xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx

QUALITY ASSURANCE

PROCESS VALIDATION PROTOCOL FOR TABLETS

Protocol No. : xxxxxxxxxxxxxxxxxRev. :00Supersedes: NILProtocol prepared on: xxxxxxxxxxEffective Date: xxxxxxxxxxxxxPage 1 of 38

PROCESSVALIDATION

PROTOCOL FOR TABLETS

Protocol No. : xxxxxxxx

Effective Date. : xxxxxxxxxxxx

Prepared By Reviewed by Approved by

Designation QA chemist Production Manager Manager QC&A Plant headDateFormat No.: xxxxxxxxxxxxxx

xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx

QUALITY ASSURANCE

PROCESS VALIDATION PROTOCOL FOR TABLETS

Protocol No. : xxxxxxxxxxxxxxxxxRev. :00Supersedes: NILProtocol prepared on: xxxxxxxxxxEffective Date: xxxxxxxxxxxxxPage 2 of 38

TABLE OF CONTENTS

S.NO. SECTION Page No

1. Protocol approval

2. Purpose

3. Responsibilities

4. Requirements

5. Personnel Responsibilities

6. Validation parameters

7. Limits

8. Conclusion report

Prepared By Reviewed by Approved by

Designation QA chemist Production Manager Manager QC&A Plant headDateFormat No.: xxxxxxxxxxxxxx

xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx

QUALITY ASSURANCE

PROCESS VALIDATION PROTOCOL FOR TABLETS

Protocol No. : xxxxxxxxxxxxxxxxxRev. :00Supersedes: NILProtocol prepared on: xxxxxxxxxxEffective Date: xxxxxxxxxxxxxPage 3 of 38

1. PROTOCOL APPROVAL

This document is prepared by the validation and the GMP compliance (QA) team of xxxxxxxxxxxxxxxxx under the authority of Manager QC & A. Hence this document before being effective shall be approved by xxxxxxxxxxxxxxx QA team.

Name Signature Date

Manager production

Manager Engineering

Manager QA

Prepared By Reviewed by Approved by

Designation QA chemist Production Manager Manager QC&A Plant headDateFormat No.: xxxxxxxxxxxxxx

xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx

QUALITY ASSURANCE

PROCESS VALIDATION PROTOCOL FOR TABLETS

Protocol No. : xxxxxxxxxxxxxxxxxRev. :00Supersedes: NILProtocol prepared on: xxxxxxxxxxEffective Date: xxxxxxxxxxxxxPage 4 of 38

2. PURPOSEProcess validation is establishing documented evidence which provides a high degree of assurance that a specific process (such as manufacturer of pharmaceutical dosages forms) will consistently produce a product meeting its predetermined specifications and quantity characteristics.

3. RESPONSIBILITIES

S.NO. Activity Responsibility

1. Preparation of protocol QA chemist

2. Chemical analysis and sampling QC chemist

3. Microbial analysis & sampling Microbiologist

4. Preparation of validation Report Dy Manager QC

5. Review of validation protocol & report QA department, Production Department

6. Approval of protocol & Report Plant Head

4. REQUIRMENTS: NIL

5. PERSONNEL RESPONSIBILITIES:The perfect validation program necessitates various departments involvement mainly to balance the total system functioning for its effective utilization for success criteria compliance on regular basis. Quality assurance department initiates validation program with protocol, specified procedure and success criteria. Quality control personnel are responsible for the validation run as per the protocol and during validation maintenance departments have to cooperate to the quality control personnel.

6. VALIDATION PARAMETERS:Prepared By Reviewed by Approved by

Designation QA chemist Production Manager Manager QC&A Plant headDateFormat No.: xxxxxxxxxxxxxx

xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx

QUALITY ASSURANCE

PROCESS VALIDATION PROTOCOL FOR TABLETS

Protocol No. : xxxxxxxxxxxxxxxxxRev. :00Supersedes: NILProtocol prepared on: xxxxxxxxxxEffective Date: xxxxxxxxxxxxxPage 5 of 38

Process Description / Flow Sheet

The information given below provides a general description of the process. Detailed information for the manufacturing will be supplied separately in the Batch Processing Record. 1 Prepare production order and according to that issue the BPR

2 RM dispensing as per Bill of material 3 Input check in presence of QA person

4 Granulation 4.1 Sifting

4.2 Pre–mixing 4.3. (a) Wet granulation Binder Preparation Mixing Wet milling Drying Dry milling Slugging, Milling (if required) Lubrication 4.3 (b) Dry Granulation Mixing Slugging, Milling (if required) Lubrication 5 Tablet compression 6 Tablet coating 7 Tablet packing

Formulation:

Batch Size:

Sr No Prepared By Reviewed by Approved by

Designation QA chemist Production Manager Manager QC&A Plant headDateFormat No.: xxxxxxxxxxxxxx

xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx

QUALITY ASSURANCE

PROCESS VALIDATION PROTOCOL FOR TABLETS

Protocol No. : xxxxxxxxxxxxxxxxxRev. :00Supersedes: NILProtocol prepared on: xxxxxxxxxxEffective Date: xxxxxxxxxxxxxPage 6 of 38

Ingredients/Excipients Unit per Tablet

Std. Qty.

Overages DispensedQuantity

Weight by

Checked by

1

2

3

4

5

6

7

8

9

10

11

12

13

14

15

16

FLOW SHEET: Prepare production order and according RM dispensing as per Bill of material to that issue the BPR

Prepared By Reviewed by Approved by

Designation QA chemist Production Manager Manager QC&A Plant headDateFormat No.: xxxxxxxxxxxxxx

xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx

QUALITY ASSURANCE

PROCESS VALIDATION PROTOCOL FOR TABLETS

Protocol No. : xxxxxxxxxxxxxxxxxRev. :00Supersedes: NILProtocol prepared on: xxxxxxxxxxEffective Date: xxxxxxxxxxxxxPage 7 of 38

Input check in presence of QA person GRANULATIONShifting

Dry Granulation Premixing

Mixing Binder preparation Wet Granulation milling Drying Dry milling Slugging, Milling (if required)

Mixing

Coating Compression Lubrication

(Blending)

Tablet packing

Sampling point

Typical Variables and responses: Granulated ProductS. No. Process step Control variables Measured responses

1. Pre-blending Blending time RPMLoad size Order of addition

Blend uniformity

2. Granulating Load sizeAmount of granulating agent

DensityYield

Prepared By Reviewed by Approved by

Designation QA chemist Production Manager Manager QC&A Plant headDateFormat No.: xxxxxxxxxxxxxx

xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx

QUALITY ASSURANCE

PROCESS VALIDATION PROTOCOL FOR TABLETS

Protocol No. : xxxxxxxxxxxxxxxxxRev. :00Supersedes: NILProtocol prepared on: xxxxxxxxxxEffective Date: xxxxxxxxxxxxxPage 8 of 38

Solvent addition rateRPMGranulation time

3. Drying Initial temperatureLoad sizeDrying temperature programAir flow programDrying timeCooling time

DensityMoisture contentYield

4. Sizing Screen typeScreen size Feed rate

Granule size distributionLoose dryingPacked density

5. Blending Load sizeRPMBlending time

Blend uniformityFlow characteristics Particle size distribution

6. Tableting Compression rateGranule feed ratePre-compression forceCompression force

Weight variation FriabilityHardness Thickness Disintegration timeDissolutionDosage from uniformity

Equipments

A detailed list of equipment used for validation together with the cleaning status will be provided in the manufacturing documents.

List of SOP’S, Validation & Qualification report used as references

Sr. No. Name of Equipment Equipment ID. Qualification details SOP No1

2

3

Prepared By Reviewed by Approved by

Designation QA chemist Production Manager Manager QC&A Plant headDateFormat No.: xxxxxxxxxxxxxx

xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx

QUALITY ASSURANCE

PROCESS VALIDATION PROTOCOL FOR TABLETS

Protocol No. : xxxxxxxxxxxxxxxxxRev. :00Supersedes: NILProtocol prepared on: xxxxxxxxxxEffective Date: xxxxxxxxxxxxxPage 9 of 38

4

5

6

7

8

9

10

11

12

Critical Process Parameters:Critical stages: Following critical stages required to be validated to provide a high degree of assurance

for the manufacturing of tablets.

Sr. No. STAGE Parameters1. Premixing RPM of mixer blade

Load size

Total time of mixing

Uniform mixing by Assay analysis

2. Granulation Mixer blade speed

Load size

Binder QuantityPrepared By Reviewed by Approved by

Designation QA chemist Production Manager Manager QC&A Plant headDateFormat No.: xxxxxxxxxxxxxx

xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx

QUALITY ASSURANCE

PROCESS VALIDATION PROTOCOL FOR TABLETS

Protocol No. : xxxxxxxxxxxxxxxxxRev. :00Supersedes: NILProtocol prepared on: xxxxxxxxxxEffective Date: xxxxxxxxxxxxxPage 10 of 38

Binder addition rate

Binder addition time

Temperature of binder

Mixing time after binder addition /Total granulation time

Uniformity of granulated mass (Visual Checking)

3. Drying Dryer outlet temperature

Dryer inlet temperature

Drying load

Total drying time

Weight of the Dried granules

4. Milling Speed of machine

Direction of knives

5. Lubrication Load size

Occupancy

Speed of equipment (RPM)

Total time of mixing

Assay - (individual sample)

6. Compression Temperature of area

Humidity of area

Machine Details

Weight variation of 20 tablets

Average weight of tablet

Disintegration time

FriabilityPrepared By Reviewed by Approved by

Designation QA chemist Production Manager Manager QC&A Plant headDateFormat No.: xxxxxxxxxxxxxx

xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx

QUALITY ASSURANCE

PROCESS VALIDATION PROTOCOL FOR TABLETS

Protocol No. : xxxxxxxxxxxxxxxxxRev. :00Supersedes: NILProtocol prepared on: xxxxxxxxxxEffective Date: xxxxxxxxxxxxxPage 11 of 38

Diameter (Length)

Thickness

Hardness

Assay

Content uniformity

Dissolution

7. Coating Temperature of area

Temperature of blower

Speed of Coating Pan (RPM)

Spray Rate

Bed Temperature

Air Pressure

Total Coating solution used

Weight Built up

Weight variation of 20 tablets

Assay

Disintegration time

Dissolution

8. Packaging Forming roller temperature. (for Blister Packing)

Sealing roller temperature

Sealing roller Pressure

Speed of machine

Seal integrity

AssayPrepared By Reviewed by Approved by

Designation QA chemist Production Manager Manager QC&A Plant headDateFormat No.: xxxxxxxxxxxxxx

xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx

QUALITY ASSURANCE

PROCESS VALIDATION PROTOCOL FOR TABLETS

Protocol No. : xxxxxxxxxxxxxxxxxRev. :00Supersedes: NILProtocol prepared on: xxxxxxxxxxEffective Date: xxxxxxxxxxxxxPage 12 of 38

Dissolution

9. Packaging (bulk packing)

Sealing temperature

Seal integrity

Counter Checking from 10 Jars at different Time intervals

Sr. No Process / Variable Machine setting( Control Variables) Remarks

1

Blend ManufacturingSifting Visually Inspection No visible foreign particulate

matter is observedPremixing Stage

Uniform mixing by Assay analysis Variation between the results shall not be more than 2%

2 Granulation

Prepared By Reviewed by Approved by

Designation QA chemist Production Manager Manager QC&A Plant headDateFormat No.: xxxxxxxxxxxxxx

xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx

QUALITY ASSURANCE

PROCESS VALIDATION PROTOCOL FOR TABLETS

Protocol No. : xxxxxxxxxxxxxxxxxRev. :00Supersedes: NILProtocol prepared on: xxxxxxxxxxEffective Date: xxxxxxxxxxxxxPage 13 of 38

Binder PreparationGranulation Finely divided material without free

powder and excessive wetted lumps.Wet milling Material was finely dividedDrying Loss on drying Between 2.0 to 5.0%Dry milling Finely divided granules are observedLubrication Assay and Sieve analysis Variation between the results

shall not be more than 2%

3 Tablet compression Physical ParameterWt. Variation, Hardness, Thickness, DT, Dissolution and Assay

4 Tablet coating Weight gain, weight variation and DT

5 Tablet packing Leak Test

PREMIXING:

Sampling Qty.: -Depends on quantity required for analysis.

Sampling Time: - (bracketing the time between 2 to 3 intervals of total mixing time)

While mixing is on: -

After ____ minutes,

After ___ minutes,

After _____ minutes

______ minutes

(Top , Middle & Bottom)

_______ minutes

(Top , Middle & Bottom)

______ minutes

(Top , Middle & Bottom)

Prepared By Reviewed by Approved by

Designation QA chemist Production Manager Manager QC&A Plant headDateFormat No.: xxxxxxxxxxxxxx

xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx

QUALITY ASSURANCE

PROCESS VALIDATION PROTOCOL FOR TABLETS

Protocol No. : xxxxxxxxxxxxxxxxxRev. :00Supersedes: NILProtocol prepared on: xxxxxxxxxxEffective Date: xxxxxxxxxxxxxPage 14 of 38

Total samples: 9 Samples

MIXING:

Sampling Qty.: -Depends on quantity required for analysis.

Sampling Time: - (bracketing the time between 2 to 3 intervals of total mixing time)

While mixing is on: -

After ____ minutes,

After ___ minutes,

After _____ minutes

______ minutes

(Top , Middle & Bottom)

_______ minutes

(Top , Middle & Bottom)

______ minutes

(Top , Middle & Bottom)

Total samples: 9 Samples

DRYING:

Sampling point for drying stage:

Top View Sampling Top

TOP VIEW

T2

B2

B3

T3T1Prepared By Reviewed by Approved by

Designation QA chemist Production Manager Manager QC&A Plant headDateFormat No.: xxxxxxxxxxxxxx

xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx

QUALITY ASSURANCE

PROCESS VALIDATION PROTOCOL FOR TABLETS

Protocol No. : xxxxxxxxxxxxxxxxxRev. :00Supersedes: NILProtocol prepared on: xxxxxxxxxxEffective Date: xxxxxxxxxxxxxPage 15 of 38

Front side Bottom

----- Sampling Points

Sampling Qty.: -Depends on quantity required for analysis.

Sampling Time: - (bracketing the time between 2 to 3 intervals of total mixing time)

While Drying is on: -

After ____ minutes,

After ___ minutes,

After _____ minutes

______ minutes

(Top , Middle & Bottom)

_______ minutes

(Top , Middle & Bottom)

______ minutes

(Top , Middle & Bottom)

Total samples: 9 Samples

MILLING:

Sampling Qty.: -Depends on quantity required for analysis.

Sampling Time: - (bracketing the time between 2 to 3 intervals of total milling time)

While milling is on: -

After ____ minutes,

After ___ minutes,

After _____ minutes

______ minutes

(Top , Middle & Bottom)

_______ minutes

(Top , Middle & Bottom)

______ minutes

(Top , Middle & Bottom)

B1

Prepared By Reviewed by Approved by

Designation QA chemist Production Manager Manager QC&A Plant headDateFormat No.: xxxxxxxxxxxxxx

xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx

QUALITY ASSURANCE

PROCESS VALIDATION PROTOCOL FOR TABLETS

Protocol No. : xxxxxxxxxxxxxxxxxRev. :00Supersedes: NILProtocol prepared on: xxxxxxxxxxEffective Date: xxxxxxxxxxxxxPage 16 of 38

Total samples: 9 Samples

SAMPLING POINT FOR LUBRICATION (BLANDING) STAGE:Name of Blender: (DOUBLE CONE BLENDER)

Loading Valve Sampling Points

B3

T2

B3

B2

T3

Prepared By Reviewed by Approved by

Designation QA chemist Production Manager Manager QC&A Plant headDateFormat No.: xxxxxxxxxxxxxx

xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx

QUALITY ASSURANCE

PROCESS VALIDATION PROTOCOL FOR TABLETS

Protocol No. : xxxxxxxxxxxxxxxxxRev. :00Supersedes: NILProtocol prepared on: xxxxxxxxxxEffective Date: xxxxxxxxxxxxxPage 17 of 38

M

Sampling points T1, T2, T3 for top T4 B4 for middle, B1, B2, B3 for bottom sampling.

T2 T1

T3T1

T4

T1 B1

B4

B1

B2 B3

Prepared By Reviewed by Approved by

Designation QA chemist Production Manager Manager QC&A Plant headDateFormat No.: xxxxxxxxxxxxxx

xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx

QUALITY ASSURANCE

PROCESS VALIDATION PROTOCOL FOR TABLETS

Protocol No. : xxxxxxxxxxxxxxxxxRev. :00Supersedes: NILProtocol prepared on: xxxxxxxxxxEffective Date: xxxxxxxxxxxxxPage 18 of 38

Sampling Qty.: -Depends on quantity required for analysis.

Sampling Time: - (bracketing the time between 2 to 3 intervals of total mixing time)

While mixing is on: -

After ____ minutes,

After ___ minutes,

After _____ minutes

______ minutes

(Top , Middle & Bottom)

_______ minutes

(Top , Middle & Bottom)

______ minutes

(Top , Middle & Bottom)

Total samples: 9 Samples

COMPRESSION:

Sampling Qty.: -Depends on quantity required for analysis.

Sampling Time: - (bracketing the time between 2 to 3 intervals of total compression time)

After ____ minutes,

After ___ minutes,

After _____ minutes

______ minutes _______ minutes ______ minutes

Total samples: 3 Samples

COATING:

Prepared By Reviewed by Approved by

Designation QA chemist Production Manager Manager QC&A Plant headDateFormat No.: xxxxxxxxxxxxxx

xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx

QUALITY ASSURANCE

PROCESS VALIDATION PROTOCOL FOR TABLETS

Protocol No. : xxxxxxxxxxxxxxxxxRev. :00Supersedes: NILProtocol prepared on: xxxxxxxxxxEffective Date: xxxxxxxxxxxxxPage 19 of 38

Sampling Qty.: -Depends on quantity required for analysis.

Sampling Time: - (Bracketing the time between 2 to 3 intervals of total coating time)

While coating is on: -

After ____ minutes,

After ___ minutes,

After _____ minutes

______ minutes _______ minutes ______ minutes

Total samples: 3 Samples

Sampling:

Stage / Test Parameter Equipment

(Size, Location & Time)

Acceptance Criteria

Premixing Stage Variation between the results of Assay shall not be more than 2%

MixingDrying Loss on drying Between 2.0 to 4.0%MixingLubrication Variation between the results of assay shall

not be more than 2%Tablet compression Physical Parameter (I.P.Q.C)Tablet coating Weight GainTablet packing Leak Test

Recording of data & Data treatment:

Data Recording:

Prepared By Reviewed by Approved by

Designation QA chemist Production Manager Manager QC&A Plant headDateFormat No.: xxxxxxxxxxxxxx

xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx

QUALITY ASSURANCE

PROCESS VALIDATION PROTOCOL FOR TABLETS

Protocol No. : xxxxxxxxxxxxxxxxxRev. :00Supersedes: NILProtocol prepared on: xxxxxxxxxxEffective Date: xxxxxxxxxxxxxPage 20 of 38

The data obtained from the various analysis & observations shall be recorded in the Data

recording sheet for first three commercial batches.

Data Recording Sheet No.

Sheet No 1 For recording Mixing stage data

Sheet No 2 For recording Loss on drying data

Sheet No 3 For recording Lubrication stage data

Sheet No 4 For recording Compression stage data

Sheet No 5 For recording Coating stage data

Sheet No 6 For recording Packing stage data

Sheet No 7 For recording of analysis report

Sheet No 8 For recording general utilities /equipment / method qualitical

/results.

Sheet No 9 For recording analytical method validation.

Prepared By Reviewed by Approved by

Designation QA chemist Production Manager Manager QC&A Plant headDateFormat No.: xxxxxxxxxxxxxx

xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx

QUALITY ASSURANCE

PROCESS VALIDATION PROTOCOL FOR TABLETS

Protocol No. : xxxxxxxxxxxxxxxxxRev. :00Supersedes: NILProtocol prepared on: xxxxxxxxxxEffective Date: xxxxxxxxxxxxxPage 21 of 38

Data recording sheet no I

Mixing Stage: Date

Equipment name :

Identification no :

Ingredients and sequence of material addition :

RPM of Mixer Blade :

Capacity :

Mixing time : Minutes

Standard Weight of Tablet :

Method reference: As per assay procedure given in finished product specification.

Blended material to be analyzed for ______________________________

Plan: Samples to be drawn of mixing from 3 different locations (Top, Middle & Bottom)

Result after mixing _________________ minutes

Sampling Detail Results

Top

Middle

Bottom

Mean

Standard Deviation

% Relative standard deviation

Prepared By Reviewed by Approved by

Designation QA chemist Production Manager Manager QC&A Plant headDateFormat No.: xxxxxxxxxxxxxx

xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx

QUALITY ASSURANCE

PROCESS VALIDATION PROTOCOL FOR TABLETS

Protocol No. : xxxxxxxxxxxxxxxxxRev. :00Supersedes: NILProtocol prepared on: xxxxxxxxxxEffective Date: xxxxxxxxxxxxxPage 22 of 38

Result after mixing _________________ minutes

Sampling Detail Results

Top

Middle

Bottom

Mean

Standard Deviation

% Relative standard deviation

Result after mixing _________________ minutes

Sampling Detail Results

Top

Middle

Bottom

Mean

Standard Deviation

% Relative standard deviation

Analyst: Date

Remarks:

Checked By: _________________________ Date: ____________________

Data recording sheet no II

Prepared By Reviewed by Approved by

Designation QA chemist Production Manager Manager QC&A Plant headDateFormat No.: xxxxxxxxxxxxxx

xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx

QUALITY ASSURANCE

PROCESS VALIDATION PROTOCOL FOR TABLETS

Protocol No. : xxxxxxxxxxxxxxxxxRev. :00Supersedes: NILProtocol prepared on: xxxxxxxxxxEffective Date: xxxxxxxxxxxxxPage 23 of 38

Loss on Drying Stage: Date

Equipment name :

Dryer outlet temperature :

Dryer inlet temperature :

Drying Load :

Total Drying time : Minutes

Weight of the dried granules :

Method reference: Loss on drying procedure by IR moisture balance.

Plan: Material to be analyzed for Loss on drying

Samples to be drawn from 3 different locations

Sample East West North South Average Limit

Weight taken

% LOD

Remarks:

Checked By: _________________________ Date: ____________________

Prepared By Reviewed by Approved by

Designation QA chemist Production Manager Manager QC&A Plant headDateFormat No.: xxxxxxxxxxxxxx

xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx

QUALITY ASSURANCE

PROCESS VALIDATION PROTOCOL FOR TABLETS

Protocol No. : xxxxxxxxxxxxxxxxxRev. :00Supersedes: NILProtocol prepared on: xxxxxxxxxxEffective Date: xxxxxxxxxxxxxPage 24 of 38

Data recording sheet III

Lubrication Stage: Date

Equipment name :

Identification no :

Capacity :

Occupancy :

Speed of equipment :

Mixing time : Minutes

Standard Weight of Tablet :

Method reference: As per assay procedure given in finished product specification.

Lubricated material to be analyzed for % of active content ______________________________

Plan: Samples to be drawn at of blender from 3 different locations (Top, Middle & Bottom)

Result after mixing _________________ minutes

Sampling Detail Results

Top

Middle

Bottom

MeanPrepared By Reviewed by Approved by

Designation QA chemist Production Manager Manager QC&A Plant headDateFormat No.: xxxxxxxxxxxxxx

xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx

QUALITY ASSURANCE

PROCESS VALIDATION PROTOCOL FOR TABLETS

Protocol No. : xxxxxxxxxxxxxxxxxRev. :00Supersedes: NILProtocol prepared on: xxxxxxxxxxEffective Date: xxxxxxxxxxxxxPage 25 of 38

Standard Deviation

% Relative standard deviation

Result after mixing _________________ minutes

Sampling Detail Results

Top

Middle

Bottom

Mean

Standard Deviation

% Relative standard deviation

Result after mixing _________________ minutes

Sampling Detail Results

Top

Middle

Bottom

Mean

Standard Deviation

Prepared By Reviewed by Approved by

Designation QA chemist Production Manager Manager QC&A Plant headDateFormat No.: xxxxxxxxxxxxxx

xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx

QUALITY ASSURANCE

PROCESS VALIDATION PROTOCOL FOR TABLETS

Protocol No. : xxxxxxxxxxxxxxxxxRev. :00Supersedes: NILProtocol prepared on: xxxxxxxxxxEffective Date: xxxxxxxxxxxxxPage 26 of 38

% Relative standard deviation

Remarks:

Checked By: _________________________ Date: ____________________

Data recording sheet IV

Compression Stage Date

________ Station compression machine :

Identification no :

Prepared By Reviewed by Approved by

Designation QA chemist Production Manager Manager QC&A Plant headDateFormat No.: xxxxxxxxxxxxxx

xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx

QUALITY ASSURANCE

PROCESS VALIDATION PROTOCOL FOR TABLETS

Protocol No. : xxxxxxxxxxxxxxxxxRev. :00Supersedes: NILProtocol prepared on: xxxxxxxxxxEffective Date: xxxxxxxxxxxxxPage 27 of 38

Capacity :

RPM : 13 to 28 RPM

Punch Size :

Temperature of area :

Humidity of area :

Weight of 20 Tablets :

Average Weight of tablet :

Disintegration Time : NMT 15 minutes

Dissolution (If required) :

Friability : NMT 1.0%

Thickness :

Hardness :

Assay :

Content of uniformity (If required) :

Method reference: As per In-process check procedure.

Plan: Compressed tablets to be analyzed for: Average weight, Weight variation and Physical parameter at an interval of 2 hours

Requirement RPM: RPM: RPM:

Time

Average weight

Thickness mm

Prepared By Reviewed by Approved by

Designation QA chemist Production Manager Manager QC&A Plant headDateFormat No.: xxxxxxxxxxxxxx

xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx

QUALITY ASSURANCE

PROCESS VALIDATION PROTOCOL FOR TABLETS

Protocol No. : xxxxxxxxxxxxxxxxxRev. :00Supersedes: NILProtocol prepared on: xxxxxxxxxxEffective Date: xxxxxxxxxxxxxPage 28 of 38

Hardness in kg./sq. cm2

Friability in %

DT in min.

Weight variation after validated RPM __________

Time Average Weight Thickness Hardness Friability Disintegration

Weight variation: Time Time Time Time Time

Prepared By Reviewed by Approved by

Designation QA chemist Production Manager Manager QC&A Plant headDateFormat No.: xxxxxxxxxxxxxx

xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx

QUALITY ASSURANCE

PROCESS VALIDATION PROTOCOL FOR TABLETS

Protocol No. : xxxxxxxxxxxxxxxxxRev. :00Supersedes: NILProtocol prepared on: xxxxxxxxxxEffective Date: xxxxxxxxxxxxxPage 29 of 38

Remarks:

Checked By: _________________________ Date: ____________________

Data recording sheet V

Coating Stage Date

Name of equipment :

Identification no :

Capacity :

Speed of coating pan :

Temperature of area :

Temperature of blower :

Prepared By Reviewed by Approved by

Designation QA chemist Production Manager Manager QC&A Plant headDateFormat No.: xxxxxxxxxxxxxx

xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx

QUALITY ASSURANCE

PROCESS VALIDATION PROTOCOL FOR TABLETS

Protocol No. : xxxxxxxxxxxxxxxxxRev. :00Supersedes: NILProtocol prepared on: xxxxxxxxxxEffective Date: xxxxxxxxxxxxxPage 30 of 38

Spray rate :

Bed temperature :

Air Pressure :

Total coating solution used :

Weight build up :

Weight of 20 Tablets :

Average Weight of tablet :

Disintegration Time : Not more than

Dissolution (If required) :

Assay

Method reference: As per In-process check procedure.

Plan: Coated tablets to be analyzed for Weight gain, weight variation and DT. At an interval of __ hours

Date Time Initial weight

Average weight

Final weight

Average weight

% Weight gain DT in min.

Prepared By Reviewed by Approved by

Designation QA chemist Production Manager Manager QC&A Plant headDateFormat No.: xxxxxxxxxxxxxx

xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx

QUALITY ASSURANCE

PROCESS VALIDATION PROTOCOL FOR TABLETS

Protocol No. : xxxxxxxxxxxxxxxxxRev. :00Supersedes: NILProtocol prepared on: xxxxxxxxxxEffective Date: xxxxxxxxxxxxxPage 31 of 38

Weight variation:

Time

Weight variation

Remark:

Checked By: _________________________ Date: ____________________

Prepared By Reviewed by Approved by

Designation QA chemist Production Manager Manager QC&A Plant headDateFormat No.: xxxxxxxxxxxxxx

xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx

QUALITY ASSURANCE

PROCESS VALIDATION PROTOCOL FOR TABLETS

Protocol No. : xxxxxxxxxxxxxxxxxRev. :00Supersedes: NILProtocol prepared on: xxxxxxxxxxEffective Date: xxxxxxxxxxxxxPage 32 of 38

Data recording sheet VI

Packing Stage Date

Name of equipment :

Identification no :

Capacity :

Forming roller temperature (For blister packing) :

Sealing roller temperature :

Sealing roller pressure :

Speed of machine :

Seal integrity (Leak test) :

Method reference: As per In-process check procedure.

Plan: Packed tablets to be analysed for Leak test at an interval of __ hours

Date Time Leak Test Results RemarksNo of strips to be taken

Prepared By Reviewed by Approved by

Designation QA chemist Production Manager Manager QC&A Plant headDateFormat No.: xxxxxxxxxxxxxx

xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx

QUALITY ASSURANCE

PROCESS VALIDATION PROTOCOL FOR TABLETS

Protocol No. : xxxxxxxxxxxxxxxxxRev. :00Supersedes: NILProtocol prepared on: xxxxxxxxxxEffective Date: xxxxxxxxxxxxxPage 33 of 38

Data recording sheet VII

Analysis Report

Product Name:Batch No.: Batch size:Mfg. Date: Exp. Date:

Composition:Test method reference: In house

Sr. No. Test Specification Results Remark01 Description

02

03

04

05

5.1

5.2

5.3

5.4

Remark:

Result: The sample referred above complies / does not comply with the standard prescribed as per In house Specification.

Data recording sheet VIII

Prepared By Reviewed by Approved by

Designation QA chemist Production Manager Manager QC&A Plant headDateFormat No.: xxxxxxxxxxxxxx

xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx

QUALITY ASSURANCE

PROCESS VALIDATION PROTOCOL FOR TABLETS

Protocol No. : xxxxxxxxxxxxxxxxxRev. :00Supersedes: NILProtocol prepared on: xxxxxxxxxxEffective Date: xxxxxxxxxxxxxPage 34 of 38

Sr

No

Name of critical equipment / Utilities Qualification /

Validation file

reference No

Date of Qualification /

Validation

Prepared By Reviewed by Approved by

Designation QA chemist Production Manager Manager QC&A Plant headDateFormat No.: xxxxxxxxxxxxxx

xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx

QUALITY ASSURANCE

PROCESS VALIDATION PROTOCOL FOR TABLETS

Protocol No. : xxxxxxxxxxxxxxxxxRev. :00Supersedes: NILProtocol prepared on: xxxxxxxxxxEffective Date: xxxxxxxxxxxxxPage 35 of 38

1

2

3

4

5

6

7

8

9

10

11

12

13

14

Sr No

Name of critical equipment / Utilities Qualification / Validation file reference No

Date of Qualification / Validation

15

16

17

18

19Prepared By Reviewed by Approved by

Designation QA chemist Production Manager Manager QC&A Plant headDateFormat No.: xxxxxxxxxxxxxx

xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx

QUALITY ASSURANCE

PROCESS VALIDATION PROTOCOL FOR TABLETS

Protocol No. : xxxxxxxxxxxxxxxxxRev. :00Supersedes: NILProtocol prepared on: xxxxxxxxxxEffective Date: xxxxxxxxxxxxxPage 36 of 38

20

21

22

23

24

25

26

27

28

Utilities:

1 AHU System

2 Water System

3 Compressed Air

4 Steam

5 Lightning

6 Drain

Data recording sheet IX

Remark:

Analytical Method Validation protocol attached

Prepared By Reviewed by Approved by

Designation QA chemist Production Manager Manager QC&A Plant headDateFormat No.: xxxxxxxxxxxxxx

xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx

QUALITY ASSURANCE

PROCESS VALIDATION PROTOCOL FOR TABLETS

Protocol No. : xxxxxxxxxxxxxxxxxRev. :00Supersedes: NILProtocol prepared on: xxxxxxxxxxEffective Date: xxxxxxxxxxxxxPage 37 of 38

Conclusion

Sr. No. Stage Acceptance criteria Observation

1. Sifting No visible foreign particulate matter is observed

2. Premixing

Stage

Variation between the results shall not be more

than 2%

3. Drying Between 2.0 to 4.0%

4. Lubrication Variation between the results shall not be more

than 2%

5. Tablet

compression

Average weight of tablets is within ± ____of std.

weight.

Tablets shall meet requirement of physical

parameter and FP specification.

6. Tablet coating Tablets shall meet the requirements for weight

gain, weight variation and disintegration.

Coated tablets shall meet FP Specification

7. Tablet

packing

Packed tablet shall meet the requirement for leak

test

Conclusion:

Product _________________________________ manufactured as per B.M.R. No _____________

meets predefined acceptance criteria.

Analysis By Approved By

Date Date

Prepared By Reviewed by Approved by

Designation QA chemist Production Manager Manager QC&A Plant headDateFormat No.: xxxxxxxxxxxxxx

xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx

QUALITY ASSURANCE

PROCESS VALIDATION PROTOCOL FOR TABLETS

Protocol No. : xxxxxxxxxxxxxxxxxRev. :00Supersedes: NILProtocol prepared on: xxxxxxxxxxEffective Date: xxxxxxxxxxxxxPage 38 of 38

7. LIMITS: As pre relative STPs

8. CONCLUSION REPORT

Summary report will contain discussion and conclusion , which clearly states the successful achievement of objective of validation studies and recommended concentrations required for sanitization, disinfections and equipment sanitization.

Note: Extra pages for conclusions can be used as per requirement.

Prepared By Reviewed by Approved by

Designation QA chemist Production Manager Manager QC&A Plant headDateFormat No.: xxxxxxxxxxxxxx