Parenteral Process Validation 1
Parenteral Process Validation 1
:
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PROCESS
VALIDATION
PROTOCOL FOR PARENTERALS
Protocol No. :
Effective Date. :
Designation
Date
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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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1. PROTOCOL APPROVAL
This document is prepared by the validation and the GMP compliance (QA) team of ______________under the
authority of _____________. Hence this document before being effective shall be approved by
____________________.
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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
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
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6. VALIDATION PARAMETERS:
Formulation: Parenterals
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.
GENERAL:
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, (find below). The results of the validation activities will be summarized in the validation report.
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FLOW SHEET:
Prepare production order and according RM dispensing as per Bill of material
to that issue the BPR
Sampling point
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FORMULATION:
Batch Size:
Sr No Quantity
Ingredients Unit per Quantity Overages with Dispensed Function
ml in Kgs Overages Quantity
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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Equipments/ Factory
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
SrNo Equipment Equipment No. SOP No
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
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Date
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Equipment Details
Make/Model:
ID. No.
S.S. Manufacturing Tank Capacity:
Tag No.
RPM
M.O.C.
Model:
Rubber stopper washing ID. No.
Capacity:
machine
Tag No.
M.O.C.
Make/Model:
ID. No.
Vials washing machine Capacity:
Speed
Tag No.
M.O.C.
Make/Model:
DHS ID. No.
Capacity:
Tag No.
M.O.C.
Designation
Date
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Make/Model:
Autoclave ID. No.
Capacity:
Tag No.
M.O.C.
Make/Model:
Membrane filter Capacity:
Tag No.
M.O.C.
Make/Model:
ID. No.
Capacity:
Filling Machine Tag No.
Speed
M.O.C.
Make/Model:
ID. No.
Lyophilizer Capacity:
Tag No.
M.O.C.
Equipment Details
Make/Model:
Designation
Date
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ID. No.
Capacity:
Sealing Machine Speed
Tag No.
M.O.C.
Make/Model:
ID. No.
Labeling Machine Capacity:
Speed
Tag No.
M.O.C.
Make/Model:
ID. No.
Cold storage Capacity:
Tag No.
M.O.C.
Remarks:
____________________________________________________________________________________________
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Date
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FINAL WASH
LOAD SIZE
LEAKAGE
ACTIVE SPEED
VOLUME SEALING
STIRRER
R.P.M. R.P.M.
CAKE
FORMATION
T MIXING
E TIME PH
M
P.
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BOTTOM VALVE
Sampling Time: -
__________ minutes ____________minutes ________ minutes
Total samples:________
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SAMPLING:
Equipment
Stage / Test Parameter (Size, Location & Time) Acceptance Criteria
Manufacturing
pH Sampling As specified in the BMR
Assay Assay 90 % to 110 %
Note: The assay value should be decided based up the product in use. If it is biological take concerned
pharmacopeia and refer to the guidance values.(Especially in case of Fertility hormones).
Leak test and its methodology must be properly understood as per equipment used.
Optical Inspection: Refer to the guidance about visual inspection methodologies and Knapp test.
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Data recording -2
Equipment Name : vial washing Machine
Identification no : _________________________ Date: ___________________
Capacity : ______________________ (vials per minutes)
Method reference: Visual inspection.
Stage Inspected by 1 2 3 4 5 6 7 8 9 10
Beginning of washing
Middle of washing
End of washing
Conclusion:
___________________________________________________________________________________________
Note: If you have a procedure or methodology to remove the vials as per non-conformity attach a table how
many vials were fed and how many were removed. This is a key point to track the vials quality and report to
your vendor. More than 0.3% of rejections is considered very high.
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Data recording -3
Equipment Name: Rubber stopper washing Machine
Identification no : _________________________ Date: ___________________
Capacity : ______________________
Method reference: Visual inspection.
Stage Inspected by 1 2 3 4 5 6 7 8 9 10
After washing
Conclusion:
_________________________________________________________________________________________
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Data recording 4
Filtration Parameters:
Type of Filter used and Its manufacturer:________________
Membrane filter holder or Cartridge housing number:________
Nitrogen gas or a Pump :________________
Details about sanitization of Pump if it is used:_____________
Integrity check details of Nitrogen filter:_____________
Capacity of Pressure vessel used:_________
Details of pressure vessel :____________
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Data recording 5
Equipment Name: Filling machine
Identification no: ________________________________
Machine Speed: _________________________________
Standard volume: ________________________________
Plan: Samples to be drawn from beginning of filling, middle of filling and end of filling (Depends upon batch size)
Inspected
Stage Volume measured in measuring Cylinder by
1 2 3 4 5 6 7 8
Beginning of
filling
Middle of filling
End of filling
Conclusion:
____________________________________________________________________________________________
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Data recording -6
Equipment Name: Lyophilization
Identification no: ________________________________
Machine Capacity: ________________________________
Procedure: Filled vials send to the lyophilizer for lyophilization process.
SAMPLING: Sampling should be done after the competition of the lyophilization cycle and check all
Parameters mentioned in BPR
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Data recording -7
Plan: Samples to be drawn from beginning of filling, middle of filling and end of filling (Depends upon batch size)
Inspected
Stage Leak test Remarks by
1 2 3 4 5 6 7 8
Beginning of
Sealing
Middle of
sealing
End of sealing
Conclusion:
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Data recording -8
Equipment Name: vial labeling machine
Identification no: ________________________________
Machine Speed: ________________________________
Procedure: Labeling should be as per the specifications.
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Data recording-10
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 pH
03 Specific Gravity
04 Uniformity Of volume
05 Assay
5.1 % 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.
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Data recording 10
Utilities:
1 AHU System
2 Water System
3 Compressed Air
4 Steam
5 Lightning
6 Drain
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Data recording 11
Remark:
Attach Analytical Method Validation protocol
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Conclusion
Sr. No. Stage Acceptance criteria Observation
1. Manufacturing Complies as per BPR
2. Vial Washing Complies as per BPR
3. Rubber stopper
washing Complies as per BPR
4. Filling Complies as per BPR
5. Lyophilization Complies as per BPR
6. Sealing Leak test
7. Labeling and
packing Complies as per BPR
Conclusion:
Product _______________________manufactured as per B.M.R. No _____________ meets predefined
acceptance criteria.
Analysis By Approved By
Date Date
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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 sanitisation, disinfections and
equipment sanitization.
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