VALIDATION
validation refers to establishing documented evidence that a process or system, when operated within established parameters, can perform effectively and reproducibly to produce a medicinal product meeting its predetermined specifications and quality attributes
Validation protocol
A written plan stating how validation will be conducted, including test parameters, product characteristics, production and packaging equipment, and decision points on what constitutes acceptable test results. This document should give details of critical steps of the manufacturing process that should be measured, the allowable range of variability and the manner in which the system will be tested. The validation protocol provides a synopsis of what is hoped to be accomplished. The protocol should list the selected process and control parameters, state the number of batches to be included in the study, and specify how the data, once assembled, will be treated for relevance. The date of approval by the validation team should also be noted. In the case where a protocol is altered or modified after its approval, appropriate reasoning for such a change must be documented.
Scheme for validation protocol
Part 1. Purpose (the validation) and prerequisites Part 2. Presentation of the entire process and subprocesses, flow diagram, critical steps/risks Part 3. Validation protocol, approval Part 4. Installation qualification, drawings
Scheme for validation protocol
Part 5. Qualification protocol/report 5.1 Subprocess 1 5.1.1 Purpose 5.1.2 Methods/procedures, list of manufacturing methods, SOPs, and written procedures, as applicable 5.1.3 Sampling and testing procedures, acceptance criteria (detailed description of, or reference to, established procedures, as described in pharmacopoeias) 5.1.4 Reporting 5.1.4.1 Calibration of test equipment used in the production process 5.1.4.2 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
Scheme for validation protocol
Part 6. Product characteristics, test data from validation batches Part 7. Evaluation, including comparison with the acceptance criteria and recommendations (including frequency of revalidation/requalification) Part 8. Certification (approval) Part 9. If applicable, preparation of an abbreviated version of the validation report for external use, for example by the regulatory authority The validation protocol and report may also include copies of the product stability report or a summary of it, validation documentation on cleaning, and analytical methods.
PHARMACEUTICAL VALIDATION AND PROCESS CONTROLS 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.
INFORMATIONS ON VALIDATION PROTOCOL
The validation protocol should be numbered, signed and dated, and should contain as a minimum the following information: objectives, scope of coverage of the validation study validation team membership, their qualifications and responsibilities 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
Informations on validation protocol (contd.)
critical process parameters and their respective tolerances description of the processing steps: copy of the master documents for the product sampling points, stages of sampling, methods of sampling, 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.
SUMMARY: Validation???
Documentation Programme. provides high degree of assurance. To check correctness of method or process.
Required by law.
To avoid possibility of rejection or recalled batches. To ensure product uniformity, reproducibility & quality
Validation protocol:
it gives Details of the critical parts of the manufacturing process. Information about the key parameter to be measured. Allowable range of variability in case of measured parameter.
Validation of facilities, equipment and services is called qualification
A) Design Qualification (D.Q.) to confirm that a design of equipment is planned properly. B) Installation qualification (I.Q.)
Performance of the tests in order to confirm that a piece of equipment is installed properly.
C)
Operational qualification (O.Q.) Performance of the tests in order to confirm that a piece of equipment is operated properly.
D)
Performance qualification (P.Q.)
Test to demonstrate the effectiveness and reproducibility of a process. E) Change Control
In short : Validation is done for:
Raw material Process product
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Product Validation: Tablet
Raw Material Packaging Material Granules Compressed Tablets Coated Tablets Packed Final Product
Raw material validation:
Raw material is validated for particle size, surface area, particle size distribution, colour , Appearance, texture, density, flowability , compressibility etc.
Organolaptic property Physical characteristic Chemical characteristic Biological characteristic Microbiological characteristic Stability testing Storage condition
Process validation
Two stage First identify the critical process parameter and design protocol Manufacture three batches of product controlling the critical parameter and test it for compliance
Process validation:
Thank you
