超高效液相色谱-串联质谱多组分检测牛奶中外源性激素残留

Simultaneous Determination of Exogenous Anabolic Steroid Residues in Milk by Ultra Performance Liquid Chromatography-Electrospray Tandem Mass Spectrometry(UPLC-MS/MS)

在多反应监测模式条件下采用正离子采集模式建立牛奶中7种激素的超高效液相色谱-质谱/质谱(UPLC-MS/MS)检测方法。样品以甲醇溶液为提取剂超声辅助提取,经LC-C18柱净化,经BEH-C18(100mm×2.1mm,1.7μm)柱分离后进行UPLC-MS/MS多反应监测模式下的定性及定量分析。7种激素方法检出限为0.01～0.25μg/kg,定量限为0.06～0.5μg/kg,添加水平为10μg/kg时,平均回收率为83%～124%,相对标准偏差为4.3%～24%。该法灵敏度高、检出限低、分析时间短、操作简便,可应用于实际样品检测。

A rapid,specific and highly sensitive method was developed for the determination of 7 exogenous anabolic steroid residues in milk based on ultra performance liquid chromatography-electrospray tandem mass spectrometry（UPLC-MS/MS） in the positive ion mode using multiple reaction monitoring（MRM）.Samples were extracted with methanol with the assistance of ultrasonic and cleaned up using LC-C18 solid phase extraction cartridge.Qualitative and quantitative analysis was carried out in the MRM mode after chromatographic separation using Waters ACQUITY UPLCTM BEH C18（1.7 μm,2.1mm × 100 mm） column.The limits of detection（LOD） of 7 exogenous anabolic steroids by the method ranged from 0.01 to 0.25μg/kg and the limits of quantification（LOQ） were in the range of 0.06-0.5 μg/kg.Average spike recoveries for 7 exogenous anabolic steroids at the level of 10 μg/kg ranged from 83% to 124%,with relative standard deviations（RSDs） between 4.3% and 24%.