A new, rapid, and sensitive gas chromatography–mass spectrometry (GC-MS) method was developed for the determination of ezetimibe (EZE) in human plasma. EZE was derivatized prior to GC-MS analysis. Various derivatization techniques such as acetylation, methylation, and silylation were tried. EZE was extracted from plasma with high recovery (–) using methyl tertbutyl ether and carbonate buffer (pH 9). Chromatographic conditions were optimized using chemometric methods. |