Validation and method validation parameter

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Validation and method validation parameter:

Validation and method validation parameter PARAS VIRANI

Validation :

Validation “Methods validation is the process of demonstrating that analytical procedures are suitable for their intended use” (ICH Topic Q2B, March 1995) The objective of validation of an analytical procedure is to demonstrate that it is suitable for its intended purpose.

Validation guidelines:

Validation guidelines 1. ICH Q2A Text on validation of analytical procedures: Definitions and terminology (March 1995) 2. ICH Q2B Validation of analytical procedures: Methodology (June1997) 3. FDA (Draft) industry: Analytical procedures and methods Validation Guidance for IND 4. Pharmacopoeias USP and indian Pharmacopoeia

Method validation:

Method validation Validation of an analytical method is the process by which it is established, by laboratory studies, that the performance characteristics of the method meet the requirements for the intended analytical applications.

EXAMPLES OF METHODS THAT REQUIRE VALIDATION DOCUMENTATION:

EXAMPLES OF METHODS THAT REQUIRE VALIDATION DOCUMENTATION CHROMATOGRAPHIC METHODS SPECTROPHOTOMETRIC METHODS CAPILLARY ELECTROPHORESIS METHODS PARTICLE SIZE ANALYSIS METHODS DISSOLUTION METHODS TITRATION METHODS AUTOMATED ANALYTICAL METHODS

TYPES OF ANALYTICAL PROCEDURES TO BE VALIDATED:

TYPES OF ANALYTICAL PROCEDURES TO BE VALIDATED Identification tests. Quantitative tests for impurities' content. Limit tests for the control of impurities. Quantitative tests of the active moiety in samples of drug

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VALIDATION PARAMETER

SPECIFICITY:

SPECIFICITY Specificity is the ability to assess unequivocally the analyte in the presence of components, which may be expected to be present. Typically these might include impurities, degradants and excipients. Stability indicating analytical methods should always be specific. An investigation of specificity should be conducted during the validation of identification tests, the determination of impurities and the assay.

Slide9:

Suitable identification tests should be able to discriminate between compounds of closely related structures which are likely to be present.

Linearity:

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. ” A linear relationship should be evaluated across the range of the analytical procedure. It may be demonstrated directly on the drug substance and/or separate of synthetic mixtures of the drug product components Linearity should be evaluated by visual inspection of a plot of signals – vs - analyte concentration

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For the establishment of linearity, a minimum of five concentrations is recommended.

RANGE:

RANGE Range of an analytical procedure is the interval between the upper and lower concentration (amounts) of analyte in the sample (including these concentrations) for which it has been demonstrated that the analytical procedure has a suitable level of precision, accuracy and linearity. The specified range is normally derived from linearity studies and depends on the intended application of the procedure.

ACCURACY:

ACCURACY Accuracy of an analytical method is the closeness of test results obtained by that method to the true value. Accuracy should be established across the specified range of the analytical procedure. Accuracy should be assessed using a minimum of 9 determinations over a minimum of 3 concentration levels covering the specified range (i.e., three concentrations and three replicates of each).

Precision:

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. The precision of an analytical procedure is usually expressed as the variance, standard deviation or coefficient of variation of a series of measurements.

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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. Repeatability is also termed intra-assay precision a minimum of 9 determinations covering the specified range for the procedure (e.g., 3 concentrations/3 replicates each) or a minimum of 6 determinations at 100% of the test concentration.

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Intermediate precision: Intermediate precision expresses within-laboratories variations: different days, different analysts, different equipment, etc. Its also called intra laboratory precision. Typical variations to be studied include days, analysts, equipment, etc. Reproducibility: Reproducibility expresses the precision between laboratories its also called inter laboratory precision. Reproducibility should be considered in case of the standardization of an analytical procedure,

DETECTION LIMIT :

DETECTION LIMIT The detection limit of an individual analytical procedure is the lowest amount of analyte in a sample which can be detected but not necessarily quantitated as an exact value. Based on Visual Evaluation Based on Signal-to-Noise Based on the Standard Deviation of the Response

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