摘要
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.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2015年第2期311-316,共6页
Chinese Journal of Pharmaceutical Analysis
基金
辽宁省自然科学基金(201102246)
证据科学教育部重点实验室(中国政法大学)开放基金资助课题(2014KFKT05)
大学生创新训练计划项目(No.201310175001)