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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 establish a method for the simultaneous determination of 7 progesterone and 5 androgen in milk by high performance liquid chromatography-tandem mass spectrometry (LC-MS / MS). Methods Homogeneous samples were extracted with acetonitrile, denatured with n-hexane, purified with HLB column, separated on a Waters Xbridge TMC18 column and detected by MRM in electrospray positive ion mode. Results The linearities of 12 hormones in the range of 0.5μg / L ~ 50μg / L were good and the correlation coefficients were both above 0.999. The limits of detection and quantification were 12.0μg / kg ~ 0.08μg / kg and 0.1μg / kg ~ 0.3 respectively μg / kg. The average recoveries were 71.3% ~ 99.0% at 1μg / kg, 2μg / kg and 10μg / kg. The relative standard deviations (RSDs) were 0.7% ~ 12.5%. Conclusion The method is simple, sensitive and accurate. It is suitable for rapid and simultaneous analysis of progestin and androgens in milk.