气相色谱法测定蔬菜中多种有机磷农药残留量研究

Measurements of Organic Phosphorus Residual Quantity in Vegetable by Using GC

在用岛津GC2010气相色谱仪、氮磷检测器（Fq＇D），采用毛细管气相色谱法测定蔬菜中甲胺磷、氧化乐果、久效磷、乐果、二嗪农、磷胺、甲基对硫磷、马拉硫磷、对硫磷、水胺硫磷等10种有机磷农药。该方法结合前处理方法较为简单、快捷的标准NY/T761-2008和灵敏度较高的上机检测[氮磷检测器（FTD）GB／T5009．145—2003]2种方法，取得了较好的结果-10种有机磷农药都能得到较好的分离，分离效果好。，采用外标法定量，测定分析方法的相对标准偏差在1．14％～6．87％。对每种农药作3种不同浓度（0．004、0．040、0．100mg／kg）添加回收率试验。结果表明，10种有机磷农药标样的添加平均回收率在80．27％～123．86％，变异系数（相对标准偏差）在O．81％。7．33％，最小检测浓度在1．05×10^-4～5．13×10^-5，比火焰光度检测器（FPD）的检出限提高了100～1000倍，符合国家农药残留量测定方法的要求。

Tests have been made by capillary gas chromatography with SHIMADZU GC2010 chromatography and nitrogen-phosphorus detector （FTD） to analyze ten kinds of organophosphorus pesticide residues in the vegetable, including Methamidophos, Omethoate, Monocrotophos, Phorate, Dimethoate, Diazinon, Phosphamidon, Parathion-methyl, Malathion, Parathion, Isocarbophos. In the test, good test results have been got through combination of simple and standard NY/T 761-2008 and FFD of high sensitivity. All of the ten kinds of organophosphorus pesticide have been separated. By an external standard method, the relative error of this test was between 1.14% and 6.87%. The added recovery rates have been studied to every kind of organophosphorus pesticide by three different concentration （0.004,0.040,0.100 mg/kg）. It showed that the average reeovery ratio was between 80.27% and 123.86%, the relative standard deviation （coefficient of variation） was 0.81%-7.33%, and the minimum detectable concentration was 1.05~10^-4- 5.13× 10^-5 with a 100 to 1000-fold inerease of the detection limit of flame photometric detection （FPD）. The results of this test had met the requirement of national method of pesticide residue analysis.