Liquid Chromatography–Mass Spectrometry Assays in the Regulated Bioanalytical Laboratory

Data derived from robust and reproducible bioanalytical assays form the foundation of all pharmaceutical marketing approval submissions to regulatory agencies. In this chapter, bioanalytical method development, validation, and sample analysis for small molecules are discussed with emphasis on high performance liquid chromatography–mass spectrometry/mass spectrometry (LC–MS/MS) assays. Considerations for assay development include selection of analyte extraction, chromatography, and mass spectrometry parameters. Relevant aspects of validation testing and documentation are covered. Sample analysis for both good laboratory practice (animal, nonclinical) and good clinical practice (human, clinical) studies is discussed. Regulatory compliance issues are addressed for assay development, validation, and sample analysis.