Liquid chromatography/tandem mass spectrometry method for the quantification of deserpidine in human plasma: Application to a pharmacokinetic study

摘要

A sensitive and rapid liquid chromatography/tandem mass spectrometric (LC/MS/MS) method was developed and validated for the determination of deserpidine in human plasma. The plasma samples were prepared using liquid-liquid extraction (LLE) with ethyl ether-dichloromethane (3:2, v/v). Chromatographic separation was accomplished on an Ultimate XB-C18 column. The mobile phase consisted of methanol-5 mM ammonium acetate-formic acid (72:28:0.036, v/v/v). Detection of deserpidine and the internal standard tropisetron was achieved by tandem mass spectrometry with an electrospray ionization interface in positive ion mode. The lower limit of quantification was 4.0 pg/ml. The linear range of the method was from 4.0 to 2000 pg/ml. The intra- and inter-day precisions were lower than 14.7% in terms of relative standard deviation (RSD), and the accuracy was within +/- 8.7% in terms of relative error (RE). This validated method was successfully applied for the evaluation of pharmacokinetics of deserpidine after a single oral administration dose of 0.25 mg deserpidine to 22 healthy volunteers.