色谱

色谱 ›› 2016, Vol. 34 ›› Issue (2): 170-175.DOI: 10.3724/SP.J.1123.2015.08033

• 研究论文 • 上一篇    下一篇

改进的高效液相色谱-串联质谱方法同时测定动物性食品中4种β2-受体激动剂残留

黎娟, 乔庆东, 庄景新, 王翠苹   

  1. 北京市昌平区疾病预防控制中心, 北京 102200
  • 收稿日期:2015-08-27 出版日期:2016-02-08 发布日期:2012-09-11
  • 通讯作者: 黎娟
  • 基金资助:

    中国科学院生态环境研究中心环境化学与生态毒理学国家重点实验室开放基金项目(KF2014-04).

Simultaneous determination of the residues of four β2-agonists in animal foods by modified high performance liquid chromatography-tandem mass spectrometry

LI Juan, QIAO Qingdong, ZHUANG Jingxin, WANG Cuiping   

  1. Beijing Changping District Center for Disease Control and Prevention, Beijing 102200, China
  • Received:2015-08-27 Online:2016-02-08 Published:2012-09-11
  • Supported by:

    Program of the State Key Laboratory of Environmental Chemistry and Ecotoxicology, Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences (Grant No. KF2014-04).

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摘要：

建立了同时测定动物性食品中克伦特罗、沙丁胺醇、莱克多巴胺和特布他林4种 β2-受体激动剂残留的高效液相色谱-串联质谱(HPLC-MS/MS)的分析方法。样品采用质量分数为5%的三氯乙酸振荡提取,用HLB与ProElut PXC固相萃取柱串联净化,采用HPLC-MS/MS在多反应监测(MRM)模式下检测,内标法定量。结果表明:克伦特罗、沙丁胺醇、莱克多巴胺和特布他林的检出限(S/N=3)分别为0.05、0.05、0.05和0.2 μ g/kg,定量限(S/N=10)分别为0.25、0.25、0.1和0.5 μ g/kg。空白基质加标水平为2.5、5、10 μ g/kg时, 4种 β2-受体激动剂的平均回收率为90.3%~120.5%,相对标准偏差为1.60%~9.33%。该方法采用酸解法提取样品,较酶解法耗时短,速度快,灵敏度高,回收率、重现性好,可有效用于动物性食品中4种 β2-受体激动剂残留的快速检测。

关键词: β2-受体激动剂, 动物性食品, 高效液相色谱-串联质谱, 固相萃取, 酸解提取法

Abstract:

An analytical method was developed to simultaneously determine the residues of four β2-agonists in animal foods by high performance liquid chromatography/electrospray-tandem mass spectrometry (HPLC-MS/MS). Samples were extracted with 5% (mass fraction) trichloracetic acid, and then cleaned up by two solid phase extraction cartridges (HLB and ProElut PXC). Quantification of the four β2-agonists was achieved by HPLC-MS/MS in multiple reaction monitoring (MRM) using internal standard method. The limits of detection (S/N=3) of clenbuterol, salbutamol, ractopamine and terbutaline were 0.05, 0.05, 0.05 and 0.2 μ g/kg, and the limits of quantification (S/N=10) were 0.25, 0.25, 0.1 and 0.5 μ g/kg, respectively. The average recoveries of the four β2-agonists spiked in blank samples at the spiked levels of 2.5, 5 and 10 μ g/kg were 90.3%-120.5% with the relative standard deviation (RSD) range of 1.60%-9.33%. The method is reliable, sensitive, good recovery and repeatability. It is suitable for the determination of the residues of the four β2-agonists in animal foods.

Key words: β2-agonists, acidolysis extraction, animal foods, high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS), solid phase extraction

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