超高效液相色谱串联质谱法快速检测鸡蛋和鸡肉中的非泼罗尼及其代谢物的残留量

Rapid determination of fipronil and its metabolite residues in eggs and chicken by ultra performance liquid chromatography tandem mass spectrometry

中文关键词:  非泼罗尼  代谢物  鸡蛋  鸡肉  残留  超高效液相色谱串联质谱法

英文关键词:fipronil  metabolites  egg  chicken  residue  ultra performance liquid chromatography tandem mass spectrometry

中文摘要:

      目的 建立超高效液相色谱串联质谱法(ultra performance liquid chromatography tandem mass spectrometry, UPLC-MS/MS)检测鸡蛋和鸡肉中非泼罗尼及其代谢物(氟甲腈、非泼罗尼硫醚和非泼罗尼砜)残留量的分析方法。方法 鸡蛋和鸡肉中的非泼罗尼及其代谢物经乙腈提取后, 加入盐析剂进行分层, 经Oasis PRiME HLB固相萃取净化后, UPLC-MS/MS法检测, 基质匹配标准曲线法定量。结果 该方法具有良好的准确度和精密度, 在鸡蛋和鸡肉中添加回收率范围分别为79.2%~103.1%和83.5%~101.4%, 相对标准偏差(relative standard deviation, RSD)低于8.1%。方法的检出限和最低定量限分别为0.5 μg/kg和1.0 μg/kg。结论 该方法具有分析时间短、样品处理简单、溶剂用量少等优点, 适用于鸡蛋和鸡肉中非泼罗尼及其代谢物残留量的常规检测。

英文摘要:

      Objective To establish a method for the determination of fipronil and its metabolite (fipronil-desulfinyl, fipronil-sulfide and fipronil-sulfone) residues in eggs and chicken by ultra performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS). Methods The fipronil and metabolites in chicken and eggs were extracted by acetonitrile, and samples were layered by joining the salting-out agent. The extracts were purified by the Oasis PRiME HLB solid phase extraction, then analyzed by UPLC-MS/MS, and the matrix-matching standard curve method was used to quantify. Results The method had good accuracy and precision, and the recovery range of egg and chicken was 79.2%~103.1% and 83.5%~101.4%, respectively, with the relative standard deviation (RSD) of lower than 8.1%. The limit of detection was 0.5 μg/kg and the limit of quantitation was 1.0 μg/kg. Conclusion This method is time-saving, simple and less solvent consumption, which is suitable for detection of fipronil and its metabolites residues in eggs and chicken.