Scribd Logo
Upload

Welcome to Scribd!

  • 490 views

    Coa Propylene Glycol

    Uploaded by

    NadaNursetiyanti
    This certificate provides the analysis of a propylene glycol reference material. It was certified to be 99.9% pure based on mass balance analysis. Various tests were performed to characterize the material and ensure it met specifications, including assays comparing it to pharmacopeial standards, identification by IR and MS, determination of water content, residue, and other properties. The material is stated to be homogeneous and its long term stability was assessed.

    Copyright:

    © All Rights Reserved
    Download as PDF, TXT or read online from Scribd

    Coa Propylene Glycol

    Uploaded by

    NadaNursetiyanti
    490 views8 pages
    This certificate provides the analysis of a propylene glycol reference material. It was certified to be 99.9% pure based on mass balance analysis. Various tests were performed to characterize the material and ensure it met specifications, including assays comparing it to pharmacopeial standards, identification by IR and MS, determination of water content, residue, and other properties. The material is stated to be homogeneous and its long term stability was assessed.

    Original Description:

    Coa Propylene Glycol

    Copyright

    © © All Rights Reserved

    Available Formats

    PDF, TXT or read online from Scribd

    Did you find this document useful?

    Is this content inappropriate?

    This certificate provides the analysis of a propylene glycol reference material. It was certified to be 99.9% pure based on mass balance analysis. Various tests were performed to characterize the material and ensure it met specifications, including assays comparing it to pharmacopeial standards, identification by IR and MS, determination of water content, residue, and other properties. The material is stated to be homogeneous and its long term stability was assessed.

    Copyright:

    © All Rights Reserved
    Download as PDF, TXT or read online from Scribd
    Download as pdf or txt
    490 views8 pages

    Coa Propylene Glycol

    Uploaded by

    NadaNursetiyanti
    This certificate provides the analysis of a propylene glycol reference material. It was certified to be 99.9% pure based on mass balance analysis. Various tests were performed to characterize the material and ensure it met specifications, including assays comparing it to pharmacopeial standards, identification by IR and MS, determination of water content, residue, and other properties. The material is stated to be homogeneous and its long term stability was assessed.

    Copyright:

    © All Rights Reserved
    Download as PDF, TXT or read online from Scribd
    Download as pdf or txt
    of 8

    Certificate of Analysis

    ISO 17034
    ANAB Cert# AR-1470
    PROPYLENE GLYCOL
    ISO/IEC 17025 CERTIFIED REFERENCE MATERIAL
    ANAB Cert# AT-1467

    CERTIFIED PURITY: 99.9%, Ucrm = ±0.2% k = 2


    (Mass Balance/as is basis)

    NOMINAL PACKAGE SIZE: 1.5g


    CATALOG #: PHR1051 LOT #: LRAB0286
    CERTIFICATE VERSION: LRAB0286.4 ISSUE DATE: 31 January 2019
    Note: Certificates may be updated due to Pharmacopeial Lot changes or the availability of new data.
    Check our website at: www.sigma-aldrich.com for the most current version.

    CRM EXPIRATION: 31 December 2020 (Proper Storage and Handling Required).


    RECEIPT DATE: ________________
    Note: this space is provided for convenience only and its use is not required.
    STORAGE: Store at Room Temperature. Transfer unused portions to a tightly closed
    container. Protect from humidity.
    CHEMICAL FORMULA: C3H8O2 MW: 76.1
    PHYSICAL DESCRIPTION: Clear liquid in amber ampule CAS #: 57-55-6
    HAZARDS: Read Safety Data Sheet before using. All chemical reference materials
    should be considered potentially hazardous and should be used only by qualified
    laboratory personnel.
    INSTRUCTIONS FOR USE: Do not dry, us on the as is basis. The internal pressure of
    the container may be slightly different from the atmospheric pressure at the user’s
    location. Open slowly and carefully to avoid dispersion of the material. This material is
    intended for Laboratory Use only. Not for drug, household or other uses.

    Page 1 of 8
    TRACEABILITY ASSAY
    Comparative assay demonstrates direct traceability to Pharmacopeial Standards
    METHOD: GC (ref.: Adapted from Propylene Glycol Monograph, Current
    Compendial Monograhs)

    ASSAY vs. USP REFERENCE STANDARD (as is basis)


    ASSAY VALUE vs. USP LOT
    99.3% R081G0
    Labeled Content = 1.00 mg/mg

    ASSAY vs. EP CRS (as is basis)


    ASSAY VALUE vs. EP BATCH
    99.3% 2.0
    Labeled Content = None
    Assigned Content = 99.1 %*

    Column: SPB-624, 30m x 0.53 mm x 3.0 µm


    Detector/Temperature: FID/280°C
    Carrier Gas: H2
    Flow: 4.0 mL/min
    Split Ratio: N/A
    Injection/Temperature: 0.5 µL/ 40°C
    Temperature Program: 40°C, 50°C/min to 100°C hold 4 min, 50°C/min to 120°C hold
    10 min, 50°C/min to 220°C and hold 6 min
    Internal Standard: 2,2,2-Trichloroethanol

    Representative Chromatogram from Lot: LRAB0286 vs. USP/EP Analysis

    Page 2 of 8
    ASSAY vs. BP CRS (as is basis)
    ASSAY VALUE vs. BP BATCH
    99.9% 3082
    Labeled Content = 99.9%
    *Assigned content was determined by comparison against the USP Reference Standard
    and BP CRS
    Column: SPB-624 30m x 0.53 mm x 1.40µm
    Detector/Temperature: FID/250°C
    Carrier Gas: H2
    Flow: 2.4mL/min
    Split Ratio: 10:1
    Injection/Temperature: 1µL/220°C
    Temperature Program: 40°C for 1min, 25°C /min to 120°C, hold 10 min, 25°C to 220°C,
    hold 6min
    Internal Standard: 2,2,2-Trichloroethanol

    Representative Chromatogram from Lot: LRAB0286 vs. BP Analysis

    PURITY DETERMINATION BY MASS BALANCE

    CHROMATOGRAPHIC IMPURITY ANALYSIS


    METHOD: GC (ref.: Adapted from Propylene Glycol Monograph, Current
    Compendial Monograhs)
    Column: SPB-624 30m x 0.53 mm x 1.40µm
    Detector/Temperature: FID/250°C
    Carrier Gas: H2
    Flow: 2.4mL/min
    Split Ratio: 10:1
    Injection/Temperature: 1µl/220°C
    Temperature Program: 40°C for 1min, 25°C /min to 120°C, hold 10 min, 25°C to 220°C,
    hold 6min

    Page 3 of 8
    Impurities Detected
    Impurity 1: 0.005% Impurity 2: 0.04%
    Impurity 3: 0.006% Impurity 4: 0.004%
    Total Chromatographic Impurities: 0.06%
    Representative Chromatogram from Lot: LRAB0286 Impurity Analysis

    RESIDUAL SOLVENTS
    Method: GC-MS Headspace (ref.: Residual Solvents USP <467>)
    Column: DB-1301
    Carrier gas: He
    Flow: 1.2mL/min
    Split Ratio: 1:5
    Injection/Temperature: 1µL/250°C
    Temperature Program: 40°C for 20min, 10°C/min to 240°C, hold 20min
    Solvents Detected: None

    WATER DETERMINATION
    Method: Karl Fisher titration (ref.: Current Compendial Monographs)
    Mean of three measurements, Water Content = 0.04%

    RESIDUE ANALYSIS
    Method: Sulfated Ash (ref.: Current Compendial Monographs)
    Sample Size: ~ 1.5 g
    Mean of three determinations, Residue = 0.001%

    CERTIFIED PURITY BY MASS BALANCE [100% - Impurities (normalized)]

    99.9% Ucrm = ±0.2%, k = 2


    (as is basis)

    Page 4 of 8
    IDENTIFICATION TESTS

    INFRARED SPECTROPHOTOMETRY (Comparative identification analysis


    demonstrates direct traceability to Pharmacopeial standards).

    Page 5 of 8
    MASS SPECTRUM
    Method: HR-QTOF; 4.0 kV ESI+; temperature: 325 °C

    Theoretical value: 77.0603 m/z

    The signal of the MS spectrum is consistent with the theoretical value and its
    interpretation is consistent with the structural formula.
    1
    H NMR (Data provided by an external laboratory; not in scope of accreditation)

    Consistent with structure

    Page 6 of 8
    BOILING POINT
    Specification: 184°C to 189°C (EP)
    Mettler Toledo FP900 Thermosystem with FP81 Measuring Cell
    Mean of three measurements = 187.3°C (corrected)

    REFRACTIVE INDEX
    Specification: 1.431 to 1.433 (EP)
    Mettler Toledo RA-510M Refractoanalyzer
    Temperature: 20°C
    Mean of three measurements = 1.432

    SPECIFIC GRAVITY
    Specification: 1.035 to 1.040 (EP)
    Anton Paar DMA38 Density Meter
    Temperature: 20°C
    Mean of three measurements = 1.038

    HOMOGENEITY ASSESSMENT
    Homogeneity was assessed in accordance with ISO Guide 35. Completed units were
    sampled using a random stratified sampling protocol. The results of chemical analysis
    were then compared by Single Factor Analysis of Variance (ANOVA). The uncertainty
    due to homogeneity was derived from the ANOVA. Heterogeneity was not detected
    under the conditions of the ANOVA.
    Analytical Method: GC Sample size: ~ 500 µL

    UNCERTAINTY STATEMENT
    Uncertainty values in this document are expressed as Expanded Uncertainty (Ucrm)
    corresponding to the 95% confidence interval. Ucrm is derived from the combined
    standard uncertainty multiplied by the coverage factor k, which is obtained from a t-
    distribution and degrees of freedom. The components of combined standard uncertainty
    include the uncertainties due to characterization, homogeneity, long term stability, and
    short term stability (transport). The components due to stability are generally considered
    to be negligible unless otherwise indicated by stability studies.

    STABILITY ASSESSMENT
    Significance of the stability assessment will be demonstrated if the analytical result of the
    study and the range of values represented by the Expanded Uncertainty do not overlap the
    result of the original assay and the range of its values represented by the Expanded
    Uncertainty. The method employed will usually be the same method used to characterize
    the assay value in the initial evaluation.

    Page 7 of 8
    Long Term Stability Evaluation - An assessment, or re-test, versus a Compendial
    Reference Standard may be scheduled, within the 3 year anniversary date of a release of a
    Secondary Standard. The re-test interval will be determined on a case-by-case basis.
    Short Term Stability Study - It is useful to assess stability under reasonably anticipated,
    short term transport conditions by simulating exposure of the product to humidity and
    temperature stress. This type of study is conducted under controlled conditions of
    elevated temperature and humidity.

    __________________________________ _______________________________
    QC Manager Head Quality Assurance

    APPENDIX

    Original Release Date: 31 March 2016


    Stability Test Date: 22 March 2018
    Requalification Test Date: 22 March 2018
    Requalification Test Date: 31 January 2019

    Manufactured and certified by Sigma-Aldrich RTC, Inc.


    2931 Soldier Springs Rd, Laramie WY, USA 82070 Page 8 of 8
    (Phone): 1-307-742-5452 (Fax): 1-855-831-9212
    email: [email protected]

    You might also like