液相色谱串接质谱联用法分析人体志愿者尿样中克仑特罗

Determination of Clenbuterol in Human Urine by High Pressure Liquid Chromatography-tandem Mass Spectrometry

目的：建立液相色谱串接质谱联用法检测人体志愿者尿样中克仑特罗检测方法。方法：尿样经过液液萃取提取,以10 mmol/L p H3.5甲酸铵和乙腈为流动相,采用Agilent Eclipse PLUS C18150 mm×4.6mm×3.5μm色谱柱分离,电喷雾离子源,正离子多反应监测模式扫描分析检测,D9-克仑特罗为内标。采用该方法分析了4名人体志愿者尿样中的克仑特罗。结果：该方法的检测限为0.02μg/L,定量限为0.04μg/L,在添加的高、中、低三种浓度的相对回收率分布在85%～100%之间。结论：分析了克仑特罗在人体尿液中代谢规律。方法满足常规检测要求,样品前处理简单、快速、可靠。

Objective To develop a method for determination of clenbuterol in human urine. Methods The urines from 4 volunteers were prepared by liquid-liquid phase extraction. Clenbuterol in urine was separated by Agilent Eclipse PLUS C18 （150 mm×4.6mm×3.5μm） column and detected by HPLC-MS/MS using D9- clenbuterol as internal standard,and ammonium formate and methyl cyanides as mobile phase. Results The detectability of the method was 0.02μg/L,and limit of quantitation was 0.04 μg/L. The relative recovery of target compounds ranged from 85 to 100% respectively at high- ,moderate- ,and low concentrations. Conclusion The method introduced in this study is simple, rapid, reliable, and suitable for routine analysis in human urine.