新农药氯溴虫腈在甘蓝和土壤中的残留检测方法  

Determination of Novel Insecticide HNPC-A3061 Residues in Cabbage and Soil

作　　者：阳承虎 欧晓明[1,3,4] 刘红玉[1,2] 梁骥[3,4] 付启明[3,4] 任竞[3,4] 聂思桥[3,4] 

机构地区：[1]湖南大学环境科学与工程学院,长沙410082 [2]湖南大学环境生物与控制教育部重点实验室,长沙410082 [3]湖南化工研究院国家农药创制工程技术研究中心,长沙410007 [4]农用化学品湖南省重点实验室,长沙410007

出　　处：《农药》2014年第3期194-196,199,共4页Agrochemicals

基　　金：“十二五”国家科技支撑计划课题(2011BAE06B01)

摘　　要：【目的】建立甘蓝和土壤中氯溴虫腈残留的检测分析法，为其合理使用准则的制定提供参考。【方法】土壤样品经乙腈提取、二氯甲烷萃取，甘蓝样品经乙腈提取、盐析作用，再用装有无水硫酸钠和弗罗里硅土一活性炭混合物（质量比50：11的层析柱净化，采用HP一1毛细管柱和带电子捕获检测器的气相色谱仪定量测定甘蓝和土壤中的氯溴虫腈残留量。【结果】在有效成分质量浓度0．01—10mg／L范围内氯溴虫腈峰面积与进样质量浓度呈现出良好的线性关系，R2=0．9995；在添加质量分数水平0．01～1.0mg／kg范围内，甘蓝和土壤中氯溴虫腈的平均回收率为96．0％～102．4％，相对标准偏差为3．4％-8．1％；方法最小检出量（LOD）为2×10^-11g，最低检测质量分数（LOQ）为0．01mg／kg。【结论】该方法简便、快速、准确度高、精密度好，符合农药残留分析的要求，适用于甘蓝和土壤中氯溴虫腈的残留分析检测。[Aims] The aim is to establish the determination method of novel insecticide HNPC-A3061 residue in cabbage and soil and provide the reference for setting of the reasonable application guideline of the insecticide. [Methods] Soil samples were extracted with acetonitrile, leached with dichloromethane, cabbage samples were extracted with acetonitrile, salted-out, and then purified by the column filled with the florisil-carbon mixture （mass ratio 50 ： 1）, and the HNPC-A3061 residues in cabbage and soil samples were quantified by GC equipped with HP-1 stainless steel colunm and ECD detector. [Results] There appeared a excellent linear relationship between the response values （peak area） of HNPC-A3061 and its mass concentrations in the concentration ranged from 0.01 to 10 mg/L with the linear correlation of 0.999 5. At the spiked concentration of 0.01-1.0 mg/kg, the average recovery rate of HNPC-A3061 in cabbage and soil sample was in the range from 96.0-102.4%, and coefficient of variation was 3.4-8.1%. The LOD of this method was 2×10^-11g, and the LOQ was 0.01 mg/kg. [Conclusions] The method was simple, fast, and very sensitive with good accuracy in compliance with pesticide residue analysis.

关 键 词：气相色谱 氯溴虫腈 甘蓝 土壤 残留分析 

分 类 号：O657.71[理学—分析化学] TQ450.263[理学—化学]