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QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS
Protocol No. : xxxxxxxxxxxxxxxxx Rev. :00 Supersedes: NIL Protocol prepared on: xxxxxxxxxx Effective Date: xxxxxxxxxxxxx Page 1 of 38
PROCESS VALIDATION PROTOCOL FOR TABLETS
Protocol No.
: xxxxxxxx
Effective Date.
: xxxxxxxxxxxx
Prepared By
Designation
QA chemist
Date Format No.: xxxxxxxxxxxxxx
Reviewed by
Production Manager
Manager QC&A
Approved by
Plant head
xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx
QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS
Protocol No. : xxxxxxxxxxxxxxxxx Rev. :00 Supersedes: NIL Protocol prepared on: xxxxxxxxxx Effective Date: xxxxxxxxxxxxx Page 2 of 38
TABLE OF CONTENTS Page No
S.NO. SECTION 1.
Protocol approval
2.
Purpose
3.
Responsibilities
4.
Requirements
5.
Personnel Responsibilities
6.
Validation parameters
7.
Limits
8.
Conclusion report
Prepared By
Designation
QA chemist
Date Format No.: xxxxxxxxxxxxxx
Reviewed by
Production Manager
Manager QC&A
Approved by
Plant head
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QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS
Protocol No. : xxxxxxxxxxxxxxxxx Rev. :00 Supersedes: NIL Protocol prepared on: xxxxxxxxxx Effective Date: xxxxxxxxxxxxx Page 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
Designation
QA chemist
Date Format No.: xxxxxxxxxxxxxx
Reviewed by
Production Manager
Manager QC&A
Approved by
Plant head
xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx
QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS
Protocol No. : xxxxxxxxxxxxxxxxx Rev. :00 Supersedes: NIL Protocol prepared on: xxxxxxxxxx Effective Date: xxxxxxxxxxxxx Page 4 of 38
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
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.
Prepared By
Designation
QA chemist
Date Format No.: xxxxxxxxxxxxxx
Reviewed by
Production Manager
Manager QC&A
Approved by
Plant head
xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx
QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS
Protocol No. : xxxxxxxxxxxxxxxxx Rev. :00 Supersedes: NIL Protocol prepared on: xxxxxxxxxx Effective Date: xxxxxxxxxxxxx Page 5 of 38
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 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: Prepared By
Designation
QA chemist
Date Format No.: xxxxxxxxxxxxxx
Reviewed by
Production Manager
Manager QC&A
Approved by
Plant head
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QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS
Protocol No. : xxxxxxxxxxxxxxxxx Rev. :00 Supersedes: NIL Protocol prepared on: xxxxxxxxxx Effective Date: xxxxxxxxxxxxx Page 6 of 38
Batch Size: Sr No 1
Ingredients/Excipients Unit per Tablet
Std. Qty.
Overages Dispensed Quantity
Weight by
Checked by
2 3 4 5 6 7 8 9 10 11 12 13 14 15 16
FLOW SHEET: Prepare production order and according to that issue the BPR
Prepared By
Designation
QA chemist
Date Format No.: xxxxxxxxxxxxxx
RM dispensing as per Bill of material
Reviewed by
Production Manager
Manager QC&A
Approved by
Plant head
xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx
QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS
Input check in presence of QA person
Protocol No. : xxxxxxxxxxxxxxxxx Rev. :00 Supersedes: NIL Protocol prepared on: xxxxxxxxxx Effective Date: xxxxxxxxxxxxx Page 7 of 38
GRANULATION Shifting
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 Product
Prepared By
Designation
QA chemist
Date Format No.: xxxxxxxxxxxxxx
Reviewed by
Production Manager
Manager QC&A
Approved by
Plant head
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QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS
Protocol No. : xxxxxxxxxxxxxxxxx Rev. :00 Supersedes: NIL Protocol prepared on: xxxxxxxxxx Effective Date: xxxxxxxxxxxxx Page 8 of 38
S. No.
Process step
Control variables
Measured responses
1.
Pre-blending
Blend uniformity
2.
Granulating
3.
Drying
4.
Sizing
5.
Blending
6.
Tableting
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
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 By
Designation
QA chemist
Date Format No.: xxxxxxxxxxxxxx
Reviewed by
Production Manager
Manager QC&A
Approved by
Plant head
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QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS
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List of SOP’S, Validation & Qualification report used as references Sr. No. 1
Name of Equipment
Equipment ID.
Qualification details
SOP No
2 3 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 Prepared By
Designation
QA chemist
Date Format No.: xxxxxxxxxxxxxx
Parameters Reviewed by
Production Manager
Manager QC&A
Approved by
Plant head
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QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS
1.
Premixing
Protocol No. : xxxxxxxxxxxxxxxxx Rev. :00 Supersedes: NIL Protocol prepared on: xxxxxxxxxx Effective Date: xxxxxxxxxxxxx Page 10 of 38
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
Prepared By
Designation
QA chemist
Date Format No.: xxxxxxxxxxxxxx
Reviewed by
Production Manager
Manager QC&A
Approved by
Plant head
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QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS
Protocol No. : xxxxxxxxxxxxxxxxx Rev. :00 Supersedes: NIL Protocol prepared on: xxxxxxxxxx Effective Date: xxxxxxxxxxxxx Page 11 of 38
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
Designation
QA chemist
Date Format No.: xxxxxxxxxxxxxx
Reviewed by
Production Manager
Manager QC&A
Approved by
Plant head
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QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS
Protocol No. : xxxxxxxxxxxxxxxxx Rev. :00 Supersedes: NIL Protocol prepared on: xxxxxxxxxx Effective Date: xxxxxxxxxxxxx Page 12 of 38
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
Sealing temperature
packing) Seal integrity Counter Checking from 10 Jars at different Time intervals
Sr. No 1
Process / Variable Blend Manufacturing Sifting
Prepared By
Designation
QA chemist
Date Format No.: xxxxxxxxxxxxxx
Machine setting ( Control Variables)
Remarks No visible foreign particulate matter is observed
Visually Inspection
Reviewed by
Production Manager
Manager QC&A
Approved by
Plant head
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QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS
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Premixing Stage Uniform mixing by Assay analysis Granulation Binder Preparation Granulation 2
Wet milling Drying Dry milling Lubrication
3
Tablet compression
4
Tablet coating
5
Tablet packing
Variation between the results shall not be more than 2%
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,
Prepared By
Designation
QA chemist
Date Format No.: xxxxxxxxxxxxxx
Reviewed by
Production Manager
Manager QC&A
Approved by
Plant head
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QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS
After ___
Protocol No. : xxxxxxxxxxxxxxxxx Rev. :00 Supersedes: NIL Protocol prepared on: xxxxxxxxxx Effective Date: xxxxxxxxxxxxx Page 14 of 38
minutes,
After _____ minutes ______ minutes
_______ minutes
______ minutes
(Top , Middle & Bottom)
(Top , Middle & Bottom)
(Top , Middle & Bottom)
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
_______ minutes
______ minutes
(Top , Middle & Bottom)
(Top , Middle & Bottom)
(Top , Middle & Bottom)
Total samples: 9 Samples
DRYING:
Sampling point for drying stage: T2
Top View Sampling Top
B2 B3
TOP VIEW Prepared By
Designation
QA chemist
Date Format No.: xxxxxxxxxxxxxx
Reviewed by
Production Manager
Manager QC&A
Approved by
Plant head
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QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS
Protocol No. : xxxxxxxxxxxxxxxxx Rev. :00 Supersedes: NIL Protocol prepared on: xxxxxxxxxx Effective Date: xxxxxxxxxxxxx Page 15 of 38
T3
T1 Front side
B1
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
_______ minutes
______ minutes
(Top , Middle & Bottom)
(Top , Middle & Bottom)
(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 Prepared By
Designation
QA chemist
Date Format No.: xxxxxxxxxxxxxx
Reviewed by
Production Manager
Manager QC&A
Approved by
Plant head
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QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS
Protocol No. : xxxxxxxxxxxxxxxxx Rev. :00 Supersedes: NIL Protocol prepared on: xxxxxxxxxx Effective Date: xxxxxxxxxxxxx Page 16 of 38
______ minutes
_______ minutes
______ minutes
(Top , Middle & Bottom)
(Top , Middle & Bottom)
(Top , Middle & Bottom)
Total samples: 9 Samples
SAMPLING POINT FOR LUBRICATION (BLANDING) STAGE: Name of Blender: (DOUBLE CONE BLENDER) T2
Loading Valve Sampling
Points B3 B2
T3 Prepared By T2 Designation
QA chemist
Date Format No.: xxxxxxxxxxxxxx
T1
Reviewed by
Production Manager
Manager QC&A
Approved by
Plant head
xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx
QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS
Protocol No. : xxxxxxxxxxxxxxxxx Rev. :00 Supersedes: NIL Protocol prepared on: xxxxxxxxxx Effective Date: xxxxxxxxxxxxx Page 17 of 38
M T4 T 1
B4 B2
T3
T1
B1
B3 B1
Sampling points T1, T2, T3 for top T4 B4 for middle, B1, B2, B3 for bottom sampling.
Prepared By
Designation
QA chemist
Date Format No.: xxxxxxxxxxxxxx
Reviewed by
Production Manager
Manager QC&A
Approved by
Plant head
xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx
QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS
Protocol No. : xxxxxxxxxxxxxxxxx Rev. :00 Supersedes: NIL Protocol prepared on: xxxxxxxxxx Effective Date: xxxxxxxxxxxxx Page 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
_______ minutes
______ minutes
(Top , Middle & Bottom)
(Top , Middle & Bottom)
(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
Designation
QA chemist
Date Format No.: xxxxxxxxxxxxxx
Reviewed by
Production Manager
Manager QC&A
Approved by
Plant head
xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx
QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS
Protocol No. : xxxxxxxxxxxxxxxxx Rev. :00 Supersedes: NIL Protocol prepared on: xxxxxxxxxx Effective Date: xxxxxxxxxxxxx Page 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
Acceptance Criteria
(Size, Location & Time) Variation between the results of Assay shall not be more than 2%
Premixing Stage Mixing Drying Mixing Lubrication
Loss on drying Between 2.0 to 4.0%
Tablet compression Tablet coating Tablet packing
Variation between the results of assay shall not be more than 2% Physical Parameter (I.P.Q.C) Weight Gain Leak Test
Recording of data & Data treatment: Data Recording: Prepared By
Designation
QA chemist
Date Format No.: xxxxxxxxxxxxxx
Reviewed by
Production Manager
Manager QC&A
Approved by
Plant head
xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx
QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS
Protocol No. : xxxxxxxxxxxxxxxxx Rev. :00 Supersedes: NIL Protocol prepared on: xxxxxxxxxx Effective Date: xxxxxxxxxxxxx Page 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
Designation
QA chemist
Date Format No.: xxxxxxxxxxxxxx
Reviewed by
Production Manager
Manager QC&A
Approved by
Plant head
xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx
QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS
Protocol No. : xxxxxxxxxxxxxxxxx Rev. :00 Supersedes: NIL Protocol prepared on: xxxxxxxxxx Effective Date: xxxxxxxxxxxxx Page 21 of 38
Data recording sheet no I Date
Mixing Stage: Equipment name
:
Identification no
:
Ingredients and sequence of material addition
:
RPM of Mixer Blade
:
Capacity
:
Mixing time
:
Standard Weight of Tablet
:
Minutes
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
Designation
QA chemist
Date Format No.: xxxxxxxxxxxxxx
Reviewed by
Production Manager
Manager QC&A
Approved by
Plant head
xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx
QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS
Protocol No. : xxxxxxxxxxxxxxxxx Rev. :00 Supersedes: NIL Protocol prepared on: xxxxxxxxxx Effective Date: xxxxxxxxxxxxx Page 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: _________________________
Prepared By
Designation
QA chemist
Date Format No.: xxxxxxxxxxxxxx
Date: ____________________
Reviewed by
Production Manager
Manager QC&A
Approved by
Plant head
xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx
QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS
Protocol No. : xxxxxxxxxxxxxxxxx Rev. :00 Supersedes: NIL Protocol prepared on: xxxxxxxxxx Effective Date: xxxxxxxxxxxxx Page 23 of 38
Data recording sheet no II Date
Loss on Drying Stage: Equipment name
:
Dryer outlet temperature
:
Dryer inlet temperature
:
Drying Load
:
Total Drying time
:
Weight of the dried granules
:
Minutes
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: _________________________
Prepared By
Designation
QA chemist
Date Format No.: xxxxxxxxxxxxxx
Date: ____________________
Reviewed by
Production Manager
Manager QC&A
Approved by
Plant head
xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx
QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS
Protocol No. : xxxxxxxxxxxxxxxxx Rev. :00 Supersedes: NIL Protocol prepared on: xxxxxxxxxx Effective Date: xxxxxxxxxxxxx Page 24 of 38
Data recording sheet III Date
Lubrication Stage: Equipment name
:
Identification no
:
Capacity
:
Occupancy
:
Speed of equipment
:
Mixing time
:
Standard Weight of Tablet
:
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
Results
Top Middle Bottom
Prepared By
Designation
QA chemist
Date Format No.: xxxxxxxxxxxxxx
Reviewed by
Production Manager
Manager QC&A
Approved by
Plant head
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QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS
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Mean 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 Prepared By
Designation
QA chemist
Date Format No.: xxxxxxxxxxxxxx
Reviewed by
Production Manager
Manager QC&A
Approved by
Plant head
xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx
QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS
Protocol No. : xxxxxxxxxxxxxxxxx Rev. :00 Supersedes: NIL Protocol prepared on: xxxxxxxxxx Effective Date: xxxxxxxxxxxxx Page 26 of 38
Standard Deviation % Relative standard deviation
Remarks:
Checked By: _________________________
Date: ____________________
Data recording sheet IV Date
Compression Stage ________ Station compression machine Prepared By
Designation
QA chemist
Date Format No.: xxxxxxxxxxxxxx
: Reviewed by
Production Manager
Manager QC&A
Approved by
Plant head
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QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS
Protocol No. : xxxxxxxxxxxxxxxxx Rev. :00 Supersedes: NIL Protocol prepared on: xxxxxxxxxx Effective Date: xxxxxxxxxxxxx Page 27 of 38
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)
:
13 to 28 RPM
NMT 15 minutes
NMT 1.0%
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
Designation
QA chemist
Date Format No.: xxxxxxxxxxxxxx
Reviewed by
Production Manager
Manager QC&A
Approved by
Plant head
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QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS
Average weight Thickness mm Hardness in kg./sq. cm2 Friability in % DT in min. Weight variation after validated RPM __________
Time
Average Weight
Weight variation: Time
Thickness
Time
Prepared By
Designation
QA chemist
Date Format No.: xxxxxxxxxxxxxx
Hardness
Time
Friability
Time
Reviewed by
Production Manager
Manager QC&A
Disintegration
Time
Approved by
Plant head
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QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS
Protocol No. : xxxxxxxxxxxxxxxxx Rev. :00 Supersedes: NIL Protocol prepared on: xxxxxxxxxx Effective Date: xxxxxxxxxxxxx Page 29 of 38
Remarks:
Checked By: _________________________
Date: ____________________
Data recording sheet V Date
Coating Stage Name of equipment
:
Identification no
:
Capacity
: Prepared By
Designation
QA chemist
Date Format No.: xxxxxxxxxxxxxx
Reviewed by
Production Manager
Manager QC&A
Approved by
Plant head
xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx
QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS
Protocol No. : xxxxxxxxxxxxxxxxx Rev. :00 Supersedes: NIL Protocol prepared on: xxxxxxxxxx Effective Date: xxxxxxxxxxxxx Page 30 of 38
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)
:
Not more than
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
Prepared By
Designation
QA chemist
Date Format No.: xxxxxxxxxxxxxx
Average weight
Final weight
Average weight
% Weight gain
Reviewed by
Production Manager
Manager QC&A
DT in min.
Approved by
Plant head
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QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS
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Weight variation: Time Weight variation
Remark: Checked By: _________________________
Prepared By
Designation
QA chemist
Date Format No.: xxxxxxxxxxxxxx
Date: ____________________
Reviewed by
Production Manager
Manager QC&A
Approved by
Plant head
xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx
QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS
Protocol No. : xxxxxxxxxxxxxxxxx Rev. :00 Supersedes: NIL Protocol prepared on: xxxxxxxxxx Effective Date: xxxxxxxxxxxxx Page 32 of 38
Data recording sheet VI Date
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
Prepared By
Designation
QA chemist
Date Format No.: xxxxxxxxxxxxxx
Leak Test No of strips to be taken
Results
Reviewed by
Production Manager
Manager QC&A
Remarks
Approved by
Plant head
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QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS
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Data recording sheet VII Analysis Report Product Name: Batch No.: Mfg. Date:
Batch size: Exp. Date: Composition:
Test method reference: In house Sr. No. Test 01
Specification
Results
Remark
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
Designation
QA chemist
Date Format No.: xxxxxxxxxxxxxx
Reviewed by
Production Manager
Manager QC&A
Approved by
Plant head
xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx
QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS
Sr
Name of critical equipment / Utilities
No
Protocol No. : xxxxxxxxxxxxxxxxx Rev. :00 Supersedes: NIL Protocol prepared on: xxxxxxxxxx Effective Date: xxxxxxxxxxxxx Page 34 of 38
Qualification /
Date of Qualification /
Validation file
Validation
reference No 1 2 3 4 5 6 7 8 9 10 11 12 13 14 Sr No 15
Name of critical equipment / Utilities
Prepared By
Designation
QA chemist
Date Format No.: xxxxxxxxxxxxxx
Qualification / Validation file reference No
Reviewed by
Production Manager
Manager QC&A
Date of Qualification / Validation
Approved by
Plant head
xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx
QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS
Protocol No. : xxxxxxxxxxxxxxxxx Rev. :00 Supersedes: NIL Protocol prepared on: xxxxxxxxxx Effective Date: xxxxxxxxxxxxx Page 35 of 38
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
Data recording sheet IX
Prepared By
Designation
QA chemist
Date Format No.: xxxxxxxxxxxxxx
Reviewed by
Production Manager
Manager QC&A
Approved by
Plant head
xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx
QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS
Protocol No. : xxxxxxxxxxxxxxxxx Rev. :00 Supersedes: NIL Protocol prepared on: xxxxxxxxxx Effective Date: xxxxxxxxxxxxx Page 36 of 38
Remark: Analytical Method Validation protocol attached
Prepared By
Designation
QA chemist
Date Format No.: xxxxxxxxxxxxxx
Reviewed by
Production Manager
Manager QC&A
Approved by
Plant head
xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx
QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS
Protocol No. : xxxxxxxxxxxxxxxxx Rev. :00 Supersedes: NIL Protocol prepared on: xxxxxxxxxx Effective Date: xxxxxxxxxxxxx Page 37 of 38
Conclusion Sr. No.
Stage
Acceptance criteria
Observation
1.
Sifting
No visible foreign particulate matter is observed
2.
Premixing
Variation between the results shall not be more
Stage
than 2%
3.
Drying
Between 2.0 to 4.0%
4.
Lubrication
Variation between the results shall not be more than 2%
5.
Tablet
Average weight of tablets is within ± ____of std.
compression
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
Packed tablet shall meet the requirement for leak
packing
test
Conclusion: Product _________________________________ manufactured as per B.M.R. No _____________ meets predefined acceptance criteria. Analysis By
Approved By
Date
Date
Prepared By
Designation
QA chemist
Date Format No.: xxxxxxxxxxxxxx
Reviewed by
Production Manager
Manager QC&A
Approved by
Plant head
xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx
QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS
Protocol No. : xxxxxxxxxxxxxxxxx Rev. :00 Supersedes: NIL Protocol prepared on: xxxxxxxxxx Effective Date: xxxxxxxxxxxxx Page 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
Designation
QA chemist
Date Format No.: xxxxxxxxxxxxxx
Reviewed by
Production Manager
Manager QC&A
Approved by
Plant head
