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当前位置: 首页 > 文章 > 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 食品科学 2010,31 (6) 208-212
Position: Home > Articles > Simultaneous Determination of Exogenous Anabolic Steroid Residues in Milk by Ultra Performance Liquid Chromatography-Electrospray Tandem Mass Spectrometry(UPLC-MS/MS) FOOD SCIENCE 2010,31 (6) 208-212

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

作  者：
张爱芝;王全林
单  位：
宁波市产品质量监督检验研究院
关键词：
超高效液相色谱-质谱/质谱;性激素;牛奶
摘  要：
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。
译  名：
Simultaneous Determination of Exogenous Anabolic Steroid Residues in Milk by Ultra Performance Liquid Chromatography-Electrospray Tandem Mass Spectrometry(UPLC-MS/MS)
作  者：
ZHANG Ai-zhi,WANG Quan-lin*(Ningbo Academy of Product Quality Supervision and Inspection,Ningbo 315041,China)
关键词：
ultra performance liquid chromatography-electrospray tandem mass spectrometry(UPLC-MS/MS);anabolic steroid;milk
摘  要：
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%.

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