LC/MS/MS电喷雾正负离子切换同时检测动物组织中的性激素

LC/MS/MS simultaneous determination of male and female hormon in animal organs with switching ES^+/ES^-

目的:固相萃取高效液相色谱-串联质谱电喷雾正负离子切换同时测定禽畜组织中已烯雌酚(DES)、甲基睾酮(MET)、丙酸睾酮(TES)的残留量。方法:样品经甲醇提取,Alltech Extract-clean columns C18,200 mg/6 ml小柱净化和富集。通过Waters SunFireTMC183.5μm 100×2.1 mm色谱柱分离,流动相为:甲醇∶水=85∶15(V/V),ES-、ES+切换,MRM方式测定,外标法定量。结果:最低检出限分别为:已烯雌酚0.15μg/kg;甲基睾酮0.15μg/kg、丙酸睾酮0.33μg/kg;回收率在94.5%～105%之间,相对标准偏差3.2%～10.2%。结论:该方法操作简便、快捷,是动物组织激素残留的快速而准确的检测方法。

Objective：A rapid,simple and sensitive SPE high performance liquid chromatography-electrospray tandem mass spectrometry with switching ES＋/ES-for the simultaneous determination of male and female hormon residues in animal tissues has been established.Metheods： Samples were extracted by Methanol.Samples concentration and purification were performed using Alltech Extract-clean columns C18,200 mg/6 ml.The separation was performed on a Discovery C18 5 μm 250×4.6 mm column,mobile phase was：Methanol∶Water=85∶15（V/V）,flowing rate was 0.3 ml/min.Results： The limits of detection（LOD） of the method were 0.15 μg/kg～0.33 μg/kg.Average recoveries for three hormone were 94.5%～105%,with relative standard deviations between 3.2% and 10.2%.Conclusion： The established method was sensitive and of good recoveries.Tt could be applied as a rapid and reliable method for determination of three hormone in animal tissues.