食品科学 ›› 2010, Vol. 31 ›› Issue (6): 208-212.doi: 10.7506/spkx1002-6630-201006049

• 分析检测 • 上一篇    下一篇

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

张爱芝,王全林*   

  1. 宁波市产品质量监督检验研究院
  • 收稿日期:2009-03-20 修回日期:2009-08-28 出版日期:2010-03-15 发布日期:2010-12-29
  • 通讯作者: 王全林 E-mail:quanlinwang@163.com
  • 基金资助:

    浙江省质检系统科技计划项目(20070106)

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

ZHANG Ai-zhi,WANG Quan-lin*   

  1. Ningbo Academy of Product Quality Supervision and Inspection, Ningbo 315041, China
  • Received:2009-03-20 Revised:2009-08-28 Online:2010-03-15 Published:2010-12-29
  • Contact: WANG Quan-lin* E-mail:quanlinwang@163.com

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(UPLCMS/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。

关键词: 超高效液相色谱- 质谱/ 质谱, 性激素, 牛奶

Abstract:

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%.

Key words: ultra performance liquid chromatography-electrospray tandem mass spectrometry (UPLC-MS/MS), anabolic steroid, milk

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