华南预防医学 ›› 2014, Vol. 40 ›› Issue (5): 425-430.doi: 10.13217/j.scjpm.2014.0425

• 论著 • 上一篇    下一篇

液相色谱串联质谱法测定食用肉类及肝脏中9种β-受体激动剂

刘桂华,毛丽莎,朱舟,刘红河,康莉   

  1. 深圳市疾病预防控制中心,广东 深圳 518055
  • 收稿日期:2014-05-14 出版日期:2014-10-20 发布日期:2014-11-07
  • 作者简介:刘桂华(1965—),女,硕士研究生,主任技师,主要从事理化检验工作

Determination of residues of nine β-agonists in edible meat and liver by liquid chromatography tandem mass spectrometry

LIU Gui-hua, MAO Li-sha, ZHU Zhou, LIU Hong-he, KANG Li   

  1. Shenzhen Center for Disease Control and Prevention, Shenzhen 518055, China
  • Received:2014-05-14 Online:2014-10-20 Published:2014-11-07

摘要: 目的 建立高效准确的液相色谱串联质谱法(LC-MS/MS)同时测定猪、牛、羊肉及其肝脏中9种β-受体激动剂(菲洛特罗、异丙喘宁、特布他林、沙丁胺醇、莱克多巴胺、克伦特罗、福马特洛、妥布特罗、苯乙醇胺A)残留的确证方法。方法 试样(10.0 g)经β-葡糖醛酸苷肽酶和芳基磺酸酯酶混合酶溶液在37 ℃酶解过夜,游离出结合态的β-激动剂,用高氯酸溶液提取后,分别经过HLB和MCX小柱2次净化处理,甲醇-0.1%甲酸水(10+90)复溶,采用d6-莱克多巴胺、d9-克仑特罗和d3-沙丁胺醇同位素作为分析的内标,采用电喷雾串联四级杆质谱进行测定。用该方法对深圳市2012—2013年市售的720份样品进行β-受体激动剂的测定。结果 9种目标β-受体激动剂在1~50 μg/L范围内该方法线性关系良好,线性相关系数均>0.995。在所测样品基质中,9种目标β-受体激动剂的方法定量限均为0.5 μg/kg,方法平均回收率为66.2%~119.4%,相对标准偏差为0.36%~10.02%。用所建立方法对720份样品进行检测,共检出9份阳性样品,总检出率为1.25%,其中莱克多巴胺检出率为0.56% (4/720)、克伦特罗检出率为0.42%(3/720)、苯乙醇胺A检出率为0.28%(2/720)。结论 该方法快速准确,可用于猪、牛、羊肉及其肝脏中9种β-受体激动剂的检测。

Abstract: Objective To develop an efficient and accurate method for simultaneous determination of multi-residues of 9 β-agonists in meat and liver by using liquid chromatography-tandem mass spectrometry (LC-MS/MS), and to investigate the residues in porcine, bovine, and ovine muscles and livers collected from local markets in Shenzhen. Methods Samples (10.0 g) were hydrolyzed by β-glucuronidase /sulfatase at 37 ℃ overnight to free bound β-agonists, extracted by perchloric acid, purified by HLB and MCX cartridges, and reconstituted with a methanol-0.1% formic acid (10+90).The residues of β-agonists were determined by electrospray ionization-trandem mass spectrometry, and quantified by internal standard method by d6-ractopamine, d9-clenbuterol and d3-salbutarnol. Results The linear relationships of the nine target β-agonists were optimal in the range of 0-50 μg/L and the linear correlation coefficient was >0.995. The limits of quantification were 0.5 μg/kg for 9 β-agonists in porcine, bovine, and ovine muscles and livers. Average recoveries were 66.2%-119.4% with relative standard deviations of 0.36%-10.02%. Nine of 720 samples detected by this method were positive, with a detection rate of 1.25%, of which the detection rates were 0.56% (4/720) for ractopamine, 0.42% (3/720) for clenbuterol, and 0.28% (2/720) for phenylethanolamine A. Conclusion This method proved to be quick and accurate for determination of the residues of 9 β-agonists in porcine, bovine and ovine muscle and liver specimens.

中图分类号: 

  • R115