Preparation of Validation and Qualification Protocols
To lay down a procedure for Preparation of Validation and Qualification protocols applicable to all aspects of manufacturing processes, equipments, control systems (including computer hardware and software), utilities, facility, temperature mapping, Shipping and any significant changes to the above mentioned elements which may affect the quality of products directly or indirectly.
This standard procedure is applicable at the QA department.
Officer/Executive-QA/Store/Production/QC/Engineering shall be responsible for implementation of this SOP.
HOD/Designee-QA/Store/Production/QC/Engineering shall be responsible for compliance to the procedure as per this SOP.
Abbreviations and Definitions
- Sr.No :Serial Number
- MACO : Maximum Allowable carry over
- URS : User required Specifications
- PLC : Programmable Logic control
- CPU : Central processing Unit
- RAM : Random Access Memory
- UPS : uninterruptible Power supply
- VR : Validation Report
- VP : Validation Protocol
- R&D : Research & Development
- MOC : Material of Construction
- HVAC : Heating, Ventilation Air Conditioning
- PQ : Performance Qualification
- OQ : Operational Qualification
- IQ : Installation Qualification
- DQ : Design Qualification
The transformation of starting materials into finished products through a single operation or a sequence of operations involving installations, personnel, documentation and environment.
Identification of equipment attributes related to the performance of particular function or functions and allocation of certain limits or restrictions to those attributes.
The act of planning, carrying out and recording the results of tests on equipment to confirm its capabilities and to demonstrate that it will perform as intended.
Design Qualification (DQ):
Documented evidence that the systems or subsystems have been designed in accordance with the requirements of GMP.
Installation Qualification (IQ):
The documented verification that the facilities, systems and equipment as installed or modified, comply with the approved design and manufacturer’s recommendations.
Operational Qualification (OQ):
The documented verification that the facilities, systems and equipment, as installed or modified, perform as intended throughout the anticipated operating ranges.
Performance Qualification (PQ):
Documented verification that the integrated system or subsystem functions as intended, in its normal operating environment.
Establishing documented evidence that a system does what it purports to do.
Repetition of validation process or a specific portion of, to ensure continued compliance with established requirements.
Equipment Qualification Protocol:
Note: Qualification protocols are prepared for those systems, utility, facility, equipment sand area defined as critical for the process. They are prepared following a structure defined in the following sections.
It shall be prepared by User department, checked by Engineering Department and approved by User department; Engineering and Quality Assurance department.
Format of URS is attached as
Equipment Name and its capacity shall be written in under the Description in header.
- Document number shall be given as per SOP.
- Equipment no shall be assign by the user department as per their numbering sequences.
- The equipment shall preciously describe the system and its intended purpose i.e. use and field of identification where this shall be located and its prescribed environmental condition and dimension of location in required specification column.
- Glossary shall be attached as annexure which contain the abbreviation and components list and its specification.
- In operational requirements column shall be written whatever the headings is applicable to the required equipment.
- The cover page shall prepared as annexure and incorporate with URS.
- (QA) shall keep the final copy of approved URS along with relevant drawings.
- The duplicate copy of approved URS shall be forwarded to the vendor or supplier for intended purpose.
- Any modification over the approved URS shall be documented with adequate supporting rationale and shall be in acceptance to the initial signatories of approval.
- Design Qualification:
- The vendor shall provide the design qualification document (including relevant drawing).
- It shall be reviewed and approved by the validation team and shall be undertaken in conjunction with other relevant department(s) against the URS sent to vendor.
- Copy of the approved document will be sent to vendor.
- If not provided by vendor then by mutually understand the design and make the document as per the format of DQ is attached as
- In format, wherever the Name of Equipment mentioned there shall be written exactly the Name of equipment and Document number as per SOP.
- Installation Qualification :
- IQ protocol and report shall be provided by the supplier or will be prepared by the validation team based on business terms and condition in Purchase order (PO).
- IQ protocol and report shall be reviewed by Validation team and approved by the Quality Assurance Head.
- The installation qualification protocol attached as
In component result – under Description, the name of parameters to be verified shall be written Eg: Make Model and Sr.No etc.
Under specification- mentioning the information given by vendor in DQ, certificate and manual shall be written.
Verification Source- shall be written how the specification meets or not from the information which are available in certificate, manual, and in name plate.
Utility verification-shall be mentioned in vendor demanded utilities e.g. compressed air, electricity etc.
It shall be Systematic check of installed equipment against equipment’s supplier specification and/ or additional criteria identified and communicated in the purchase order (PQ).
OQ protocol shall be provided by the supplier or will be prepared by the validation team based on business terms and condition in Purchase order (PO).
OQ protocol will be reviewed by Validation team and approved by the QA shall keep the final copy of approved OQ document along with relevant drawings.
The operational qualification protocol The operational qualification report is as
IQ Protocol and Report wherever the Name of equipment mentioned it shall be written the exact name of the equipment.
Protocol shall be written the main operation parameter verification test procedure for controlled and operated by PLC or manual.
From the instruction given by operating manual or by the instruction provided by vendor representative the test and acceptance column shall be written.
It shall be Systematic check of installed equipment against equipment’s supplier operating specification and/ or additional criteria identified and communicated in the purchase order and DQ as a functional specification.
PQ protocol shall be prepared by the validation team and approved by Head of Production, QC and Quality Assurance.
QA shall keep the final copy of approved PQ document along with relevant drawings.
The performance qualification protocol and cover page attached as
- Validation Report cover page, Index page for Validation Report, Approval Sheet, Name of validation team members, Parameter recording sheet, Deviations and Investigations, if any, Qualification Reports and Certification of completion of validation shall be the content of PQ report.
- Parameter Recording Sheet in report shall be written the Selected Product, Batch Number, Batch size, MFC Number, Date of Manufacturing, Critical parameters which directly impact on the quality of the product.
- Document number mentioned in References, shall be the respective doc number of equipment.
- Computer Hardware and Software (DQ/IQ/OQ/PQ) qualification:
- Computer hardware and software used as part of the equipment and systems to control equipment or system must be validated. Design, Installation, Operational qualification of hardware and software should be executed prior to Performance qualification of the associated equipment or system.
- For reasons of expediency, computer validation can be executed as part of the systems or equipment validation. It shall be done by external party and they will provide the necessary documents of validation systems.
- Process Validation/ Qualification Documents:
- Process Validation Protocol format attached as
- Results of the validation study shall be documented in a validation report.
- The header of Protocol and Report Product Name (Generic name or Brand name should be mentioned.
- The protocol Number shall be mentioned as per SOP.
- Batch Size shall be mentioned either in Numbers or in Kg & Numbers as per technical direction of the Product.
- Master formula Number is taken from MFR of the particular product.
- The Validation Report shall contain the following components which are incorporated in protocol.
- Validation team members-shall be written the name of the members from different department will be involved in the validation activity.
- Equipment list shall be written the name and it’s ID of all the equipments and instruments used from dispensing to final packing process including the Instruments which are used in Process controls.
- Approved raw material list should have the name of all API’s, Excipients and their vendor name & in house item codes.
- Process flow chart-it shall be interlinked between Equipment type and sizes, process step and process variables as a flow chart .
- Critical process variables-Stages of process with respective equipment and its variables shall be written in observation column.
- Sampling plan and analytical data compilation &acceptance Criteria-It shall be contained stage sampling plan location of sampling (diagram of location), frequency of sampling, quantity of sample, analysis plan shall be written the parameter to be tested as per respective STP number to be filled. Under record the analytical findings the equipment used for testing and its calibration status sampling interval individual sample and their test result checked by name/ sign of person and date while compiling the data shall be the test parameters and results shall be compared with their acceptance criteria.
- Environmental monitoring record (holding studies)
- Process validation report cover page-the name of the product of Export, generic name and their strength shall be mentioned if its for domestic market then the brand name with active material and their strength shall be mentioned.
- Process validation report approval sheet shall be filled.
- Process validation Report shall be prepared by the cumulative of all stages and all batch numbers.
- Summarize the findings and observations of the validation studies with conclusion of process capability.
- Statistics can be made to interpret data obtained and provide meaningful information during validation exercise.
- Mentioned the Details of equipment usage and in-process steps
- Mentioned the Details of the current Specs No and STP no. for the respective product.
- Mentioned the Details of manufacturing procedure shall be written as per MFR briefly without skipping or missing any steps.
- Mentioned the Details of process requirement and the sequences of Process step to be mentioned under process step and the critical process parameter which are identified earlier shall mentioned under the process parameter and justifies the process step consideration by what parameters &how those parameters are justified by the test parameters and sampling methods, location of sampling and quantity of samples.
- Mentioned the Details of Process steps and sampling analysis plan and acceptance shall be written for all steps.
- Mentioned the Details of Holding studies shall be clearly mentioned the Quantity of material to be kept under these studies, Frequency of sampling, test parameter, packaging type, and area of storage, test method and acceptance criteria of test method.
- Process validation/ Qualification program (plan and number of batches to be monitored) should be a part of Validation Master Plan (VMP).
- Cleaning Validation:
- Protocol format attached as an annexure-11.
- Title: shall be written as ‘Cleaning validation protocol for the area (applicable area name to be mentioned e.g.Production block.) and the dosage forms eg. Tablet & Capsule section.
- Document number shall be written as per SOP.
- Heading of Objective: it shall be written as the procedure being followed for cleaning of equipment and accessories is effective and remove all residues of previous batch, cleaning agent and holding of equipment in dirty and cleaned conditions to a pre-determined acceptance level thereby avoiding the risk of cross contamination and no microbial proliferation in equipments.
- In Scope: it shall be written specifically area of consideration for the study with highlighting the major concerns of this activity.
- In Responsibility: shall be written clear and specific activity and their role of every department.
- shall be written the Dosage forms eg. Tablet & Capsule and Area Eg. Production Block.
- Prepare the Product matrix.
- Prepare the Equipment matrix.
- Prepare the Pre-Cleaning Validation requirements.
- Prepare for the chemical rinse/swab test report for products and for hold time report and for total carry over.
- Prepare the Sampling plan.
- Test record for the equipments used in the product manufacturing shall be prepared.
- Test Procedure shall be prepared for the drug which are considered for validation.
- Summarize the findings and observations of the validation studies with conclusion.
- After completion of validation, the report shall be included the certificate of application.
- Mapping of the Environmental Conditions
- The Protocol format attached as
- The header of Protocol the Title shall be written and the area of the mapping to be address with the title Eg: Mapping of the Environmental Conditions (Temperature and Relative Humidity) in WareHouse Area.
- Protococl number shall be written as per SOP.
- Protocol approval sheet under the heading of Functional Area, the persons who are responsible for the activity to be done Eg.Warehouse.
- Objective shall be mentioned as per specific condition to be validated Eg.Temperature and Relative humidity or only temperature or only Relative humidity with the area.
- Scope shall be mentioned specific condition to be validated, area of validation and duration of validation
- shall be written the condition to be validated, no of days the reading to be taken, frequency of reading
- The following components are incorporated protocol .
- Validation Team Members
- Equipment/ Instrument List
- Design Conditions and Acceptance Criteria
- Locations for Monitoring
- Cover page of the Report
- Validation Report Approval Sheet
- Validation Report Summary Conclusion
- Deviation form
- Temperature and RH Recording Sheet
- Report shall be prepared by end of activity in every quarter and final report shall be prepared at end of the year..
- Shipping Validation
- The Protocol format
- Protocol number shall be written as per SOP.
- Objective shall be mentioned the specific condition to be validated with the final destination. e.g. both temperature and %RH or Temperature only.
- Scope shall be mentioned specific condition to be validated, frequency of validation.
- The following components are incorporated protocol and it can be numbered as per requirement.
- Arrangement of Data Loggers
- Details of Shipping Validation Study
- Cover page of the Report
- Validation Report Approval Sheet
- Validation Report Summary & Conclusion.
- Validation report number shall be as per SOP .
- Report shall be prepared end of activity in every quarter and final report shall be end of the year.
- Cover page
- Details of Shipping Validation Study
- Summary and conclusion
- Forms and Records
- Not Applicable
- Quality Assurance, Production, Quality Control
Date Revision Number Reason for Revision – 00 New SOP