xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx

Protocol No. : xxxxxxxxxxxxxxxxx

Rev. :00
QUALITY ASSURANCE Supersedes: NIL
PROCESS VALIDATION PROTOCOL Protocol prepared on: xxxxxxxxxx
FOR TABLETS Effective Date: xxxxxxxxxxxxx
Page 1 of 37

PROCESS
VALIDATION
PROTOCOL FOR TABLETS

Protocol No. : xxxxxxxx

Effective Date. : xxxxxxxxxxxx

Prepared By Reviewed by Approved by

Designation QA chemist Production Manager Manager QC&A Plant head

Date
Format No.: xxxxxxxxxxxxxx
 xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx

Protocol No. : xxxxxxxxxxxxxxxxx

Rev. :00
QUALITY ASSURANCE Supersedes: NIL
PROCESS VALIDATION PROTOCOL Protocol prepared on: xxxxxxxxxx
FOR TABLETS Effective Date: xxxxxxxxxxxxx
Page 2 of 37

TABLE OF CONTENTS

Page
S.NO. SECTION
No
1. Protocol approval

2. Purpose

3. Responsibilities

4. Requirements

5. Personnel Responsibilities

6. Validation parameters

7. Limits

8. Conclusion report

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Date
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 xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx

Protocol No. : xxxxxxxxxxxxxxxxx

Rev. :00
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PROCESS VALIDATION PROTOCOL Protocol prepared on: xxxxxxxxxx
FOR TABLETS Effective Date: xxxxxxxxxxxxx
Page 3 of 37

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

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Date
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 xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx

Protocol No. : xxxxxxxxxxxxxxxxx

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PROCESS VALIDATION PROTOCOL Protocol prepared on: xxxxxxxxxx
FOR TABLETS Effective Date: xxxxxxxxxxxxx
Page 4 of 37

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.

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Date
Format No.: xxxxxxxxxxxxxx
 xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx

Protocol No. : xxxxxxxxxxxxxxxxx

Rev. :00
QUALITY ASSURANCE Supersedes: NIL
PROCESS VALIDATION PROTOCOL Protocol prepared on: xxxxxxxxxx
FOR TABLETS Effective Date: xxxxxxxxxxxxx
Page 5 of 37

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
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
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 xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx

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Page 6 of 37

6 Tablet coating
7 Tablet packing

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

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Date
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 xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx

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Page 7 of 37

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

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

Coating Compression Lubrication

(Blending)

Tablet packing

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 xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx

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Page 8 of 37

Sampling point

Typical Variables and responses: Granulated Product

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Page 9 of 37

S. No. Process step Control variables Measured responses

1. Pre-blending Blending time Blend uniformity
RPM
Load size
Order of addition
2. Granulating Load size Density
Amount of granulating agent Yield
Solvent addition rate
RPM
Granulation time
3. Drying Initial temperature Density
Load size Moisture content
Drying temperature program Yield
Air flow program
Drying time
Cooling time
4. Sizing Screen type Granule size distribution
Screen size Loose drying
Feed rate Packed density
5. Blending Load size Blend uniformity
RPM Flow characteristics
Blending time Particle size distribution
6. Tableting Compression rate Weight variation
Granule feed rate Friability
Pre-compression force Hardness
Compression force Thickness
Disintegration time
Dissolution
Dosage from uniformity
Equipments

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Date
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 xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx

Protocol No. : xxxxxxxxxxxxxxxxx

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PROCESS VALIDATION PROTOCOL Protocol prepared on: xxxxxxxxxx
FOR TABLETS Effective Date: xxxxxxxxxxxxx
Page 10 of 37

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

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

Sr. No. Name of Equipment Equipment ID. Qualification details SOP No
1
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 Parameters

1. Premixing RPM of mixer blade
Load size
Total time of mixing
Uniform mixing by Assay analysis
2. Granulation Mixer blade speed
Load size

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 xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx

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Page 11 of 37

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
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
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 xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx

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Page 12 of 37

7. Coating Temperature of area

Temperature of blower
Speed of Coating Pan (RPM)
Spray Rate
Bed Temperature
Air Pressure
Total Coating solution used
Weight Built up
Weight variation of 20 tablets
Assay
Disintegration time
Dissolution
8. Packaging Forming roller temperature. (for Blister Packing)
Sealing roller temperature
Sealing roller Pressure
Speed of machine
Seal integrity
Assay
Dissolution
9. Packaging (bulk Sealing temperature
packing)
Seal integrity
Counter Checking from 10 Jars at different Time intervals

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

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 xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx

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Page 13 of 37

Sifting No visible foreign particulate

Visually Inspection
matter is observed
Premixing Stage
Variation between the results
Uniform mixing by Assay analysis
shall not be more than 2%
Granulation
Binder Preparation
Granulation Finely divided material without free
powder and excessive wetted lumps.
4 Wet milling Material was finely divided
Drying Loss on drying Between 2.0 to 5.0%
Dry milling Finely divided granules are observed
Lubrication Variation between the results
Assay and Sieve analysis
shall not be more than 2%
Wt. Variation, Hardness,
5 Tablet compression Physical Parameter Thickness, DT, Dissolution
and Assay
Weight gain, weight variation
6 Tablet coating
and DT
7 Tablet packing Leak Test

PREMIXING:

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Page 14 of 37

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

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:

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Page 15 of 37

Sampling point for drying stage:

T2
Top View Sampling
Top B2

B3
TOP VIEW

T1 T3

B1
Front side Bottom

----- Sampling Points

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

Sampling Time: - (bracketing the time between 2 to 3 intervals of total mixing time)
While Drying is on: -
After ____ minutes,
After ___ minutes,
After _____ minutes

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 xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx

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Page 16 of 37

______ 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

______ minutes _______ minutes ______ minutes

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

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Date
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 xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx

Protocol No. : xxxxxxxxxxxxxxxxx

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FOR TABLETS Effective Date: xxxxxxxxxxxxx
Page 17 of 37

SAMPLING POINT FOR LUBRICATION (BLANDING) STAGE:

Name of Blender: (DOUBLE CONE BLENDER)

T2
Loading Valve
Sampling Points
B3
B3
B2

T3

T2 T1
M

T4 T3
T1

T
1 B1
B4
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 xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx

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Page 18 of 37

B2 B3

B1

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

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 xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx

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Page 19 of 37

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

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Date
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 xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx

Protocol No. : xxxxxxxxxxxxxxxxx

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PROCESS VALIDATION PROTOCOL Protocol prepared on: xxxxxxxxxx
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Page 20 of 37

COATING:
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)
Premixing Stage Variation between the results of Assay shall
not be more than 2%
Mixing
Drying Loss on drying Between 2.0 to 4.0%
Mixing
Lubrication Variation between the results of assay shall
not be more than 2%
Tablet compression Physical Parameter (I.P.Q.C)
Tablet coating Weight Gain
Tablet packing Leak Test

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Date
Format No.: xxxxxxxxxxxxxx
 xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx

Protocol No. : xxxxxxxxxxxxxxxxx

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PROCESS VALIDATION PROTOCOL Protocol prepared on: xxxxxxxxxx
FOR TABLETS Effective Date: xxxxxxxxxxxxx
Page 21 of 37

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.

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.

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 xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx

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Page 22 of 37

Data recording sheet no I

Mixing Stage: Date
Equipment name :
Identification no :
Ingredients and sequence of material addition :
RPM of Mixer Blade :
Capacity :
Mixing time : Minutes
Standard Weight of Tablet :
Method reference: As per assay procedure given in finished product specification.
Blended material to be analyzed for ______________________________
Plan: Samples to be drawn of mixing from 3 different locations (Top, Middle & Bottom)
Result after mixing _________________ minutes
Sampling Detail Results
Top
Middle
Bottom

Mean
Standard Deviation
% Relative standard deviation

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 xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx

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Page 23 of 37

Result after mixing _________________ minutes

Sampling Detail Results
Top
Middle
Bottom

Mean
Standard Deviation
% Relative standard deviation

Result after mixing _________________ minutes

Sampling Detail Results
Top
Middle
Bottom

Mean
Standard Deviation
% Relative standard deviation

Analyst: Date
Remarks:
Checked By: _________________________ Date: ____________________

Data recording sheet no II

Loss on Drying Stage: Date
Equipment name :
Dryer outlet temperature :
Dryer inlet temperature :
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Page 24 of 37

Drying Load :
Total Drying time : Minutes
Weight of the dried granules :

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

Plan: Material to be analyzed for Loss on drying

Samples to be drawn from 3 different locations

Sample East West North South Average Limit

Weight taken
% LOD

Remarks:

Checked By: _________________________ Date: ____________________

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 xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx

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Page 25 of 37

Data recording sheet III

Lubrication Stage: Date
Equipment name :
Identification no :
Capacity :
Occupancy :
Speed of equipment :
Mixing time : Minutes
Standard Weight of Tablet :

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

Lubricated material to be analyzed for % of active content ______________________________

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

Result after mixing _________________ minutes

Sampling Detail Results
Top
Middle
Bottom

Mean
Standard Deviation
% Relative standard deviation
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 xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx

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Page 26 of 37

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

Remarks:

Checked By: _________________________ Date: ____________________

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Date
Format No.: xxxxxxxxxxxxxx
 xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx

Protocol No. : xxxxxxxxxxxxxxxxx

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PROCESS VALIDATION PROTOCOL Protocol prepared on: xxxxxxxxxx
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Page 27 of 37

Data recording sheet IV

Compression Stage Date
________ Station compression machine :
Identification no :
Capacity :
RPM : 13 to 28 RPM
Punch Size :
Temperature of area :
Humidity of area :
Weight of 20 Tablets :
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 xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx

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Page 28 of 37

Average Weight of tablet :

Disintegration Time : NMT 15 minutes
Dissolution (If required) :
Friability : NMT 1.0%
Thickness :
Hardness :
Assay :
Content of uniformity (If required) :
Method reference: As per In-process check procedure.

Plan: Compressed tablets to be analyzed for: Average weight, Weight variation and Physical parameter
at an interval of 2 hours
Requirement RPM: RPM: RPM:
Time
Average weight
Thickness mm
Hardness in kg./sq. cm2
Friability in %
DT in min.
Weight variation after validated RPM __________

Time Average Weight Thickness Hardness Friability Disintegration

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 xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx

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Page 29 of 37

Weight variation:
Time Time Time Time Time

Remarks:

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 xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx

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Page 30 of 37

Checked By: _________________________ Date: ____________________

Data recording sheet V

Coating Stage Date
Name of equipment :
Identification no :
Capacity :
Speed of coating pan :
Temperature of area :
Temperature of blower :
Spray rate :
Bed temperature :
Air Pressure :
Total coating solution used :
Weight build up :
Weight of 20 Tablets :
Average Weight of tablet :
Disintegration Time : Not more than
Dissolution (If required) :
Assay

Method reference: As per In-process check procedure.

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 xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx

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Page 31 of 37

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

Date Time Initial Average Final Average % Weight gain DT in min.

weight weight weight weight

Weight variation:

Time
Weight variation

Remark:

Checked By: _________________________ Date: ____________________

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 xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx

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Page 32 of 37

Data recording sheet VI

Packing Stage Date
Name of equipment :
Identification no :
Capacity :
Forming roller temperature (For blister packing) :
Sealing roller temperature :
Sealing roller pressure :
Speed of machine :
Seal integrity (Leak test) :

Method reference: As per In-process check procedure.

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

Date Time Leak Test Results Remarks

No of strips to be
taken

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 xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx

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Page 33 of 37

Data recording sheet VII

Analysis Report
Product Name:
Batch No.: Batch size:
Mfg. Date: Exp. Date:
Composition:
Test method reference: In house
Sr. No. Test Specification Results Remark
01 Description
02
03
04
05
5.1

5.2

5.3

5.4

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

Data recording sheet VIII

Sr Name of critical equipment / Utilities Qualification / Date of Qualification /

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 xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx

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Page 34 of 37

No Validation file Validation

reference No
1
2
3
4
5
6
7
8
9
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11
12
13
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Sr Name of critical equipment / Utilities Qualification / Validation Date of Qualification /
No file reference No Validation
15
16
17
18
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21
22
23
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25
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27
Prepared By Reviewed by Approved by

Designation QA chemist Production Manager Manager QC&A Plant head

Date
Format No.: xxxxxxxxxxxxxx
 xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx

Protocol No. : xxxxxxxxxxxxxxxxx

Rev. :00
QUALITY ASSURANCE Supersedes: NIL
PROCESS VALIDATION PROTOCOL Protocol prepared on: xxxxxxxxxx
FOR TABLETS Effective Date: xxxxxxxxxxxxx
Page 35 of 37

28
Utilities:
1 AHU System
2 Water System
3 Compressed Air
4 Steam
5 Lightning
6 Drain

Data recording sheet IX

Remark:
Analytical Method Validation protocol attached

Prepared By Reviewed by Approved by

Designation QA chemist Production Manager Manager QC&A Plant head

Date
Format No.: xxxxxxxxxxxxxx
 xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx

Protocol No. : xxxxxxxxxxxxxxxxx

Rev. :00
QUALITY ASSURANCE Supersedes: NIL
PROCESS VALIDATION PROTOCOL Protocol prepared on: xxxxxxxxxx
FOR TABLETS Effective Date: xxxxxxxxxxxxx
Page 36 of 37

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

7. LIMITS: As pre relative STPs

Prepared By Reviewed by Approved by

Designation QA chemist Production Manager Manager QC&A Plant head

Date
Format No.: xxxxxxxxxxxxxx
 xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx

Protocol No. : xxxxxxxxxxxxxxxxx

Rev. :00
QUALITY ASSURANCE Supersedes: NIL
PROCESS VALIDATION PROTOCOL Protocol prepared on: xxxxxxxxxx
FOR TABLETS Effective Date: xxxxxxxxxxxxx
Page 37 of 37

8. CONCLUSION REPORT

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

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

Prepared By Reviewed by Approved by

Designation QA chemist Production Manager Manager QC&A Plant head

Date
Format No.: xxxxxxxxxxxxxx