HPLC-MS/MS法测定人血浆中尼古丁浓度

目的建立简单、快速且灵敏的液质联用法检测人血浆中尼古丁的浓度。方法 血浆样品经二氯甲烷萃取后,采用Thermo Hypurity CN柱(2.1mm×150mm,5μm)分离,以乙腈-20mmol.L-1甲酸铵(50∶50,v/v)为流动相,流速为0.30mL·min-1。采用电喷雾离子源(ESI源)正离子多反应监测(MRM)扫描分析,尼古丁和d-4-尼古丁的离子选择通道分别为:m/z163→130和m/z 167→133.9。结果尼古丁的线性范围为0.597～76.48ng·mL-1,最低检测浓度为0.597ng·mL-1,平均提取回收率为70.7%～86.8%,日内和日间变异均<15%。结论本方法简单、灵敏、快速、重现性好,适用于尼古丁的人体临床药物代谢动力学及生物等效性研究。

HPLC-MS/MS method for the determination of nicotine in human plasma

Objective To establish a simple, rapid and sensitive HPLC-MS/MS method to determine nicotine in human plasma. Methods The plasma samples were extraced with dichloromethane. The nicotine and internal standard were separated on a Thermo Hypurity CN column （2.1 minx 150 ram, 5 μm） with the mobile phase containing acetonitrile and 20 mmol · L^-1 ammonium （50 ： 50, v/v） at 0.30 mL · min^-1. The electrospray ionization with positive mode and multiple reaction monitor （MRM） were used. The most intense M-H]＋ MRM transition for niciotine and d4 nicotine was m/z163→130 and m/z 167→133.9. Results The linear range of the calibration curves for nicotine was 0. 597- 76.48 ng · mL^-1. The method recovery was 70.7%-86.8%. The intra-day and inter-day RSD was less than 15%. Conclusion This method is simple, sensitive, rapid and reproducible. It is suitable for the pharmacokinetic studies of nicotine.