气相色谱法测定水产品中4种三唑类农药残留

Determination of four triazole pesticides residues in aquatic products by gas chromatography spectrometry

本文建立了一种水产品中4种三唑类农药残留的固相萃取-气相色谱检测方法,4种三唑类农药包括三唑酮、三唑醇、环丙唑醇和联苯三唑醇。采用乙腈提取样品,石墨化碳黑-弗罗里硅土复合柱净化,丙酮-正己烷(1∶9,V/V)溶液洗脱,以及利用气相色谱法测定和外标法定量。研究显示,三唑酮在1.25~125.00 ng/m L,三唑醇、环丙唑醇和联苯三唑醇在25~2 500 ng/m L范围内响应值与质量浓度的线性关系良好,相关系数为0.999 7~0.999 8。当添加浓度分别为三唑酮0.4~8.0μg/kg,三唑醇、环丙唑醇和联苯三唑醇8~160μg/kg时,鳗鲡、日本对虾、鲍鱼和龙须菜加标样品的日内和日间平均回收率为78.8%~95.0%,相对标准偏差为1.48%~11.4%;三唑醇、环丙唑醇和联苯三唑醇检出限均为4.0μg/kg,最低定量限均为8.0μg/kg;三唑酮的检出限为0.2μg/kg,最低定量限为0.4μg/kg。研究结果表明,本文建立的固相萃取-气相色谱检测方法可以有效检测出水产品中4种三唑类农药的残留。

A Gas Chromatography Spectrometry method（ GC） for determination of 4 kinds of triazole pesticides residues including triazolone,triadimenol,cyproconazole and bitertanol in aquatic products was established in this study. The triazole pesticides were extracted with acetonitrile,then purified by graphitizing carbon-florisil column and eluted with acetone-n-hexane（ 1∶ 9,V/V）. Then the prepared samples were analyzed by gas chromatography spectrometry and quantified through external standard method. Results showed that the response value of triazolone has good linear relationship with mass concentration in the range of 1. 25～ 125. 00 ng/m L,and that of the other three pesticides were 25 ～2500 ng/m L. The correlation coefficients were all in the range of 0. 999 7 ～ 0. 999 8. When triazolone was spiked within 0. 4 ～ 8. 0 μg/kg and the others were spiked within 8 ～ 160 μg/kg,the average recoveries of intraday and interday of eel,Penaeus japonicus,abalone and asparagus were 78. 8% ~ 95. 0%, and their relative standard deviations were 1. 48% ～11. 4%. The limits of detection and quantitation of triadimenol、 cyproconazole and bitertanol were4. 0 μg/kg and 8. 0 μg/kg respectively,and that of triazolone was 0. 2 μg/kg and 0. 4 μg/kg respectively.These results suggested that the GC method established in this study could effectively detect the residues of 4 kinds of triazole pesticides in aquatic products.