同位素稀释-液相色谱-串联质谱快速测定猪肝中4种β_(2)-受体激动剂残留

Rapid Determination of Residues of Four β_(2)-agonists in Pig Liver by Isotope Dilution-Liquid Chromatography-Tandem Mass Spectrometry

[目的]建立同位素稀释-液相色谱-串联质谱(LC/MS/MS)测定猪肝中沙丁胺醇、克伦特罗、莱克多巴胺和氯丙那林的分析方法。[方法]样品经5%高氯酸水解后,加入固体缓冲剂,用乙酸乙酯-叔丁基甲醚(3∶2,V/V)提取,氮吹复溶后,正己烷净化,采用Agilent ZORBAX SB-Aq色谱柱分离。[结果]沙丁胺醇、克伦特罗、莱克多巴胺、氯丙那林在0.25~10.00μg/L线性良好(r≥0.9975);方法的定量限为0.50μg/kg。在3个添加水平下回收率为82.5%~109.7%,RSD为1.0%~12.2%。[结论]该方法灵敏、快速、准确,适用于猪肝中4种β_(2)-受体激动剂快速定性和定量筛查。

[Objective]To establish an analytical method for the determination of salbutamol,clenbuterol,ractopamine and cloprenaline in pig liver by isotope dilution-liquid chromatography-tandem mass spectrometry(LC/MS/MS).[Method]The sample was hydrolyzed with 5%perchloric acid,and the solid buffet was added,and extracted with a mixture of ethyl acetate-tert-butyl methyl ether(3∶2,V/V),the extraction solution was dried under a stream of nitrogen,and dissolved with initial moble phase,then purified with N-hexane.The target analytes were separated by the Agilent ZORBAX SB-Aq.[Result]The salbutamol,clenbuterol,ractopamine and clorprenalin had good linearity at 0.25-10.00μg/L(r≥0.9975);the limit of quantification of the method was 0.50μg/kg.The average recoveries at the three leves of addition were 82.5%-109.7%,RSD was 1.0%-12.2%.[Conclusion]The method is sensitive,rapid and accurate,and is suitable for the rapid qualitative and quantitative screening of four β_(2)-receptor agonists in pig liver.