基于QuEChERS净化-气相色谱法检测蔬菜中16种有机磷农药残留  

GC Determination of 16 Organophosphorus Pesticide Residues in Vegetables Using QuEChERS Purification

作　　者：邹昀[1] 何明辉[1] 周锦[1] 张德新[2] 

机构地区：[1]天门市疾病预防控制中心,湖北天门431700 [2]湖北中医药大学检验学院,武汉430065

出　　处：《湖北农业科学》2017年第4期736-739,755,共5页Hubei Agricultural Sciences

摘　　要：建立了蔬菜中16种有机磷农药的气相色谱检测方法,探讨不同色谱柱、衬管、基质效应对分析效果的影响,检测了Qu ECh ERS净化管对16种农药的吸附情况,利用乙腈超声抽提,Qu ECh ERS法净化,采用火焰光度检测器(FPD)气相色谱法测定了植物性食品中16种有机磷农药的残留量。该方法回收率为84.0%~104.0%,相对标准偏差(RSD)为1.7%~3.2%。16种有机磷类农药的测定检出限为0.001~0.008mg/kg,定量限为0.003~0.024 mg/kg。16种农药运用TR-1701分离柱能完全分离,氧化乐果、乙酰甲胺磷、甲胺磷等在TR-PESTICIDEⅡ柱上有严重的拖尾现象。超高惰性衬管比普通脱活衬管减少的样品基质效应强;韭菜对16种有机磷农药有不同程度的基质减弱或增强效应;净化结果前后无显著差异。该方法快速、准确、灵敏,适于蔬菜中16种有机磷农药残留量的分析。To establish a gas chromatography method for the multi-residues analysis of 16 kinds of organophosphorus pesticides in plant food, we discuss different chromatographic column, liner, effect of matrix on the effect of the analysis and QuECh- ERS tube adsorption for 16 kinds of pesticides. Plant food were extracted by acetonitrile, purified on a QuEChERS pipe, and determined by GC-FPD. The average spiked recoveries ranged from 84.0% to 104.0% with relative standard deviations of 1.7%-3.2%. The limits of detection were in the range of more than 0.001~0.008 mg/kg and the limit of quantitation were in the range of less than 0.003-0.024 mg/kg. Using the TR-1701 can completely separate 16 kinds of pesticides, however omethoate, acephate, methamidophos has serious trailing phenomenon onTR-PESTICIDE H column. Ultra high inertia liner can reduce the sample matrix effect compared to ordinary living off liner. Chinese chives have effect of matrix for 16 organophos- pborus pesticides and there was no significant difference between before and after purification results. This method was rapid, sensitive and accurate, and met the detection requirement of 16 kinds of organophosphorus pesticides in plant.

关 键 词：QU ECH ERS 气相色谱 蔬菜 有机磷农药 

分 类 号：O657.71[理学—分析化学]