SAMSON LABORATORIES PVT. LTD.

, SANSIWALA

Process Validation Protocol

Protocol No. : PVP/ET132 Process Validation Protocol

For Page 1 of 14
Revision No. : 00 Prednisolone 5mg Tablets BP

PROCESS VALIDATION PROTOCOL

FOR

PREDNISOLONE 5MG TABLETS BP

Generic Name Prednisolone 5 mg Tablets BP

Type of Validation Prospective validation

Standard Batch Size 20,00,000 Tablets

Effective Date

SAMSON LABORATORIES PVT. LTD.

Plot No. 152, Village Sansiwala,
Barotiwala, Tehsil Baddi,
Distt.-Solan, H.P. -174103, India

(SOP/QA/029/F01-01)
 SAMSON LABORATORIES PVT. LTD., SANSIWALA

Process Validation Protocol

Protocol No. : PVP/ET132 Process Validation Protocol

For Page 2 of 14
Revision No. : 00 Prednisolone 5mg Tablets BP

Table of Content

1.0 Protocol Approval............................................................................................................................................3

2.0 Objective:.........................................................................................................................................................4
3.0 Scope:..............................................................................................................................................................4
4.0 Responsibility Of Validation Team...................................................................................................................4
5.0 Validation Criteria............................................................................................................................................4
6.0 References:.....................................................................................................................................................5
7.0 Training:...........................................................................................................................................................5
8.0 Detail of Manufacturer Name OF Active Material To Be Used:.......................................................................6
9.0 Product Profile:................................................................................................................................................6
10.0 Details Of Equipment Used:..........................................................................................................................7
11.0 Weighment Sheet :........................................................................................................................................8
12.0 Manufacturing Process Flow: :......................................................................................................................9
13.0 Sampling Plan:............................................................................................................................................11
14.0 Methodology of Sampling:...........................................................................................................................13
15.0 Sampling Location Of Blender Diagram:.....................................................................................................14
16.0 Validation Report:........................................................................................................................................14
17.0 Stability Study:.............................................................................................................................................14
18.0 Deviation / OOS :.........................................................................................................................................14
19.0 Abbreviations:..............................................................................................................................................15
20.0 Revision History:..........................................................................................................................................15

1.0 Protocol Approval

Prepared by:
Functional Area Name Designation Signature & Date

Quality Assurance

Reviewed by:
Functional Area Name Designation Signature & Date

Quality Assurance

(SOP/QA/029/F01-01)
 SAMSON LABORATORIES PVT. LTD., SANSIWALA

Process Validation Protocol

Protocol No. : PVP/ET132 Process Validation Protocol

For Page 3 of 14
Revision No. : 00 Prednisolone 5mg Tablets BP

Head Production

Head Quality Control

Head Engineering

Approved by:
Functional Area Name Designation Signature & Date

Head QA

Plant Head

2.0 OBJECTIVE:
The objective of this protocol is to validate the manufacturing process or to collect sufficient data to
establish that the proposed manufacturing process for Prednisolone 5mg Tablets BP using qualified
equipment and utilities by studying three consecutive batches consistently produces the product of its
predetermined quality parameters.

3.0 Scope:
This protocol is based on SOP No. SOP/QA/029 and the scope of this process validation is limited to
validate the manufacturing process of Prednisolone 5mg Tablets BP

4.0 Responsibility Of Validation Team

Departments Responsibilities

Preparation of Process Validation Protocol.

Co-ordination with Production and QC to carryout Process Validation.

Monitoring and sampling at the different stages of Manufacturing as per

QA
Process Validation Protocol.

Preparation of a Summary Report on Process Validation Batch (s).

To impart training of protocol to concerned department/persons.

(SOP/QA/029/F01-01)
 SAMSON LABORATORIES PVT. LTD., SANSIWALA

Process Validation Protocol

Protocol No. : PVP/ET132 Process Validation Protocol

For Page 4 of 14
Revision No. : 00 Prednisolone 5mg Tablets BP

Review of protocol, testing of samples, recording of results and final

Quality Control
result submission.
Review of protocol, operation of equipments and manufacture as per the
Production
batch manufacturing record and packing as per batch packing record.

Head QA Approval of Process Validation Protocol.

Plant Head Approval of Process Validation Protocol.

5.0 VALIDATION CRITERIA

First Validation

6.0 REFERENCES:
The following document has been referred to prepare the process validation protocol:

Sr. No. Title of Document *Document No.

1. Master Formula Record MFR/ET132-01

2. Batch Manufacturing Record No. BMR/ET132-01

3. Batch Packing Record No. BMR/ET132-01

4. Finished Product Specification FPT/ET132-01

* All approved current version of relevant document(s) must be referred.

7.0 Training:
Training to be provided to all concern person and record shall be attached in report.

(SOP/QA/029/F01-01)
 SAMSON LABORATORIES PVT. LTD., SANSIWALA

Process Validation Protocol

Protocol No. : PVP/ET132 Process Validation Protocol

For Page 5 of 14
Revision No. : 00 Prednisolone 5mg Tablets BP

8.0 Detail of Manufacturer Name of Active Material to be used:

Sr. No. Ingredient Approved Manufacturer Name

Tianjin Tianyao Pharmaceuticals

1. Prednisolone BP
Henan Lihua Pharmaceuticals

9.0 Product Profile:

Product Name Prednisolone 5mg Tablets BP

Generic name Prednisolone 5mg Tablets BP
Product Code ET132
Active Ingredient Prednisolone
Batch Size 20,00,000 Tablets.
Dosages form Oral Solid Dosage Form (Tablets)
Each Uncoated tablet contains:

Label Claim Prednisolone BP 5mg.

Excipients q.s.
Round shaped, White coloured, Biconvex, Uncoated tablet, having
Product Description
break line on one side and other side plain

Theoretical Tablet weight 200 ± 5%

(SOP/QA/029/F01-01)
 SAMSON LABORATORIES PVT. LTD., SANSIWALA

Process Validation Protocol

Protocol No. : PVP/ET132 Process Validation Protocol

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Revision No. : 00 Prednisolone 5mg Tablets BP

Product Name Prednisolone 5mg Tablets BP

Dimensions and Shape Round shaped,

Punch Tooling Details Upper Punch 8.0 mm ± 0.2

Lower Punch 8.0 mm ± 0.2

10.0 Details of Equipment used:

Sr. Equipment Ref. Operation &

Equipment Name Capacity Make
No. ID No. Cleaning SOP No.
Dispensing Area:
1. RLAF Dispensing - SL/WH/EQP/002 Multi tech SOP/WH/040

2. RLAF Dispensing - SL/WH/EQP/003 Multi tech SOP/WH/040

Granulation Area:
3. Sifter - SL/TB/EQP/075 Amar Engg. SL/PD/001

4. Blender 1200 lit. SL/TB/EQP/006 Brilliant Pharma SL/PD/008

Compression Area:
SL/TB/EQP/023
5. Compression Machine 75,000/hr. Fluid Pack SL/PD/011
SL/TB/EQP/016
SL/TB/EQP/027
6. Dedusting Machine 1.00 Lac/hr Fluid Pack SL/PD/013
SL/TB/EQP/025
7. Metal Detectors - SL/TB/EQP/070 Unique SOP/PR/036
Inspection Area:
8. Inspection belt - SL/TB/EQP/069 Unique SL/PD/055
Packing Area
9. Blister Machine 6.0 lac/8hr. SL/TB/EQP/048 Rapid Pack SL/PD/018

(SOP/QA/029/F01-01)
 SAMSON LABORATORIES PVT. LTD., SANSIWALA

Process Validation Protocol

Protocol No. : PVP/ET132 Process Validation Protocol

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Revision No. : 00 Prednisolone 5mg Tablets BP

Sr. Equipment Ref. Operation &

Equipment Name Capacity Make
No. ID No. Cleaning SOP No.

10. Leak test Apparatus - SL/QA/INS/003 Lt -101 P SL/PD/021

11.0 Weighment Sheet :

Sr. No. Raw Materials Qty. /Tablet in mg Qty Per 20.0 Lac.(kg)

1. Prednisolone BP 5.1 10.200

2. Colloidal Silicon Dioxide BP 3 6.000

3. Lactose BP (Super 200 Mesh) 24.99 49.980

4. Microcrystalline Cellulose BP (PH102) 142.91 285.820

5. Sodium Starch Glycolate BP (Type A) 5 10.000

6. Talcum BP 2 4.000

7. Magnesium Stearate BP 2 4.000

8. Sodium Lauryl Sulphate BP 1.5 3.000

9. Kyron-T 314/Tulsion 671 2.5 5.000

10. Crospovidone -XL 10 BP 7 14.000

11. Croscarmellose sodium BP 4 8.000

(SOP/QA/029/F01-01)
 SAMSON LABORATORIES PVT. LTD., SANSIWALA

Process Validation Protocol

Protocol No. : PVP/ET132 Process Validation Protocol

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Revision No. : 00 Prednisolone 5mg Tablets BP

12.0 Manufacturing Process Flow: With critical control point:

Critical Control Parameter Critical quality attributes (CQA)/

Stage Equipment Use/Process
(CCP) Check Point

Dispensing of Dispensing of Raw Material Calibrated weighing balance  AR Nos. of material

Material  Weight of dispensed
material
 Manufacturer Name

Vibro-sifter
Sifting  Sift the dispensed matirial  Sieve Size  Sieve Integrity (Before &
After)

Blender Bin
Blending  Mixing Time  Blend uniformity
 Load the sifted material in Blender
for 25 minutes

 Blend uniformity
 Assay
Blender Bin  Bulk density
Lubrication  Add sifted Magnesium stearate  Mixing Time
 Tapped density
blended material and mix for 5  Compresibility index
minutes

(SOP/QA/029/F01-01)
 SAMSON LABORATORIES PVT. LTD., SANSIWALA

Process Validation Protocol

Protocol No. : PVP/ET132 Process Validation Protocol

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Revision No. : 00 Prednisolone 5mg Tablets BP

Stage Critical Control Parameter Critical quality attributes (CQA)/

Equipment Use/Process
(CCP) Check Point

 Description,
Compression Process  Average weight
 weight of 20 tablets,
Compression Process  Load the blend into the hopper of the  Machine Speed  Thickness
tablet compression machine and
 Hardness
compressed into tablets by using punch
 Friability
 Assay
 Dissolution
 CU

Tablet Inspection Tablet Inspection belt Visual verification

process

 Machine speed  Appearance of blister

Blister Packing Machine  Leak test
 Forming temperature
Packing  Tablet are packed into blister using  Sealing Temperature  Cut –pockets
blister packing machine  Missing Tablets

(SOP/QA/029/F01-01)
 SAMSON LABORATORIES PVT. LTD., SANSIWALA

Process Validation Protocol

Protocol No. : PVP/ET132 Process Validation Protocol

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Revision No. : 00 Prednisolone 5mg Tablets BP
13.0 Sampling Plan:

Manufacturing Brief detail of Sampling Procedure, Location, Time &

Test Parameter Acceptance criteria
Stage Manufacturing Process Quantity
Dispensing as per approved
Dispensing Dispensing of material -------------- --------------
BMR
 Process monitoring as
Sifting of material as Not applicable
per approved BMR
Sifting defined in BMR and record  Material passing (Visual check during the
 All material should pass
the observation in BMR process)
through the desire sieve

 Sample size: Collect 10 samples in

Triplicate with a unit dose sampler
 Qty 3x : X = avg. weight
 Sampling Time: After 25 minutes of mixing  All ingredient should mix
Load the sifted material
 Theoretical Quantity of blend is 198 mg: properly
Blending load in blender bin and
record the observation in Actual Sampled quantity should be  Blend uniformity  Individual value should be
between 198 mg to 596 mg per location. NMT ± 10 of the absolute
BMR
 Device : Sampling thief mean
 Sampling point: 10 location from as per
pictorial diagram

 Sample size: Collect 10 samples in

Triplicate with a unit dose sampler.
 Sampling Time: After 5 minutes of mixing
Add the lubricant in  Theoretical Quantity of blend is 200 mg:  Individual value should
Lubrication blended material and mix Actual Sampled quantity should be  Blend uniformity be NMT ± 10 of the
as per BMR ad record the between 200 mg to 600 mg per location. absolute mean
observation in BMR
 Device : Sampling thief
 Sampling point: 10 location from as per
pictorial diagram

(SOP/QA/029/F01-01)
 SAMSON LABORATORIES PVT. LTD., SANSIWALA

Process Validation Protocol

Protocol No. : PVP/ET132 Process Validation Protocol

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Revision No. : 00 Prednisolone 5mg Tablets BP

Manufacturing Brief detail of Sampling Procedure, Location, Time &

Test Parameter Acceptance criteria
Stage Manufacturing Process Quantity
 Assay  95.0- 110%
 Bulk density  Informative
 Composite sample : 50 g  Tapped density  Informative
 Compresibility index  Informative
 Water content  Informative
 Speed Challenge study:
 Appearance  Round shaped, White
 Sampling plan: Start the machine as per coloured, Biconvex,
Uncoated tablet, having
BMR and perform the initial checks as per
break line on one side
BMR. After the initial checks are found and other side plain.
satisfactory perform the machine speed  200 ± 5% (190mg to
 Average weight 210mg )
 Set the machine as per challenge test study at three different
machine speeds and run the machine  Weight of 20 tablets  4.00 ± 5 % ( 3.80gm to
Compression BMR and start the 4.20gm )
compression process about 5-10 minute for at each speed
 3.5 mm ± 0.3 ( 3.20 mm
challenge and at the end of compression  Thickness to 3.80 mm)
run collect sample for checking of Physical  NLT 3 kg/cm2
 Hardness
and chemical parameter  NMT 1 % w/w
 Friability
 ± 5 % of average weight
 Sample Quantity: 150tablets after each  Uniformity of weight
 DT  NMT15 min.
run.

 Composite sample:  As per finished product  As per finished product

specification specification
 Mix of initial, middle, end of Compression
 Water content  Informative

(SOP/QA/029/F01-01)
 SAMSON LABORATORIES PVT. LTD., SANSIWALA

Process Validation Protocol

Protocol No. : PVP/ET132 Process Validation Protocol

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Revision No. : 00 Prednisolone 5mg Tablets BP

Manufacturing Brief detail of Sampling Procedure, Location, Time &

Test Parameter Acceptance criteria
Stage Manufacturing Process Quantity
 Composite sample: 150 tablet
Sampling Plan: When initial check is  Appearance  Should be ok
 Start the machine as completed successfully collect the sample at
 Pocket formation  Proper packet formation
per SOP, perform the following condition.
 Blister cutting  Cutting should be proper
initial checks. After the
 Minimum machine speed and maximum
initial checks are forming & sealing temperature  Leak test  No pocket should fail in
Primary Packing leak test
 High machine speed and minimum forming
satisfactory perform the
& sealing temperature
packing validation  Sample Qty.: Nos. of blister per cut
equivalent to 26 Blister
Compete testing as per Finish product  As per Finished  To comply with Finished
specification (Release) Product specification Product specification

14.0 Methodology of Sampling:

Follow the current version of Batch manufacturing record and Batch packing record during the manufacturing and packing process

(SOP/QA/029/F01-01)
 SAMSON LABORATORIES PVT. LTD., SANSIWALA

Process Validation Protocol

Protocol No. : PVP/ET132 Process Validation Protocol

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Revision No. : 00 Prednisolone 5mg Tablets

15.0 Sampling Location of Blender Diagram:

S1 S2
Top
S3 S4

S5

Middle
S8 S9 S6
S7

S10 Bottom

Where:
L1= Top Left L4= Top Center L7= Top Right

L2= Middle Left L5= Middle Center L8= Middle Right

L3= Bottom Left L6= Bottom Center L9= Bottom Right

L10= Discharge Point

16.0 Validation Report:

A validation report shall be prepared after completion of three consecutive batches, mentioning
recommendations (if any) and conclusions of the Process validation study. Final Validation report will
comprise of following documents.

 Test data slip (In process and Analytical).

 Copy of finished product COA

17.0 Stability Study:

For stability study separate protocol is generated. The stability study of the validation batches shall be
conducted as per stability protocol.

18.0 DEVIATION / OOS (if any):

(SOP/QA/029/F01-01)
 SAMSON LABORATORIES PVT. LTD., SANSIWALA

Process Validation Protocol

Protocol No. :PVP/ET132 Process Validation Protocol

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Revision No. : 00 Prednisolone 5mg Tablets
Any deviations, OOS or changes that may occur during the process, shall be investigated and to be
addressed in the report.

19.0 ABBREVIATIONS:

Abbreviation Full Form

BMR Batch Manufacturing Record

mg Milligram

mm Millimeter

NLT/NMT Not less than/Not More than

QA Quality Assurance

QC Quality control

Qty. Quantity

Ref. No. Reference Number

RM Raw Material

rpm Revolution per minute

SOP Standard Operating Procedure

Sr. No. Serial Number

20.0 Revision History:

Revision No. Details of Changes Reason for change

00 Nil Introduction of New Document

(SOP/QA/029/F01-01)