PVP - Prednisolone BP 5 MG

SAMSON LABORATORIES PVT. LTD.
, SANSIWALA
Process Validation Protocol
Protocol No. : PVP/ET132 Process Validation Protocol

For Page 1 of 17
Revision No. : 00 Metformin Hydrochloride Tablets 1000mg BP
PROCESS VALIDATION PROTOCOL
FOR
Metformin Hydrochloride Tablets 1000mg BP
Generic Name Metformin Hydrochloride Tablets 1000mg BP
Type of Validation Prospective validation
Standard Batch Size 6,00,000 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

For Page 2 of 17
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:
Quality Assurance
(SOP/QA/029/F01-01)

For Page 3 of 17
Head Production
Head Quality Control
Head Engineering
Approved by:
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 Metformin Hydrochloride Tablets 1000mg 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 Metformin Hydrochloride Tablets 1000mg 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)

For Page 4 of 17
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)

For Page 5 of 17
8.0 Detail of Manufacturer Name of Active Material to be used:
Sr. No. Ingredient Approved Manufacturer Name
1. Metformin Hydrochloride BP
9.0 Product Profile:
Product Name Metformin Hydrochloride Tablets 1000mg BP

Generic name Metformin Hydrochloride Tablets 1000mg BP
Product Code ET404
Active Ingredient Metformin Hydrochloride
Batch Size 6,00,000 Tablets.
Dosages form Oral Solid Dosage Form (Tablets)
Each Film coated tablet contains:

Metformin Hydrochloride BP 1000mg
Label Claim (As sustained release form)
Excipients q.s.
Colour: Titanium Dioxide
(SOP/QA/029/F01-01)

For Page 6 of 17
Product Name Metformin Hydrochloride Tablets 1000mg BP

White Colour Capsule shaped, biconvex,uncoated tablet,having
Product Description
central break line on one side and other side plain.
Theoretical Tablet weight 1183 ± 5%
Dimensions and Shape Elongated Shaped
Punch Tooling Details Upper Punch 19.5 x 10.00mm
Lower Punch 19.5 x 10.00mm
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
(SOP/QA/029/F01-01)

For Page 7 of 17
Sr. Equipment Ref. Operation &

Equipment Name Capacity Make
No. ID No. Cleaning SOP No.
9. Blister Machine 6.0 lac/8hr. SL/TB/EQP/048 Rapid Pack SL/PD/018
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 6,00,000 Lac.(kg)
1. Metformin Hydrochloride BP
2. Maize Starch BP
3. Sodium Starch Glycolate BP
4. Maize Starch BP
5. Povidone k -30 BP
6. Maize Starch BP
7. Povidone k -30 BP
8. Purified Talcum BP
9. Magnesium Stereate BP
10. Croscarmellose sodium BP
11. Colloidal anhydrous Silica BP
12. Film coating material
13. Titanium Dioxide BP
14. PEG-6000 BP
15. Hydroxy Propyl Methyl Cellulose (E15)
(SOP/QA/029/F01-01)

For Page 8 of 17
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
& Mix for 25 minutes
 Blend uniformity
 Assay
Blender Bin  Bulk density
Lubrication  Add sifted Magnesium stearate in  Mixing Time
 Tapped density
blended material and mix for 5  Compresibility index
minutes
(SOP/QA/029/F01-01)

For Page 9 of 17
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
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)

For Page 10 of 17
13.0 Sampling Plan:
Manufacturin Brief detail of

Sampling Procedure, Location, Time & Quantity Test Parameter Acceptance criteria
g Stage Manufacturing Process
Dispensing as per approved
Dispensing Dispensing of material -------------- --------------
BMR
Sifting of material as  Process monitoring as
Not applicable
defined in BMR and per approved BMR
Sifting  Material passing (Visual check during the
record the observation in  All material should pass
process)
BMR 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: Actual properly
Blending load in blender bin and
record the observation in Sampled quantity should be between 198 mg to 596  Blend uniformity  Individual value should
BMR mg per location. be NMT ± 10 of the
 Device : Sampling thief absolute mean
 Sampling point: 10 location from as per pictorial
diagram
 Sample size: Collect 10 samples in Triplicate with a
unit dose sampler.
Add the lubricant in  Sampling Time: After 5 minutes of mixing
blended material and  Theoretical Quantity of blend is 200 mg: Actual  Individual value should
Lubrication mix as per BMR ad Sampled quantity should be between 200 mg to 600  Blend uniformity be NMT ± 10 of the
record the observation in mg per location. absolute mean
BMR  Device : Sampling thief
 Sampling point: 10 location from as per pictorial
diagram
(SOP/QA/029/F01-01)

For Page 11 of 17

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

For Page 12 of 17

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

For Page 13 of 17
(SOP/QA/029/F01-01)

For Page 14 of 17
15.0 Physical Process Parameter at Compression Stage:

Uniformity of weight : ± 4 % of average weight
Low Speed Optimum Speed High Speed
Date: ……………….. Date: ……………….. Date: ………………..
Sr. No.
Machine RPM : ………… Machine RPM : ………… Machine RPM : …………
LHS RHS LHS RHS LHS RHS
1.
2.
3.
4.
5.
6.
7.
8.
9.
10.
11.
12.
13.
14.
15.
16.
17.
18.
19.
20.
Average weight
(mg)
Observed Min.
Weight
(mg) Max.
DT.
Sign. /Date By
QA

For Page 15 of 17
Thickness:
Locat Thickness (mm) : 3.8 ± 0.3 (3.5mm to 4.1mm) Checked By

ion Q.A.
1 2 3 4 5 6 7 8 9 10
Low Speed LHS
RHS
Optimum LHS
Speed
RHS
High Speed LHS
RHS
Inprocess Sheet
Hardness
Locat Resistance to Crushing : NLT 4 kg/cm2 Checked By
ion 1 2 3 4 5 6 7 8 9 10 Prod/Q.A.
Low Speed LHS
RHS
Optimum LHS
Speed
RHS
High Speed LHS
RHS
Inprocess Sheet
Friability: (NMT 1 % w/w):
LHS RHS
Wt. of 24 Wt. of 24 Wt. of 24 Wt. of 24 Checked
Calculation Calculation
Tabs Tabs Tabs Tabs
Date Time (A-B) x 100 (A-B) x 100 By
before After before After
=-------------- =-------------- Prod/Q.A.
Test (A) Test (B) Test (A) Test (B)
(A) (%w/w) (A) (%w/w)
(g) (g) (g) (g)
Low Speed
Optimum
Speed
High Speed

For Page 16 of 17
Revision No. : 00 Prednisolone 5mg Tablets
16.0 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
17.0 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
18.0 Stability Study:

For stability study separate protocol is generated. The stability study of the validation batches shall be
conducted as per stability protocol.
19.0 DEVIATION / OOS (if any):

Protocol No. :PVP/ET132 Process Validation Protocol

For Page 17 of 17
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.
20.0 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
21.0 Revision History:
Revision No. Details of Changes Reason for change

00 Nil Introduction of New Document

PVP - Prednisolone BP 5 MG

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SAMSON LABORATORIES PVT. LTD.

Process Validation Protocol

Protocol No. : PVP/ET132 Process Validation Protocol

PROCESS VALIDATION PROTOCOL

Metformin Hydrochloride Tablets 1000mg BP

Generic Name Metformin Hydrochloride Tablets 1000mg BP

Type of Validation Prospective validation

Standard Batch Size 6,00,000 Tablets

SAMSON LABORATORIES PVT. LTD.

Process Validation Protocol

Protocol No. : PVP/ET132 Process Validation Protocol

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

1.0 Protocol Approval

Process Validation Protocol

Protocol No. : PVP/ET132 Process Validation Protocol

Head Quality Control

4.0 Responsibility Of Validation Team

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

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

To impart training of protocol to concerned department/persons.

Process Validation Protocol

Protocol No. : PVP/ET132 Process Validation Protocol

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

Head QA Approval of Process Validation Protocol.

Plant Head Approval of Process Validation Protocol.

5.0 VALIDATION CRITERIA

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

Process Validation Protocol

Protocol No. : PVP/ET132 Process Validation Protocol

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

Sr. No. Ingredient Approved Manufacturer Name

9.0 Product Profile:

Product Name Metformin Hydrochloride Tablets 1000mg BP

Each Film coated tablet contains:

Process Validation Protocol

Protocol No. : PVP/ET132 Process Validation Protocol

Product Name Metformin Hydrochloride Tablets 1000mg BP

Theoretical Tablet weight 1183 ± 5%

Dimensions and Shape Elongated Shaped

Punch Tooling Details Upper Punch 19.5 x 10.00mm

Lower Punch 19.5 x 10.00mm

10.0 Details of Equipment used:

Sr. Equipment Ref. Operation &

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

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

Process Validation Protocol

Protocol No. : PVP/ET132 Process Validation Protocol

Sr. Equipment Ref. Operation &

9. Blister Machine 6.0 lac/8hr. SL/TB/EQP/048 Rapid Pack SL/PD/018

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

11.0 Weighment Sheet :

3. Sodium Starch Glycolate BP

10. Croscarmellose sodium BP

11. Colloidal anhydrous Silica BP

12. Film coating material

13. Titanium Dioxide BP

15. Hydroxy Propyl Methyl Cellulose (E15)