Tablet Process Validation 2d3e5z
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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 33
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 33
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
1. PROTOCOL APPROVAL 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 33
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
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
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 4 of 33
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: 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
Protocol No. : xxxxxxxxxxxxxxxxx Rev. :00 Supersedes: NIL Protocol prepared on: xxxxxxxxxx Effective Date: xxxxxxxxxxxxx Page 5 of 33
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 1 2 3 4 5 6 7
Ingredients/Excipients
Unit per Tablet
Prepared By
Designation QA chemist Date Format No.: xxxxxxxxxxxxxx
Std. Qty.
Overages Dispensed Quantity
Weight by
Reviewed by
Production Manager
Manager QC&A
Checked by
Approved by
Plant head
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QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS
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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
Dry Granulation
Premixing Mixing
Binder preparation
Wet Granulation milling
Drying Dry milling
Slugging, Milling (if required)
Mixing
Prepared By
Coating
Designation QA chemist Date Format No.: xxxxxxxxxxxxxx
Reviewed by
Compression
Production Manager
Lubrication
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 7 of 33 (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
S. No. 1.
Process step Pre-blending
2.
Granulating
3.
Drying
4.
Sizing
5.
Blending
6.
Tableting
Protocol No. : xxxxxxxxxxxxxxxxx Rev. :00 Supersedes: NIL Protocol prepared on: xxxxxxxxxx Effective Date: xxxxxxxxxxxxx Page 8 of 33
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 by List of SOP’S, Validation &By Qualification report usedReviewed as references Designation QA chemist Date Format No.: xxxxxxxxxxxxxx
Production Manager
Manager QC&A
Approved by
Plant head
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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
Protocol No. : xxxxxxxxxxxxxxxxx Rev. :00 Supersedes: NIL Protocol prepared on: xxxxxxxxxx Effective Date: xxxxxxxxxxxxx Page 9 of 33
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. 1.
STAGE Premixing
2.
Granulation
3.
Drying Prepared By
Designation QA chemist Date Format No.: xxxxxxxxxxxxxx
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
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QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS
4.
Milling
5.
Lubrication
6.
Compression
7.
Coating
8.
Packaging Prepared By
Designation QA chemist Date Format No.: xxxxxxxxxxxxxx
Protocol No. : xxxxxxxxxxxxxxxxx Rev. :00 Supersedes: NIL Protocol prepared on: xxxxxxxxxx Effective Date: xxxxxxxxxxxxx Page 10 of 33
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
Production Manager
Manager QC&A
Plant head
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QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS
9.
Packaging (bulk
Protocol No. : xxxxxxxxxxxxxxxxx Rev. :00 Supersedes: NIL Protocol prepared on: xxxxxxxxxx Effective Date: xxxxxxxxxxxxx Page 11 of 33
Speed of machine Seal integrity Assay Dissolution Sealing temperature
packing) Seal integrity Counter Checking from 10 Jars at different Time intervals
Sr. No
Process / Variable Blend Manufacturing Sifting
1
4
Machine setting ( Control Variables) Visually Inspection
No visible foreign particulate matter is observed
Uniform mixing by Assay analysis
Variation between the results shall not be more than 2%
Premixing Stage Granulation Binder Preparation Granulation Wet milling Prepared By
Designation QA chemist Date Format No.: xxxxxxxxxxxxxx
Remarks
Finely divided material without free powder and excessive wetted lumps. Material was finelyReviewed divided 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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Drying Dry milling Lubrication
Loss on drying Finely divided granules are observed
5
Tablet compression
Physical Parameter
6
Tablet coating
7
Tablet packing
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
Assay and Sieve analysis
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
_______ minutes
______ minutes
(Top , Middle & Bottom) Total samples: 9 Samples
(Top , Middle & Bottom)
(Top , Middle & Bottom)
MIXING: Sampling Qty.: -Depends on quantity required for analysis. Prepared By Reviewed by
Designation QA chemist Date Format No.: xxxxxxxxxxxxxx
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 13 of 33
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) Total samples: 9 Samples
(Top , Middle & Bottom)
(Top , Middle & Bottom)
DRYING: Sampling point for drying stage: T2
Top View Sampling Top
B2
TOP VIEW
B3
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) By Reviewed by While Drying is on: Prepared Designation QA chemist Date Format No.: xxxxxxxxxxxxxx
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 14 of 33
After ____ minutes, After ___ minutes, After _____ minutes ______ minutes
_______ minutes
______ minutes
(Top , Middle & Bottom) Total samples: 9 Samples MILLING:
(Top , Middle & Bottom)
(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
_______ minutes
______ minutes
(Top , Middle & Bottom) Total samples: 9 Samples
(Top , Middle & Bottom)
(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
Protocol No. : xxxxxxxxxxxxxxxxx Rev. :00 Supersedes: NIL Protocol prepared on: xxxxxxxxxx Effective Date: xxxxxxxxxxxxx Page 15 of 33
SAMPLING POINT FOR LUBRICATION (BLANDING) STAGE: Name of Blender: (DOUBLE CONE BLENDER) T2
Loading Valve Sampling Points
B3
B3 B2 T3 T1
T2
M T4
B2
T3
T1 T 1
B4 B3
B1
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
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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 33
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) Total samples: 9 Samples
(Top , Middle & Bottom)
(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: Sampling Qty.: -Depends on quantity required for analysis. Sampling Time: - (Bracketing the time between 2 to 3 intervals of total coating time) By Reviewed by While coating is on:Prepared Designation QA chemist Date Format No.: xxxxxxxxxxxxxx
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 17 of 33
After ____ minutes, After ___ minutes, After _____ minutes ______ minutes
_______ minutes
______ minutes
Total samples: 3 Samples Sampling: Stage / Test Parameter
Equipment
Acceptance Criteria
(Size, Location & Time) Premixing Stage
Variation between the results of Assay shall not be more than 2%
Mixing Drying Mixing Lubrication
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
Tablet compression Tablet coating Tablet packing
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
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 18 of 33
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
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 19 of 33
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
Results
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
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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 20 of 33
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 Standard Deviation % Relative standard deviation Analyst: Remarks:
Date
Checked By: _________________________
Date: ____________________
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
Prepared By procedure by IR moisture Reviewed by Method reference: Loss on drying balance. Designation QA chemist Date Format No.: xxxxxxxxxxxxxx
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 21 of 33
Plan: Material to be analyzed for Loss on drying Samples to be drawn from 3 different locations Sample
Ea
W
No
So
st
est
rth
ut
Average
Limit
h 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
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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 22 of 33
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
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 23 of 33
Sampling Detail Top Middle Bottom
Results
Mean Standard Deviation % Relative standard deviation Result after mixing _________________ minutes Sampling Detail Top Middle Bottom
Results
Mean Standard Deviation % Relative standard deviation Remarks: Checked By: _________________________
Prepared By
Designation QA chemist Date Format No.: xxxxxxxxxxxxxx
Date: ____________________
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 24 of 33
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.
Prepared By
Designation QA chemist Date Format No.: xxxxxxxxxxxxxx
Date : : : : : : : : : : : : : : : :
13 to 28 RPM
NMT 15 minutes NMT 1.0%
Reviewed by
Production Manager
Manager QC&A
Approved by
Plant head
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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
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
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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 Weight of 20 TabletsPrepared By
Designation QA chemist Date Format No.: xxxxxxxxxxxxxx
Date : : : : : : : : : : : : 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 33
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.
Weight variation: Time Weight variation Remark: Checked By: _________________________ Prepared By
Designation QA chemist Date Format No.: xxxxxxxxxxxxxx
Date: ____________________ Reviewed by Approved by
Production Manager
Manager QC&A
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 28 of 33
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
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
Protocol No. : xxxxxxxxxxxxxxxxx Rev. :00 Supersedes: NIL Protocol prepared on: xxxxxxxxxx Effective Date: xxxxxxxxxxxxx Page 29 of 33
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 Description
Specification
Results
Remark
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
Name of critical equipment / Utilities
No
Qualification /
Date of Qualification /
Validation file
Validation
reference No 1 2 3
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
4 5 6 7 8 9 10 11 12 13 14 Sr No 15
Name of critical equipment / Utilities
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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
Designation QA chemist Date Format No.: xxxxxxxxxxxxxx
Data recording Reviewed sheet IX 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 31 of 33
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
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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 32 of 33
Conclusion Sr. No. 1. 2.
Stage Sifting Premixing
Acceptance criteria No visible foreign particulate matter is observed Variation between the results shall not be more
3. 4.
Stage Drying Lubrication
than 2% Between 2.0 to 4.0% Variation between the results shall not be more
5.
Tablet
than 2% Average weight of tablets is within ± ____of std.
compression
weight.
Observation
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
packing Conclusion:
Coated tablets shall meet FP Specification Packed tablet shall meet the requirement for leak test
Product _________________________________ manufactured as per B.M.R. No _____________ meets predefined acceptance criteria.
7.
Analysis By
Approved By
Date
Date
LIMITS: As pre relative STPs 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
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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
QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS
Protocol No. : xxxxxxxxxxxxxxxxx Rev. :00 Supersedes: NIL Protocol prepared on: xxxxxxxxxx Effective Date: xxxxxxxxxxxxx Page 1 of 33
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 33
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
1. PROTOCOL APPROVAL 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 3 of 33
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
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
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 33
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: 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
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 33
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 1 2 3 4 5 6 7
Ingredients/Excipients
Unit per Tablet
Prepared By
Designation QA chemist Date Format No.: xxxxxxxxxxxxxx
Std. Qty.
Overages Dispensed Quantity
Weight by
Reviewed by
Production Manager
Manager QC&A
Checked by
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 6 of 33
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
Dry Granulation
Premixing Mixing
Binder preparation
Wet Granulation milling
Drying Dry milling
Slugging, Milling (if required)
Mixing
Prepared By
Coating
Designation QA chemist Date Format No.: xxxxxxxxxxxxxx
Reviewed by
Compression
Production Manager
Lubrication
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 7 of 33 (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
xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx
QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS
S. No. 1.
Process step Pre-blending
2.
Granulating
3.
Drying
4.
Sizing
5.
Blending
6.
Tableting
Protocol No. : xxxxxxxxxxxxxxxxx Rev. :00 Supersedes: NIL Protocol prepared on: xxxxxxxxxx Effective Date: xxxxxxxxxxxxx Page 8 of 33
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 by List of SOP’S, Validation &By Qualification report usedReviewed as references Designation QA chemist Date Format No.: xxxxxxxxxxxxxx
Production Manager
Manager QC&A
Approved by
Plant head
xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx
QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS
Sr. No. 1 2 3 4 5 6 7 8 9 10 11 12
Name of Equipment
Protocol No. : xxxxxxxxxxxxxxxxx Rev. :00 Supersedes: NIL Protocol prepared on: xxxxxxxxxx Effective Date: xxxxxxxxxxxxx Page 9 of 33
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. 1.
STAGE Premixing
2.
Granulation
3.
Drying Prepared By
Designation QA chemist Date Format No.: xxxxxxxxxxxxxx
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
xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx
QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS
4.
Milling
5.
Lubrication
6.
Compression
7.
Coating
8.
Packaging Prepared By
Designation QA chemist Date Format No.: xxxxxxxxxxxxxx
Protocol No. : xxxxxxxxxxxxxxxxx Rev. :00 Supersedes: NIL Protocol prepared on: xxxxxxxxxx Effective Date: xxxxxxxxxxxxx Page 10 of 33
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
Production Manager
Manager QC&A
Plant head
xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx
QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS
9.
Packaging (bulk
Protocol No. : xxxxxxxxxxxxxxxxx Rev. :00 Supersedes: NIL Protocol prepared on: xxxxxxxxxx Effective Date: xxxxxxxxxxxxx Page 11 of 33
Speed of machine Seal integrity Assay Dissolution Sealing temperature
packing) Seal integrity Counter Checking from 10 Jars at different Time intervals
Sr. No
Process / Variable Blend Manufacturing Sifting
1
4
Machine setting ( Control Variables) Visually Inspection
No visible foreign particulate matter is observed
Uniform mixing by Assay analysis
Variation between the results shall not be more than 2%
Premixing Stage Granulation Binder Preparation Granulation Wet milling Prepared By
Designation QA chemist Date Format No.: xxxxxxxxxxxxxx
Remarks
Finely divided material without free powder and excessive wetted lumps. Material was finelyReviewed divided 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 12 of 33
Drying Dry milling Lubrication
Loss on drying Finely divided granules are observed
5
Tablet compression
Physical Parameter
6
Tablet coating
7
Tablet packing
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
Assay and Sieve analysis
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
_______ minutes
______ minutes
(Top , Middle & Bottom) Total samples: 9 Samples
(Top , Middle & Bottom)
(Top , Middle & Bottom)
MIXING: Sampling Qty.: -Depends on quantity required for analysis. Prepared By Reviewed by
Designation QA chemist Date Format No.: xxxxxxxxxxxxxx
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 13 of 33
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) Total samples: 9 Samples
(Top , Middle & Bottom)
(Top , Middle & Bottom)
DRYING: Sampling point for drying stage: T2
Top View Sampling Top
B2
TOP VIEW
B3
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) By Reviewed by While Drying is on: Prepared Designation QA chemist Date Format No.: xxxxxxxxxxxxxx
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 14 of 33
After ____ minutes, After ___ minutes, After _____ minutes ______ minutes
_______ minutes
______ minutes
(Top , Middle & Bottom) Total samples: 9 Samples MILLING:
(Top , Middle & Bottom)
(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
_______ minutes
______ minutes
(Top , Middle & Bottom) Total samples: 9 Samples
(Top , Middle & Bottom)
(Top , Middle & Bottom)
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 15 of 33
SAMPLING POINT FOR LUBRICATION (BLANDING) STAGE: Name of Blender: (DOUBLE CONE BLENDER) T2
Loading Valve Sampling Points
B3
B3 B2 T3 T1
T2
M T4
B2
T3
T1 T 1
B4 B3
B1
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 16 of 33
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) Total samples: 9 Samples
(Top , Middle & Bottom)
(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: Sampling Qty.: -Depends on quantity required for analysis. Sampling Time: - (Bracketing the time between 2 to 3 intervals of total coating time) By Reviewed by While coating is on:Prepared Designation QA chemist Date Format No.: xxxxxxxxxxxxxx
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 33
After ____ minutes, After ___ minutes, After _____ minutes ______ minutes
_______ minutes
______ minutes
Total samples: 3 Samples Sampling: Stage / Test Parameter
Equipment
Acceptance Criteria
(Size, Location & Time) Premixing Stage
Variation between the results of Assay shall not be more than 2%
Mixing Drying Mixing Lubrication
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
Tablet compression Tablet coating Tablet packing
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
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 33
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
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 33
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
Results
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 20 of 33
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 Standard Deviation % Relative standard deviation Analyst: Remarks:
Date
Checked By: _________________________
Date: ____________________
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
Prepared By procedure by IR moisture Reviewed by Method reference: Loss on drying balance. Designation QA chemist Date Format No.: xxxxxxxxxxxxxx
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 33
Plan: Material to be analyzed for Loss on drying Samples to be drawn from 3 different locations Sample
Ea
W
No
So
st
est
rth
ut
Average
Limit
h 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 22 of 33
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
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 23 of 33
Sampling Detail Top Middle Bottom
Results
Mean Standard Deviation % Relative standard deviation Result after mixing _________________ minutes Sampling Detail Top Middle Bottom
Results
Mean Standard Deviation % Relative standard deviation 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 33
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.
Prepared By
Designation QA chemist Date Format No.: xxxxxxxxxxxxxx
Date : : : : : : : : : : : : : : : :
13 to 28 RPM
NMT 15 minutes NMT 1.0%
Reviewed by
Production Manager
Manager QC&A
Approved by
Plant head
xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx Protocol No. : xxxxxxxxxxxxxxxxx Rev. :00 Supersedes: NIL Protocol prepared on: xxxxxxxxxx Effective Date: xxxxxxxxxxxxx Page 25 of 33
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
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
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 33
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 Weight of 20 TabletsPrepared 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 27 of 33
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.
Weight variation: Time Weight variation Remark: Checked By: _________________________ Prepared By
Designation QA chemist Date Format No.: xxxxxxxxxxxxxx
Date: ____________________ Reviewed by Approved by
Production Manager
Manager QC&A
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 28 of 33
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
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
xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx
QUALITY ASSURANCE PROCESS VALIDATION PROTOCOL FOR TABLETS
Protocol No. : xxxxxxxxxxxxxxxxx Rev. :00 Supersedes: NIL Protocol prepared on: xxxxxxxxxx Effective Date: xxxxxxxxxxxxx Page 29 of 33
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 Description
Specification
Results
Remark
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
Name of critical equipment / Utilities
No
Qualification /
Date of Qualification /
Validation file
Validation
reference No 1 2 3
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
4 5 6 7 8 9 10 11 12 13 14 Sr No 15
Name of critical equipment / Utilities
Protocol No. : xxxxxxxxxxxxxxxxx Rev. :00 Supersedes: NIL Protocol prepared on: xxxxxxxxxx Effective Date: xxxxxxxxxxxxx Page 30 of 33
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
Designation QA chemist Date Format No.: xxxxxxxxxxxxxx
Data recording Reviewed sheet IX 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 31 of 33
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 32 of 33
Conclusion Sr. No. 1. 2.
Stage Sifting Premixing
Acceptance criteria No visible foreign particulate matter is observed Variation between the results shall not be more
3. 4.
Stage Drying Lubrication
than 2% Between 2.0 to 4.0% Variation between the results shall not be more
5.
Tablet
than 2% Average weight of tablets is within ± ____of std.
compression
weight.
Observation
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
packing Conclusion:
Coated tablets shall meet FP Specification Packed tablet shall meet the requirement for leak test
Product _________________________________ manufactured as per B.M.R. No _____________ meets predefined acceptance criteria.
7.
Analysis By
Approved By
Date
Date
LIMITS: As pre relative STPs 8. CONCLUSION REPORT 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 33 of 33
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
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