超高效液相色谱-串联质谱方法同时测定猪肉中7种β-受体激动剂残留量

Determination of Seven β-Agonist Residues including Phenylethanolamine A in Pork by UPLC-MS/MS

建立同时测定猪肉中苯乙醇胺A、盐酸克伦特罗、沙丁胺醇、莱克多巴胺、特布他林、西马特罗和氯丙那林7种β-受体激动剂残留量的超高效液相色谱-串联质谱方法(UPLC-MS/MS)。样品采用1%甲酸-乙腈一次性振荡提取,用β-受体激动剂专用固相萃取柱净化、多反应监测(MRM)、内标法定量。结果表明:7种β-受体激动剂检出限均为0.2μg/kg,定量限为0.5μg/kg。空白猪肉中添加1、2、10μg/kg水平,7种β-受体激动剂总体平均回收率72.2%～116.9%,总体相对偏差均小于2.5%。该方法不需要酶解,分析速度快,灵敏度高,重现性好,各项技术指标均满足国内外相关法规要求,可用于猪肉中7种β-受体激动剂残留的快速检测。

An ultra performance liquid chromatography-tandem mass spectrometry （UPLC-MS/MS） method was established for the simultaneous determination of phenylethanolamine A, clenbuterol, salbutamol, ractopamine, terbutaline, cimaterol and clorprenaline residues in pork. Samples were extracted with 1% fomic acid- acetonitrile, cleaned up using a solid phase extraction cartridge. Quantification of seven β-agonists was achieved by UPLC-MS/MS with multiple reaction monitoring （MRM） using internal standard method. The detection limit and quantification limit of the developed method for seven analytes were 0.2 μ g/kg and 0.5 μ g/kg, respectively. The average recovery rates of seven β-agonists from blank pork at the spiked levels of 1, 2 μ g/kg and 10 μ g/kg were 72.2%--116.9%, with relative standard deviation （RSD） of less than 2.5%. This method had the advantages of rapid analysis, high sensitivity, good reproducibility and no need for enzymatic hydrolysis. Its various technical indexes could meet the requirements of relevant domestic and international regulations. Therefore, this method is applicable for rapid determination of β -agonist residues in pork.