Home / QA & QC / SOP on writing & approval of Qualification and validation protocol & reports

SOP on writing & approval of Qualification and validation protocol & reports

  • Objective:
    • To describe the procedure for writing & approval of qualification and validation protocols & reports.
  • Scope:
  • This SOP is applicable to all type of qualification and validation protocol & report for all department to Formulation plant of pharmaceutical Company.
  • Responsibility:
    • The officer / executive / section in-charge who initiates the operation or activity of the department.
  • Accountability:
    • Head –QA shall be accountable for compliance of this SOP.
  • Procedure:

1.Periodic Validation:

  • All type of validation protocol should be on A4 size paper. The protocol should be written with font type Times New Roman only and font size 11.
  • Cover page of protocol:
  • The cover page of the protocol shall consist of the equipment name and equipment Id or area where activity performed.
  • There is double space between them and the font type is in Times New roman and font size is 20.
  • Header
  • Header must be on each & every page of the protocol & report as per details given below for:
  • The header of validation protocol shall consist of the following :
Company Logo Company Name Protocol No. PR/VL/AA/BB/CC
Equipment No.
Effective Date DD-MM-YYYY
Validation Protocol Page X of Y
Equipment Name:
  • Protocol No. be written in format PR/VL/AA/BB/CC and report No. should be written in format RP/VL/AA/BB/CC,
  • PR refers for Protocol and RP refers for report, VL refers to validation, AA refers to type of study performed BB refers to Number of the Protocol and CC refers to revision no. of the protocol. Revision no. of the protocol shall be done with proper change control procedure refer SOP on change control procedure SOP.
  • Protocol numbering shall be done as per SOP on document numbering.
Company Logo Company Name Report  No.   RT/VL/XX/01/YY
Equipment No.
  Validation report Page X of Y
Equipment name:
  • The header for validation report
  • The company name  should be at centre in capital, bold letters with font type Times New Roman font size 11.
  • The page no. shall be written in right side corner in front of validation protocol/validation report  with font type Times New Roman with font size 11.

2. Validation Protocol (General Content)

  • Header
  • Header must be on each & every page of the protocol & report as per details given below for:
  • The header consists of the following :
Company Logo Company Name Protocol No. PR/AA/BB/CC
Market
TYPE OF VALIDATION PROTOCOL Effective Date
Page X of Y
Product Name Product Name
  • Protocol No. for should be written in format PR/ AA/BB/CC and report No. should be written in format RP /AA/BB/CC,
  • PR refers for Protocol and RP refers for report, AA refers to type of study , BB refers to Number of the Protocol and CC refers to revision no. of the protocol. Revision No. of the protocol go through the proper change control procedure refer SOP on change control procedure SOP.For details of Protocol No. SOP on document numbering.
  • The company name should at centre in capital & bold letters with font type Times New Roman font size 11.
  • The page no. shall be placed at the bottom right corner in front of validation protocol with font type Times New Roman with font size 11.
  • Table of contents:
  • The title ‘TABLE OF CONTENTS’ shall be written in with font type Times New Roman font size 11.
  • The following below minimum table of contents for process validation, but not limited to shall be covered.
S. No. Description Page No.
1.0 Protocol approval
2.0 Overview
2.1 Objective
2.2 Purpose
2.3 Scope
3.0 Responsibility and Validation team
4.0 Training
5.0 System Description
6.0 Validation Test Procedures
7.0 Discrepancy and corrective action report
8.0 References
9.0 Summary
10.0 Conclusions
11.0 Appendix
12.0 Periodic Validation Criteria
13.0 Revision History
  • Body of protocol / report:
    • The line spacing between Heading / Subheading / note = single.
    • The heading, sub-heading and note shall be in bold letter.
    • The text body of protocol or report shall be written with font type Times New Roman and size 11 including bullets and numbering also.
    • Paragraph spacing (before & after) = 6 pt.
    • The numbering indent from left = 0 inch & the hanging indent / left tab 0.5”
    • For example the details of body text are given below:

 

paragraph

  • Protocol Approval :

In the approval sheet of the protocol/Report, representative of following departments shall do the  signing:-

Signing of this approval page of protocol indicates agreement with the validation approach described in this document. If any modification in the equipment validation approach becomes necessary, a revision through change control shall be prepared, checked and approved. This protocol cannot be executed unless approved by following personnel.
Department Name Designation Signature /Date
Prepared by
User Department
Quality Assurance
Reviewed by
HOD-Engineering
HOD-Production
HOD –Quality control
Quality Assurance
Approved by
HOD – QA
  • Protocol writing with respect to activity:
  • Overview
  • To establish the methodology to provide documentary evidence w.r.t. activity in details of specification, component & features etc.
  • Objective
  • The objective of the protocol i.e. procedure and plan for validation on the Equipment with Equipment ID is defined.
  • Purpose
  • The purpose of this Protocol for which the validation is carried out shall be defined .
  • Scope
  • The scope of the protocol is limited to for which validation and where the validation is performed shall defined.
  • Responsibility and Validation Team: – In this section responsibilities of various departments during validation activity shall be defined.
  • Training: Training shall be conducted formally by concern expert or QA person which involve in the validation activity and she / he must have knowledge of that activity. Training record shall be attached with validation report.
  • Equipment /System Description: – In this section equipment make, model, capacity, location, dimensions and there working principle and design specification shall be defined.
  • Validation procedure: Under this detail procedure of the validation shall be mentioned that what are the actives shall be done in the validation and what is the testing procedure, acceptance criteria and recording of the result.
  • Pre- Validation Requirements: in this section what are the requirements to be completed prior to validation activity shall be defined.
  • Discrepancy and corrective action report: Under this section if any Discrepancy is observed during the validation shall be reported and corrective action must be documented and it must be verified by the department Head and QA head.
  • References
  • All the references which are prefer during the validation activity for the preparation for the protocol and testing procedure must be documented in the validation protocol not in the report.
  • Summary
  • The validation summary report shall include Protocol reference , Dates of validation activities, Pre-validation testes performed, Confirmation of calibration and preventive maintenance,  and result obtained and acceptance criteria .
  • Conclusion
  • The validation report shall include statement for conclusion of the validation activity based on result and observation from the validation activity.
  • Appendix
  • All the attachments such as test data sheet with S.No. Title and No. of pages must be mention in the form of Tables. It mention in the protocol not in the report
  • Abbreviation used are must be mention with abbreviation and there definition
  • Format of Test data sheets of Process validation:
  • The format of the test data sheet is as follows
  • Periodic Validation Criteria
  • The periodic and revalidation criteria are mention in the protocol with the name of test and frequency.
  • Revision History
  • In the revision history for which the protocol is revised is mention.

 

3. Installation qualification /operational qualification and Performance qualification Protocol cum Report :

  • All type of validation protocol cum report should be on A4 size paper. The protocol should be written with font type Times New Roman only and font size 11.
  • Cover page
    • The cover page should consist of following content which shall be written in font size of 20 with Times new Roman of font type  bold in capital letter. This format shall be used where one time validation is required.
      • In this page following content shall be mentioned:
      • Type of qualification i.e. Installation qualification, operational qualification or performance qualification.
      • Equipment Name and equipment ID.
      •  Header
      • The header should consist of the following contents. For example:
Company logo Company Name  Page X of Y
INSTALLATION  QUALIFICATION PROTOCOL CUM REPORT
Equipment name
Protocol cum Report No. PRCR/IQ/EQ.ID/XX/YY Effective Date DD-MM-YYYY

 

  • The details of Header content shall be written in font theme of Times New Roman and font size  of 11 .
  • The Protocol Cum Report No. shall be written in format PRCR/Type of Qualification/Equipment ID/Number of the Protocol/revision no. of the protocol.
  • For installation qualification write IQ, for operational qualification write OQ, for performance qualification write PQ, for operational cum performance qualification refer OQ-PQ.
  • Table of contents for Installation Qualification:

The title ‘TABLE OF CONTENTS ‘shall be written in font theme of Times New Roman   with font size of 11.

The following minimum table of contents but not limited to shall be covered .

S. No.    TITLE PAGE NO.
1.0 Pre Approval
2.0 Overview
2.1 Purpose
2.2 Responsibility

2.3 Re-qualification

2.4 Equipment Description

3.0 Equipment Specification
4.0 Equipment Identification
5.0 Equipment Location
6.0

 

 

 

 

 

 

 

 

 

 

Installation Qualification Procedure
6.1 Inspection Checklist
6.2 Installation Qualification
6.2.1 Major Component Verification
6.2.2  Material Of Construction Verification Checklist
6.2.3 Verification of utility supply
6.2.4 Critical instrument list with calibration requirements
6.2.5 Verification of Installation
6.2.6 Levelling and Alignment
6.2.7 Drawing & Manual
6.2.8 Deviation (if any) and corrective Action
7.0  Acceptance criteria
8.0 Remarks (If Any)
9.0 Summary
10.0 Appendix
11.0 Post Approval Signature

 

  • Approval Page: For Installation Qualification /Operational Qualification and Performance Protocol cum Report following department shall review the document:
    • Pre Approval
Signing of this approval page of protocol cum report indicates agreement with the qualification approach described in this document. If any modification in the equipment qualification approach becomes necessary, a revision through change control shall be prepared, checked and approved. This protocol cannot be executed unless approved by following personnel.
Department Name Designation Signature /Date
Prepared by
Quality Assurance
Reviewed by
Engineering
Production
Quality Assurance
Approved by
HOD – QA
  • Overview: To establish the methodology to provide documentary evidence with respect to activity in details of specification, component & features etc.
  • Purpose – The purpose of the protocol to provide an outline for the Installation Qualification static attributes
  • Responsibility:- It consists of Responsibilities of various department in the qualification
  • Requalification: – It consists of requalification of the equipment.
  • Equipment Description:- It consists of purpose of the equipment ,Basic mode of operation ,GMP feature ,major component verification, ,capacity ,location ,dimensions.
  • Equipment specification: Under this specification of the machine shall be defined
  • Equipment Identification: Under this equipment ID, make, capacity, Name of the supplier, purchase order and date shall be mentioned.
  • Equipment Location : Under this facility, floor, Area, Room Name room ID shall be mentioned
  • Installation Qualification procedure : Under this Inspection check list, major component verification with make, model capacity dimension material of construction is defined ,LCD or control Panel or HMI keys display must be defined , Material of construction verification ,verification of Utility supply, i.e. electrical supply, Compressed air, water ,Critical instrument with calibration check list ,location assembly, leveling of the equipment ,Installation Verification, Drawing and manuals,
  • Deficiency (if any) and corrective action report: Under this section the Deficiency if any shall be reported.
  • Acceptance criteria: under this section check the acceptance criteria for installation
  • Summary: under this section summarized all the installation qualification activity.
  • Conclusion: under this section give the result of all the qualification activity and data that should be mentions that it under goes for operational qualification activity.
  • Post approval signatures: after the installation qualification all the data reviewed by the head of the engineering, production and quality head and take the certification of its approval.
  • Appendix : Under this section mention the abbreviation and list of the document

4. Operational qualification protocol cum report shall consist minimum contents but not limited to .

S. No.    TITLE PAGE NO.
1.0 Pre Approval
2.0 Overview
2.1 Purpose
2.2 Background

2.3 Responsibility

2.4 Re qualification

2.5 System Description

3.0 Operational Qualification Procedure

3.1 Training Date

3.2 Calibration Review

3.3 Key Functionality

3.4 Safety Features

3.5 SOP verification

3. 6 Preventive maintenance procedure verification

3.7 Operational testing

3.8 Deficiency (if any) and Corrective action Report

4.0 Acceptance criteria
5.0 Summary
6.0 Post Approval
7.0 Appendix
7.1 Abbreviations
7.2 List of Document
  •  For operational Qualification Protocol cum report writing with respect to activity
  • Pre Approval: It is described above.
  • Overview: under this section purpose, background about the installation qualification responsibility, requalification and system description is come.
  • Operational Qualification procedure : Under this section training ,calibration review, Key functionality ,challenge test ,safety feature, SOP verification, Operational testing
  • Deficiency (if any) and corrective action report: Under this section the Deficiency if any shall be reported.
  • Acceptance criteria: under this section check the acceptance criteria for operational qualification.
  • Summary: under this section summarized all the operational qualification activity.
  • Conclusion: under this section give the result of all the qualification activity and data that should be mentions that it under goes for performance qualification activity.
  • Post approval signatures: after the operational qualification all the data reviewed by the head of the engineering, production and quality head and take the certification of its approval.
  • Appendix : Under this section mention the abbreviation and list of the document

5. Performance qualification protocol cum report shall consist minimum contents but  not limited to 

S. No.    TITLE PAGE NO.
1.0 Pre Approval
2.0 Overview
2.1 Purpose
2.2 Background

2.3 Responsibility

2.4 Re qualification

2.5 System Description

3.0 Performance  Qualification Procedure

3.1 Training Date

3.2 Performance Qualification results for Run-1

3.3 Performance Qualification results for Run -2

3.4 Performance Qualification results for Run-2

3.5  Deficiency (if any) and Corrective action Report

4.0 Acceptance criteria
5.0 Summary
6.0 Post Approval
7.0 Appendix
7.1 Abbreviations
7.2 List of Document
  •  For performance Protocol cum report writing with respect to activity
  • Pre Approval: It is described above.
  • Overview: under this section purpose, background about the operational for performance qualification responsibility, requalification and system description is come.
  • Performance Qualification procedure: Under this section training, performance qualification test at three run shall be mention.
  • Deficiency (if any) and corrective action report: Under this section the Deficiency if any shall be reported.
  • Acceptance criteria: under this section check the acceptance criteria for performance qualification.
  • Summary: under this section summarized all the performance qualification activity.
  • Conclusion: under this section give the result of all the qualification activity and data that should be mentions that it under goes for operational use.
  • Post approval signatures: after the Performance qualification all the data reviewed by the head of the engineering, production and quality head and take the certification of its approval.
  • Appendix : Under this section mention the abbreviation and list of the document

6. Operation cum performance qualification protocol cum report shall consist minimum contents ,but not limited to.

S. No.    TITLE PAGE NO.
1.0 Pre Approval
2.0 Overview
2.1 Purpose
2.2 Background

2.3 Responsibility

2.4 Re qualification

2.5 System Description

3.0 Operational Qualification Procedure

3.1 Training Date

3.2 Calibration Review

3.3 Key Functionality

3.4 Safety Features

3.5 SOP verification

3. 6 Preventive maintenance procedure verification

3.7 Operational testing

3.8 Performance Qualification results

3.9 Deficiency (if any) and Corrective action Report

4.0 Acceptance criteria
5.0 Summary
6.0 Post Approval
7.0 Appendix
7.1 Abbreviations
7.2  List of Document

 

  • Appendix: Under this section mention the abbreviation and list of the document.
  • Post approval signatures: after the operation cum performance qualification all the data reviewed by the head of the engineering, production and quality head and take the certification of its approval.
  • Conclusion: under this section give the result of all the qualification activity and data that should be mentions that it under goes for operational use.
  • Summary: under this section summarized all the operation cum performance qualification activity.
  • Acceptance criteria: under this section check the acceptance criteria for performance qualification.
  • Deficiency (if any) and corrective action report: Under this section the Deficiency if any shall be reported.
  • Operation Qualification procedure: Under this section training, Calibration Review, key functionality of equipments, safety feature, SOP verification. operational testing and performance qualification test at three run shall be mention.
  • Overview: under this section purpose, background about the operational for performance qualification responsibility, requalification and system description is come.
  • For operation cum performance qualification Protocol writing with respect to activity

7.Cleaning validation

  • consists of the following :-
  • Protocol No. for cleaning validation should be written in format PRT/CLV/AA/ CC/DD .PRT refers to protocol ,CLV refers to cleaning validation, CC refers Protocol no. DD refers to revision no. of the protocol. Revision No. of the protocol go through the proper change control procedure refer SOP on change control procedure SOP.For details of Protocol No. SOP on document numbering.
  • Protocol of the cleaning validation consists of the following
S. No.    TITLE PAGE NO.
1.0 Pre Approval
2.0 Objective
2.1 Purpose

2.2 scope

2.3 Responsibility

2.4 Revalidation

2.5 Equipment description/Product Description

3.0 Cleaning validation Procedure

3.1 Training Date

3.2 Cleaning validation for Equipment/Product

3.3 product matrix for Maximum allowable residue

3.4 Product detail

3.5 , Sampling Procedure

4.0 Result
5.0 Deficiency if any and corrective action report
6.0 Acceptance criteria
7.0 Conclusion
8.0 Post Approval
9.0 Appendix
  • Pre Approval: It is same as installation qualification.
  • Overview: under this section purpose, scope, responsibility, revalidation criteria and Equipment description/Product Description is define.
  • Cleaning validation Procedure : Under this section training, Cleaning validation for Equipment/Product, product matrix for Maximum allowable residue, Product detail, Sampling Procedure shall be mention.
  • Deficiency (if any) and corrective action report: Under this section the Deficiency if any shall be reported.
  • Acceptance criteria: under this section check the acceptance criteria for cleaning validation.
  • Summary: Under this section summarized all the cleaning validation activity.
  • Conclusion: Under this section give the result of all the cleaning validation activity and data that should be mentions that it under goes for operational use.
  • Post approval signatures: After the cleaning validation activity all the data reviewed by the head of the engineering, production and quality head and take the certification of its approval.
  • Appendix : Under this section mention the abbreviation and list of the document

8.Process validation protocol

  • Protocol No. for process validation should be written in format PR/PV/AA/ CC/DD and report No. should be written in format RP/PV/AA/ CC/DD.PRT refers to protocol ,PV refers to Process validation, AA refers to study done , CC refers Protocol no. DD refers to revision no. of the protocol. Revision No. of the protocol go through the proper change control procedure refer SOP on change control procedure SOP.For details of Protocol No. SOP on document numbering.
  • Protocol of the Process validation consists of the following

 

S. No. TITLE PAGE No.
1.0 Approval  Signatures
2.0 Overview
3.0 Responsibilities
4.0 Background
5.0 Validation Approach
6.0 Equipment List
7.0 Product details
8.0 Manufacturing Location
9.0 Unit Formula and Batch Calculation
10.0 Process Flow Chart
11.0 Manufacturing Procedure
12.0 Proposed Requirements
13.0 Methodology
14.0 Result recording and evaluation
15.0 Preparation of Report
16.0 Handling of Deviations
17.0 Change management
18.0 Reference documents

 

  • Protocol Approval: It is same as equipment validation protocol
  • Overview: The overview of protocol consists of critical processing stage during the manufacturing and sampling at different stage for assurance of the reproducibility and reparability.
  • Objective :The objective of  the Protocol is to provide the methodology to validate the manufacturing process .
  • Scope : The scope of this Protocol is limited to for which validation what is it process and for which market it shall be incused where the validation is performed
  • Responsibilities : The various department what is there responsibilities is must be defined in the protocol.
  • Background:
  • When the process validation is performed there is clearly mention about for which market it is applicable and what is the back up data for that validation is available is defined.
  • Validation Approach: the validation approach concists of the following
  • The selected validation approach for which type of validation.
  • Three batches for each strength proposed for validation study using different API lots, to assess the process parameters and quality attributes of the product.
  • It includes the division of the manufacturing process into unit operations, and the analysis of sample from potentially critical points in the manufacturing process.
  • Study will be carried out in which these steps and critical points are simulated and the effect on the process is assessed.
  • The study may include upper and lower processing conditions that will be encountered normally in the routine production operations (in case of oral section).
  • This study may include worst case conditions but not necessarily simulate the failure range of the product processing conditions (in case of oral section).
  • The steps of Validation methodology and acceptance criteria for each step are described in the following sections.
  • EQUIPMENT & SOP LIST: The equipment which are used during the validation are defined and there SOP is defined.
  • PRODUCT DETAILS: The product details consists of Product Name, Generic Name, Formulation Design, Category: Storage & Environmental Conditions
  • Unit Formula And Batch Calculation:
  • The unit formulation of the batch and per dose calculation and API calculation is defined in protocol.
  • Process Flow Chart : The manufacturing process must be defined in flow chart.
  • Manufacturing Procedure :The manufacturing procedure is mention in the protocol.
  • Sampling Plan :In this section sampling plan should be defined .Under this section qty.test description shall be defined.
  • Methodology:
  • What are the critical steps during the validation stage, Critical processing steps, Control variables, Sampling plan, Test Parameters, Acceptance Criteria are mention in this section.
  • Result Recording and Evaluation:
  • Record all the observation and results as per the Monitoring Methodology given in the After completion of  recording all the relevant data a final conclusion shall be drawn to assure all the data collected supports that  the all the batches thus produced meets the pre-defined specifications and  quality attributes. There by consistent quality of the commercial batch production is assured.
  • Preparation of report:
  • Upon successful execution of process validation batches a consolidated report shall be prepared. This shall include summary of all the intended activities define in the protocol, results of each test performed at different unit operational stages, details of instruments / equipments used during the process validation activity, intended environmental monitoring data, resolution of deviation if any, conclusion of process validation activity. Appropriate yield at manufacturing and packaging stage shall be defined and shall form a base line for commercial batches.

9. Handling of Deviations:

  • Any deviations / critical changes to the approved protocol during the execution of process validation shall be handled as per handling of deviation procedure. Details of deviation shall be documented in the report with details such as, description of deviation, reason / cause, corrective and preventive action, and status of the deviation.
  • All the deviations shall be closed or resolution shall be specified prior to release of product for intended purpose.

10.Change management:

  • Any changes to specified process during post validation period with respect to key process parameters, key raw material & packaging components, critical quality attributes of the product, equipments, and facility related changes shall be handled as per applicable change control procedure.

11. Reference documents: what are the reference documents are used for the validation activity and test procedure are used must be kept in reference document

12. BET and sterility validation of microbiology  consists of the following:-

  • Protocol No. for BET and sterility validation should be written in format PR/MV/AA/ BB/CC/DD and report No. should be written in format RP/MV/AA/ CC/DD .PR refers to protocol, RP refers to Report, MV refers to microbiology validation. AA refers to type of validation or Product name, BB refers for the Product code ,CC refers Protocol no. DD refers to revision no. of the protocol. Revision No. of the protocol go through the proper change control procedure refer SOP on change control procedure SOP.For details of Protocol No. SOP on document numbering.
  • Protocol of the validation consists of the following
S. No.    TITLE PAGE NO.
1.0 Protocol Approval
2.0 Overview
2.1  Objective
2.2 scope
2.3 Responsibility
2.4  Validation Team
3.0 Training Record
4.0 Pre – Validation Requirements
5.0 Acceptance Criteria
6.0 Validation Procedure
7.0 Validation Report & List of Exhibit
8.0 Revalidation Criteria
9.0 Observed Deviation
10 Reference Documents (If Any)
11 Abbreviations

 

13. Validation Status Label

  • Validation status label affix on the equipment.

14. References (If any):

  • SOP on SOPs
  • SOP on document numbering.
  • SOP on Change Control Procedure.

15.Reason for revision:

  • Not Applicable.

16.Abbreviation:

  • IQ :    Installation Qualification
  • OQ :  Operational Qualification
  • PQ :   Performance Qualification
  • BET : Bacterial Endotoxin test
  • PV :   Process Validation
  • r.t :     With respect to

 

 

 

 

 

 

 

 

 

 

 

 

 

About Pharmaceutical Guidanace

Mr. Shiv Kumar is the Author and founder of pharmaceutical guidance, he is a pharmaceutical Professional from India having more than 14 years of rich experience in pharmaceutical field. During his career, he work in quality assurance department with multinational company’s i.e Zydus Cadila Ltd, Unichem Laboratories Ltd, Indoco remedies Ltd, Panacea Biotec Ltd, Nectar life Science Ltd. During his experience, he face may regulatory Audit i.e. USFDA, MHRA, ANVISA, MCC, TGA, EU –GMP, WHO –Geneva, ISO 9001-2008 and many ROW Regularities Audit i.e.Uganda,Kenya, Tanzania, Zimbabwe. He is currently leading a regulatory pharmaceutical company as a head Quality. You can join him by Email, Facebook, Google+, Twitter and YouTube

Check Also

Document Management System in Quality Assurance Department in Pharma Industry

Document Management System in Quality Assurance Department Standard Operating Procedure (SOP) Objective: To lay down …