High-throughput bioanalytical method using automated sample preparation and liquid chromatography–atmospheric pressure ionspray mass spectrometry for quantitative determination of glybenclamide in human serum

A liquid chromatographic–mass spectrometric (LC–MS) method with rapid automated sample preparation was developed and validated for determination of glybenclamide in human serum. Glybenclamide and its deuterated labelled internal standard were extracted from human serum samples by automated solid-phase extraction. The extract was injected into the LC–MS system for analysis. Glybenclamide and its internal standard were measured in multiple ion monitoring mode. The method was validated over a range of 10–1000 ng/ml with good accuracy and precision and was applicable for pharmacokinetic studies.