高效液相色谱串联质谱联用法测定人血浆中克仑特罗的浓度

Determination of clenbuterol in human plasma by liquid chromatography tandem mass spectrum

目的建立简单、快速和灵敏的高效液相色谱串联质谱联用法测定人血浆中克仑特罗的浓度。方法采用Agilent Eclipse XDB-C18色谱柱（4．6mm×50mm，1．8μm），流动相为乙腈-0．1％甲酸=30：70（v/v），流速为0．5mL·min^-1，柱温为25℃，通过电喷雾离子源进入质谱，以二级质谱多反应监测（MRM）方式对克仑特罗进行检测。结果克仑特罗的线性范围为5．4541090pg·mL^-1，LLOQ为5．45pg·mL^-1，平均相对回收率在80％～120％范围内，日内和日间变异均〈15％。结论本法简单、快速、灵敏、重现性好，能够用于克仑特罗的人体药物动力学和生物等效性研究。

Abstract： Objective To develop a simple, quick and sensitive method of liquid chromatography -electrospray tandem mass spectrometry to determine Clenbuterol in human plasma. Methods Agilent Eclipse XDb-C18 column （4.6 mm×50 mm, 1.8μm） was used; the mobile phase was composed of acetonitrile-0.1% formate acid= 30 ： 70 （v/v）, and the flow rate was 0. 5 mL · min^-1, and the column temperature was 25℃. The eletronspray tandem mass spectrum in the positive mode and multiple reaction monitor （ MRM ） were used to detect the concentration of clenbuterol. Results The response was linear at 5.45-1 090 pg · mL^-1 for clenbuterol; the LLOQ was 5.45 pg · mL^-1. The relative re covery of clenbuterol was 80%-120%, and it had a good precision with relative standard deviation of intra-day and inter-day RSD of less than 15%. Conclusion This method is simple, quick, sensitive and reproducible for pharmacoki netics and bioequivalence study of clenbuterol.