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

Determination of imidocarb residue in animal tissues and milk by HPLC and HPLC-MS/MS

中文关键词:  咪唑脲苯  动物组织  牛奶  固相萃取  高效液相色谱法；高效液相色谱-串联质谱法

英文关键词:imidocarb  animal tissues  milk  solid-phase extraction(SPE)  high performance liquid chro-matography(HPLC)  high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)

中文摘要:

      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10 μg/kg(S/N≥3), 定量限为25 μg/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。

英文摘要:

      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 10 μg/kg (S/N≥3) and 25 μg/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.