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QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS

PROCESS VALIDATION PROTOCOL FOR TABLETS

Protocol No. Effective Date.

: xxxxxxxx : xxxxxxxxxxxx

Prepared By

Reviewed by

Approved by

Designation QA chemist Date Format No.: xxxxxxxxxxxxxx

Production Manager

Manager QC&A

Plant head

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QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS

TABLE OF CONTENTS
S.NO. SECTION 1. 2. 3. 4. 5. 6. 7. 8. Protocol approval Purpose Responsibilities Requirements Personnel Responsibilities Validation parameters Limits Conclusion report Page No

1. PROTOCOL APPROVAL
Prepared By

Reviewed by

Approved by

Designation QA chemist Date Format No.: xxxxxxxxxxxxxx

Production Manager

Manager QC&A

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QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS

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 Manager production Manager Engineering Manager QA

Signature

Date

2. PURPOSE
Process 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. Prepared By Reviewed by Approved by

Designation QA chemist Date Format No.: xxxxxxxxxxxxxx

Production Manager

Manager QC&A

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QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS

3. RESPONSIBILITIES
S.NO. Activity 1. 2. 3. 4. 5. 6. Preparation of protocol Chemical analysis and sampling Microbial analysis & sampling Preparation of validation Report Review of validation protocol & report Approval of protocol & Report Responsibility QA chemist QC chemist Microbiologist Dy Manager QC QA department, Production Department 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:
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 Prepared By Approved by 3 Input check in presence of QA person Reviewed by

Designation QA chemist Date Format No.: xxxxxxxxxxxxxx

Production Manager

Manager QC&A

Plant head

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QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS

4 Granulation 4.1 Sifting 4.2 Premixing 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 1 2 3 4 5 6 7 Ingredients/Excipients Unit per Tablet Std. Qty. Overages Dispensed Quantity Weight by Checked by

Prepared By

Reviewed by

Approved by

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Production Manager

Manager QC&A

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QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS

8 9 10 11 12 13 14 15 16

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

Input check in presence of QA person

GRANULATION Shifting Premixing Mixing Binder preparation

Dry Granulation

Wet Granulation milling

Drying Dry milling Mixing Slugging, Milling (if required)

Prepared By

Coating

Compression

Reviewed by

Lubrication

Approved by

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(Blending)

QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS

Tablet packing

Sampling point Typical Variables and responses: Granulated Product

Prepared By

Reviewed by

Approved by

Designation QA chemist Date Format No.: xxxxxxxxxxxxxx

Production Manager

Manager QC&A

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QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS

S. No. 1.

Process step Pre-blending

2.

Granulating

3.

Drying

4. 5. 6.

Sizing Blending Tableting

Control variables Blending time RPM Load size Order of addition Load size Amount of granulating agent Solvent addition rate RPM Granulation time Initial temperature Load size Drying temperature program Air flow program Drying time Cooling time Screen type Screen size Feed rate Load size RPM Blending time Compression rate Granule feed rate Pre-compression force Compression force

Measured responses Blend uniformity

Density Yield

Density Moisture content Yield

Granule size distribution Loose drying Packed density Blend uniformity Flow characteristics Particle size distribution Weight variation Friability Hardness Thickness Disintegration time Dissolution Dosage from uniformity

Equipments A detailed list of equipment used for validation together with the cleaning status will be provided in the manufacturing documents. Prepared Qualification report usedReviewed by List of SOPS, Validation &By as references Designation QA chemist Date Format No.: xxxxxxxxxxxxxx Production Manager Manager QC&A Approved by

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QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS

Sr. No. 1 2 3 4 5 6 7 8 9 10 11 12

Name of Equipment

Equipment ID.

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. 1. STAGE Premixing Parameters RPM of mixer blade Load size Total time of mixing Uniform mixing by Assay analysis Mixer blade speed Load size Binder Quantity Binder addition rate Binder addition time Temperature of binder Mixing time after binder addition /Total granulation time Uniformity of granulated mass (Visual Checking) Dryer outlet temperature Dryer inlet temperature Drying load Reviewed by Approved by Total drying time Production Manager Manager QC&A Plant head

2.

Granulation

3.

Drying Prepared By

Designation QA chemist Date Format No.: xxxxxxxxxxxxxx

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QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS

4. 5.

Milling Lubrication

6.

Compression

7.

Coating

8.

Packaging Prepared By

Weight of the Dried granules Speed of machine Direction of knives Load size Occupancy Speed of equipment (RPM) Total time of mixing Assay - (individual sample) Temperature of area Humidity of area Machine Details Weight variation of 20 tablets Average weight of tablet Disintegration time Friability Diameter (Length) Thickness Hardness Assay Content uniformity Dissolution 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 Forming roller temperature. (for Blister Packing) Sealing roller temperature Sealing roller Pressure Reviewed by Approved by

Designation QA chemist Date Format No.: xxxxxxxxxxxxxx

Production Manager

Manager QC&A

Plant head

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QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS

9.

Packaging (bulk packing)

Speed of machine Seal integrity Assay Dissolution Sealing temperature Seal integrity Counter Checking from 10 Jars at different Time intervals

Sr. No

Process / Variable Blend Manufacturing Sifting

Machine setting ( Control Variables) Visually Inspection Uniform mixing by Assay analysis

Remarks No visible foreign particulate matter is observed Variation between the results shall not be more than 2%

Premixing Stage Granulation Binder Preparation Granulation Wet milling Prepared By

Finely divided material without free powder and excessive wetted lumps. Material was finely divided by Reviewed

Approved by

Designation QA chemist Date Format No.: xxxxxxxxxxxxxx

Production Manager

Manager QC&A

Plant head

xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx Protocol No. : xxxxxxxxxxxxxxxxx Rev. :00 Supersedes: NIL Protocol prepared on: xxxxxxxxxx Effective Date: xxxxxxxxxxxxx Page 12 of 33 Between 2.0 to 5.0% Variation between the results shall not be more than 2% Wt. Variation, Hardness, Thickness, DT, Dissolution and Assay Weight gain, weight variation and DT Leak Test

QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS

Drying Dry milling Lubrication 5 6 7 Tablet compression Tablet coating Tablet packing

Loss on drying Finely divided granules are observed Assay and Sieve analysis Physical Parameter

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) Total samples: 9 Samples MIXING: Sampling Qty.: -Depends on quantity required for analysis. Prepared By Reviewed by Approved by _______ minutes (Top , Middle & Bottom) ______ minutes (Top , Middle & Bottom)

Designation QA chemist Date Format No.: xxxxxxxxxxxxxx

Production Manager

Manager QC&A

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QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS

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) Total samples: 9 Samples DRYING: Sampling point for drying stage: Top View Sampling Top TOP VIEW B2 B3 T2 _______ minutes (Top , Middle & Bottom) ______ minutes (Top , Middle & Bottom)

T1 Front side ----- Sampling Points Sampling Qty.: -Depends on quantity required for analysis. Sampling Time: - (bracketing the time between 2 to 3 intervals of total mixing time) Reviewed by While Drying is on: Prepared By Designation QA chemist Date Format No.: xxxxxxxxxxxxxx Production Manager Manager QC&A Bottom B1

T3

Approved by

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QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS

After ____ minutes, After ___ minutes, After _____ minutes ______ minutes (Top , Middle & Bottom) Total samples: 9 Samples MILLING: _______ minutes (Top , Middle & Bottom) ______ minutes (Top , Middle & Bottom)

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) Total samples: 9 Samples _______ minutes (Top , Middle & Bottom) ______ minutes (Top , Middle & Bottom)

Prepared By

Reviewed by

Approved by

Designation QA chemist Date Format No.: xxxxxxxxxxxxxx

Production Manager

Manager QC&A

Plant head

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QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS

SAMPLING POINT FOR LUBRICATION (BLANDING) STAGE: Name of Blender: (DOUBLE CONE BLENDER) Loading Valve Sampling Points B3 B2 T3 T2 T1 M T4 T3 B3 T2

T1 T 1

B2 B1

B4 B3

B1

Sampling points T1, T2, T3 for top T4 B4 for middle, B1, B2, B3 for bottom sampling. Prepared By Reviewed by Approved by

Designation QA chemist Date Format No.: xxxxxxxxxxxxxx

Production Manager

Manager QC&A

Plant head

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QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS

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) 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 Total samples: 3 Samples _______ minutes ______ minutes _______ minutes (Top , Middle & Bottom) ______ minutes (Top , Middle & Bottom)

COATING: Sampling Qty.: -Depends on quantity required for analysis. Sampling Time: - (Bracketing the time between 2 to 3 intervals of total coating time) Reviewed by While coating is on:Prepared By Designation QA chemist Date Format No.: xxxxxxxxxxxxxx Production Manager Manager QC&A Approved by

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QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS

After ____ minutes, After ___ minutes, After _____ minutes ______ minutes Total samples: 3 Samples Sampling: Stage / Test Parameter Premixing Stage Mixing Drying Mixing Lubrication Tablet compression Tablet coating Tablet packing Equipment (Size, Location & Time) Variation between the results of Assay shall not be more than 2% Loss on drying Between 2.0 to 4.0% Variation between the results of assay shall not be more than 2% Physical Parameter (I.P.Q.C) Weight Gain Leak Test Acceptance Criteria _______ minutes ______ minutes

Recording of data & Data treatment: Data Recording: The data obtained from the various analysis & observations shall be recorded in the Data recording sheet for first three commercial batches.

Prepared By

Reviewed by

Approved by

Designation QA chemist Date Format No.: xxxxxxxxxxxxxx

Production Manager

Manager QC&A

Plant head

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QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS

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 Sheet No 9 /results. For recording analytical method validation.

Prepared By

Reviewed by

Approved by

Designation QA chemist Date Format No.: xxxxxxxxxxxxxx

Production Manager

Manager QC&A

Plant head

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QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS

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 Top Middle Bottom Mean Standard Deviation % Relative standard deviation Results

Prepared By

Reviewed by

Approved by

Designation QA chemist Date Format No.: xxxxxxxxxxxxxx

Production Manager

Manager QC&A

Plant head

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QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS

Result after mixing _________________ minutes Sampling Detail Top Middle Bottom Mean Standard Deviation % Relative standard deviation Result after mixing _________________ minutes Sampling Detail Top Middle Bottom Mean Standard Deviation % Relative standard deviation Analyst: Remarks: Checked By: _________________________ Date Date: ____________________ Results Results

Data recording sheet no II Loss on Drying Stage: Equipment name Dryer outlet temperature Dryer inlet temperature Drying Load Total Drying time Weight of the dried granules Date : : : : : :

Minutes Approved by

Prepared By Reviewed by Method reference: Loss on drying procedure by IR moisture balance. Designation QA chemist Date Format No.: xxxxxxxxxxxxxx Production Manager Manager QC&A

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QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS

Plan: Material to be analyzed for Loss on drying Samples to be drawn from 3 different locations Sample Ea st Weight taken % LOD W est No rth So ut h Average Limit

Remarks: Checked By: _________________________ Date: ____________________

Prepared By

Reviewed by

Approved by

Designation QA chemist Date Format No.: xxxxxxxxxxxxxx

Production Manager

Manager QC&A

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QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS

Data recording sheet III Lubrication Stage: Equipment name Identification no Capacity Occupancy Speed of equipment Mixing time Standard Weight of Tablet Date : : : : : : :

Minutes

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 Top Middle Bottom Results

Mean Standard Deviation % Relative standard deviation Result after mixing _________________ minutes Prepared By Reviewed by Approved by

Designation QA chemist Date Format No.: xxxxxxxxxxxxxx

Production Manager

Manager QC&A

Plant head

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QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS

Sampling Detail Top Middle Bottom Mean Standard Deviation % Relative standard deviation Result after mixing _________________ minutes Sampling Detail Top Middle Bottom Mean Standard Deviation % Relative standard deviation Remarks: Checked By: _________________________

Results

Date: ____________________

Prepared By

Reviewed by

Approved by

Designation QA chemist Date Format No.: xxxxxxxxxxxxxx

Production Manager

Manager QC&A

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QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS

Data recording sheet IV Compression Stage ________ Station compression machine Identification no Capacity RPM Punch Size Temperature of area Humidity of area Weight of 20 Tablets Average Weight of tablet Disintegration Time Dissolution (If required) Friability Thickness Hardness Assay Content of uniformity (If required) Method reference: As per In-process check procedure. Date : : : : : : : : : : : : : : : :

13 to 28 RPM

NMT 15 minutes NMT 1.0%

Prepared By

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Production Manager

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QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS

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 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 Prepared By

Time

Time Reviewed by

Time Approved by

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QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS

Remarks:

Checked By: _________________________

Date: ____________________

Data recording sheet V Coating Stage Name of equipment Identification no Capacity Speed of coating pan Temperature of area Temperature of blower Spray rate Bed temperature Air Pressure Total coating solution used Weight build up Prepared By Weight of 20 Tablets Date : : : : : : : : : : : : Reviewed by

Approved by

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Production Manager

Manager QC&A

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QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS

Average Weight of tablet Disintegration Time Dissolution (If required) Assay Method reference: As per In-process check procedure.

Not more than

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.

Weight variation: Time Weight variation Remark: Checked By: _________________________ Prepared By Date: ____________________ Reviewed by Approved by

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Production Manager

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QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS

Data recording sheet VI Packing Stage 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 No of strips to be taken Results Remarks Date : : : : : : : :

Prepared By

Reviewed by

Approved by

Designation QA chemist Date Format No.: xxxxxxxxxxxxxx

Production Manager

Manager QC&A

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QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS

Data recording sheet VII Analysis Report Product Name: Batch No.: Mfg. Date: Test method reference: In house Sr. No. Test 01 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 Sr No 1 2 3 Name of critical equipment / Utilities Qualification / Validation file reference No Prepared By Reviewed by Approved by Date of Qualification / Validation Batch size: Exp. Date: Composition: Specification Results Remark

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QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS

4 5 6 7 8 9 10 11 12 13 14 Sr No 15

Name of critical equipment / Utilities

Qualification / Validation file reference No

Date of Qualification / Validation

16 17 18 19 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 Prepared By Data recording Reviewed by sheet IX Production Manager Manager QC&A Approved by

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QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS

Remark: Analytical Method Validation protocol attached

Prepared By

Reviewed by

Approved by

Designation QA chemist Date Format No.: xxxxxxxxxxxxxx

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QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS

Conclusion Sr. No. 1. 2. 3. 4. 5. Stage Sifting Premixing Stage Drying Lubrication Tablet compression Acceptance criteria No visible foreign particulate matter is observed Variation between the results shall not be more than 2% Between 2.0 to 4.0% Variation between the results shall not be more than 2% Average weight of tablets is within ____of std. weight. Tablets shall meet requirement of physical 6. Tablet coating parameter and FP specification. Tablets shall meet the requirements for weight gain, weight variation and disintegration. 7. Tablet Coated tablets shall meet FP Specification Packed tablet shall meet the requirement for leak test Observation

packing Conclusion:

Product _________________________________ manufactured as per B.M.R. No _____________ meets predefined acceptance criteria. Analysis By Date 7. Approved By Date

LIMITS: As pre relative STPs 8. CONCLUSION REPORT

Prepared By Reviewed by Approved by

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QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS

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 Date Format No.: xxxxxxxxxxxxxx

Production Manager

Manager QC&A

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