We provide customized method validation services per applicable ICH/ICH/EPA/other regulatory agency guidelines at your site. Some methods require only partial validation, while others require full validation. This usually depends on the stage of product readiness at the point of submission for approval. The objective of validation of an analytical procedure is to demonstrate that it is suitable for its intended purpose. A tabular summation of the characteristics applicable to identification, control of impurities and assay procedures need to be included.
Specificity- Specificity is the ability to assess unequivocally the analyte in the presence of components which may be expected to be present. Typically these include impurities, degradants, matrix, etc. Typical analytes evaluated include; solvent blanks, mobile phase, API(s), impurities, placebo, forced degradation studies (acid/base/peroxide/heat/light degradants), filters, etc. Peak purity is assessed for standard/product samples.
Identity- Suitable identification tests are intended to ensure the identity of an analyte in a sample. This is normally achieved by comparison of a property of the sample (e.g., spectrum, chromatographic behavior, chemical reactivity, etc) to that of a reference standard.
Assay and Impurity Test(s)- Assay procedures are intended to measure the analyte present in a given sample (e.g. quantitative measurement of the major component(s) in the drug substance). For the drug product, similar validation characteristics also apply when assaying for the active or other selected component(s). Testing for impurities can be either a quantitative test or a limit test for the impurity in a sample. Either test is intended to accurately reflect the purity characteristics of the sample.
Linearity- The linearity of an analytical procedure is its ability (within a given range) to obtain test results which are directly proportional to the concentration (amount) of analyte in the sample. Depending on the type of sample being evaluated linearity will cover the applicable range for products (e.g. 50-150% or 80-120%) and impurities (e.g. from the QL to 120% of impurity specification for impurity assays and impurity/assay methods)
Accuracy - The accuracy of an analytical procedure expresses the closeness of agreement between the value which is accepted either as a conventional true value or an accepted reference value and the value found. Again depending on the type of sample being evaluated accuracy will cover the applicable range for products (e.g. typically 98-102%) and impurities (e.g. normally a wider acceptance criteria).
Precision - The precision of an analytical procedure expresses the closeness of agreement (degree of scatter) between a series of measurements obtained from multiple sampling of the same homogeneous sample under the prescribed conditions. Precision may be considered at three levels: repeatability, intermediate precision and reproducibility.
Repeatability - Repeatability expresses the precision under the same operating conditions over a short interval of time; or agreement between the results of successive measurements of the same measurement carried out under the same set of conditions. . Repeatability is also termed intra-assay precision.
Method Validation Services (1)
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