针对吡虫啉、啶虫脒、噻虫嗪、噻虫胺、噻虫啉、呋虫胺等6种新烟碱类和乐果、敌敌畏、毒死蜱等3种有机磷类杀虫剂建立了蜂蜜中分散固相萃取法－超高效液相色谱?串联质谱的残留分析方法．前处理方法利用乙腈为提取剂，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，9种杀虫剂在5—800μg·L－1浓度范围内均具有良好的线性关系（R≥0．994）；在0．005—0．200 mg·kg－1添加，水平范围内平均回收率在80．4％—107．5％之间，相对标准偏差在1．2％—6．8％之间；方法检出限（LOD）在0．1—1．5μg·kg－1范围内；定量限（LOQ）在0．3—4．5μg·kg－1范围内．该方法分析速度快、灵敏度高、重现性好，适用于蜂蜜中多种农药残留的快速检测和确证．
A method was developed for the simultaneous determination of 6 neonicotinoid insecticides and 3 organophosphorus insecticides including imidacloprid, acetamiprid, thiamethoxam, clothianidin, thiacloprid, dinotefuran, dimethoate, DDVP and chlorpyrifos in honey. The residues were extracted from the samples with acetonitrile and cleaned up with dispersive method on PSA, then detected by ultra liquid chromatography?mass spectrometry under multiple reaction monitoring mode, and quantified by matrix?match standard solution. The results showed the method had good linearity ( R≥0.994) from 5—800μg·L-1 . Average fortified recoveries in samples were in the range of 80. 4%—107. 5% at three fortified levels from 0. 005—0. 200 mg·kg-1 , with relative standard deviations of 1.2%—6.8% ( n=5) . The limits of detection ( LOD) of these 9 insecticides were in the range of 0.1—1.5 μg·kg-1, while limits of quantification (LOQ) were in the range of 0.3—4.5 μg·kg-1 . The method is rapid and simple with high sensitivity and good reproducibility, and suitable for determination of different insecticides in honey.
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