PROCESS VALIDATION REPORT

Document # VP/CAP/PV/024
TITLE: Issue # 01
Effective Date 15-02-2019
XREX 50mg Review Date 15-02-2023
(PREGABALIN) Supersede # 00
Page 1 of 20
CAPSULE
REVIEWED BY:
PREPARED BY: APPROVED BY:

QA Officer Sr. Q.C Manager Sr. Q.A Manager Sr. Production Manager GM
Engineering G.M Quality
Operation

TABLE OF CONTENTS
Section Description PAGE NO.
1.0 SCOPE 2
2.0 DOCUMENTATION 2
3.0 VALIDATION APPROACH 2
3.1 PROCESS VALIDATION 2
3.2 VALIDATION STRATEGY 3
4.0 PRODUCT DESCRIPTION 3
5.0 LIST OF MAJOR EQUIPMENT USED IN 3
MANUFACTURING
6.0 PROCESS DETAILS 4
6.1 PROCESS SCALE 4
7.0 PROCESS FLOW DIAGRAM 4
7.1 PROCESS FLOW DIAGRAM OF X-REX 50mg CAPSULE 4-6
7.2 MANUFACTURING PROCESS 7-8
8.0 CRITICAL QUALITY ATTRIBUTES 8
9.0 PROCESS PARAMETERS TO BE QUALIFIED 9
9.1 PROCESS PARAMETERS 9-10
10.0 MANUFACTURING CONDITIONS-REQUIREMENTS AND 11-18
RESULTS
11.0 PACKAGING 19
11.1 BLISTERING & PACKING 19
12.0 STABILITY 19
13.0 SUMMARY AND CONCLUSION 19

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 PROCESS VALIDATION REPORT
Document # VP/CAP/PV/024
TITLE: Issue # 01
Effective Date 15-02-2019
XREX 50mg Review Date 15-02-2023
(PREGABALIN) Supersede # 00
Page 2 of 20
CAPSULE
REVIEWED BY:
PREPARED BY: APPROVED BY:

QA Officer Sr. Q.C Manager Sr. Q.A Manager Sr. Production Manager GM
Engineering G.M Quality
Operation

2
 PROCESS VALIDATION REPORT
Document # VP/CAP/PV/024
TITLE: Issue # 01
Effective Date 15-02-2019
XREX 50mg Review Date 15-02-2023
(PREGABALIN) Supersede # 00
Page 3 of 20
CAPSULE
REVIEWED BY:
PREPARED BY: APPROVED BY:

QA Officer Sr. Q.C Manager Sr. Q.A Manager Sr. Production Manager GM
Engineering G.M Quality
Operation

1.0 SCOPE
This protocol will document at least the critical steps and parameters of manufacturing process,
i.e. those that may have an impact on the quality of the product.Complete manufacturing
processes, including Blending, Filling and Encapsulation will be validated.

2.0 DOCUMENTATION:
All batch documents should be in compliance with standard documents.
2.1 Mfg. Directions
2.2 Manufacturing Order
2.3 Standard Operating Procedure
2.4 Standard Control Procedures
2.5 Standard Test Method
2.6 Packaging Order
All of the above stated documents are understood by all responsible persons, as applicable.
All related operating procedures must be in compliance with the product requirement.

3.0 VALIDATION APPROACH

3.1 Process Validation
This is a new product an approach of concurrent validation with a single lot acceptance
will be adopted. This will be three lot concurrent validation and all three lots will be
subjected to stability studies.
Rationale: Establishing documented evidence with a high degree of assurance, that a
specific process will consistently produce a product meeting its predetermined
specifications and quality characteristics, based on preplanned protocols following are
the pre-requisites:
o Equipment, production environment and analytical testing methods – already fully
validated.
o appropriately trained personnel and batch manufacturing documentation prepared
after these critical parameters have been identified, and machine settings, component
specifications and environmental conditions have been determined and specified
o Data within the finally agreed parameters.
 from at least three consecutive batches, giving product of the desired quality
may be considered acceptable.

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 PROCESS VALIDATION REPORT
Document # VP/CAP/PV/024
TITLE: Issue # 01
Effective Date 15-02-2019
XREX 50mg Review Date 15-02-2023
(PREGABALIN) Supersede # 00
Page 4 of 20
CAPSULE
REVIEWED BY:
PREPARED BY: APPROVED BY:

QA Officer Sr. Q.C Manager Sr. Q.A Manager Sr. Production Manager GM
Engineering G.M Quality
Operation

o Same size batches will be considered for validation.

o Commercial batch sizes will be considered.
 Validity of assumptions made should be demonstrated when commercial
production starts.
o Extensive testing at various stages in the manufacturing process _ including on the
final product and its package.
3.2 Validation strategy
Focuses on:
3.2.1 Filling of capsule bodies in capsule feeder plate
3.2.2 Transfer of Pregabalin (Powdered) into hopper of filling machine.
3.2.3 Filling:
3.2.3.1 Fill weight variation.
3.2.4 Sealing of the bodies and caps of the capsules.
3.2.5 Blistering.

4.0 PRODUCT DESCRIPTION

4.1 Active ingredients
Each Film coated tablet contains: Pregabalin (powdered) 50mg/capsule.
4.2 Indication
Xrex (Pregabalin) is used to treat pain caused by Fibromyalgia or nerve pain in people
with Diabetes.(Diabetic neuropathy).
.
5.0 LIST OF MAJOR EQUIPMENTS USED IN MANUFACTURING

6.0 S. No. Qualification

Equipment Description Asset Number
Status
1. Ribbon mixer,50 kg 1-01-03-25-0006 Qualified
2. Capsule Filling and Sealing Machine 1-01-03-03-0002 Qualified
3. Capsule polishing machine 1-01-03-44-0004 Qualified
4 China Blister Machine, ALU ALU 1-01-03-02-0003 Qualified
PROCESS DETAILS
6.1 Process scale
S. No. Scale Drug Name Drug Code Unit of Quantity:82.00
mg/tab. No. Measure kg /200,000

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 PROCESS VALIDATION REPORT
Document # VP/CAP/PV/024
TITLE: Issue # 01
Effective Date 15-02-2019
XREX 50mg Review Date 15-02-2023
(PREGABALIN) Supersede # 00
Page 5 of 20
CAPSULE
REVIEWED BY:
PREPARED BY: APPROVED BY:

QA Officer Sr. Q.C Manager Sr. Q.A Manager Sr. Production Manager GM
Engineering G.M Quality
Operation

Capsules
Pregabalin RM-API-
1 50.0 kg 5.00
(powdered) 0205
RM-XCP-
2 95.0 Lactose kg 9.50
0047
RM-XCP-
3 47 Maize Starch kg 4.7
0071
RM-XCP-
4 3.00 Talcum kg 0.300
0078
EG Capsules # 3,
RM-XCP-
5 - white body and green Nos. 105000
0364
cap
Compliance to Specification of all (new & already in use) codes used will be checked.
I - Verify the material is received from the approved source.
II - Successful completion of shelf life of the product will confirm the validation of the raw
materials.

7.0 PROCESS FLOW DIAGRAM

7.1 Process flow diagram of Xrex 50mg Capsule

- PREGABALIN
Pass following through 16 mesh 16 mesh screen:
(powdered)
- LACTOSE screen:
-MAIZE STARCH

Collect in Mixer and mix for 20 Mixer, 50kg

minutes

Add by sieving
through 40 mesh sieve
Blend for 05 minutes 40 mesh screen:
-Talcum powder

Submit sample to Blended granules transfer to Polyethylene

Q.C. for analysis Polyethylene lined Plastic Containers. lined plastic
Containers

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 PROCESS VALIDATION REPORT
Document # VP/CAP/PV/024
TITLE: Issue # 01
Effective Date 15-02-2019
XREX 50mg Review Date 15-02-2023
(PREGABALIN) Supersede # 00
Page 6 of 20
CAPSULE
REVIEWED BY:
PREPARED BY: APPROVED BY:

QA Officer Sr. Q.C Manager Sr. Q.A Manager Sr. Production Manager GM
Engineering G.M Quality
Operation

Fill E.G. Capsule Capsule Filling

No.3 Fill into Capsule and Sealing
feeder plate Machine

Separate Bodies and Caps through

machine

Capsule Filling
Transfer:
Hopper of Capsule and Sealing
- Xrex blend
filling machine Machine

Filling of Xrex powder into Capsule Filling

bodies of E.G. Capsules. and Sealing
Machine

Sealing of bodies and caps of

filled Capsules. Fill Weight:
195mg /Cap. ± 7.5%

Polishing of filled and sealed Capsule Polishing

capsules Machine

Transfer to PVC Containers and PVC Containers

close tightly.

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 PROCESS VALIDATION REPORT
Document # VP/CAP/PV/024
TITLE: Issue # 01
Effective Date 15-02-2019
XREX 50mg Review Date 15-02-2023
(PREGABALIN) Supersede # 00
Page 7 of 20
CAPSULE
REVIEWED BY:
PREPARED BY: APPROVED BY:

QA Officer Sr. Q.C Manager Sr. Q.A Manager Sr. Production Manager GM
Engineering G.M Quality
Operation

China Blister
Send Sample to Q.C Blistering and Machine,
Packing 2 X 7’S ALU ALU

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 PROCESS VALIDATION REPORT
Document # VP/CAP/PV/024
TITLE: Issue # 01
Effective Date 15-02-2019
XREX 50mg Review Date 15-02-2023
(PREGABALIN) Supersede # 00
Page 8 of 20
CAPSULE
REVIEWED BY:
PREPARED BY: APPROVED BY:

QA Officer Sr. Q.C Manager Sr. Q.A Manager Sr. Production Manager GM
Engineering G.M Quality
Operation

7.2 Manufacturing process

Batch No.1: M001 Mfg. started on: 01-12-2018 Mfg. completed on: 04-12-2018
Batch No 2:M002 Mfg. started on: 01-12-2018 Mfg. completed on: 06-12-2018
Batch No.3:N001 Mfg. started on: 29-01-2019 Mfg. completed on: 01-02-2019

Step #01:
Pass the following materials through Mesh # 16 a mixer and blend for 20 minutes.
Material Quantity
Pregabalin (powdered) 5.00Kg
Lactose 9.50Kg
Maize Starch 2.80Kg

Step #02:
Add the following material through sieve # 40 in mixer and blend for 05 minutes.
Material Quantity
Talcum powder 0.30Kg

Step #03:
Weigh the powder and record net weight of powder and calculate yield.
Batch #. Theoretical yield Actual yield % Yield
M001 19.50Kg 19.45Kg 99.74%
M002 19.50Kg 19.35Kg 99.23%
N001 19.50Kg 19.30Kg 98.97%

Step #04:
Intimate QC to collect blended powder sample for analysis.

Step # 05: Encapsulation

Start filling operation using semi-automatic capsule filling machine as per standard parameters:
Parameters Specifications
Fill weight of powder 195 mg / cap + 7.50 %.
Empty Capsules Size 03
Empty shell w 50
Color of Cap Green

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 PROCESS VALIDATION REPORT
Document # VP/CAP/PV/024
TITLE: Issue # 01
Effective Date 15-02-2019
XREX 50mg Review Date 15-02-2023
(PREGABALIN) Supersede # 00
Page 9 of 20
CAPSULE
REVIEWED BY:
PREPARED BY: APPROVED BY:

QA Officer Sr. Q.C Manager Sr. Q.A Manager Sr. Production Manager GM
Engineering G.M Quality
Operation

Color of body White

Printing on Cap and body None
Wt. of powder to be filled in Capsule 195mg
Wt. of 10 filled capsule (With shell) 2.45g
Av. Wt. of filled capsule (With shell) 245mg
Encapsulation Individual Range 245mg ± 7.50% (226.625–263.375mg)

Step # 06:
Seal the bodies and Caps of Capsules, check the weight of individual Capsules and record in
Capsules filling in-Process sheet.

Step # 07:
After completion of filling operation, transfer filled capsules in polythene lined container, close it
tightly and securely.

Step # 08:
Intimate to Q.C for sampling through intimation form.

Step # 09:
Check and record weight after completion of Encapsulation
Batch #. Theoretical weight Actual weight % Yield
M001 100000 Tablets 23.95Kg/97755 Capsules 97.70%
M002 100000 Tablets 23.70Kg/96734 Capsules 96.73%
N001 100000 Tablets 23.54Kg/96081 Capsules 96.08%

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 PROCESS VALIDATION REPORT
Document # VP/CAP/PV/024
TITLE: Issue # 01
Effective Date 15-02-2019
XREX 50mg Review Date 15-02-2023
(PREGABALIN) Supersede # 00
Page 10 of 20
CAPSULE
REVIEWED BY:
PREPARED BY: APPROVED BY:

QA Officer Sr. Q.C Manager Sr. Q.A Manager Sr. Production Manager GM
Engineering G.M Quality
Operation

8.0 CRITICAL QUALITY ATTRIBUTES

Rationale/
Critical Quality Attribute How Measured
Reference
Before capsule filling

Content : 195mg of powder per capsule As Per STM

Pregabalin(powdered)
Filling process
Weight Variation Fill Weight with shell: 195mg+ shell As Per STM
weight ± 7.5%. Record of in-process
inspection during entire filling
operation.
Filled capsules

Disintegration Time NMT 15 minutes As Per STM

Content of Pregabalin Within specification limit As Per STM

9.0 PROCESS PARAMETERS TO BE QUALIFIED

9.1 Process Parameters
Process Parameter Process Operating How Monitored Rationale/
Range Reference

Pass the following Mixing Time 20 Uniform mixing As per manufacturing

materials through minutes direction
Mesh # 16 in mixer
- PREGABLIN
- LACTOSE
- MAIZE STARCH
Add the following Mixing Time , 5 Uniform mixing As per manufacturing
material through minutes direction
sieve # 40 in mixer
- TALCUM
POWDER

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 PROCESS VALIDATION REPORT
Document # VP/CAP/PV/024
TITLE: Issue # 01
Effective Date 15-02-2019
XREX 50mg Review Date 15-02-2023
(PREGABALIN) Supersede # 00
Page 11 of 20
CAPSULE
REVIEWED BY:
PREPARED BY: APPROVED BY:

QA Officer Sr. Q.C Manager Sr. Q.A Manager Sr. Production Manager GM
Engineering G.M Quality
Operation

Fill E.G Capsules No. Uniform size of body Check Uniform size As per process
3 in the capsule and cap of capsule of body and cap of requirement
feeder plate. Separate capsule
the bodies and caps
through machine.
Transfer Pregabalin Smooth filling of Uniform filling in As per process
powder in hopper and pellets into body of the bodies of E.G requirement
fill uniformly in the capsule. caps
bodies of E.G caps by -Check machine
vibrating the Filling setting
machine. -Check Machine
- Capsule machine speed.
settings - Check feeding
- Machine speed system
(caps/hr)
- Feeding system
Seal the bodies and Proper sealing of Take Sample for As per process
Caps of Capsules, body and cap sealing check requirement
Weight variation
checks - Filling
Operation
Seal the bodies and Weight of Filled Take Sample for fill As per process
Caps of Capsules, Capsule 245mg/ cap weight checks requirement
check the weight of + 7.5%
individual Capsules
and record in
Capsules filling in-
Process sheet.

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 PROCESS VALIDATION REPORT
Document # VP/CAP/PV/024
TITLE: Issue # 01
Effective Date 15-02-2019
XREX 50mg Review Date 15-02-2023
(PREGABALIN) Supersede # 00
Page 12 of 20
CAPSULE
REVIEWED BY:
PREPARED BY: APPROVED BY:

QA Officer Sr. Q.C Manager Sr. Q.A Manager Sr. Production Manager GM
Engineering G.M Quality
Operation

10.0 MANUFACTURING CONDITIONS -REQUIREMENT AND RESULTS

S. No. Section
10.1 Xrex capsules 50 mg – Blend uniformity
 Pregabalin Content
10.2 During filling operation:
 Weight variation during filling operation.
10.3 Disintegration Time
 Disintegration Time of Xrex Capsule
10.4 % Dissolution
 % dissolution of filled capsule
10.5 Content of Pregabalin
 Content of Pregabalin per Capsule.
10.6 Assay
 of filled capsule
10.7 Environmental monitoring – throughout manufacturing process
 To check Temperature and Relative Humidity of the Capsule
Manufacturing and Filling Area.

10.1 Assay of blended powder

Objective:
To verify Content Uniformity of blended powder
Test and sampling plan
Take sample of powder after blending.
Test method
as per test method: HP/QC/SPFG-202.
Acceptance criteria
45.0mg/195mg-55.0mg/195mg, 90%-110% of L.C.
Data

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 PROCESS VALIDATION REPORT
Document # VP/CAP/PV/024
TITLE: Issue # 01
Effective Date 15-02-2019
XREX 50mg Review Date 15-02-2023
(PREGABALIN) Supersede # 00
Page 13 of 20
CAPSULE
REVIEWED BY:
PREPARED BY: APPROVED BY:

QA Officer Sr. Q.C Manager Sr. Q.A Manager Sr. Production Manager GM
Engineering G.M Quality
Operation

Product: Xrex 50mg Capsule

Sr. No. Batch No. Location Assay (%) Acceptance Criteria
51.945mg/195mg Tab,
1 Top
103.89%
50.5490mg/195mg Tab,
2 Middle
101.09%
M001
50.4158mg/195mg Tab,
3 Bottom
100.83%
50.5561mg/195mg Tab,
4 Composite
101.11%
49.5405mg/195mg Tab,
5 Top
99.08%
49.5517mg/195mg Tab, Pregabalin:
6 Middle
99.10% 45.0mg/195mg-
M002
49.5019mg/195mg Tab, 55.0mg/195mg,
7 Bottom
99.00% 90%-110% of L.C.
49.592mg/195mg Tab,
8 Composite
99.18%
9 51.21mg/195mg Tab,
Top
102.43%
10 50.92mg/195mg Tab,
Middle
101.85%
N001
11 51.18mg/195mg Tab,
Bottom
102.13%
12 51.21mg/195mg Tab,
Composite
102.43%
Conclusion Result complies with acceptance criteria.
Performed S.M. Shahid
by
Verified Shakeel Ahmed
by

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 PROCESS VALIDATION REPORT
Document # VP/CAP/PV/024
TITLE: Issue # 01
Effective Date 15-02-2019
XREX 50mg Review Date 15-02-2023
(PREGABALIN) Supersede # 00
Page 14 of 20
CAPSULE
REVIEWED BY:
PREPARED BY: APPROVED BY:

QA Officer Sr. Q.C Manager Sr. Q.A Manager Sr. Production Manager GM
Engineering G.M Quality
Operation

Equipment Calibration
Test Instrument description Instrument ID #. Calibration status
HPLC Q.C.D-033 Calibrated

10.2 Weight variation during filing operation

Objective:
To verify weight variation during filing operation.
Test and sampling plan
Take sample of filled capsule after filing.
Test method
As per test method: HP/QC/SPFG-202.
Acceptance criteria
Parameters Specifications
Theoretical Weight 245mg
Variation from theoretical weight 245mg ± 7.50% (227–263mg)
Data
Product: Xrex 50mg Capsule B#. M001
Sample Weight/ 10 Capsules Individual weight/ Capsule
(g) (mg)
1 2.43 236
2 2.42 244
3 2.50 228
4 2.46 246
5 2.42 240
6 2.43 242
7 2.45 246
8 2.27 232
9 2.51 240
10 2.43 240
Conclusion Result complies with acceptance criteria.
Performed by Mehmeen Maryam/ S.M. Shahid
Verified by Aamir Zaidi/ Shakeel Ahmed
Product: Xrex 50mg Capsule B#. M002
Sample Weight/ 10 Capsules Individual weight/ Capsule

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 PROCESS VALIDATION REPORT
Document # VP/CAP/PV/024
TITLE: Issue # 01
Effective Date 15-02-2019
XREX 50mg Review Date 15-02-2023
(PREGABALIN) Supersede # 00
Page 15 of 20
CAPSULE
REVIEWED BY:
PREPARED BY: APPROVED BY:

QA Officer Sr. Q.C Manager Sr. Q.A Manager Sr. Production Manager GM
Engineering G.M Quality
Operation

(g) (mg)
1 2.45 240
2 2.43 243
3 2.46 243
4 2.47 250
5 2.42 246
6 2.43 243
7 2.45 253
8 2.45 243
9 2.46 245
10 2.40 244
Conclusion Result complies with acceptance criteria.
Performed by Mehmeen Maryam/ S.M. Shahid
Verified by Aamir Zaidi/ Shakeel Ahmed

Product: Xrex 50mg Capsule B#. N001

Sample Weight/ 10 Capsules Individual weight/ Capsule
(g) (mg)
1 2.44 242
2 2.41 249
3 2.39 250
4 2.45 241
5 2.39 244
6 2.41 246
7 2.46 250
8 2.40 243
9 2.47 245
10 2.41 244
Conclusion Result complies with acceptance criteria.
Performed by Mehmeen Maryam/ S.M. Shahid
Verified by Aamir Zaidi/ Shakeel Ahmed
Equipment Calibration
Test Instrument description Instrument ID #. Calibration status
N/A N/A N/A

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 PROCESS VALIDATION REPORT
Document # VP/CAP/PV/024
TITLE: Issue # 01
Effective Date 15-02-2019
XREX 50mg Review Date 15-02-2023
(PREGABALIN) Supersede # 00
Page 16 of 20
CAPSULE
REVIEWED BY:
PREPARED BY: APPROVED BY:

QA Officer Sr. Q.C Manager Sr. Q.A Manager Sr. Production Manager GM
Engineering G.M Quality
Operation

10.3 Disintegration Test: Disintegration Time of coated tablets

Objective:
To verify disintegration time of filled capsule.
Test and sampling plan
Collect 18 filled capsules (composite sample) after completion of filing operation
different location.
Test method
As per test method: HP/QC/SPFG-202.
Acceptance criteria
Disintegration time: NMT 15min.
Data
Product: Xrex 50mg Capsule
Batch #. Disintegration time- Capsule Acceptance criteria
(min)

M001 5
Disintegration time: NMT
M002 5
15min.
N001 5
Conclusion Result complies with acceptance criteria.
Performed by S.M. Shahid
Verified by Shakeel Ahmed

Equipment Calibration
Test Instrument description Instrument ID #. Calibration status
Disintegration test apparatus Q.C.D-029 Calibrated

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 PROCESS VALIDATION REPORT
Document # VP/CAP/PV/024
TITLE: Issue # 01
Effective Date 15-02-2019
XREX 50mg Review Date 15-02-2023
(PREGABALIN) Supersede # 00
Page 17 of 20
CAPSULE
REVIEWED BY:
PREPARED BY: APPROVED BY:

QA Officer Sr. Q.C Manager Sr. Q.A Manager Sr. Production Manager GM
Engineering G.M Quality
Operation

10.4 Dissolution: % dissolution of capsule

Objective:
To verify % dissolution of capsule.
Test and sampling plan
For dissolution, 6 capsules collected.
Test method
As per test method: HP/QC/SPFG-202.
Acceptance criteria
NLT 80% of L.C
Data
Product: Xrex 50mg Capsule
Batch #. % Dissolution Acceptance criteria
M001 100.58%
M002 90.98% NLT 80% of L.C.
N001 91.42%
Conclusion Result complies with acceptance criteria.
Performed by S.M. Shahid
Verified by Shakeel Ahmed

Equipment Calibration
Test Instrument description Instrument ID #. Calibration status
Dissolution apparatus Q.C.D-058 Calibrated

10.5 Content uniformity

Objective:
To verify content uniformity of Pregabalin in filled capsule.
Test and sampling plan
Take samples of filled capsule for content uniformity.
Test method
As per test method: HP/QC/SPFG-202.
Acceptance criteria
L1= NMT 15
Data
Product: Xrex 50mg Capsule

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 PROCESS VALIDATION REPORT
Document # VP/CAP/PV/024
TITLE: Issue # 01
Effective Date 15-02-2019
XREX 50mg Review Date 15-02-2023
(PREGABALIN) Supersede # 00
Page 18 of 20
CAPSULE
REVIEWED BY:
PREPARED BY: APPROVED BY:

QA Officer Sr. Q.C Manager Sr. Q.A Manager Sr. Production Manager GM
Engineering G.M Quality
Operation

Batch #. Assay (Coated tablets) Acceptance criteria

M001 8.96
L1= NMT 15
M002 8.86
N001 6.84
Conclusion Result complies with acceptance criteria.
Performed by S.M. Shahid
Verified by Shakeel Ahmed

Equipment Calibration
Test Instrument description Instrument ID #. Calibration status
HPLC Q.C.D-033 Calibrated

10.6 Assay of Pregabalin in filled capsule (% of L.C. per Cap)

Objective:
To verify Pregabalin in filled capsule.
Test and sampling plan
For Assay, 24 filled capsule (composite sample) collected after completion of filing
from different location.
Test method
As per test method: HP/QC/SPFG-202.
Acceptance criteria
Pregabalin: 45.0mg/tab-55.0mg/tab, 90%-110% of L.C.
Data

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 PROCESS VALIDATION REPORT
Document # VP/CAP/PV/024
TITLE: Issue # 01
Effective Date 15-02-2019
XREX 50mg Review Date 15-02-2023
(PREGABALIN) Supersede # 00
Page 19 of 20
CAPSULE
REVIEWED BY:
PREPARED BY: APPROVED BY:

QA Officer Sr. Q.C Manager Sr. Q.A Manager Sr. Production Manager GM
Engineering G.M Quality
Operation

Product: Xrex 50mg Capsule

Batch #. Assay (Coated tablets) Acceptance criteria
M001 49.042mg/cap, 98.08% Pregabalin:
M002 50.12mg/cap, 100.25% 45.0mg/tab-55.0mg/tab, 90%-
N001 50.68mg/cap, 101.36% 110% of L.C
Conclusion Result complies with acceptance criteria.
Performed by S.M. Shahid
Verified by Shakeel Ahmed

Equipment Calibration
Test Instrument description Instrument ID #. Calibration status
HPLC Q.C.D-033 Calibrated

10.7 Environmental monitoring – throughout manufacturing process To check

Temperature and Relative Humidity of the Capsule Manufacturing and Filling
Area.
Objective:
To check Temperature and Relative Humidity of the Capsule Manufacturing and
Filling Area..
Test and sampling plan
Check temperature and humidity periodically.
Test method
Nil
Acceptance criteria
Temperature: 25°C ± 2°C
Relative humidity: NMT 60%
Data
Product: Xrex 50mg Capsule
Batch #. Result Acceptance criteria
M001 Complies with acceptance criteria
Temperature: 25°C ± 2°C
M002 Complies with acceptance criteria
Relative humidity: NMT 60%
N001 Complies with acceptance criteria
11.0 PACKAGING
11.1 Blistering and packing

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Document # VP/CAP/PV/024
TITLE: Issue # 01
Effective Date 15-02-2019
XREX 50mg Review Date 15-02-2023
(PREGABALIN) Supersede # 00
Page 20 of 20
CAPSULE
REVIEWED BY:
PREPARED BY: APPROVED BY:

QA Officer Sr. Q.C Manager Sr. Q.A Manager Sr. Production Manager GM
Engineering G.M Quality
Operation

Capsules are blistered by using blistering machine in Aluminium Foil Printed Xrex
Capsules 50 mg, 220mm, 20µ, and Cold Forming Printed Aluminium Foil 220mm,
150µ and then packed in printed cartons as 2 x 7’s pack.

Name of Blistering Blister Sealing

Batch #. Equipment No.
Machine Checks
M001 Satisfactory
M002 China Alu Alu Blister - Satisfactory
N001 Machine 3 Satisfactory

12.0 STABILITY DATA

X-rex 50mg capsule B#. M001 kept on on-going stability.

13.0 SUMMARY AND CONCLUSION :

13.1 Process validation of consecutive batches of Xrex 50mg Capsule (B#. M001, M002,
N001), Product Code: CP-HLX-0315 as per concurrent approach.
13.2 All physical and chemical tests were performed and found within specification limit.
13.3 All quality attributes and critical process parameters were found within specified
limits.
13.4 Assay was performed on all batches, as per approved test method and results found
within specified limits.

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