Professional Documents
Culture Documents
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CONTENT
Introduction
Validation Study Phases
Master Validation Protocol
Dissolution Apparatus Validation
Conclusion
References
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INTRODUCTION
A validation programme involves various components in
pharmaceutical organisation related to process, equipment and
product.
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EQUIPMENT VALIDATION
Definition (US-FDA):- Validation is the establishment of
documentary evidence which provide a high degree
assurance of specified process will consistently produce the
product meeting with predetermined specification and
quality attributes.
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CYCLE OF VALIDATION
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VALIDATION STUDY PHASES
Phase 1:
Pre-Validation Phase (Qualification Phase)
Phase 2:
Process Validation Phase (Process Qualification phase)
Phase 3:
Validation Maintenance Phase
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VALIDATION PLAN
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PHASE-1(QUALIFICATION)
DESIGN QUALIFICATION:
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DQ REVIEW DOCUMENTS
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INSTALLATION QUALIFICATION
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COMPUTER AND SOFTWARE IQ
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Phase-2
(process qualification phase)
OPERATIONAL QUALIFICATION
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How may runs are to be performed during Operational
Qualification (OQ) testing?
Guidelines stress the importance of equipment qualification simulating
actual production conditions, including 'worst case' situations and that
"tests and challenges should be repeated a sufficient number of times to
assure reliable and meaningful results."
"three consecutive batches" is recommended for process validation rather
than for equipment qualification. No specific number of "runs" for
equipment qualification, but multiple tests to simulate actual operating
ranges and to establish consistency are expected
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PERFOMANCE QUALIFICATION
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Performance Qualification
Purpose- To define testing requirements in a product/
process/performance/qualification/validation protocol.
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RE-VALIDATION
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PHASE-3
(VALIDATION MAINTENANCE PHASE)
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MASTER VALIDATION PROTOCOL
MVP :
Identifies which items are subjects to validation.
Defines the nature and extent of testing expected to be done on each
item.
Outlines the test procedures and protocols to be followed to
accomplish validation.
Describes functional responsibilities and requirements to document
the work carried out and the results obtained.
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Installation Qualification
Installation qualification consists of documented
verification that all key aspects of the dissolution
apparatus are in working condition and have been
properly installed in accordance with manufacturer’s
specifications in the proper operating environment.
Calibration
The installation qualification should document that
specific devices contained within the dissolution
apparatus (e.g., speed, time, and temperature displays)
have been calibrated to traceable standards.
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INSTALLATION QUALIFICATION-
Environmental Conditions
Computerized System
Equipment Information
Preventive maintenance
SOP
Utilities
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DISSOLUTION APPARATUS
VALIDATION
Dissolution is defined as the process by which a known
amount of drug substance goes into solution per unit of
time under standardized conditions.
The primary goal of dissolution testing is to be used as a
qualitative tool to provide measurements of the
bioavailability of a drug as well as to demonstrate
bioequivalence from batch-to-batch.
Validation is achieved by performing a series of validation
activities; for a dissolution apparatus, validation is obtained
through installation qualification and operational
qualification.
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DISSOLUTION APPARATUS
• Apparatus 1
• Vessel: cylindrical, 160-210 mm height, inside diameter 98-
106 mm, nominal capacity is 1000 mL; sides are flanged at
the top. Shaft: positioned so that its axis is not more than 2
mm at any point from the vertical axis of the vessel and
rotates smoothly and without significant wobble.
Materials of Construction: Shaft and basket components
are stainless steel, type 316 or equivalent. Basket position:
the distance between the inside bottom of the vessel and the
basket is maintained at 25 +/- 2 mm during the test.
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DISSOLUTION APPARATUS
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• Temperature Distribution Study
A temperature distribution study should be conducted
during the operational qualification. The study should
include temperature mapping of each vessel contained
within the dissolution apparatus. Temperature should
be mapped using a data system for a minimum time
that is based on the monograph or 1 hour, whichever is
greater. The temperature must remain at 37°C ± 0.5°C;
Rotation Speed Study
A rotation speed study should be conducted during the
operational qualification. The study should include a
measurement of the speed of the shaft rotation for each
vessel contained within the dissolution apparatus.
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SYSTEM SUITABILITY
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CONCLUSION
Validation provide the good quality product and the equipment .
Validation data should be generated for the all types of the product
process
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REFERENCES
1. Potdar Manohar A. “Pharmaceutical quality assurance” 2 nd Edition, Nirali
Prakashan, p-8.1-8.7
2. Nash Robert A. “Pharmaceutical Process Validation”3 rd Edition, Marcel Dekker Inc,
p-442
3. Cole Graham C. ‘Pharmaceutical Production Facilities” 2 nd Edition, CRC Press, p-
199
4. Despautz Joseph F. “Automation And Validation Of Information In Pharmaceutical
Processing” Vol-90, Marcel Dekker Inc, p-221
5. Berry And Harpaz “ Validation Of Active Pharmaceutical Ingredient”2 nd Edition,
CRC Press, p-429
6. Sharon M.Averell Frost, “ Introduction to the Validation of a Dissolution
Apparatus.”p-19.
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