液相色谱-串联质谱法测定策划药物MDPV及其代谢物

Simultaneous analysis of designer drug methylenedioxy-pyrovalerone and its metabolites by liquid chromatography-mass spectrometry

目的：建立日益流行的策划药物亚甲二氧吡咯戊酮（MDPV）及其体外代谢产物的液相色谱-质谱（LC-MS）联用测定方法。方法：采用Thermo Gold ODS色谱柱（150 mm×2.1 mm,5μm）,以0.1 mmol·L^-1醋酸铵-甲酸缓冲溶液（p H 4.5）为流动相A,甲醇为B进行梯度洗脱（0～1 min,10%B;1～6 min,10%B→90%B;6～14 min,90%B）,流速0.20 mL·min^-1;采用电喷雾离子化源,正离子检测方式,全离子扫描、选择反应监测扫描模式检测并鉴定MDPV及其代谢产物。结果：在大鼠肝微粒体S9组分中鉴定得到MDPV的4种体外代谢产物。结论：所建立的方法用于策划药物及其代谢物的分析,不仅可以节省分析时间、减少实验成本,而且具有高效、灵敏和选择性好等特点。

Objective： To develop a method for the simultaneous analysis of designer drug methylenedioxy-pyrovalerone（ MDPV） and its in vitro metabolites by liquid chromatography-mass spectrometry（ LC-MS）. Methods：The separation was carried out on a Thermo Gold ODS column（ 150 mm × 2. 1 mm,5 μm） with the mobile phase consisting of 0. 1 mmol·L^-1ammonium acetate-formic acid（ p H 4. 5） solution（ A） and methanol（ B） by gradient elution（ 0-1 min,10% B; 1-6 min,10% B→90% B; 6-14 min,90% B） at a flow rate of 0. 20 mL·min^-1.MDPV and its metabolites were detected by positive ESI-MS with full scan and MRM modes. Results： There were four metabolites that were identified in the rat liver S9 fraction. Conclusion： The obtained results indicated that the method was time-and cost-saving,and it could be applied in the determination of designer drugs and their metabolites with advantages of efficiency,sensitivity and good selectivity.