食品科学 ›› 2013, Vol. 34 ›› Issue (8): 216-219.doi: 10.7506/spkx1002-6630-201308046

• 分析检测 • 上一篇    下一篇

高效液相色谱-串联质谱法测定卤肉中3种β-受体激动剂残留

王 远,邢丽杰,郝家勇,鲁立良,唐宗贵,罗小玲   

  1. 新疆农垦科学院 农业部食品质量监督检验测试中心,新疆 石河子 832000
  • 收稿日期:2011-12-15 修回日期:2013-03-15 出版日期:2013-04-25 发布日期:2013-05-07
  • 通讯作者: 邢丽杰 E-mail:xinglj2010@sina.com
  • 基金资助:
    基于金磁微粒检测农兽药多残留蛋白质芯片及其信息读取仪的研制

Determination of β-Agonists in Cooked Meat by HPLC-MS/MS

WANG Yuan,XING Li-jie,HAO Jia-yong,LU Li-liang,TANG Zong-gui,LUO Xiao-ling   

  1. Food Quality Supervision and Testing Center of Ministry of Agriculture, Xinjiang Academy of Agricultural Reclamation Science, Shihezi 832000, China
  • Received:2011-12-15 Revised:2013-03-15 Online:2013-04-25 Published:2013-05-07
  • Contact: Xing Li-jie E-mail:xinglj2010@sina.com

摘要: 建立卤肉中3种β-受体激动剂(克仑特罗、莱克多巴胺、沙丁胺醇)残留检测的高效液相色谱-串联质谱方法。样品经β-盐酸葡萄糖醛甙酶/芳基硫酯酶水解,MCX固相萃取柱净化,以乙腈-0.1%甲酸溶液作为流动相洗脱,采用电喷雾离子源,多反应监测方式进行采集,外标法定量。结果表明:3种β-受体激动剂在1~100ng/mL质量浓度范围内呈现良好的线性关系,R2均大于0.99,方法检测限均为0.25μg/kg,从0.5、1μg/kg和2μg/kg添加水平检测结果可以看出,方法平均回收率为80%~120%,相对标准偏差为1.0%~10.0%。

关键词: β-受体激动剂, 卤肉, 高效液相色谱-串联质谱

Abstract: A high performance liquid chromatography-mass/mass (HPLC-MS/MS) method was established for the determination of 3 β-agonists (clenbuterol, ractopamine and salbutamol) in cooked meat. The β-agonists were hydrolyzed by β-glucuronidase, purified by MCX, and analyzed with a methanol-0.1% formic acid-acetonitrile mobile phase. The residues of β-agonists were determined by electrospray ionization-trandem mass spectrometry, and quantified by external standard method. The calibration curve revealed an excellent linear range between peak areas and concentrations in the range of 1–100 ng/mL with correlation coefficient (R2) higher than 0.99. The limit of detection of the developed method was 0.25 μg/kg. The average recovery rate from spiked cooked meat at three concentrations of 0.5, 1, 2 μg/kg was in the range of 80%–120% with relative standard deviations of 1.0%–10.0%.

Key words: β-agonists, cooked meat, high performance liquid chromatography-mass/mass (HPLC-MS/MS)

中图分类号: