色谱

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大葱中25种有机磷农药多残留的微波净化-气相色谱测定

姜俊,李安,李海燕,佟克兴,周丽丽,周慧敏,赵彤

  

  1. Dalian Institute of Product Quality Supervision and Inspection, Dalian 116021, China
  • 收稿日期:2007-01-15 修回日期:2007-03-01 出版日期:2007-05-30 发布日期:1985-09-25
  • 通讯作者: 姜俊

Determination of Organic Phosphorus Pesticide Residues in Scallion by Gas Chromatography Coupled with Microwave Clean-Up

JIANG Jun, LI An, LI Haiyan, TONG Kexing, ZHOU Lili, ZHOU Huimin, ZHAO Tong   

  1. Dalian Institute of Product Quality Supervision and Inspection, Dalian 116021, China
  • Received:2007-01-15 Revised:2007-03-01 Online:2007-05-30 Published:1985-09-25

摘要:

采用微波净化去除大葱中硫醚干扰、气相色谱-火焰光度检测(GC-FPD)实现了大葱基质中25种有机磷农药多残留的快速检测。25种有机磷的加标回收率为85.2%~119.6%,相对标准偏差为2.1%~14.8%。大多数农药在0.1~5.0 mg/L范围内线性关系良好,相关系数不低于0.9910,检出限为0.025~0.200 mg/L。

关键词: 大葱 , 气相色谱法, 微波净化, 有机磷农药残留

Abstract:

A method for the determination of organic phosphorus pesticide residues is described. It covers 25 residues in scallion including dichlorvos, ethoprophos, phorate, diazinon, disulfoton, dimethoate, pirimiphos-methyl, chlorpyrifos, malathion, fenitrothion, parathion, chlorfenvinphos, ethion, EPN, dyfonate, chlorpyrifos-methyl, parathion-methyl, fenthion, quinalphos, gardona, methidathion, carbophenothion, phosmet, phosalone, and coumaphos. After the scallion samples were heated for 30 s in microwave oven, the residues were extracted with acetonitrile, and then the organic phase was salted out from the matrix. As a result, most of the interfering impurities were abolished in the heating process. In this study, these pesticides were categorized into two groups for analysis. The gas chromatographic analysis was performed on a capillary column (DB-1701, 30 m×0.25 mm×0.25 μm) and determined with a flame photometric detector. Linear correlation coefficients of the 25 organic phosphorus pesticides were not lower than 0.9910 and the linear ranges for most of the compounds were between 0.1 to 5.0 mg/L. The detection limits were between 0.025 and 0.200 mg/L. In recovery study, average recoveries ranged from 85.2% to 119.6% at the fortification levels of 0.05, 0.2 and 0.5 mg/kg and the relative standard deviations were in the range of 2.1% and 14.8%. The method is a simple, rapid and highly efficient one to determine organic phosphorus pesticide residues in scallion.

Key words: gas chromatography (GC), microwave clean-up, organic phosphorus pesticide residues, scallion