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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

Production Manager

Manager QC&A

Plant head

Date Format No.: xxxxxxxxxxxxxx

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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

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QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS

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 Manager production Manager Engineering

Signature

Date

Manager QA

Prepared By

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Approved by

Designation

QA chemist

Production Manager

Manager QC&A

Plant head

Date Format No.: xxxxxxxxxxxxxx

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QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS

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.

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.

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QA chemist

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Manager QC&A

Plant head

Date Format No.: xxxxxxxxxxxxxx

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QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS

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 3 Input check in presence of QA person 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: Prepared By Reviewed by Approved by

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QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS

Batch Size: Sr No 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 Ingredients/Excipients Unit per Tablet Std. Qty. Overages Dispensed Quantity Weight by Checked by

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

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Production Manager

Manager QC&A

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QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS

Input check in presence of QA person

GRANULATION Shifting

Dry Granulation

Premixing

Mixing Wet Granulation milling

Binder preparation

Drying Dry milling Mixing Slugging, Milling (if required)

Coating

Compression

Lubrication (Blending)

Tablet packing

Sampling point Typical Variables and responses: Granulated Product

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QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS

S. No. 1.

Process step Pre-blending

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

2.

Granulating

Density Yield

3.

Drying

Density Moisture content Yield

4.

Sizing

5.

Blending

6.

Tableting

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 By Reviewed by Approved by

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QA chemist

Production Manager

Manager QC&A

Plant head

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QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS

List of SOPS, Validation & Qualification report used as references Sr. No. 1 2 3 4 5 6 7 8 9 10 11 12 Name of Equipment Equipment ID. Qualification details SOP No

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 Prepared By Parameters Reviewed by Approved by

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QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS

1.

Premixing

RPM of mixer blade Load size Total time of mixing Uniform mixing by Assay analysis

2.

Granulation

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)

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

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QA chemist

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Manager QC&A

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QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS

Assay - (individual sample) 6. Compression 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 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 Prepared By Reviewed by Approved by

Designation

QA chemist

Production Manager

Manager QC&A

Plant head

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QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS

Assay Disintegration time Dissolution 8. Packaging Forming roller temperature. (for Blister Packing) Sealing roller temperature Sealing roller Pressure Speed of machine Seal integrity Assay Dissolution 9. Packaging (bulk packing) Seal integrity Counter Checking from 10 Jars at different Time intervals Sealing temperature

Sr. No 1

Process / Variable Blend Manufacturing Sifting

Machine setting ( Control Variables) Visually Inspection

Remarks No visible foreign particulate matter is observed

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QA chemist

Production Manager

Manager QC&A

Plant head

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QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS

Premixing Stage Uniform mixing by Assay analysis Granulation Binder Preparation Granulation 2 Wet milling Drying Dry milling Lubrication

Variation between the results shall not be more than 2%

3 4 5

Tablet compression Tablet coating Tablet packing

Finely divided material without free powder and excessive wetted lumps. Material was finely divided Loss on drying Between 2.0 to 5.0% Finely divided granules are observed Variation between the results Assay and Sieve analysis shall not be more than 2% Wt. Variation, Hardness, Physical Parameter Thickness, DT, Dissolution and Assay Weight gain, weight variation and DT 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,

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QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS

After ___

minutes,

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

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

DRYING:

Sampling point for drying stage: Top View Sampling Top B2 TOP VIEW Prepared By Reviewed by B3 Approved by T2

Designation

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Manager QC&A

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QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS

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) While Drying is on: After ____ minutes, After ___ minutes, Bottom B1

T3

After _____ minutes ______ 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, _______ minutes (Top , Middle & Bottom) ______ minutes (Top , Middle & Bottom)

After _____ minutes Prepared By Reviewed by Approved by

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Manager QC&A

Plant head

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QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS

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

_______ minutes (Top , Middle & Bottom)

______ minutes (Top , Middle & Bottom)

SAMPLING POINT FOR LUBRICATION (BLANDING) STAGE: Name of Blender: (DOUBLE CONE BLENDER) Loading Valve Sampling Points B3 B2 T3 Prepared By T2 Designation QA chemist T1 Reviewed by Approved by T2

Production Manager

Manager QC&A

Plant head

Date Format No.: xxxxxxxxxxxxxx

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QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS

M T4 T 1 T3

T1

B1

B4 B2 B1

B3

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

Prepared By

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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 _______ minutes (Top , Middle & Bottom) ______ minutes (Top , Middle & Bottom)

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

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QA chemist

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 coating time) While coating is on: After ____ minutes, After ___ minutes,

After _____ minutes ______ minutes Total samples: 3 Samples _______ minutes ______ minutes

Sampling: Stage / Test Parameter Equipment (Size, Location & Time) Premixing Stage Mixing Drying Mixing Lubrication Tablet compression Tablet coating Tablet packing 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

Recording of data & Data treatment: Data Recording: Prepared By Reviewed by Approved by

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Manager QC&A

Plant head

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QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS

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 Sheet No 2 Sheet No 3 Sheet No 4 Sheet No 5 Sheet No 6 Sheet No 7 Sheet No 8 For recording Mixing stage data For recording Loss on drying data For recording Lubrication stage data For recording Compression stage data For recording Coating stage data For recording Packing stage data For recording of analysis report For recording general utilities /equipment / method qualitical /results. Sheet No 9 For recording analytical method validation.

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QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS

Data recording sheet no I Mixing Stage: Equipment name Identification no Ingredients and sequence of material addition RPM of Mixer Blade Capacity Mixing time Standard Weight of Tablet : : : : : : : Minutes Date

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

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QA chemist

Production Manager

Manager QC&A

Plant head

Date Format No.: xxxxxxxxxxxxxx

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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 Results

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

Prepared By

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Approved by

Designation

QA chemist

Production Manager

Manager QC&A

Plant head

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QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS

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 : : : : : : Minutes Date

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 Weight taken % LOD

East

West

North

South

Average

Limit

Remarks:

Checked By: _________________________

Date: ____________________

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QA chemist

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Manager QC&A

Plant head

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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 : : : : : : : Minutes Date

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

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QA chemist

Production Manager

Manager QC&A

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QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS

Mean Standard Deviation % Relative standard deviation

Result after mixing _________________ minutes

Sampling Detail Top Middle Bottom

Results

Mean Standard Deviation % Relative standard deviation

Result after mixing _________________ minutes

Sampling Detail Top Middle Bottom

Results

Mean Prepared By Reviewed by Approved by

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QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS

Standard Deviation % Relative standard deviation

Remarks:

Checked By: _________________________

Date: ____________________

Data recording sheet IV Compression Stage ________ Station compression machine Prepared By : Reviewed by Approved by Date

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Manager QC&A

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QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS

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)

: : : : : : : : : : : : : : : NMT 1.0% NMT 15 minutes 13 to 28 RPM

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 Prepared By Reviewed by Approved by

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QA chemist

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Manager QC&A

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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

Time

Time

Time

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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 Prepared By : : : Reviewed by Approved by Date

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QA chemist

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Manager QC&A

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Speed of coating pan Temperature of area Temperature of blower Spray rate Bed temperature Air Pressure Total coating solution used Weight build up Weight of 20 Tablets Average Weight of tablet Disintegration Time Dissolution (If required) Assay

: : : : : : : : : : : : Not more than

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.

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QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS

Weight variation: Time Weight variation

Remark: Checked By: _________________________ Date: ____________________

Prepared By

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QA chemist

Production Manager

Manager QC&A

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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) : : : : : : : : Date

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

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QA chemist

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 02 03 04 05 5.1 Description Batch size: Exp. Date: Composition: Specification Results Remark

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

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QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS

Sr No

Name of critical equipment / Utilities

Qualification / Validation file reference No

Date of Qualification / Validation

1 2 3 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

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Approved by

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QA chemist

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Manager QC&A

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16 17 18 19 20 21 22 23 24 25 26 27 28 Utilities: 1 2 3 4 5 6 AHU System Water System Compressed Air Steam Lightning Drain

Data recording sheet IX

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QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS

Remark: Analytical Method Validation protocol attached

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Conclusion Sr. No. 1. 2. Stage Sifting Premixing Stage 3. 4. Drying Lubrication 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% 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 Conclusion: Product _________________________________ manufactured as per B.M.R. No _____________ meets predefined acceptance criteria. Analysis By Date Approved By Date Packed tablet shall meet the requirement for leak test Observation

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QA chemist

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QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS

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.

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Date Format No.: xxxxxxxxxxxxxx