthly if system is in- prescribed in Section 10.3.3 of perform maintenance and a series of
are applicable house. the QAPP. checks before putting back in service.
Catalog any affected samples and
Negative Control < 1 CFU/g reanalyze.
Water Baths Temperature checked 45°C ± 1°C or test If temperature windows are exceeded,
1. APC twice a day separated by temperature ± 1°C catalog contents of incubator and re-
2. Total Coliforms 4 hours when in use. prepare. If there is not enough sample
3. Bile-tolerant Gram-negative mass to reanalyze, qualify the results on
Bacteria the client report.
Incubator Temperature checked 1. 35°C ± 2°C If temperature windows are exceeded,

1. APC twice a day separated by 2. 25°C ± 2°C catalog contents of incubator and re-
2. Yeast and Mold 4 hours when in use. 3. 20°C -25°C prepare. If there is not enough sample
3. Total Coliforms (pre-incubation) mass to reanalyze, qualify the results on
4. Bile-tolerant Gram-negative 4. 30°C -35°C (test for the client report.
Bacteria absence and quantitative)

Autoclave Every batch Content Defined Criteria If maximum pressure and/or temperature
 Method requirements  Media are not reached or not held for the required
pertaining to pressure,  Waste amount of time, perform maintenance on
temperature, autoclave time  Plates/Bottles the autoclave and use indicators to ensure
at temperature, and total time. effectiveness before re-sterilizing contents.
Consider running weekly spore
ampule to assess sterility.
Ambient Air Checks Weekly Not to exceed 15 CFU/plate Catalogue samples analyzed since last
 General media plate (HPC) check. Investigate source of
exposed for 15 minutes contamination and assess data quality on
affected samples by examining negative
control records. Qualify samples that had
affected data quality on client report.
Lab Duplicates 1 per preparation batch up For results expressed as MPN, Inform the client. If possible, reanalyze
to 20 samples. For MPN, both results should be within the associated samples. If reanalysis is not
one per 10 samples 95% confidence interval (if possible due to available sample, quality
available) for at least one of the the affected sample in the batch on the
results. client report.
Duplicate Count Every 10% of samples Same person < 5% RPD Both analysts should repeat their counts.
Different person < 10% RPD If the results are still outside of control,
assess the counting procedures and
perform corrective action as necessary in
the form of procedural change and/or
training, as indicated by the root cause
analysis.
Positive Controls Every batch Detected Perform checks on quality control

1. APC indicators to assign source of
2. Yeast and Mold contamination or inhibition. Reanalyze
3. Total Coliforms associated samples after appropriate
4. Bile-tolerant Gram-negative corrective action is taken.

Bacteria
Negative Controls Every batch Negative Control < 1 CFU/g Perform checks on quality control
1. APC indicators to assign source of
2. Yeast and Mold contamination. Reanalyze associated
3. Total Coliforms samples after appropriate corrective action
4. Bile-tolerant Gram-negative is taken.
Bacteria

MDPH Microbiology by PCR and ELISA

Dilution Water or Buffer Ongoing checks Meet all ongoing criteria prescribed in Section Reject lot of water. If system is in-house,
 All methods where 9.1 of the QAPP. perform maintenance and a series of
dilutions are checks before putting back in service.
applicable Negative Control Catalog any affected samples and
Every lot or batch 1. Not detected in 1 g reanalyze.
1. Pathogenic E.coli 2. Not detected in 1 g
2. Salmonella 3. > 20 ppb of sum of aflatoxin B1 (AFB1)
3. Mycotoxins B2 (AFB2), G1 (AFG1) and G2 (AFG2)
Water Baths Twice a day 1. N/A If temperature windows are exceeded

1. Pathogenic E.coli separated by 4 2. 49 ± 1°C; 43 ± 0.2 °C; 42 ± 0.2°C during the relevant step of the method,
2. Salmonella hours when in use 3. N/A catalog contents of incubator and re-
3. Mycotoxins prepare. If there is not enough sample
mass to reanalyze, qualify the results on
the client report.
Incubator Twice a day 1. 35 ± 1.0°C and 44 ± 1.0°C If temperature windows are exceeded
1. Pathogenic E.coli separated by 4 2. 35.0°C ± 2 °C during the relevant steps of the method,
2. Salmonella hours when in use 3. N/A catalog contents of incubator and re-
3. Mycotoxins prepare. If there is not enough sample
mass to reanalyze, qualify the results on
the client report.
Autoclave Every batch Content Defined Criteria If maximum pressure and/or temperature
 Method requirements  Media are not reached or not held for the
pertaining to pressure,  Waste required amount of time, perform
temperature, autoclave  Plates/Bottles maintenance on the autoclave and use
time at temperature, indicators to ensure effectiveness before
and total time. Consider running weekly spore ampule re-sterilizing contents.
to assess sterility

MDPH Microbiology by PCR and ELISA

Ambient Air Checks Monthly Not to exceed 15 CFU/plate Catalogue samples analyzed since last
 General media plate check. Investigate source of
exposed for 15 minutes contamination and assess data quality on
affected samples by examining negative
control records. Qualify samples that had
affected data quality on client report.
Lab Duplicates Every Batch <20% RPD Inform the client. Reanalyze associated
samples. If reanalysis is not possible due
to available sample, quality the affected
sample in the batch on the client report.
Positive Controls Every batch 1. Detected Perform checks on quality control

1. Pathogenic E.coli 2. Detected indicators to assign source of
2. Salmonella 3. 90-110% recovery for aflatoxin B1 (AFB1) contamination or inhibition. Reanalyze
3. Mycotoxins B2 (AFB2), G1 (AFG1) and G2 (AFG2) associated samples after appropriate
corrective action is taken.
Negative Controls Every Batch 1. Not Detectable in 1 g and IC, if Perform checks on quality control
1. Pathogenic E.coli applicable, is positive indicators to assign source of
2. Salmonella 2. Not Detectable in 1 g and IC, if contamination. Reanalyze associated
3. Mycotoxins applicable, is positive samples after appropriate corrective action
3. < 5ppm of each individual aflatoxin or is taken.
< 20 ppb of sum of aflatoxin B1 (AFB1) B2
(AFB2), G1 (AFG1) and G2 (AFG2)

Quality Assurance Program Plan for Analytical Testing Laboratories Performing Analyses of Finished Medical Marijuana
Products and Marijuana-Infused Products in Massachusetts
Appendix B
Data Review Instructions and Checklists
Version 5.0 May 15, 2018 Page B-1

Chemistry Data Review Checklist Template Instruction
1) Data Review Templates are examples that can be used for method data review or internal audits.
2) Each checklist should be customized to the analysis requirements and criteria set out in the MDPH
protocols, the text of this document, the MDPH QAPP DQO tables
(Appendix A of this document), or laboratory generated limits.
3) Reference SOP section should be supplemented with any additional requirements for the relevant
samples.
4) Checks that may be considered for addition include but are not limited to interference checks, dilution
checks, dual column checks, varying CCV concentrations, historical agreement, or data agreement
such as MeHg<Total Hg.
5) Font in red indicates areas of example only and should be replaced with parallel or additional QC
checks.
6) Delete any QC checks that are not performed in method.
7) Client Sample sections can be simplified by Project ID, Preparation Batch IDs or Analytical Batch IDs if
all are included in the method review.
8) Sample IDs used for QC samples such as matrix spikes or matrix duplicates should be recorded in the
comment sections.
9) Standard and Traceability records should include the record reviewed that contained the traceability to
standards and reagents. The identification should be contained in batch records and preparation
logbooks. If not included in other review procedures, such as logbook review, this review should
include a review traceability back to the specific Certificate of Analysis on file for each standard and
reagent used in the analysis.
10) For use as an internal audit checklist, specific supporting elements should be added from the quality
management system and supporting technical SOPs. These include but are not limited to current
analyst DOC record references, support equipment logbook reviews, and, record of training records
reviewed.

Insert Organic Method Name

I. Analytical Batch Information Analytical
SOP: Sequence/s:
Version: Date: Instrument ID:
Method File(s): Analysis Date: Analyst:
Electronic Filename(s): Analyte Group:
**Review sheet includes current QA O & M anager instructio n; SOP revsn pending date Reference SOP q ( ) q (())
II. Client Samples (items) listed by Prep Batch
P Batch: P Batch: P Batch:
III. Standards & Reagents

Traceability Records:
(()) Preparation Logbook ID:
Analyst Analyst Comments (see below as well) Reviewer (Review notes)
IV. Calibrations Pass Fail* N/A Agree C.A.R**
Corr. Coef. (all analytes)≥ 0.990 q q q q
(()) Analytes all w ithin RE%? q q q q q
<LOQ (or are a verified impurity) q q q q q
Retention Time of Mid-Standard Int. Std.? q q q q q
ICV (2nd Source) Recovery: 70%-130% q q q q
ICB/CCB Conc < ½LOQ or <LOD q q q q
CCV Recovery: 70%-130% q q q q
((CCV concentration 2)) Recovery: 70%-130% q q q q
((CCV low concentration))70-130%, q q q q q
Internal Standards 50%-150% q q q q q
Instrument Replicate %RPD <%% q q q q q
RT of all Surrogates within 6 secs or 0.4 RRT of MidStandard? q q q q q
V. Analytical Quality Control Pass Fail* Agree C.A.R**
Batch Size ≤ 20 samples q q q q

Method Blank (BLK,LRB)Conc < ½LOQ or <LOD q q q q
LCS (BS,LFB) Matrix1: 85-115% Matrix 2 80-120%
Surrogate(s) Matrix1: 85-115% Matrix 2 80-120% q q q q
VI. Sample QC Pass Fail* Agree C.A.R**
MS/MSD RPD: ± 30% q q q q
Matrix Spikes †† Matrix 1 : 70-130% Matrix 2: 75-125% q q q q
(()) Matrix 1 : 70-130% Matrix 2: 75-125% q q q q q
†† (unless spike < 30% background)
VII. Field QC Pass Fail* Verified N/A Agree C.A.R**
Field/Equipment Blank(s) Conc < ½LOQ or <LOD q q q q q q

Field Duplicates RPD: ±40% (±2LOQ if <5LOQ) q q q q q q
Data Agreement (w ithin 20%RPD or LOQ) q q q q q q
VIII. Data Management Yes N/A Agree C.A.R**
Manual Integrations Reviewed and Recorded? q q q q
Data Calculations/Entry/Upload Complete & Accurate q q q q
LIMS: Chemist initials; Instrument ID; Update status q q q q
Is optional batch narrative attached? q q q q
IX. Follow up after initial review Yes N/A
Corrective actions that were required (C.A.R.) by the reviewer have been completed: q q
Signatures & Dates
Analyst Date Review er Date:
See back for additional comments
Additional Analyst Comments Reviewer Comments


The batch was selected for an internal audit: q
* If a QC element fails and data is reported with a qualifier, include in the comments the QC result value, the qualifier code, and the
Insert Inorganic/Metals Method Name

I. Analytical Batch Information Analytical
SOP: Sequence/s:
Version: Date: Instrument ID:
Method File(s): Analysis Date: Analyst:
Electronic Filename(s): Analyte Group:
**Review sheet includes current QA O & M anager instructio n; SOP revsn pending date Reference SOP q ( ) q (())
II. Client Samples (items) listed by Prep Batch
P Batch: P Batch: P Batch:
III. Standards & Reagents

Traceability Records:
(()) Preparation Logbook ID:
Analyst Analyst Comments (see below as well) Reviewer (Review notes)
IV. Calibrations Pass Fail* N/A Agree C.A.R**
Corr. Coef. (all analytes)≥ 0.998 q q q q
(()) Analytes ±20% of true or ± LOQ q q q q q
((Interference Check)) <LOQ (or are a verified impurity) q q q q q
no t<LOQ, but interf's lo w so data no t affected q q q q q
ICV (2nd Source) Recovery: 90-110% q q q q
ICB/CCB Conc < ½LOQ or <LOD q q q q
CCV Recovery: 90-110% q q q q
((CCV concentration 2)) Recovery: 90-110% q q q q
((CCV low concentration))90-110%, q q q q q
Internal Standards 50%-150% q q q q q
Instrument Replicate %RPD <%% q q q q q
q q q q q
V. Analytical Quality Control Pass Fail* Agree C.A.R**
Batch Size ≤ 20 samples q q q q
Method Blank (BLK,LRB)Conc < ½LOQ q q q q
LCS (BS,LFB) Matrix1: 85-115% Matrix 2 80-120% q q q q
VI. Sample QC Pass Fail* Agree C.A.R**
MS/MSD RPD: ± 20% q q q q
Matrix Spikes †† Matrix 1 : 70-130% Matrix 2: 75-125% q q q q
(()) Matrix 1 : 70-130% Matrix 2: 75-125% q q q q q
†† (unless spike < 30% background)
VII. Field QC Pass Fail* Verified N/A Agree C.A.R**
Field/Equipment Blank(s) Conc < ½LOQ q q q q q q

Field Duplicates RPD: ±40% (±2LOQ if <5LOQ) q q q q q q
Data Agreement (w ithin 20%RPD or LOQ) q q q q q q
C.A.R.*
VIII. Data Management Yes N/A Agree *
Data Calculations/Entry/Upload Complete & Accurate q q q
LIMS: Chemist initials; Instrument ID; Update status q q q
Is optional batch narrative attached? q q
IX. Follow up after initial review Yes N/A
Corrective actions that were required (C.A.R.) by the reviewer have been completed: q q
Signatures & Dates

The batch was selected for an internal audit: q

* If a QC element fails and data is reported with a qualifier, include in the comments the QC result value, the qualifier code, and the
grade. If data is not reported, comment "Affected data not reported".
** C.A.R = Corrective Actions Required--Comment should state if a "green sheet" or "issue" was created.

Appendix C
Report Template
Version 5.0 May 15, 2018 Page C-1

A. REPORT HEADING
LAB NAME REPORT TITLE

LAB
REVISION #
SAMPLE ID
LAB ADDRESS
REPORT DATE
D. PICTURE OF SAMPLE
B. RMD INFO C. SAMPLE IDENTIFICATION
RMD NAME
RMD
SAMPLE ID
RMD OPTIONAL
ADDRESS (not required at this time)
BATCH ID
MANIFEST/CoC
NUMBER PARENT
DATE BATCH ID
RECEIVED
E. SAMPLE F. PRODUCT PRODUCTION

G. TEST TYPES RUN
PROPERTIES CHARACTERIZATION STAGE
For Plant
Other: (CN) Cannabinoid Profile
SAMPLE Material:
SIZE PRODUCT For Conc. (HM) Heavy Metals Analysis
Other:
Units= CLASS & Resin: (MB) Microbiological Test
(PT) Pathogen Screen
NUMBER of For MIP: Other:
SERVINGS (MY) Mycotoxin Test
INTENDED ROUTE OF
PRODUCT TYPE (VC) Residual Solvents Test
*MIP only CONSUMPTION
Other: (PS) Pesticide Screen
MATRIX RETAIL NAME
(TP) Terpene Profile
Other: Specify:
EXTRACTION
SAMPLE GROW MATERIAL SOLVENT
CONDITION *flower only
RE-TEST YES/NO
REMEDIATED YES/NO
Description
H. AUTHORIZATION
CASE NARRATIVE, LABORATORY NOTES, and STATEMENTS
MAY be dispensed LAB AUTHORIZATION SIGNATURE
MAY be dispensed as
THIS PRODUCT: INGESTION ONLY product
MAY NOT be dispensed

TABLE I. CANNABINOID PROFILE Analysis Date:

Lab Sample ID: <equal to heading> Analytical Method: Lab SOP #: Analyst:
Narrative Summary of Analysis
Concentration "Dose" weight LOD LOQ

Test ID Analyte
unit= %wt unit= mg/serving unit= %wt unit= %wt
Δ9-THC
THCa
CBD
CBDa
<to add>
<to add>
<to add>
<to add>
<to add>
<to add>
<to add>
- MAX THC
- MAX CBD
- CBD:THC RATIO
TABLE J. HEAVY METALS Analysis Date:

Concentration LOD LOQ Limits - All Use Limits - Ingestion Only

Test ID Analyte
unit= ppb unit= ppb unit= ppb Limits (ppb) Test Limits (ppb) Test
As 200 PASS/FAIL 1500 PASS/FAIL
Cd 200 PASS/FAIL 500 PASS/FAIL
Hg 100 PASS/FAIL 1500 PASS/FAIL
Pb 500 PASS/FAIL 1000 PASS/FAIL
TABLE K. MICROBIOLOGICAL CONTAMINANTS Analysis Date:

Analyte Standard Limits

Test ID Test Analysis Result Unit Limit Test
Symbol unit= CFU/g
AC Total Viable Aerobic Bacteria CFU/g PASS/FAIL
YM Total Yeast & Mold CFU/g PASS/FAIL
CC Total Coliforms CFU/g PASS/FAIL
Total Bile-Tolerant Gram
EB CFU/g PASS/FAIL
Negative Bacteria
TABLE L. PATHOGENIC BACTERIA Analysis Date:

Analyte
Test ID Test Analysis Result Standard Limits Limit Test
Symbol
ECPT E. coli (O157) Not detected in 1g PASS/FAIL
SPT Salmonella Not detected in 1g PASS/FAIL
TABLE M. MYCOTOXINS Analysis Date:

Analyte Result LOD LOQ Standard Limits

Test ID Test Analysis Limit Test
Symbol unit= ppb unit= ppb unit= ppb unit= ppb
<20 PASS/FAIL
<20 PASS/FAIL
<20 PASS/FAIL
<20 PASS/FAIL
<20 PASS/FAIL

TABLE N. RESIDUAL SOLVENTS Analysis Date:

Result LOD LOQ Standard Limits

Test ID Analyte Limit Test
unit= ppm unit= ppm unit= ppm unit= ppm
n-Butane - -
Iso-Butane - -
Propane - -
<to add if necessary> PASS/FAIL
- Total Hydrocarbons (Sum) 0 - - 12 PASS/FAIL
TABLE O. PESTICIDES Analysis Date:

Method
Result LOD LOQ Standard Limits
Test ID Analyte QA/QC
unit= ppb unit= ppb unit= ppb unit= ppb Test Test
Bifenazate 10 PASS/FAIL
Bifenthrin 10 PASS/FAIL
Cyfluthrin 10 PASS/FAIL
Etoxazole 10 PASS/FAIL
Imazalil 10 PASS/FAIL
Imidacloprid 10 PASS/FAIL
Myclobutanil 10 PASS/FAIL
Spiromesifen 10 PASS/FAIL
Trifloxystrobin 10 PASS/FAIL
<to add if necessary> 10 PASS/FAIL
TABLE P. TERPENE PROFILE Analysis Date:

Concentration LOD LOQ

Test ID Analyte CAS Number
unit= %wt unit= wt% unit= wt%
<to add>
<to add>
<to add>
<to add>
<to add>
<to add>
<to add>
<to add>
<to add>
<to add>
<to add>
<to add>
<to add>
<to add>
<to add>
<to add>
<to add>
<to add>
<to add>
<to add>

QA/QC RESULTS
TABLE Q. QC RESULTS - CANNABINOID PROFILE Analysis Date:

Analytical Method: Lab SOP #: Analyst:
Notes describing QC test
Prep Concentration Measured Concentration

Analyte RECOVERY (%)
unit= unit=
Δ9-THC
THCa
CBD
CBDa
<to add>
<to add>
<to add>
<to add>
<to add>
<to add>
<to add>
TABLE R. QC RESULTS - HEAVY METALS Analysis Date:


unit= unit=
As
Cd
Hg
Pb
TABLE S. QC RESULTS - MICROBIOLOGICAL CONTAMINANTS Analysis Date:

Date of most recent QC check:

Status:
TABLE T. QC RESULTS - PATHOGENIC BACTERIA

DATE QC CHECK PATHOGEN RESULT STATUS
Control (+) E. coli (O157)

Control (-) E. coli (O157)
Standard 1 E. coli (O157)
Standard 2 E. coli (O157)
Control (+) Salmonella
Control (-) Salmonella
Standard 1 Salmonella
Standard 2 Salmonella

TABLE U. QC RESULTS - MYCOTOXINS Analysis Date:

Reference Concentration Measured Concentration

Analyte STATUS
unit= unit=
<to add>
<to add>
<to add>
<to add>
TABLE V. QC RESULTS - RESIDUAL SOLVENTS Analysis Date:


unit= unit=
<to add>
<to add>
<to add>
<to add>
<to add>
<to add>
TABLE W. QC RESULTS - PESTICIDES Analysis Date:

Prep Concentration Measured Concentration RECOVERY

Analyte STATUS
unit= unit= (%)
Bifenazate
Bifenthrin
Cyfluthrin
Etoxazole
Imazalil
Imidacloprid
Myclobutanil
Spiromesifen
Trifloxystrobin
<to add>
<to add>
<to add>
<to add>
<to add>
<to add>
<to add>
<to add>
<to add>
<to add>

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Quality Assurance Program Plan for Analytical Testing Laboratories Performing Analyses of Finished Medical

Marijuana Products and Marijuana-Infused Products in Massachusetts

Title: Quality Assurance Program Plan for Analytical Testing Laboratories

The Protocol contains the following sections:

Version 5.0 May 15, 2018 Page i

8.2 Accuracy .....................................................................................................................28

Version 5.0 May 15, 2018 Page ii

11.5.3 Monitoring of Corrective Actions ..........................................................................62

Appendix A Data Quality Objective (DQO) Tables .................................................................. A-1

Version 5.0 May 15, 2018 Page iii

Version 5.0 May 15, 2018 Page iv

1.0 SCOPE AND APPLICATION

In order to outline the required Good Practices more clearly in

2.0 PROBLEM STATEMENT

Version 5.0 May 15, 2018 Page 5

appropriate quality. Within laboratory quality management systems such as ISO/IEC

3.0 DECISION RULE

 Exhibit 4. Analysis Requirements and Recommended Limits for Metals in Finished

Direction, on which materials are to be subjected to given protocol sections (Exhibits), is

4.0 MONITORING REQUIREMENTS

Version 5.0 May 15, 2018 Page 6

Table 1 Monitoring Requirements of Finished Plant Material for Massachusetts

Product Type Analyte Class Analyte(s) Action Limit Comment

Version 5.0 May 15, 2018 Page 7

Table 2 Monitoring Requirements of Marijuana Resin and Concentrates for

Product Analyte Class Analyte Action Comment

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Table 3 Monitoring Requirements of Marijuana Infused Products (MIPs) for

Product Type Analyte Class Analyte Action Limit Comment

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Table 4 Monitoring Requirements of Environmental Media and Water

Product Type Analyte Class Analyte Action Limit Comment

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5.0 QUALITY MANAGEMENT SYSTEM

5.1 Laboratory Quality Assurance Manual

5.2 General Requirements and Responsibilities for Laboratory Staff

5.2.1 Laboratory Staff

Laboratory staff members are responsible for the following activities:

 Performing procedures in accordance with the SOPs, project-specific

 Understanding and implementing the QA/QC requirements that pertain to their

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 Each technical staff member is to have a combination of experience, education,

5.2.2 Laboratory Management

The laboratory management is responsible for the following activities:

 Appointing of a technical manager that has appropriate education and experience to

 Providing supervision or providing for supervision of all personnel employed by the

 Safety training and maintenance of safety records.

5.2.3 Laboratory Quality Officer

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5.2.4 Deputies and Points of Contact

The laboratory management, however defined in the laboratory procedures, is to appoint

 Initiating frequent communications with appropriate RMD personnel or the

 Providing prompt verbal, text, or e-mail communication of any nonconformance

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 The POC is responsible for day-to-day activities associated with the