超高效液相色谱-串联质谱法测定柑橘及柑橘精油中4种农药残留

摘要

A simple and rapid method was developed for the simultaneous determination of 4 residues, imidacloprid, carbendazim, prochloraz and β-cypermethrin, in citrus fruit and citrus essential oil. The residues were extracted from samples with acetonitnle and cleaned up with dispersive method on primary secondary amine, then detected by ultra liquid chromatography-mass spectrometry under multiple reaction monitoring mode, and quantified by matrix-match standard solution. Average fortified recoveries in samples were found in the range of 72. 6% -113. 3% at three fortified levels from 0. 01 to 1 mg/kg, with relative standard deviations of 0. 9%-19. 6% (n = 5). The limits of detection (LOD) of these four pesticides were in the range of 0. 02 -0. 6 μg/kg, while limits of quantification (LOQ) were in the range of 0. 06-2 μg/kg.%建立了柑橘及柑橘精油中吡虫啉、多菌灵、咪鲜胺和高效氯氰菊酯4种农药的多残留分析方法.前处理方法以乙腈为提取剂、N-丙基乙二胺(PSA)为分散净化剂的QuEChERS方法,并利用超高效液相色谱-串联质谱(UPLC- MS/MS)在多反应离子监测模式(MRM)下进行检测,外标法定量.结果表明:在0.01～1.00 mg/kg添加水平范围内,4种农药的平均回收率为72.6％～113.3％；相对标准偏差(RSD,n=5)为0.9％～19.6％；方法检出限(LOD)在0.02～0.60 μg/kg范围内；定量限(LOQ)在0.06～2.00μg/kg范围内.