Validation and Validation Protocol

8/3/2019 Validation and Validation Protocol

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VALIDATION

validation refers to establishingdocumented evidence that a process or

system, when operated withinestablished parameters, can performeffectively and reproducibly to produce a

medicinal product meeting its pre-determined specifications and qualityattributes


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Validation protocol

A written plan stating how validation will be conducted,including test parameters, product characteristics,production and packaging equipment, and decisionpoints on what constitutes acceptable test results. Thisdocument should give details of critical steps of themanufacturing process that should be measured, theallowable range of variability and the manner in which

the system will be tested.The validation protocol provides a synopsis of what ishoped to be accomplished. The protocol should list theselected process and control parameters, state thenumber of batches to be included in the study, andspecify how the data, once assembled, will be treatedfor relevance. The date of approval by the validationteam should also be noted.In the case where a protocol is altered or modifiedafter its approval, appropriate reasoning for such achange must be documented.


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Scheme for validation protocol

Part 1. Purpose (the validation) andprerequisites

Part 2. Presentation of the entireprocess and subprocesses, flowdiagram, critical steps/risksPart 3. Validation protocol, approvalPart 4. Installation qualification,drawings


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Scheme for validation protocolPart 5. Qualification protocol/report

5.1 Subprocess 15.1.1 Purpose5.1.2 Methods/procedures, list of manufacturing

methods, SOPs, and written procedures, asapplicable

5.1.3 Sampling and testing procedures,acceptance criteria (detailed description of, orreference to, established procedures, asdescribed in pharmacopoeias)

5.1.4 Reporting5.1.4.1 Calibration of test equipmentused in the production process5.1.4.2 Test data (raw data)5.1.4.3 Results (summary)

5.1.5 Approval and requalification procedure

5.2 Subprocess 2 (same as for Subprocess 1)5.n Subprocess n


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Scheme for validationprotocol

Part 6. Product characteristics, test data fromvalidation batchesPart 7. Evaluation, including comparison with the

acceptance criteria and recommendations (includingfrequency of revalidation/requalification)Part 8. Certification (approval)Part 9. If applicable, preparation of an abbreviatedversion of the validation report for external use, forexample by the regulatory authorityThe validation protocol and report may also includecopies of the product stability report or a summary ofit, validation documentation on cleaning, and

analytical methods.


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PHARMACEUTICAL VALIDATION AND PROCESSCONTROLS IN DRUG DEVELOPMENT

OBJECTIVE

In drug development, pharmaceutical validation and process controls are important to assure that the drug product can meet standards for the identity, strength,quality, purity, and stability of the drug product.

Pharmaceutical validation includes analytical method validation and (manufacturing) process validation.

A validated analytical method is often employed for product testing at various critical stages of a manufacturing process to evaluate whether the manufacturing process does what it purports to do.

For a validated manufacturing process, the current good manufacturing practice requires that a well-written procedure for process controls be established to monitor the performance of the manufacturing process.

The concept can be applied to new drugs, new dosage

forms, and generic drug development.


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INFORMATIONS ON VALIDATION PROTOCOL

The validation protocol should be numbered, signedand dated, and should contain as a minimum thefollowing information:

objectives, scope of coverage of the validation study

validation team membership, their qualifications andresponsibilities type of validation: prospective, concurrent,

retrospective, re-validation number and selection of batches to be on the validation

study a list of all equipment to be used; their normal and worst

case operating parameters outcome of IQ, OQ for critical equipment requirements for calibration of all measuring devices


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Informations on validationprotocol (contd.)

critical process parameters and their respectivetolerances

description of the processing steps: copy of themaster documents for the product

sampling points, stages of sampling, methods ofsampling, sampling plans statistical tools to be used in the analysis of data training requirements for the processing operators validated test methods to be used in in-process

testing and for the finished product specifications for raw and packaging materials and

test methods forms and charts to be used for documenting results format for presentation of results, documenting

conclusions and for approval of study results.


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SUMMARY: Validation??? Documentation Programme.provides high degree of assurance.

To check correctness of method orprocess.

Required by law.To avoid possibility of rejection orrecalled batches.To ensure product uniformity, reproducibility &

quality


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Validation protocol :

it gives Details of the critical parts of the

manufacturing process.Information about the key parameter tobe measured.

Allowable range of variability in case ofmeasured parameter.


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Validation of facilities, equipment and

services is called qualification

to confirm that a design of equipment is planned properly.

A) Design Qualification (D.Q.)

B) Installation qualification (I.Q.)

Performance of the tests in order to confirm that a piece of equipment isinstalled properly.


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Performance of the tests in order to confirm that a piece of equipment is operated properly.

C) Operational qualification (O.Q.)

D) Performance qualification (P.Q.)

Test to demonstrate the effectiveness and reproducibility of a process .

E) Change Control


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In short : Validation is done

for: Raw material

Process

product

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Product Validation: Tablet

Raw MaterialPackaging Material

GranulesCompressed TabletsCoated TabletsPacked Final Product


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Raw material validation:

Raw material is validated for particle size,surface area, particle size distribution, colour, Appearance, texture, density, flowability ,compressibility etc.

Organolaptic propertyPhysical characteristicChemical characteristicBiological characteristicMicrobiological characteristicStability testingStorage condition


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Process validation Two stage First identify the critical process

parameter and design protocol Manufacture three batches of product

controlling the critical parameter andtest it for compliance


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Process validation:


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Thank you

Validation and Validation Protocol

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