Documentation

It is essential that the validation program is documented and is properly maintained. So a written protocol should be established that specifies how qualification and validation will be conducted. The protocol should be reviewed and approved. The protocol should specify critical steps and acceptance criteria.34 Each stage of the validation process should be fully documented, reviewed, authorized and ―signed off‖. There should be a formal review of each stage of validation and documented approval before proceeding to the next stage.

The reports should reflect the protocols followed and include atleast the title and objective of the study; reference to the protocol; details of material, equipment, programmes and cycles used; procedures and test methods. The results should be evaluated, analyzed and compared against the pre-determined acceptance criteria. The results should meet the acceptance criteria; deviations and out-of-limit results should be investigated. If these deviations are accepted, this should be justified and where necessary further studies should be performed. Usually, the department responsible for the qualification and validation work should approve the completed work. And the conclusion of the report should state whether or not the outcome of the qualification and/or validation was considered successful. The quality assurance department approves the report after the final review. The criteria for approval should be in accordance with the company‘s quality assurance system. Any deviations found during the validation process should be acted upon and documented as such and corrective actions be taken, where required. 35

38 Usually, a report that cross-references the qualification and/or validation protocol is prepared summarizing the results obtained, commenting on any deviations observed, and drawing necessary conclusions, including recommending changes necessary to correct deficiencies. For e.g. in routine production, it is important to adequately record process details (e.g. time, speed, temperature, & equipment used) and any changes which have record. A maintenance log is also maintained, which is useful in performing failure investigations concerning a specific manufacturing lot.

The document (i.e. validation report) on completion of the installation and operation qualification consists of:

 Validation plan and protocols.

 User requirement and functional specifications.  Evidence of vendor qualification.

 The IQ document (includes description of hardware and software).  Operating and maintenance manuals and SOPs for testing.

 Qualification test reports with signatures and dates.

 Summary of test results and a formal statement that the system has been accepted.  Approval of user, validation department and quality assurance.36

39 Installation Qualification (IQ)

Name of company: The White Horse Pharmaceuticals Address: Raj-fulbaria, Savar, Dhaka.

Check list for installation Qualification for: HPLC

Qualification Protocol No:………WHP: 002 Date:10-11-2013

Has the equipment been delivered according to purchase order?

Yes No

Has the equipment been checked for damage (Equipment should be undamaged).

Yes No

Has the required documentation been supplied? Is it of correct issue and identified properly by model

number, serial number and date? Yes No.

Have details of all the services and utilities required to operate equipment been provided?

Yes No.

Have methods and instructions for maintenance been provided along with spare parts and contact points for

service? Yes No.

Is the selected environment suitable for the

equipment? Have appropriate utilities (e.g. electricity,

gas, steam, water, etc.) been provided? Yes No.

Has information regarding health, safety and environment in relation to the operation of the

equipment been provided? Yes No.

√

40 In case of OQ and PQ, qualification protocol has to be prepared which will include:

 SOP for OQ and PQ  References to SOPs for:

o Calibration of measuring devices, if the equipment has them o Operator‘s training;

o Preventive maintenance; o Cleaning and sanitization;

 Formats for documentation and certification.

{Formats suggested below are based on WHO publication. A WHO guide to Good Manufacturing Practice (GMP) requirements Part 2; Validation.}

Signature:

Name of the person: Designation:

Date:

(On the behalf the company) Signature:

Name of the person: Designation:

Date:

(On the behalf of manufacturer of equipment)

41 Operational Qualification (OQ)

Name and address of Company: The White Horse Pharmaceuticals Validation Protocol No: WHP 006

Operational Qualification:

Name of Equipment /System: Mass Mixture A. Materials, Equipment‘s, Documents:  List of Calibration equipment required.

 Materials and Supplies needed to perform OQ.

 SOPs and Data Sheets for normal operation of equipment/System.  Records of training of operators.

 Manuals‘ for equipment. B. Procedure:

 Test and record calibration data for such instruments which need calibration.

 Test and record operation conditions of control points and alarms (e.g. temp., rotation, velocity, etc.).

 Test and record output.

 Measure and record the results of Challenge to the system in normal and worst case situation where required.

 Following:

o Record any deviations to the procedure, if made.

o Prepare a deviation report giving justification of acceptance of deviation and its impact on operation.

o Report.

 Prepare a report on OQ.

42 Performance Qualification (PQ)

Name and Address of Company: Validation Protocol No:

Performance Qualification:

A. Materials, Equipment‘s, Documents:  List of Materials.

 List of equipment.  List of SOPs

(SOPs which are specific to the performance tests including data sheets, charts predetermined specifications and acceptance limits)

B. Procedure:

 Equipment‘s: Run three times employing normal procedure for each uses (configuration or load) and records the data on data sheet. Also record deviation to the procedure, if made.

 System: Run for 20 consecutive working days and record data on datasheet. Also record deviation to procedure, if made. (Prepare summary of the data).

C. Evaluation:

 Perform required calculation and statistical analyses,  Compare the results with acceptance limits.

 If there has been deviation to the procedure, prepare deviation report including justification of acceptance and its impact on performance.

 Prepare a PQ report.

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