Process Validation of Liquid
March 14, 2017 | Author: asit_m | Category: N/A
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its working document....
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XXXXXXXXXXXXXXXXXXXXXXX Protocol No.:
Process Validation Protocol for Oral liquid/Suspension
Quality Assurance Department
Page 1 of 24
Title : Validation Protocol for
B. No. :
Formulation: Oral Liquid Product’s Name: Reason for Performing the Validity Study: Reason ( tick which ever is applicable)
Remarks
Department New product Modification in the manufacturing process. Change in Facility and / or location of manufacturing. Batch fails to meet product & process specifications.
Number of batches studied: First Three Batches Batch numbers:
1.
2.
3.
Validation activity Approved by: _____________________________Date:_______________________ Validation Team: Department
Validation Team
Production
Quality Control
Quality Assurance
Approvals: Department
Sign & Date
Production Engineering Quality Control Quality Assurance
Prepared By
Checked By
Approved By
XXXXXXXXXXXXXXXXXXXXXXX Protocol No.:
Process Validation Protocol for Oral liquid/Suspension
Quality Assurance Department
Page 2 of 24
Title : Validation Protocol for
B. No. :
1.0 General: 1.1
Introduction: The process validation will be performed as prospective validation. The complete documentation for the validation comprises several independent documents; references to relevant documents will be given as part of this protocol, (see below). The results of the validation activities will be summarized in the validation report.
1.2
List of Documents for Validation: Validation protocol, Details of sampling for the validation batches, test parameters (Product performance characteristics) with reference to test methods & Acceptance criteria. (acceptable Limit) Methods for recording / evaluating results including statistical analysis. Reference to relevant documents.
1.2.2
Batch manufacturing records.
Detailed manufacturing instructions for the production of the validation batches. 2.0
Sr
Personnel Responsibilities:
Activity
Responsibility
Remarks
No 1
Preparation of validation protocol
QA Department
2
Review of validation report.
Q.A In charge
3
Production of validation Batches
Production In charge
4
Testing of validation samples &
Q.C In charge
Preparation of validation report 5
Approval of Validation protocol
Prepared By
Manager (Q.A)
Checked By
Approved By
XXXXXXXXXXXXXXXXXXXXXXX Protocol No.:
Process Validation Protocol for Oral liquid/Suspension
Quality Assurance Department
Page 3 of 24
Title : Validation Protocol for 3.0
B. No. :
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 manufacturing record.
1
DISPENSING OF MATERIAL
2
SUGAR SYRUP PREPARATION
3
BULK MANUFACTURING
4
PH ADJUSTMENT
5
VOLUME MAKE UP
6
FILTRATION
7
WASHING, FILLING AND SEALING
3.1
Formulation: Batch Size:
Sr No
Ingredients/Excipients
Unit per ml
Quantity in Kgs
Overages
Quantity with Overages
Dispensed Function Quantity
1 2 3 4 5
Prepared By
Checked By
Approved By
XXXXXXXXXXXXXXXXXXXXXXX Protocol No.:
Process Validation Protocol for Oral liquid/Suspension
Quality Assurance Department
Page 4 of 24
Title : Validation Protocol for
B. No. :
6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 Note:
Prepared By
Checked By
Approved By
XXXXXXXXXXXXXXXXXXXXXXX Protocol No.:
Process Validation Protocol for Oral liquid/Suspension
Quality Assurance Department
Page 5 of 24
Title : Validation Protocol for
B. No. :
3.2 FLOW SHEET: MANUFACTURING PROCESS DIAGRAM:- _________________syrup
Receipt and holding of materials
Dispensing Of Raw Material
Syrup Preparation Excipient and active addition
Colour & Flavour Materials
Bulk Preparation & Final Volume Make up
Final Mixing
Filtration Through Filter Press
Cleaning And Setting Of Filling, Sealing, Labeling Machine
Prepared By
Filling Of Bulk Into Bottles
Checked By
Inspection
Approved By
Testing
XXXXXXXXXXXXXXXXXXXXXXX Protocol No.:
Process Validation Protocol for Oral liquid/Suspension
Quality Assurance Department
Page 6 of 24
Title : Validation Protocol for
4.0
B. No. :
Equipments/ Factory
A detailed list of equipment used for validation together with the cleaning status will be provided in the manufacturing documents. 4.1
List of SOP’S, Validation & Qualification report used as references
SrNo 1
Equipment
Equipment No.
SOP No
2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23
Prepared By
Checked By
Approved By
XXXXXXXXXXXXXXXXXXXXXXX Protocol No.:
Process Validation Protocol for Oral liquid/Suspension
Quality Assurance Department
Page 7 of 24
Title : Validation Protocol for
B. No. :
4.2 Details of equipment to be used. Equipment S.S. Manufacturing Tank
Details Type : Model: Capacity: Manufacturer: Tag No. RPM M.O.C.
S.S. Storage Tank
Type : Model: Capacity: Manufacturer: Tag No. RPM M.O.C.
Filter Press
Type : Model: Capacity: Manufacturer: Tag No. Type of filter M.O.C.
Transfer Pump
Type : Model: Capacity: Manufacturer: Tag No.
Washing Machine
Prepared By
M.O.C. Type :
Checked By
Approved By
XXXXXXXXXXXXXXXXXXXXXXX Protocol No.:
Process Validation Protocol for Oral liquid/Suspension
Quality Assurance Department
Page 8 of 24
Title : Validation Protocol for
B. No. :
Model: Capacity: Manufacturer: Tag No. Speed M.O.C. Filling Machine
Type : Model: Capacity: Manufacturer: Tag No. Speed M.O.C.
Sealing Machine
Type : Model: Capacity: Manufacturer: Tag No. M.O.C.
Labeling Machine
Type : Model: Capacity: Manufacturer: Tag No. M.O.C.
Remarks:
Prepared By
Checked By
Approved By
XXXXXXXXXXXXXXXXXXXXXXX Protocol No.:
Process Validation Protocol for Oral liquid/Suspension
Quality Assurance Department
Page 9 of 24
Title : Validation Protocol for 4.3
B. No. :
Identification of Critical process variables parameter.
4.3.1 Probable causes that may effect final product: DISPENSING OF MATERIAL
SUGAR SYRUP PREPARATION
ADDITION OF ACTIVE
WASHING, FILLING & SEALING
ADDITION OF FLAVOUR & COLOUR
LOAD SIZE SPEED
FINAL WASH
ACTIVE
STIRRER
CLARITY
PH & TEMP. R.P.M.
EXCIPIENT
VOLUME
MIXING TIME
LEAKAGE SEALING & THRADING
CLARITY MIXING TIME
R.P.M.
R.P.M.
DIP STICK
T E M P.
ADDITION OF EXCIPEINT
Prepared By
PH
MIXING TIME
SCREEN SIZE
pH ADJUSTMENT
Checked By
VOLUME
VOLUME MAKEUP & FINAL MIXING
Approved By
XXXXXXXXXXXXXXXXXXXXXXX Protocol No.:
Process Validation Protocol for Oral liquid/Suspension
Quality Assurance Department
Page 10 of 24
Title : Validation Protocol for
B. No. :
Critical Process PARAMETERS:
Sr No
Critical process variable
Response parameter
Sugar Syrup Preparation 1
Final mixing and volume make up 2
Fixed speed.
Mixing time Load charge in to a Blender
Mixing time Load charge in to a Blender
Remarks
Uniformity of sugar
Uniformity of Active Drugs
Fixed batch size
Fixed speed.
Fixed batch size Washing
Fixed pressure for washing.
D.M. Water pressure
Fixed temperature for washing
D.M. Water temperature
Cleaning Of Bottle
3
Fixed pressure of air Fixed cycle
Compressed air pressure
Washing efficiency
Washing cycle
Fixed direction
Alignment & blockage of needles Fixed speed
Filling & Sealing 4
Speed of filling machine Leak test
5
Labeling & Packing
Volume Uniformity
Volume variation Leakage
Clean, Position &
Clean Label
Proper Sealing
Position Sealing
Prepared By
Checked By
Approved By
XXXXXXXXXXXXXXXXXXXXXXX Protocol No.:
Process Validation Protocol for Oral liquid/Suspension
Quality Assurance Department
Page 11 of 24
Title : Validation Protocol for
Sr
Sugar syrup preparation Manufacturing
2
Machine setting
Process / Variable
No 1
B. No. :
Load time
( Control Variables)
Remarks
Mixing Time Temperature Mixing Time
Mixing time
3 4
Bottle washing
Washing Pressure
Bottle filling & Sealing
Adjustment Of Volume
Prepared By
Checked By
Approved By
XXXXXXXXXXXXXXXXXXXXXXX Protocol No.:
Process Validation Protocol for Oral liquid/Suspension
Quality Assurance Department
Page 12 of 24
Title : Validation Protocol for
B. No. :
5.0
Sampling, Test Parameters, Acceptance criteria
5.1
Sampling locations:
1. TOP –SAMPLE A
2. MIDDLE –SAMPLE B
3. BOTTAM –SAMPLE C
BOTTOM VALVE Sampling site: - Top (A), Middle (B), Bottom(C) position; use the sample tube for A&B and bottom valve for Position C Sampling Qty.: -About 100 ml from each sample site Sampling Time: - While mixing is on: - After ____ minutes, after ____ minutes, After _____ minutes __________ minutes A,B & C
____________minutes A,B & C
________ minutes A,B & C
Checked By
Approved By
Total samples:________
Prepared By
XXXXXXXXXXXXXXXXXXXXXXX Protocol No.:
Process Validation Protocol for Oral liquid/Suspension
Quality Assurance Department
Page 13 of 24
Title : Validation Protocol for 5.2
B. No. :
Sampling:
Stage / Test Parameter
Equipment
Acceptance Criteria
(Size, Location & Time) Sugar syrup Preparation
Manufacturing
Determination on each sample, for
Not more than ______
temperature, & Clarity
minutes
Sampling thief
Appearance
As specified in the BMR
pH
Ref. std. :
weight per ml
As specified in the BMR
Identification
As per standard testing procedure Assay 90 % to 110 %
Assay
Bottle washing
Visual inspection
inspected for particulate matter
Filling & sealing Volume
Measuring cylinder
Not less than label claim.
Appearance
Visual inspection,
As specified in the BMR.
Odour
Visual inspection
As specified in the BMR
Colour
Visual inspection
As specified in the BMR
Capping
Leak test
Complies leak test
Cap breaking and recapping Labeling & Packing
Prepared By
Clean, Position & Proper Sealing
Clean label and proper sealing
Checked By
Approved By
XXXXXXXXXXXXXXXXXXXXXXX Protocol No.:
Process Validation Protocol for Oral liquid/Suspension
Quality Assurance Department
Page 14 of 24
Title : Validation Protocol for 6.0
B. No. :
Recording of data & Data treatment: 6.1
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 sugar syrup preparation & results
Sheet No 2
For recording of bulk manufacturing and results
Sheet No 3
For recording of bottle washing and results
Sheet No 4
For recording of bottle filling and sealing
Sheet No 5
For recording of capping
Sheet No 6
For recording of labeling and packing
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
Checked By
Approved By
XXXXXXXXXXXXXXXXXXXXXXX Protocol No.:
Process Validation Protocol for Oral liquid/Suspension
Quality Assurance Department
Page 15 of 24
Title : Validation Protocol for
B. No. : Data recording sheet no I
Sugar syrup preparation: Equipment name
:_______________________
Identification no
:_______________________
Capacity
: ______________________lt.
Date:____________________
Ingredients and sequence of material addition: ____________________ Total Volume of ingredients : _______________ltr. Mixing time
: _______ minutes
Setting – stirrer
: slow
Procedure
: As outlined in the batch manufacturing record.
Plan
: Samples to be drawn at of ___ minutes of mixing from 3 x 100 ml different
locations For Sugar syrup preparation: Result after mixing _________________ minutes Temperature
Points
Clarity
Weight per ml
Sample A Sample B Sample C
Analyst:
Date
Conclusions:
Checked By: _________________________
Prepared By
Date: ____________________
Checked By
Approved By
XXXXXXXXXXXXXXXXXXXXXXX Protocol No.:
Process Validation Protocol for Oral liquid/Suspension
Quality Assurance Department
Page 16 of 24
Title : Validation Protocol for
B. No. : Data recording sheet no II
Manufacturing (Manufacturing Tank): Equipment Name
:_________________________
Identification no
:_________________________
Capacity
: ______________________lt.
Date:___________________
Ingredients and sequence of material addition: ____________________ Total weight of ingredients
: _______________ltr.
Mixing time
: ______ minutes
Setting – stirrer
: slow
Procedure
: As outlined in the batch manufacturing record.
Plan
: Samples to be drawn at of _______ minutes, _______ minutes, & ______
minutes of mixing from 3 different locations For manufacturing tank result: Assay of after mixing ____________ minutes Location
Appearance
pH
Weight per ml
Between
Between
to
to
Identification
Assay 90 to 110%
Top Middle Bottom Mean Standard Deviation % Relative standard deviation
N.B. Calculation sheet attached
Assay of after mixing ____________ minutes Prepared By
Checked By
Approved By
XXXXXXXXXXXXXXXXXXXXXXX Protocol No.:
Process Validation Protocol for Oral liquid/Suspension
Quality Assurance Department
Page 17 of 24
Title : Validation Protocol for Location
B. No. :
Appearance
pH
Weight per ml
Between
Between
to
to
Identification
Assay 90 to 110%
Top Middle Bottom Mean Standard Deviation % Relative standard deviation
N.B. Calculation sheet attached Assay of after mixing ____________ minutes Location
Appearance
pH
Weight per ml
Between
Between
to
to
Identification
Assay 90 to 110%
Top Middle Bottom Mean Standard Deviation % Relative standard deviation
N.B. Calculation sheet attached Conclusion:
Prepared By
Checked By
Approved By
XXXXXXXXXXXXXXXXXXXXXXX Protocol No.:
Process Validation Protocol for Oral liquid/Suspension
Quality Assurance Department
Page 18 of 24
Title : Validation Protocol for
B. No. : Data recording sheet III
Equipment Name: Bottle washing Machine Identification no
:_________________________
Date:___________________
Capacity
: ______________________ (Bottle per minutes)
Method reference: Visual inspection. Observation : Washed bottle shall be inspected for particulate matter. Stage
Inspected
1
2
3
4
5
6
7
8
9
by After
machine
setting Beginning
of
washing Middle
of
washing End of washing
Conclusion:
Data recording sheet IV Equipment Name: Monoblock filling & sealing machine Identification no: ________________________________ Machine Speed:____________________ Standard volume: ________________ ml Procedure: As per In-process check procedure for volume check. Observation: Volume shall be more than label claimed. Plan: Samples to be drawn from each roller as set for sealing at after machine setting , Beginning of filling, Middle of filling and end of filling.
Prepared By
Checked By
Approved By
10
XXXXXXXXXXXXXXXXXXXXXXX Protocol No.:
Process Validation Protocol for Oral liquid/Suspension
Quality Assurance Department
Page 19 of 24
Title : Validation Protocol for Stage
B. No. :
Volume measured in measuring Cylinder
Appearance
Inspected by
1
2
3
4
5
6
7
8
After machine setting Beginning of filling Middle
of
filling End of filling Conclusion:
Checked by: ___________________________
Prepared By
Checked By
Date_________________________
Approved By
XXXXXXXXXXXXXXXXXXXXXXX Protocol No.:
Process Validation Protocol for Oral liquid/Suspension
Quality Assurance Department
Page 20 of 24
Title : Validation Protocol for
B. No. :
Data recording sheet V Equipment Name: Monoblock filling & sealing machine Identification no: ________________________________ Machine Speed:____________________ Procedure: Capped bottles to be checked for seal breaking and recapping. Method reference: Leak test procedure for Capped bottles.
stage
No of bottle
Recapping
Seal breaking
No of Leakers
tested After machine Setting Beginning of Capping Middle of Capping At the end of Capping
Prepared By
Checked By
Approved By
XXXXXXXXXXXXXXXXXXXXXXX Protocol No.:
Process Validation Protocol for Oral liquid/Suspension
Quality Assurance Department
Page 21 of 24
Title : Validation Protocol for
B. No. :
Data recording sheet VI Equipment Name: Bottle labeling machine / Domino printing machine Identification no: ________________________________ Machine Speed: ____________________ Procedure: Labeled bottles to be checked for clean, position of label and crossed label. Method reference: Leak test procedure for Capped bottles.
stage
No of bottle
Clean
Position of label
Crossed label
tested After machine Setting Beginning of Capping Middle of Capping At the end of Capping
Prepared By
Checked By
Approved By
XXXXXXXXXXXXXXXXXXXXXXX Protocol No.:
Process Validation Protocol for Oral liquid/Suspension
Quality Assurance Department
Page 22 of 24
Title : Validation Protocol for
B. No. :
Data recording sheet VII Analysis Report Product Name: Batch No.:
Batch size:
Mfg. Date:
Exp. Date:
Composition: Test method reference: In house Sr.
Test Specification
No. 01
Description
02
pH
03
Specific Gravity
04
Uniformity Of volume
05
Assay
5.1
Results
Remark
% Labeled amount: 90 % - 110 % Quantity Found:
5.2
% Labeled amount: 90 % - 110 % Quantity Found:
5.3
% Labeled amount: 90 % - 110 % Quantity Found:
5.4
% Labeled amount: 90 % - 110 % Quantity Found:
Remark: Result: The sample referred above complies / does not comply with the standard prescribed as per In house Specification. N.B. Calculation sheet attached
Prepared By
Checked By
Approved By
XXXXXXXXXXXXXXXXXXXXXXX Protocol No.:
Process Validation Protocol for Oral liquid/Suspension
Quality Assurance Department
Page 23 of 24
Title : Validation Protocol for
B. No. : Data recording sheet VIII
Sr
Name of critical equipment / Utilities
No
Qualification /
Date of Qualification /
Validation file
Validation
reference No 1
S.S. Manufacturing tank
2
S.S. Storage vessel
3
Filter press
4
Transfer Pump
5
Washing Machine
6
Filling Machine
7
Sealing Machine
8
Labeling Machine
Utilities: 1
AHU System
2
Water System
3
Compressed Air
4
Steam
5
Lightning
6
Drain
Prepared By
Checked By
Approved By
XXXXXXXXXXXXXXXXXXXXXXX Protocol No.:
Process Validation Protocol for Oral liquid/Suspension
Quality Assurance Department
Page 24 of 24
Title : Validation Protocol for
B. No. : Data recording sheet IX
Remark: Analytical Method Validation protocol attached Conclusion Sr.
Stage
Acceptance criteria
Observation
No. 1.
Sugar Syrup
Uniformity of sugar
Preparation 2.
Manufacturing
Complies as per BMR
3.
Bottle
No particulate matter observed
Washing 4.
Filling and
Volume shall be more than labeled
Sealing
claim
5.
Capping
Leak test
6.
Labelling and Crossed label shall not be more than 2 packing
mm at the edge, label shall not be peeled off after drying
Conclusion: Product _________________________________ manufactured as per B.M.R. No _____________ meets predefined acceptance criteria.
Analysis By
Approved By
Date
Date
Prepared By
Checked By
Approved By
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