Chemistry Reference
In-Depth Information
tested. Examples include loss on drying, residue on ignition, various wet chemical
procedures such as acid value, and simple instrumental methods such as pH mea-
surements. New or different sample-handling or solution-preparation requirements
should also be taken into consideration if used, and may require verification.
The verification process is made up of several individual components: laboratory
personnel, an approved procedure or protocol, data comparison, acceptance criteria
evaluation, the final summary documentation, and corrective action, if necessary.
9.4.1.1 laboratory personnel
Laboratory personnel need to have the appropriate experience, knowledge, and
training to be able to carry out the procedure [12]. They must be able to accomplish
the given functions in the lab, such as operating instrumentation and signing off that
analyses were performed as required. It is important to note that it is not enough just
to be able to push buttons to make instrumentation function and follow the SOPs
(standard operating procedures). GMP requirements put pressure on lab manage-
ment and personnel to understand the background or basics of any analytical tech-
nique that is used in the lab [13,14]. But in spite of these requirements, the FDA still
frequently cites firms for a lack of trained personnel.
9.4.1.2 Approved procedure
An approved procedure in the form of a verification document or SOP is needed
that describes the procedure to be verified, establishes the number and identity of
lots or batches of articles that will be used in the verification, details the analytical
performance characteristics to be evaluated, and specifies the range of acceptable
results. The document should also establish the acceptance criteria that will be used
to determine that the compendial procedure performs suitably.
9.4.1.3 verification documentation
Once samples are analyzed, the data must be scrutinized and compared to the prede-
termined acceptance criteria in the approved verification document. The final sum-
mary documentation should include a summary of the data, the assessment of the
results compared to the acceptance criteria, and a decision of whether or not the data
is acceptable, which is a final indication that the laboratory personnel are capable
of successfully performing the compendial procedure in the particular laboratory.
Acceptable results are final proof that the USP procedure will perform as intended.
If the acceptance criteria are not satisfied, it may be necessary to identify the source
of the problem, take corrective action, amend the verification document if necessary,
and repeat the analysis. The initial unacceptable results, the probable cause, and any cor-
rective actions implemented should also be described in the final summary document.
Of course, there is another possible outcome where, after several attempts, the
verification of the compendial procedure cannot be made. If the source of the prob-
lem cannot be identified and rectified, then it may be concluded that the procedure
may not be suitable for use with the article being tested. It may then be necessary to
revise the current procedure, or redevelop and validate an alternative procedure. In
any case, the final verification document should summarize the inability to verify the
compendial procedure and describe the action taken.
