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[目的]研究油菜及土壤中氨氯吡啶酸残留量的气相色谱分析方法,为全面评价氨氯吡啶酸的环境效应及合理使用提供依据。[方法]向样品中加入1 mol/L硫酸溶液,用乙酸乙酯-石油醚(体积比1∶1)提取。甲基化后,将提取的有机相通过气相色谱-电子俘获检测器(GC-ECD)测定,面积外标法定量。[结果]确定方法检出限为2.0×10-3mg/kg,平均回收率为87.8%~108.4%,相对标准偏差为2.1%~7.8%。[结论]方法准确度高、精密度好,是一种较为实用的分析方法。
[Objective] The research aimed to study the gas chromatographic analysis of clopyralid residues in rapeseed and soil, and provide a basis for the comprehensive evaluation of the environmental effects and reasonable use of clidin. [Method] 1 mol / L sulfuric acid solution was added to the sample and extracted with ethyl acetate - petroleum ether (1: 1 by volume). After methylation, the extracted organic phase was determined by gas chromatography-electron capture detector (GC-ECD) and area external standard method. [Result] The detection limit of determination method was 2.0 × 10-3mg / kg, the average recovery was 87.8% -108.4% and the relative standard deviation was 2.1% -7.8%. [Conclusion] The method has high accuracy and good precision, which is a more practical analysis method.