气相色谱质谱联用法测定鱼组织中5种苯甲酰脲类杀虫剂残留  

Simultaneous Analysis of Five Benzoylurea Insecticide Residues in Fish by Gas Chromatography-Mass Spectrometry

作　　者：王晓琳[1] 丁双阳[2] 宋幸辉[1] 裴亚玲[1] 

机构地区：[1]河南牧业经济学院,郑州450046 [2]中国农业大学,北京100094

出　　处：《农药》2016年第10期757-759,766,共4页Agrochemicals

摘　　要：[目的]建立鳗鱼、泥鳅、黄鳝和鲶鱼组织中5种苯甲酰脲类杀虫剂的气相色谱质谱联用（GC-MS）检测方法。[方法]样品组织经提取、净化等步骤,七氟丁酸酐（HFBA）衍生化,GC-MS分析。对衍生化条件进行了细致的探索。[结果]经验证,方法线性良好,检测限0.3~1.5μg/kg,定量限1.0~5.0μg/kg。在3个添加水平下,5种目标化合物在4种组织中的变异系数均小于10.3%,平均回收率81.5%~98.7%。并在实测样品中成功检测出目标化合物。[结论]该方法可用于鱼组织中目标化合物的检测。[Aims ] A method for detection of 5 benzoylurea insecticide residues in eel, catfish, loach and monopterus tissues by gas chromatography-mass spectrometry was established. [Methods ] The residues of target compounds were extracted, cleaned up, derivatized with heptafluorobutyric anhydride（HFBA） and detected by GC-MS. Optimal conditions for the derivatization were investigated. [Results ] The linearity of the analytical method was excellent. The limit of detection（LOD） was 0.3-1.5 μg/kg, and the limit of quantification（LOQ） was 1.0-5.0 μg/kg. At three fortification levels, the average recoveries for this four kinds of samples ranged from 81.5 to 98.7%, and the relative standard deviation（RSD） were all below 10.3%. This method was successively applied to the determination of the five compounds in real samples from markets. [Conclusions ] The method is suitable for the simultaneous determination of five benzoylurea insecticide residues in fish tissues.

关 键 词：苯甲酰脲类杀虫剂 鱼 衍生化 气相色谱-质谱联用 

分 类 号：O657.63[理学—分析化学] TS254.7[理学—化学]