VALIDATION METHODOLOGY
VALIDATION :
Validation is defined as the establishment of
documented evidence which provides a high
degree of assurance that, a planned process
will consistently perform according to the
intended specified outcomes.
Once the system or process has been validated, it
is expected that it remains in control, provided
no changes are made.
Incase of any modifications, or problems or
equipment replacement/ relocation,
Re – Validation is performed.
VALIDATION ACTIVITIES
Validation Activities Mainly consists of :
a)
b)
c)
d)
Utilities & Equipment Qualification
Cleaning Validations
Analytical Instrument & Method Validations
Process Validations
The Utility/Equipment Qualification consists of
Installation Qualification (IQ),
Operational Qualification (OQ) &
Performance Qualification (PQ).
Equipment, Utility Qualification
• Some equipment, whose correct operation itself
is a measure of its performance and which is
calibrated at regular intervals, may need only
Installation Qualification (IQ) & Operational
Qualification (OQ).
Example : pH meter
• IQ, OQ & PQ on major equipment, systems and
Utilities must be completed and approved prior
to the use of the same for manufacturing
purpose.
• Protocols shall be prepared, reviewed &
approved for IQ, OQ &PQ studies.
INSTALLATION QUALIFICATION (IQ)
Installation Qualification is the documented
evidence that the installed equipment conforms to
the purchase specifications, manufacturer’s
literature.
The IQ should list and document all the Identification
information of all major components, their locations,
utility requirements, connections and any safety
features of the equipment.
IQ is intended to verify that the installed equipment
matches with purchase specifications, drawings,
manuals, spare parts list, supplier address and contact
numbers etc.
OPERATIONAL QUALIFICATION (OQ)
Operational Qualification is the documented evidence
that all the components of a system or piece of
equipment operate according to the specifications.
The OQ should provide a listing of SOPs for Operation,
Maintenance and Calibration.
Before initiation of OQ of an Equipment or Utility, its IQ
must be completed.
PERFORMANCE QUALIFICATION (PQ)
• Performance Qualification is the
documented evidence that a system/ piece
of equipment can consistently perform and
meet the required specifications under
routine operation and, where appropriate,
under worst-case situations.
• The PQ document should include a description
of the preliminary procedures required, the
detailed performance tests to be performed, and
the acceptance criteria for each test.
PROCESS VALIDATION
• Process Validation is the documentary evidence that
processes are capable of repeatedly and reliably
producing a Finished Product of the required Quality.
• Process Validation studies examine a process under
normal operating conditions to prove that the process
is in control. Once the process has been validated, it
is expected that it remains in control, provided no
changes are made.
Types of Process Validation
Process validation consists of either of
• Prospective Validation
• Concurrent Validation
• Retrospective Validation
Prospective Validation :
The execution and documentation of pre – approved test
protocol, which is designed to prove that a process
performs as intended, prior to the release of a
manufactured product for distribution.
CONCURRENT VALIDATION
•
Concurrent Validation is based on data collected
during actual performance of a process already
implemented in the manufacturing facility.
Validation data are collected during several runs of
the on-going process and evaluated to determine if the
process is valid.
A Protocol should be written to define the information to
be collected and evaluated.
RETROSPECTIVE VALIDATION
•
Retrospective Validation is performed
whenever a product has been in production
since a long time, and has not been validated
either prospectively (or) concurrently.
A minimum of 10 to 12 Consecutive
batches will be evaluated for Consistency of
Test results, Quality & Yield against
Acceptance Criteria.
ANALYTICAL INSTRUMENT VALIDATION
The Validation of Analytical Instruments consists of
Installation Qualification (IQ),
Operational Qualification (OQ) &
Performance Qualification (PQ).
• Some Instruments, whose correct operation itself is a
measure of its performance, may need only Installation
Qualification (IQ) & Operational Qualification (OQ).
Example : pH meter, Incubator, Freezer
• IQ, OQ & PQ of the Analytical instruments must be
completed and approved prior to the use of the same for
other validation activities/ product testing purpose.
• Protocols shall be prepared, reviewed & approved for IQ,
OQ &PQ studies.
ANALYTICAL METHOD VALIDATION
•
Analytical Method Validation is to be conducted
for all identification, quantitative analytical procedures
such as product strength/assay, impurity and
degradation analysis etc.
Validation of Analytical Method is the process of
establishing any four or more of :
Accuracy, Precision, Linearity, Range, Limit of
Detection, Limit of Quantitation, Specificity and
Ruggedness as appropriate to the type of Assay/Test.
The results of Validation must be documented in an
Approved Method Validation Protocol.
CLEANING METHOD VALIDATION
•
Cleaning validation program is to be conducted for
each product/ for each grouping of products to ensure
that the cleaning procedures effectively remove residual
products and cleaning agents from the equipment that
is in contact with the product (the cleaned equipment
contains an acceptable limit of previous product only).
SWAB Samples / RINSE Samples are obtained &
analyzed in order to prove that the cleaned equipment
contains an acceptable limit of previous product only).
The method of sample drawing, no. of samples to be
drawn, location &equipment for sampling etc. must be
documented in an Approved Method Validation
Protocol.