目的建立牛奶中7种孕激素和5种雄激素类药物的高效液相色谱-串联质谱(LC-MS/MS)同时测定方法。方法均质样品用乙腈提取,采用正己烷除脂,HLB柱净化后,经Waters XbridgeTMC18色谱柱分离,在电喷雾正离子模式下以多反应监测(MRM)方式检测。结果 12种激素类物质在0.5μg/L~50μg/L范围内线性良好,相关系数均大于0.999,检出限和定量限分别为0.02μg/kg~0.08μg/kg和0.1μg/kg~0.3μg/kg。在1μg/kg、2μg/kg、10μg/kg三个浓度水平下的平均回收率为71.3%~99.0%,相对标准偏差(RSD)为0.7%~12.5%。结论该方法操作简便、灵敏度高、定量准确,适合于牛奶中孕激素类和雄激素类药物残留的同时快速分析。
Objective To develop a detection method of 7 progesterone and 5 androgen in milk by liquid chromatography-tandem mass spectrometry(LC-MS/MS).Methods The milk sample was extracted with acetonitrile,the lipids in the extract solution were removed by n-hexane,and the analytes were purified by HLB extraction cartridges.The separation was conducted on a Waters Xbridge TMC18 column.Determination was operated by electrospry ionization mass spectrometry in the positive mode using multiple reaction monitoring(MRM).Results Good linearity was found in a range of 0.5 μg/L~50 μg/L,with correlation coefficients above 0.999.The limits of detection(LOD) and quantitation(LOQ) were 0.02 μg/kg~0.08 μg/kg and 0.1 μg/kg~0.3 μg/kg respectively.The average recoveries of the 12 anlytes were 71.3%~99.0% at the concentrations of 1,2 and 10 μg/kg,with relative standard deviation(RSD) of 0.7%~12.5%.Conclusion This method was accurate and sensitive,rapid and easy to operate.It was feasible for the simultaneous and rapid determination of progesterone and androgen residues in milk.