1 validation of analytical method – K-Patents PR-23 for K-Patents User Manual

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An essential element of pharmaceutical product development, manufacturing process design
and process scale-up design is the knowledge of how the product behaves during all stages
of manufacture. This requires establishing the analytical parameters required to monitor the
process. Awareness of product Refractive Index changes are extremely important as it can
facilitate in-line monitoring and control of the full-scale manufacturing process. The Refractive
Index’s relevance to acceptable variations in the process must first be established.

Once the refractometer system has passed the qualification with refractive index liquids, the
accuracy of an analytical method may be determined by applying that method to samples or
mixtures of excipients to which known amounts of analyte have been added both above and
below the normal levels expected in the samples. The accuracy is then calculated from the
test results as the percentage of analyze recovered by the assay. Robustness tests (sample
temperature and/or concentration parameters are deliberately varied to give an indication of
method reliability).

9.1 Validation of Analytical Method

Analytical methods are validated unless the method employed is included in the relevant
pharmacopoeia or other recognized standard reference.

Methods should be validated to include consideration of characteristics included within The
International Conference on Harmonisation of Technical Requirements for Registration
of Pharmaceuticals for Human Use (ICH) guidelines on validation of analytical methods.
The United States Food and Drug Administration (USFDA) have also proposed guidelines
on submitting samples and analytical data for methods validation. And The United
States Pharmacopoeia (USP) has published specific guidelines for method validation for
compound evaluation.

The validity of an analytical method can be verified only by laboratory studies. The suitability
of all testing methods used should nonetheless be verified under actual conditions of use
and documented.

Complete records should be maintained of any modification of a validated analytical
method. Such records should include the reason for the modification and appropriate data
to verify that the modification produces results that are as accurate and reliable as the
established method.

Analytical Method Validation:

Establishing product refractive index

monitoring validation protocols