高效液相色谱-串联质谱法测定猪肉和猪肝中 22种β-激动剂

Determination of 22 β-agonists in pork and pork liver by high performance liquid chromatography-tandem mass spectrometry

中文关键词:  高效液相色谱-串联质谱法  β-激动剂  猪肉  猪肝

英文关键词:high performance liquid chromatography-tandem mass spectrometry  β-agonists  pork  liver

中文摘要:

      目的 建立一种用高效液相色谱-串联质谱法检测猪肉和猪肝中22 种β-激动剂(特布他林、西马特罗、沙丁胺醇、非诺特罗、氯丙那林、莱克多巴胺、克仑特罗、妥布特罗、喷布特罗、福莫特罗、异丙喘宁、苯乙醇胺A、沙美特罗、马喷特罗、马布特罗、溴布特罗、苯氧丙酚胺、班布特罗、溴代克伦特罗、克仑潘特、赛布特罗和卡布特罗)的方法。方法 样品粉碎后, 在pH 5.2的乙酸铵缓冲液中, 用β-盐酸葡萄糖醛苷酶-芳基硫酸酯酶水解, 水解液经正己烷除脂后, 用阳离子交换柱净化, 再浓缩复溶后用高效液相色谱-串联质谱测定。采用内标法对克仑特罗、沙丁胺醇、莱克多巴胺、西马特罗、马布特罗、马喷特罗、赛布特罗和沙美特罗进行定量, 其余化合物采用外标法进行定量。结果 目标化合物的回收率为80%~125%, 线性范围为0.5~100 μg/kg, 相关系数均大于0.992。方法的定量限均不大于0.5 μg/kg。结论 本方法灵敏、快速、简便, 适合于同时定量检测猪肉和猪肝中多种β-激动剂。

英文摘要:

      Objective An analytical method was developed for determination of 22 β-agonists in pork and pork liver, including terbutaline, cimaterol, salbutamol, fenoterol, clorprenaline, ractopamine, clenbuterol, tulobutero, penbutolol, formoterol, metaproterenol, phenylethanolamine A, salmeterol, mapenterol, mabuterol, brombuterol, isoxsuprine, bambuterol, bromoclenbuterol, clenpenterol, cimbuterol and carbuterol by high performance liquid chromatography-tandem mass spectrometry. Methods Samples were enzymatically hydrolysed and extracted by acetic acid buffer (pH5.2). The supernatant was transferred and defatted by n-hexane, and then MCX was used as solid phase extraction cartridges to purify. The eluate was dried and reconstituted. Ractopamine, clenbuterol, salbutamol, salmeterol, mapentero, mabuterol, cimbuterol and cimaterol were determined by internal standard, others were determined by external standard. Results Average recoveries of the 22 β-agonists ranged from 80% to 125%, and the calibration curves were between the concentrations of 0.5?100.0 μg/kg with the correlation coefficient r>0.992. The limit of quantitation is not more than 0.5 μg/kg. Conclusion Due to its high sensitivity, accuracy and efficiency, the method is suitable for food safety control.