液相色谱-串联质谱法检测毛发中的克仑特罗___

摘要  目的:建立液相色谱-串联质谱法(LC-MS/MS)检测毛发中的克仑特罗。方法:毛发经碱水解，固相萃取分离、纯化、浓缩后，进行LC-MS/MS分析。色谱柱为Agilent Zorbax SB C18柱(150 mm×21 mm，35 μm)；流动相为乙腈-甲醇-04%甲酸水溶液(22∶4∶74)；流速03 mL·min-1；进样量10 μL；样品在三重四级杆串联质谱中经电喷雾正离子源离子化后，以多反应监测模式(MRM)测定，定量离子对为2271/2030，定性离子对为2771/1681和2771/2591。结果:克仑特罗浓度在1～1000 ng·g-1范围内线性关系良好，方法回收率大于9957%，提取回收率大于5108%，日内和日间RSD均小于89%，最低定量限为1 ng·g-1。随机采样人发20份，检出克仑特罗4份。结论:本方法准确，专属性强，灵敏度高，适用于毛发中克仑特罗的检测。

关键词：毛发；克仑特罗；液相色谱-质谱联用

AbstractObjective:To develop a method of liquid chromatography tandem mass spectrometry(LC-MS/MS）for the determination of clenbuterol in hair.Method:After alkaline hydrolysis，the hair sample was extracted,purified,concentrated by SPE and detected using LC-MS/MS.The separation was performed with an Agilent Zorbax SB C18 column(150 mm×21 mm，35 μm）and acetonitrile-methanol-04% formic acid(22∶4∶74）as mobile phase at a flow rate of 03 mL·min-1；The injection volume was 10 μL;The sample was ionized by positive electrospray ionization(ESI）source in the triple quadruple tandem mass spectrometer,confirmed and quantified with multiple reaction monitoring(MRM）mode.Ion transition for quantification is 227.1/203.0 and ion transitions for qualitation are 277.1/168.1，277.1/259.1.Results:The calibration curve was linear in the range of 1-1000 ng·g-1;The method recovery was more than 9957% and the extraction recovery was more than 5108%;The RSDs of inter- and intra-day were less than 89%;The limit of quantitation was 1 ng·g-1.This method has been applied to analysis 20 human hair samples and the result showed that 4 samples contained clenbuterol.Conclusion:The method is accurate,specific,sensitive,and suitable for the determination of clenbuterol in hair.

Key words:hair;clenbuterol;liquid chromatography tandem mass spectrometry(LC-MS/MS)