动物肌肉、内脏和牛奶中咪唑脲苯残留量的高效液相色谱测定及液相色谱-串联质谱确证

摘要

目的：建立固相萃取净化-高效液相色谱和液相色谱-串联质谱测定动物组织和牛奶中咪唑脲苯残留量的分析方法。方法残留的咪唑脲苯采用1%三氟乙酸-乙腈(1：4, v/v)提取, Oasis WCX固相萃取柱净化,高效液相色谱外标法定量,并经液相色谱-串联质谱确证。结果咪唑脲苯检出限为10μg/kg(S/N≥3),定量限为25μg/kg(S/N≥10)；在LOQ、MRL和2MRL三个添加水平下重复分析6次,回收率为72.7%~101%,相对标准偏差为1.2%~6.9%。结论该方法稳定、可靠,适用于动物组织和牛奶中咪唑脲苯的测定。%Objective A method for determination of imidocarb in animal tissues and milk by SPE-HPLC-MS/MS confirmation was developed. Methods The sample was extracted by 1% trifluoroacetic acid-acetonitrile(1:4, v/v), purified by SPE, detected by HPLC and quantified by the external standard. Results The LOD and LOQ of imidocarb were 10μg/kg (S/N≥3) and 25μg/kg (S/N≥10). The average recoveries range of imidocarb at three levels of LOQ, MRL and 2MRL was 72.7%~101%with the relative standard deviations (RSDs) of 1.2%~6.9%. Conlusion This method is convenient, accurate and sensitive so it can be applied to determinate imidocarb residues in animal tissues and milk.