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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1~50μg/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0.5μg/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。
OBJECTIVE To establish a high performance liquid chromatography-tandem mass spectrometry (LC-MS / MS) method for the simultaneous determination of nine β-agonists in porcine, bovine, mutton and liver (floroterol, Albuterol, ractopamine, ractopamine, clenbuterol, fopratolol, terbutaline, phenylethanolamine A). Method The sample (10.0 g) was enzymatically digested overnight at 37 ° C with a β-glucuronidase and aryl sulfonate esterase solution to liberate the bound β-agonist and extracted with perchloric acid solution After two passes through HLB and MCX cartridge respectively, the methanol-0.1% formic acid water (10 + 90) was reconstituted and d6-ractopamine, d9-clenbuterol and d3-salbutamol isotopes were used as the internal standard , Using electrospray tandem quadrupole mass spectrometry. Using this method, 720 samples commercially available in Shenzhen City from 2012 to 2013 were assayed for beta-agonists. Results The linearity of the nine target β-agonists in the range of 1 ~ 50 μg / L was good with linear correlation coefficients> 0.995. The method limits of 9 target β-agonists in the sample matrix tested were 0.5μg / kg, the average recoveries were 66.2% ~ 119.4% and the relative standard deviations were 0.36% ~ 10.02%. 720 samples were detected by the established method. A total of 9 positive samples were detected with a total detection rate of 1.25%. The detection rate of ractopamine was 0.56% (4/720). The detection rate of clenbuterol was 0.42% (3/720), phenylethanolamine A detection rate was 0.28% (2/720). Conclusion The method is rapid and accurate and can be used for the detection of nine β-agonists in pigs, cattle, mutton and their liver.