Validation of assay methodology used in pharmacokinetic studies.

Statistical methods for validating assays used in pharmacokinetic studies are discussed. Methods for assessing linearity, variability, and sensitivity are derived. It is proposed that a calibration experiment, in which samples are replicated at three different concentrations, will provide the necessary information to validate an assay prior to commencement of a pharmacokinetic study and during its routine use. A two-stage weighted least squares regression is used to analyze the calibration data. High performance liquid chromatography calibration data are used to illustrate the principles and techniques involved.