Chemistry Reference
In-Depth Information
• Description of the applicability and speciicity, along with any special pre-
cautions (e.g., safety, storage, and handling)
• List of reagents, including source and purity/grade
• Equipment, including the HPLC and any other equipment necessary
(balances, centrifuges, pH meters, etc.)
• Detailed instrument operating conditions, including integration parameters
• Detailed description of the preparation of all solutions (mobile phases,
diluents), standards, and samples
• System suitability test description and acceptance criteria
• Example chromatograms, spectra, or representative data
• Detailed procedures, including an example sample queue (the order in
which standards and samples are run)
• Representative calculations
• Revision history
• Approvals
Once drafted, methods often are subjected to a prevalidation stage, to demonstrate
that they are capable of being validated. The prevalidation stage typically consists of
an evaluation of linearity and accuracy. Sometimes a test of robustness, if it has not
already been evaluated during method development, is then carried out. The valida-
tion process usually will proceed more smoothly, and with lower risk of failure, if
the ability to pass all the key validation criteria is confirmed during the prevalidation
stage. A draft method will become an official test method after a full validation of
its intended purpose.
4.5.3 v
AlIdAtIon
r
ePort
The validation report is a summary of the results obtained when the proposed test
method is used to conduct the validation protocol. The report includes representative
calculations, chromatograms, calibration curves, and other results obtained from the
validation process. Tables of data for each step in the protocol and a pass or fail
statement for each of the acceptance criteria are also included. A validation report
generally consists of the following sections:
• Cover page with the title, authors, and afiliations.
• Signature page dated and signed by appropriate personnel, which may
include the analyst, the group leader, a senior manager, and a quality con-
trol and/or a quality assurance representative.
• An itemized list of the validation parameters evaluated, often in the form
of a table of contents.
• An introduction or objective.
• Method summary including instrument and solution preparation speciics.
• Validation results in subsections organized by the parameter studied. Each
subsection should include a brief summary of the applicable protocol, and
the mean, standard deviation, relative standard deviation, acceptance crite-
ria, and assessment (pass or fail).
