液相色谱-串联质谱法同时测定动物源性食品中9种β-受体激动剂

Simultaneous determination of 9β-agonists in animal derived food by liquid chromatography/tandem mass spectrometry

目的:建立对肉类食品中9种β-受体激动剂的高效液相色谱-串联质谱测定方法。方法:捣碎的样品用酶水解后,高氯酸提取,经离心后过滤,滤液用HLB和MCX固相萃取柱净化,氮气吹干,流动相溶解,液相色谱-串联质谱仪测定,选用D3-沙丁胺醇、D6-莱克多巴胺、D9-克伦特罗作为内标,峰面积定量。对样品前处理和色谱、质谱条件进行了优化。结果:样品测定的相对标准偏差在0.7%~9.6%,加标回收率在74.9%~106.9%,检出限和定量限分别为0.01μg/kg-0.05μg/kg和0.03μg/kg-0.20μg/kg。结论:方法灵敏度高、定性及定量准确,满足肉类食品中9种β-受体激动剂的测定要求。

Objective：Established a method for determination of 9β-agonists in meat foods by highperformance liquid chromatography/tandem mass spectrometry.Methods：The sample was cut into small slices and hydrolyzed by enzyme,then extracted by perchloric acid,centrifuged and filtered.The filtrate was purified by two kind of solid phase extraction cartridges,HLB and MCX,and then determined by HPLC-MS/MS with D3-salbutamol,D6-ractopamine and D9-clenpenterol as internal standards,quantitated by the peak area.Results：Sample preparation and the operation parameters of the instrument have been optimized,and the relative standard deviations of detection were at 0.7%~9.6%,the recoveries of analytes were at 74.9%-106.9%.The limits of detection and quantification were 0.01μg/kg^0.05μg/kg and 0.03μg/kg^0.20μg/kg,respectively.Conclusion：The method has high sensitivity,accurate quantitative and qualitative analysis,it can meet the determination requirements of 9β-agonists in meat foods.