PVPR

DALLAS DRUGS PVT. LTD.
BADDI
DOCUMENT NO. PROCESS VALIDATION PROTOCOL EFFECTIVE DATE
DD/PVPR/APS/001 CUM REPORT OF ACLOG-SP REVISION No. 00
PROCESS VALIDATION
PROTOCOL CUM
REPORT OF ACLOG-SP
DALLAS DRUGS PVT. LTD.

156, DIC Industrial Area,
Hanuman Temple Chowk Road,
B/h Sai Road, Baddi ‐ 173205. HP
PRODUCT NAME
GENERIC NAME
BATCH No.
F01/QA/025-00 Page 1 of 47
DALLAS DRUGS PVT. LTD. BADDI
B.SIZE
Table of Contents
Sr. No. Subjects

1.0 Pre Approval Sheet
2.0 Objective
3.0 Scope
4.0 Validation Team
5.0 Responsibility of Validation Team
6.0 Validation Criteria
7.0 Revalidation Criteria
8.0 Batches Under Validation
9.0 Reason for Validation
10.0 Product Profile
11.0 Description of the Equipments used
12.0 List of References SOP/Specification/STP
13.0 Name of Approved Vender of Raw Materials
14.0 Quantity of Raw Materials Used
15.0 Process flow diagram
16.0 Sampling Summary
17.0 Manufacturing Procedure, Sampling Points and Acceptance Criteria
18.0 Compression Rational
19.0 Finished Product Analysis Report
20.0 Packing Rational
21.0 Training Status of person involved
22.0 Abbreviation
23.0 List of Annexure
24.0 Summary and Conclusion
F01/QA/025-00 Page 2 of 47
25.0 Post Approval of Process Validation
1.0 Pre-Approval :
Prepared By:
Functional Area Name Signature Date
Validation
Reviewed By:
Date
Functional Area Name Signature
Validation
Production
Engineering
Quality Control
Quality Assurance
Approved By:
Head Engineering
Head
Manufacturing
F01/QA/025-00 Page 3 of 47
Head Quality
2.0 Objective:
To ensure that the critical process variables are checked during validation and to demonstrate
the process capability on equipment and utility ensuring that the product meets it predetermined
specifications and quality attributes.
3.0 Scope:
The scope of this protocol is limited to the Process Validation of ACLOG-SP formulation in
Manufacturing Area, which defines the procedural aspects to be followed while carrying out
process validation activity that includes prerequisites before commencing the actual work like,
Master Formula Record, Approved Vendors, Specifications and Standard Testing Procedures.
It also defines the acceptance criteria, re-validation criteria and justification for critical process
parameters.
4.0 Validation Team
Department Name
Validation
Production
Engineering
Quality Control
Quality Assurance
5.0 Responsibility of Validation Team:

5.1 Validation:
 Prepares the protocol and Ensures that the protocol is in compliance
with current policies and procedures.
F01/QA/025-00 Page 4 of 47
 Ensures that the content is sufficient, clearly defined, and technically

accurate.
 Distributes the finalized protocol for review and approval signatures.
 Execution of protocol, withdrawing samples, compilation of reports and
submitting summary and conclusion.
5.2 Quality Control:
 Review of protocol, testing of samples, recording of Results and final
result submission.
5.3 Production:
 Review of protocol, operation of equipments and manufacture as per the batch manufacturing
record.
5.4 Engineering:
 Review of protocol and ensures availability of utilities required for this
study.
 Ensure the proper functioning of all the equipments and measuring
devices used in the process.
5.5 Quality Assurance:
 Review & Approval of protocol
 Issuance of approved copy for execution & document control.
 Review of executed protocol, the completed data package, and final
report.
6.0 Validation Criteria:

 Process validation batch shall be manufactured as per process steps standardized as
per the master manufacturing Formula and Batch Manufacturing Record.
 The batches manufactured during process validation shall meet the criteria defined in
the specifications.
7.0 Revalidation Criteria:

The process shall be revalidated whenever there shall be change in;
F01/QA/025-00 Page 5 of 47
 Manufacturing process and the product formula

 Manufacturing site or location
 Critical parameter is out of predetermined specifications
 Change in critical equipment in manufacturing process
 Change in API source
8.0 Batches under Validation:
Sr. Batch
Product Name Batch No. Mfg. Date Exp. Date
No. Size
9.0 Reason for validation:
____________________________________________________________________________
____________________________________________________________________________
____________________________________________________________________________
____________________________________________________________________________
__________________________
10.0 Product Profile:

Name of the Product : ACLOG-SP
Generic Name : Aceclofenac, Serratiopeptidase & Paracetamol Tablets
Label Claim : Each Film coated tablet contains:
Aceclofenac I.P. …….100 mg
Serratiopeptidase I.P. ……..15 mg
(As enteric coated granules 30,000 units)
Paracetamol I.P……..325 mg
F01/QA/025-00 Page 6 of 47
Batch Size : 400,000 Tablets (280.0 kg)

Shelf-Life : 24 Months
Category : Analgesic & Paragesic
Product Code : APS/001
Storage : Store in a cool, dry & dark place

11.0 Description of the Equipments Used:
Sr.
Equipments Name Equipment ID No. Qualification Status Checked By
No.
1.
Vibro Sifter
2.
RMG
3.
Multimill
4.
Fluid Bed Dryer
5.
Octagonal Blender
6.
Compression Machine
7.
Tablet Inspection Machine
8.
ALU-ALU Packing Machine
Remarks:
_______________________________________________________________________________
_______________________________________________________________________________
_______________________________________________________________________________
___________________________
Verified By: ______________
(Sign./Date)
F01/QA/025-00 Page 7 of 47
12.0 List of Reference Standard Operating Procedure (SOP)/Specification/STP:

Sr. Title of SOP/Specification/STP SOP/Specification/STP Approval Checked By
No. No. Status
01.
02.
03.
04
05.
06.
07.
08.
09.
10.
11.
12.
13.
14.
15.
F01/QA/025-00 Page 8 of 47
Remarks:
_________________________________________________________________________________
_____________________________________________________________________________
Verified By: ____________

(Sign/Date)
13.0 Name of Approved Vender of Raw Materials:
Sr. Ingredients Specification Approved vendor Checked By

No.
01 Aceclofenac I.P
02 Paracetamol I.P
03 Serratiopeptidase I.P
04 Starch I.P
05 Dibasic Calcium Phosphate I.P
06 Starch for Paste I.H.S
07 PVP K-30 I.P
08 Methyl Paraben Sodium I.P
09 Propyl Paraben Sodium I.P
10 *Purified Water* I.H.S
11 Talcum I.P
12 Magnesium Stearate I.P
13 Sodium Starch Glycolate I.P
14 Colloidal Silicon Dioxide I.P
15 Readymix Film Coating (White) I.H.S
16 Sunset Yellow Lake I.H.S
17 Tartrazine Lake I.H.S
18 IPA I.P
19 MDC I.P
F01/QA/025-00 Page 9 of 47
13.1 Used API Details:
Assay LOD % w/w

API Batch No A.R. No Checked By
Limit_______ Limit_______
ACECLOFENAC IP
PARACETAMOL IP
SERRATIOPEPTIDASE
IP
F01/QA/025-00 Page 10 of 47
14.0 Quantity of Raw Materials Used: Std. Batch Size : 100,000 Tablets , Actual Batch Size:______
Std. Qty./ Batch No. Batch No. Batch No.
Std. Qty
Sr.No. Raw Materials Batch
Mg/ Tab
(Kg)
1. Aceclofenac
2. Paracetamol
3. Serratiopeptidase
4. Starch
5. Dibasic Calcium Phosphate
6. Starch for Paste
7. PVP K-30
8. Methyl Paraben Sodium
9. Propyl Paraben Sodium
10. *Purified Water*
11. Talcum
12. Magnesium Stearate
13. Sodium Starch Glycolate
14. Colloidal Silicon Dioxide
Readymix Film Coating
15.
(White)
16. Sunset Yellow Lake
17. Tartrazine Lake
18. IPA
19. MDC
Total
Remarks:
F01/QA/025-00 Page 11 of 47
_______________________________________________________________________________
_______________________________________________________________________________
Verified By: _______________
(Sign./Date)
15.0 Process Flow Diagram:
Equipment Process Flow Diagram Critical Step
Dispensing raw materials AR No., Grade &

Calibrated Balance Vender details
Rechecking of weights
Calibrated Balance
Sieve Integrity before
Sifting & After Sifting
Sifting
Dry mixing (Mix at fast

RMG speed of impeller and Mixing time and
chopper for 2 mins.) RPM
Mixing Time and Mixing

RMG Wet mixing
Speed
Dr
yin
Tray Dryer g
Drying time, temperature and LOD
16 # S.S Sieve Sieve Integrity, Sifting time

Vibratory shifter & 2.5 mm
Screen
Lubrication
Blender 20min at 05 RPM Blending time & RPM
Compression 17.5 x
Thickness, Hardness,
8.5mm Oval, Elongated
Compression Machine Friability,
Bi concave, on upper
Disintegration time,
punches and breakline
Compression Machineon Average weight,
lower punch
Uniformity of weight
F01/QA/025-00 Page 12 of 47
Packaging Forming/Sealing
Blister/Strip Packing Temp.
16.0 Sample Summary:
Sampling shall be done from the predefined locations as described in the Annexure – I.
17.0 Manufacturing Procedure, Sampling Points and Acceptance Criteria:

17.1 Weighing, Sifting, Dry Mixing, Wet Mixing, Drying, Milling and Sifting, Blending, as per
MFR.
17.1.1 WEIGHING AND CHECKING OF WEIGHTS

Check the weights of all ingredients as per respective SOP.
17.1.2 SIFTING
Sift the following ingredients; through S.S. Sieve fitted to a Mechanical sifter and
collect separately in double polythene lined labeled containers.
Sr. No. Ingredients Spec. Sieve size#
1 Aceclofenac I.P
2 Paracetamol I.P
3 Starch I.P
5 Microcrystalline Cellulose I.P
6 Talcum I.H.S
9 Cross Carmilose Sodium I.P
10 Colloidal Silicon Dioxide I.H.S
11 Aceclofenac I.P
12 Paracetamol I.P
13 Starch I.P
15 Microcrystalline Cellulose I.H.S
16 Talcum I.H.S
F01/QA/025-00 Page 13 of 47

19 Cross Carmilose Sodium I.P
Check the sieve integrity before and after sifting operation.

17.1.3 DRY MIXING
Load the above sifted material into RMG in following order as Nimesulide,
Paracetamol, starch & Dibasic Calcium Phosphate mix for 30 minutes at fast speed of
impeller and fast speed of chopper.
TL TR
ML MR
Impeller Chopper Discharge port
Where, TR - Top Right, TL - Top Left, MR - Middle Right, ML - Middle Left

B - Bottom
(D-1 Diagram of Rapid Mixer Granulator with Sampling Points)
F01/QA/025-00 Page 14 of 47
17.1.3.1 Test Results of Samples collected at Dry Mixing stage:
Assay%
Sample Batch No.: Batch No.: Batch No.:
TR
TL
MR
ML
B
Mean
SD
RSD
Checked By
Acceptance Criteria: RSD <5.0 % and all individuals are within ± 10% of mean (absolute)
17.1.3.2 Result of Composite Sample collected at Dry Mixing stage:

Results Of Bulk Density (Tapped and Untapped)
Acceptance Tapped Bulk Density
Sample
Criteria
B.No: B.No: B.No:
To Record
Composite Untapped Bulk Density
To Record
Checked By
F01/QA/025-00 Page 15 of 47
17.1.3.3 Result of Sieve Analysis (Lubricated Granules):
Sieve Acceptance % W/W Retention
Analysis Criteria B.No: B.No: B.No:
20#
40#
60# To Record
80#
100#
% W/W Passed Through
All Through
To Record
Checked By
Remarks:
_______________________________________________________________________________
_______________________________________________________________________________
_______________________________________________________________________________
_______________________________________________________________________________
___________________________
Verified By: _______________
(Sign./Date)
F01/QA/025-00 Page 16 of 47
17.1.4 GRANULATION
Granulate the dry mix of above step with the granulating medium (Purified water) in
Rapid Mixer Granulator by keeping impeller at slow speed and chopper at slow speed
over a period of 3 minutes (Note down the amperage reading).
After complete addition of purified water rake the material and continue mixing of
wet mass for 2 minutes with impeller and chopper at fast speed. Discharge the wet
mass by operating impeller at slow speed and chopper at fast speed.
Unload the wet mass into the FBD Bowl of FBD.
Granulation Batch No Batch No Batch No
Impeller amperage at
granulation end point
Total Granulation time
17.1.5 DRYING
Dry the wet mass prepared in above step using Fluid Bed Dryer(FBD) by maintaining
the inlet temperature NMT 80°C and Outlet temperature NMT 50°C, till the LOD is
achieved NMT 3.0%w/w (at 105°C, 5 min).
Powder
Bed
TL TR
ML MR
FBD Bowl
F01/QA/025-00 Page 17 of 47
Result of LOD/ (at the end of drying) of Dried Granules (Fluid Bed Dryer)
Sample Acceptance B. No. B. No. B. No.
Location Criteria Lot I Lot II Lot I Lot II Lot I Lot II
LOD
Top Right
(TR)
Top Left (TL)
Middle Right NMT 3.0%
(MR)
Middle Left
(ML)
Bottom (B)
Checked By
# Strike out which ever is not applicable
Reamrks:
___________________________________________________________________________
___________________________________________________________________________
____
Verified By: ______________
(Sign/Date)
17.1.6 SIZING OF GRANULES
Sift the dried granules obtained from above step through 16# sieve in Vibro sifter.
Pass the 16# sieve retained material through Multimill by using 2.5 mm screen with
knives forward configuration, at slow speed. The milled granules to be resifted through
16# sieve in Vibro sifter.
Collect the granules in air tight double polythene lined labeled HDPE container of sized
granules, record the weight.
Check the sieve and Multimill screen integrity before and after sifting operation.
F01/QA/025-00 Page 18 of 47
17.1.7 SIFTING OF EXTRA GRANULAR MATERIAL
Sr.
Ingredients Specification Sieve Size #
No.
1. Talcum IP 100
2. Magnesium Stearate IP 100
3. Sodium Starch Glycolate IP 100
4. Crosss Carmilose Sodium IP 100
5. Colloidal Silicon Dioxide IP 100
through specified S.S. sieve fitted to a Vibro sifter and collect in double Polythene lined
labeled HDPE containers
Check the sieve integrity before and after sifting operation.
F01/QA/025-00 Page 19 of 47
17.1.8 LUBRICATION
Load the granules and sifted materials (Talcum, SSG, CCS & Aerosil) in a blender and
blend for 15 minutes at 05 RPM and then add Magnesium Stearate in a blender and
Blend for 5 minutes.
Unload the lubricated granules into double polythene lined pretared labeled.
Store in HDPE containers, well covered with lid and protected from moisture.
Where,
TL = Top Left
TM = Top Middle
TL TM TR TR = Top Right
MR = Middle Right
ML MM MR MM=Middle Middle
ML = Middle Left
BL BM BR BL = Bottom Left
BM =Bottom Middle
DP BR = Bottom Right
DP =Discharge Point
(Diagram of Octagonal blender with sampling points)
F01/QA/025-00 Page 20 of 47
17.2.1 Test Result of samples collected after lubrication:
Assay%
B. No.: B. No.: B. No.:
Sample After lubrication (20 min) After lubrication (20 min) After lubrication (20 min)
TL
TM
TR
MR
MM
ML
BL
BM
BR
DP
Composite
Mean
SD
RSD
Checked By
Acceptance Criteria: NLT 98.0% and NMT 102.0 % of the labeled amount of ACECLOFENAC 100 MG
NLT 98.0% and NMT 102.0 % of the labeled amount of PARACETAMOL 325 MG
NLT 98.0% and NMT 102.0 % of the labeled amount of SERRATIOPEPTIDASE 15MG
Remarks:
________________________________________________________________________________
________________________________________________________________________________
________________________________________________________________________________
_________
F01/QA/025-00 Page 21 of 47
Verified By: ______________

(Sign/Date)
17.2.2 Result of Assay (Lubricated Granules):
Test Acceptance B.No. B.No. B.No.

Criteria
Assay NLT 98.00 mg

Aceclofenac and NMT
102.00 mg
Assay NLT 98.00 mg
Serratiopeptidase and NMT
102.00 mg
Assay NLT 98.00 mg
Paracetamol and NMT
102.00 mg
Remarks:
________________________________________________________________________________
________________________________________________________________________________
________________
Verified By: ______________
(Sign/Date)
17.2.3 Result Of Bulk Density-Untapped/Tapped (Lubricated Granules):
Sample Sample Qty. Acceptance Result of bulk density (untapped)

Criteria B.No. B.No. B.No.
To Record
Composite 100 gm
Result of bulk density (tapped)
To Record
Checked By
Remarks:
________________________________________________________________________________
________________________________________________________________________________
________________
Verified By:________________
F01/QA/025-00 Page 22 of 47
(Sign/Date)
17.2.4 Calculation of Compressibility Index & Hausner Ratio of Final Lubricated Blend:
*Compressibility Index & **Hausner Ratio Of Lubricated Blend

(For Information Only)
B.No. B.No. B.No.
Sample
Compressibility Hausner Compressibility Hausner Compressibi Hausner
Index Ratio Index Ratio lity Ratio
Index
Composite
Sample
Checked
By
*Compressibility =(Tapped Density-Bulk Density) x100 ** Hausner Ratio = Tapped Density
Tapped Density Bulk Density
17.2.5 Result of Sieve Analysis (Lubricated Granules):
Sieve Acceptance % W/W Retention

Analysis Criteria B.No: B.No. B.No.
16#
40#
60# To Record
80#
100#
% W/W Passed Through
All
Through To Record
Checked By
F01/QA/025-00 Page 23 of 47
17.2.6 Result of LOD (Lubricated Granules):
Acceptance Result Of LOD

Sample
Criteria B. No.: B. No.: B. No.:
NMT 3.0% W/W
Composite (at 105°C for 5
minutes)
Remarks:
________________________________________________________________________________
________________________________________________________________________________
________
Verified By:_____________
(Sign/Date)
17.2.7 Final Yield after Lubrication:
Yield B. No. B. No. B. No.
Yield Obtained
Checked By
Remarks:
___________________________________________________________________________
___________________________________________________________________________
________
Verified By: _____________
Sign/Date
F01/QA/025-00 Page 24 of 47
18.0 Compression Rationale:

To validate the compression process for ACLOG-SP TABLETS, run the compression machine on
optimum speed and optimum pressure and collect samples from Initial stage, Middle stage, End
stage as per sample summary Annexure-I.
Procedure:
Set the machine and adjust the compression parameters. After Stabilization of the compression
machine, check the parameters mentioned below and record in the report.
Parameters of Evaluation
1 Description 6 Friability
2 Group Weight 7 Disintegration Time
3 Thickness 8 Pre Dissolution
4 Hardness 9 Dissolution
5 Individual Weight 10 Assay
After the start of the compression, collect tablets at regular Intervals s till the end of the
compression cycle as per the sample summary (Refer: Annexure - I). Record the sample details or
in the manufacturing Record.
F01/QA/025-00 Page 25 of 47
18.1 Validation of compression for 1st Batch (Batch No. :__________________)

18.1.1 Compression hardness challenge for 1st Batch
18.1.1.1 At Low Hardness: i.e. (………Kg/cm2 and speed……. RPM)
Test Acceptance Criteria Left Side Right Side
Description Oval, Elongated &
Biconvex Tablet
Average weight(mg) (700mg) 686 – 714 mg
Individual Low (700mg±5%) 665mg
weight High to 735mg
variation
Thickness(mm) 5.50mm(5.30 - Range:_____to_______ Range:_____to______
5.70mm)
Hardness(Kg/cm2) NLT 3 Kg/cm2 Range:_____to_______ Range:_____to_______
Friability(%w/w) NMT 1.0%
Disintegration Test NMT 15 mints.
18.2.1.2 At High Hardness: i.e. (……….Kg/cm2and speed …….. RPM)

Biconvex Tablet
variation
5.70mm)
F01/QA/025-00 Page 26 of 47
18.2.2 Compression speed challenge for 1st batch

18.2.2.1 At Low speed …… RPM (RPM range 10-30)
Biconvex Tablet
variation
5.70mm)
Content uniformity (%)
Tablet No LHS Tablet No RHS

1. 1.
2. 2.
3. 3.
4. 4.
5. 5.
6. 6.
7. 7.
8. 8.
9. 9.
10. 10.
Mean Mean
F01/QA/025-00 Page 27 of 47
RSD RSD
Checked By Checked By
Acceptance criteria: As per Finished product specification
Evaluation of compression at Low speed

_________________________________________________________________________________
_________________________________________________________________________________
_______
Verified by: _____________________

(Sign/Date)
18.2.2.2 At High speed………..RPM (RPM range 10-30)

Biconvex Tablet
variation
5.70mm)
Tablet No LHS Tablet No RHS
F01/QA/025-00 Page 28 of 47
1. 1.
2. 2.
3. 3.
4. 4.
5. 5.
6. 6.
7. 7.
8. 8.
9. 9.
10. 10.
Mean Mean
RSD RSD
Checked By
Acceptance criteria: As per Finished product specification
Evaluation of compression at High speed

_________________________________________________________________________________
_________________________________________________________________________________
________
Verified by: _____________________

(Sign/Date)
F01/QA/025-00 Page 29 of 47
18.3.1 Validation of compression under optimum condition for 1st Batch (Batch .:________)
18.3.2 Average mass of 20 Tablets (gm) (Limit: 700 mg, 686-714mg)
After After After After After After After After After

Initial 60 120 180 240 300 360 420 480 540
RHS minutes minutes minutes minutes minutes minutes minutes minutes minutes

Initial 60 120 180 240 300 360 420 480 540
LHS minutes minutes minutes minutes minutes minutes minutes minutes minutes
18.3.3 Uniformity of mass (On 20 tablets): NMT 2/20 tablets may deviate from the average
mass by more than 5%

RHS Initial 60 120 180 240 300 360 420 480 540
minutes minutes minutes minutes minutes minutes minutes minutes minutes
Min.
Max
LHS Initial 60 120 180 240 300 360 420 480 540
Min
Max
F01/QA/025-00 Page 30 of 47
18.3.4 Thickness (5.50mm, 5.30 -5.70mm)

RHS Initial 60 120 180 240 300 360 420 480 540
Min
Max
LHS Initial 60 120 180 240 300 360 420 480 540
Min
Max
18.3.5 Hardness (NLT 3 Kg/cm2)

RHS Initial 60 120 180 240 300 360 420 480 540
Min
Max
LHS Initial 60 120 180 240 300 360 420 480 540
Min
Max
F01/QA/025-00 Page 31 of 47
18.3.6 Friability (Limit: NMT 1.0 % mass is lost after 4 minutes)

Initial 60 120 180 240 300 360 420 480 540

Initial 60 120 180 240 300 360 420 480 540
18.3.7 Disintegration Time (Limit: NMT 15 minutes)

Initial 60 120 180 240 300 360 420 480 540

Initial 60 120 180 240 300 360 420 480 540
18.4.1 Validation of compression under optimum condition for 2nd Batch (Batch No.:________)
F01/QA/025-00 Page 32 of 47

Initial 60 120 180 240 300 360 420 480 540

Initial 60 120 180 240 300 360 420 480 540

RHS Initial 60 120 180 240 300 360 420 480 540
Min
Max
LHS Initial 60 120 180 240 300 360 420 480 540
Min
Max
18.4.4 Thickness (5.50mm, 5.30 -5.70mm)
F01/QA/025-00 Page 33 of 47

RHS Initial 60 120 180 240 300 360 420 480 540
Min
Max
LHS Initial 60 120 180 240 300 360 420 480 540
Min
Max

RHS Initial 60 120 180 240 300 360 420 480 540
Min
Max
LHS Initial 60 120 180 240 300 360 420 480 540
Min
Max
F01/QA/025-00 Page 34 of 47

Initial 60 120 180 240 300 360 420 480 540

Initial 60 120 180 240 300 360 420 480 540

Initial 60 120 180 240 300 360 420 480 540

Initial 60 120 180 240 300 360 420 480 540
18.5.1 Validation of compression under optimum condition for 3rd Batch (Batch .:___________)
F01/QA/025-00 Page 35 of 47

Initial 60 120 180 240 300 360 420 480 540

Initial 60 120 180 240 300 360 420 480 540

RHS Initial 60 120 180 240 300 360 420 480 540
Min
Max
LHS Initial 60 120 180 240 300 360 420 480 540
Min
Max
18.5.4 Thickness (5.50mm, 5.30 -5.70mm)

RHS Initial After After After After After After After After After
60 120 180 240 300 360 420 480 540
F01/QA/025-00 Page 36 of 47

Min
Max
LHS Initial 60 120 180 240 300 360 420 480 540
Min
Max

RHS Initial 60 120 180 240 300 360 420 480 540
Min
Max
LHS Initial 60 120 180 240 300 360 420 480 540
Min
Max
RHS Initial After After After After After After After After After
60 120 180 240 300 360 420 480 540
F01/QA/025-00 Page 37 of 47

Initial 60 120 180 240 300 360 420 480 540

Initial 60 120 180 240 300 360 420 480 540

Initial 60 120 180 240 300 360 420 480 540
18.5.8 Final Yield after Compression:
Yield B. No. B. No. B. No.
F01/QA/025-00 Page 38 of 47
Yield Obtained
Checked By
Remarks:
__________________________________________________________________________
__________________________________________________________________________
__________
Verified by: ____________________
(Sign/Date)
19.0 Finished Product Analysis Report:
F01/QA/025-00 Page 39 of 47
S.No Test Specification Results

1ST 2nd 3rd
Oval, Elongated & Biconvex
1.
Description Tablet.
By HPLC: The retention time of

the Aceclofenac, Serratopeptidase
Identification by & Paracetamol Tablets peak in the
2. chromatogram of the test
preparation corresponds to that in
the chromatogram of the standard
preparation, as obtained in assay.
3. Average Weight 700 mg (686-714mg)
4. Thickness 5.50mm(5.30 – 5.70mm)
5. Hardness NLT 3 Kg/cm2
6. Friability NMT 1.0%

NMT 2/20 tablets may deviate from
7. Uniformity of mass average mass by more than 5% and
no tablet by more than 15%
The active content of each tablet
should lie between 85% and 115%
of the stated amount. If the content
of one tablet falls outside the above
limit and if the content of none of
the tablets falls beyond 75% and
8. Uniformity of Content
125% of the stated amount then
each of the remaining 20 tablets
must be assayed. The requirements
are met if the content of each of the
additional 20 tablets assayed falls
within the limit of
Disintegration Time 85% and 115% of the stated
a) NMT 5 minutes
9. a) In house
b) NMT 15 minutes
b) BP method
NLT 70% (Q) of labeled amount is
10. Dissolution Test
dissolved in 45 minutes.
F01/QA/025-00 Page 40 of 47
S.No Test Specification Results

1ST 2nd 3rd
Related substances NMT 1.0%
(By TLC BP method)
5-Chloro-1-methyl-4-
11. nitroimidazole and 6-
mercaptopurone
Total impurity NMT 1.0%

Not less than 95.0% and not more
Assay
than 105.0%
12. ( By HPLC %w/w)
Not less than 47.5 mg and not more
than 52.50 mg
Remarks:
___________________________________________________________________________
___________________________________________________________________________
___________________________________________________________________________
_____________________
Verified by: ____________________
(Sign/Date)
F01/QA/025-00 Page 41 of 47
20.0 Packing Rationale:

Packing is done by Blister Packing. During Packing of ACLOG-SP, forming, sealing
temperature and pack size is to be checked for physical appearance and leak test.
(Temperature challenge study for sealing temperature will be conducted for first batch only)
20.1 Batch 1st _____________ Batch Size: _____________ Date: __________

Temperature challenge study for PVC pack
Sealing roller temp. Speed (Cuts/min) Leak Test Knurling/Rattling Checked By
Stage Sealing roller Forming roller Physical Appearance Leak Test Checked
temp. temp. (Sealing/ Cutting By
Limit:________ Limit:________ /Knurling / Coding)
Initial
Middle
End
Remarks:
________________________________________________________________________________
________________________________________________________________________________
________________________________________________________________________________
________________________

(Sign/Date)
F01/QA/025-00 Page 42 of 47
Result for Related Substances (At maximum sealing temperature)
Sr. no. Test Limits Batch no.
Related compounds (By TLC BP

method) NMT 1.0%
1.
5-chloro-1-methyl-4nitroimidazole
and 6- mercaptopurine
20.2 Batch 2nd _____________ Batch Size: _____________ Date: __________

Initial
Middle
End
Remarks:
________________________________________________________________________________
________________________________________________________________________________
________________________________________________________________________________
________________________
Verified By: __________________
(Sign/Date)
F01/QA/025-00 Page 43 of 47
20.3 Batch 3rd _____________ Batch Size: _____________ Date: __________

Initial
Middle
End
Remarks:
________________________________________________________________________________
________________________________________________________________________________
________________________________________________________________________________

(Sign/Date)
21.0 Training Status of Person involved:

S.No. Name of Trainee Status Checked By
F01/QA/025-00 Page 44 of 47
22.0 Abbreviation:
Abbreviation Full form
SOP Standard Operating Procedure
PVP Process Validation Protocol
No. Number
Sign. Signature
LOD Loss On Drying
23.0 List of Annexure:

Annexure No. Title
F01/QA/025-00 Page 45 of 47
24.0 Summary and Conclusion:

24.1 Summary:
____________________________________________________________________________
____________________________________________________________________________
____________________________________________________________________________
____________________________________________________________________________
____________________________________________________________________________
____________________________________________________________________________
____________________________________________________________________________
____________________________________________________________________________
____________________________________________________________________________
____________________________________________________________________________
____________________________________________________________________________
____________________________________________________________________________
____________________________________________________________________________
____________________________________________________________________________
____________________________________________________________________________
____________________________________________________________________________
____________________________________________________________________________
____________________________________________________________________________
____________________________________________________________________________
____________________________________________________________________________
____________________________________________________________________________
____________________________________________________________________________
____________________________________________________________________________
____________________________________________________________________________
____________________________________________________________________________
______________________________________________
Verified By: ______________
(Sign./Date)
F01/QA/025-00 Page 46 of 47
24.2 Conclusion:
ACLOG-S tablets of Batch No.:____________/_____________/___________ were manufactured in
the facility. All the three validation batches meet the specification for ACLOG-S tablets & desire
results obtained. Since the product meets the predefined specification hence it is concluded that the
manufacturing process of ACLOG-SP tablets is validated.
The Certificate of analysis for the batches are attached.
Batch No. A.R. No.
25.0 Post Approval of Process Validation:
Validation
Production
Quality Control
Quality Assurance
Head Engineering
Head Manufacturing
Head Quality
F01/QA/025-00 Page 47 of 47

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DALLAS DRUGS PVT. LTD.

DD/PVPR/APS/001 CUM REPORT OF ACLOG-SP REVISION No. 00

DALLAS DRUGS PVT. LTD.

DD/PVPR/APS/001 CUM REPORT OF ACLOG-SP REVISION No. 00

Sr. No. Subjects

DD/PVPR/APS/001 CUM REPORT OF ACLOG-SP REVISION No. 00

25.0 Post Approval of Process Validation

Functional Area Name Signature Date

Functional Area Name Signature Date

DD/PVPR/APS/001 CUM REPORT OF ACLOG-SP REVISION No. 00

4.0 Validation Team

5.0 Responsibility of Validation Team:

DD/PVPR/APS/001 CUM REPORT OF ACLOG-SP REVISION No. 00

 Ensures that the content is sufficient, clearly defined, and technically

6.0 Validation Criteria:

7.0 Revalidation Criteria:

DD/PVPR/APS/001 CUM REPORT OF ACLOG-SP REVISION No. 00

 Manufacturing process and the product formula

9.0 Reason for validation:

10.0 Product Profile:

DD/PVPR/APS/001 CUM REPORT OF ACLOG-SP REVISION No. 00

Batch Size : 400,000 Tablets (280.0 kg)

Category : Analgesic & Paragesic

Product Code : APS/001

Storage : Store in a cool, dry & dark place

DD/PVPR/APS/001 CUM REPORT OF ACLOG-SP REVISION No. 00

12.0 List of Reference Standard Operating Procedure (SOP)/Specification/STP:

DD/PVPR/APS/001 CUM REPORT OF ACLOG-SP REVISION No. 00

Verified By: ____________

Sr. Ingredients Specification Approved vendor Checked By

DD/PVPR/APS/001 CUM REPORT OF ACLOG-SP REVISION No. 00

13.1 Used API Details:

Assay LOD % w/w

DD/PVPR/APS/001 CUM REPORT OF ACLOG-SP REVISION No. 00

DD/PVPR/APS/001 CUM REPORT OF ACLOG-SP REVISION No. 00

Dispensing raw materials AR No., Grade &

Dry mixing (Mix at fast

Mixing Time and Mixing

16 # S.S Sieve Sieve Integrity, Sifting time

DD/PVPR/APS/001 CUM REPORT OF ACLOG-SP REVISION No. 00

17.0 Manufacturing Procedure, Sampling Points and Acceptance Criteria:

17.1.1 WEIGHING AND CHECKING OF WEIGHTS

DD/PVPR/APS/001 CUM REPORT OF ACLOG-SP REVISION No. 00

17 Magnesium Stearate I.P

Check the sieve integrity before and after sifting operation.

Impeller Chopper Discharge port

Where, TR - Top Right, TL - Top Left, MR - Middle Right, ML - Middle Left

DD/PVPR/APS/001 CUM REPORT OF ACLOG-SP REVISION No. 00

17.1.3.1 Test Results of Samples collected at Dry Mixing stage:

17.1.3.2 Result of Composite Sample collected at Dry Mixing stage:

Composite Untapped Bulk Density

DD/PVPR/APS/001 CUM REPORT OF ACLOG-SP REVISION No. 00

17.1.3.3 Result of Sieve Analysis (Lubricated Granules):

Sieve Acceptance % W/W Retention

Analysis Criteria B.No: B.No: B.No:

% W/W Passed Through

DD/PVPR/APS/001 CUM REPORT OF ACLOG-SP REVISION No. 00

Granulation Batch No Batch No Batch No

Total Granulation time

DD/PVPR/APS/001 CUM REPORT OF ACLOG-SP REVISION No. 00