气相色谱法测定柑橘与土壤中氟啶虫胺腈的残留量  

Determination of Sulfoxaflor Residue in Citrus Fruits and Soil by Gas Chromatography with Electron Capture Detector

作　　者：黄庆[1,2,3] 欧晓明[3,4] 陈力华[3,4] 梁骥[3,4] 付启明[3,4] 聂思桥[3,4] 欧阳承虎[1,2,3] 刘红玉[1,2] 张贵群[3,4] 

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

出　　处：《光谱实验室》2013年第2期985-990,共6页Chinese Journal of Spectroscopy Laboratory

基　　金：国家十二五科技支撑计划课题(2011BAE06B01);湖南省自然科学基金项目(09JJ3015)

摘　　要：建立了柑橘和土壤中氟啶虫胺腈残留量的气相色谱测定方法。柑橘全果、果肉和土壤样品中的氟啶虫胺腈用乙腈提取,果皮样品用乙腈-水(4:1,V/V)混合溶剂提取,经中性氧化铝柱净化,浓缩后采用气相色谱-电子捕获检测器(GC-ECD)检测。结果表明,在添加浓度为0.05—1.0mg/kg时,氟啶虫胺腈在样品中的平均回收率为81.3%—101.2%,相对标准偏差为0.9%—4.9%。方法的检出限(LOD)为5.0×10^(-11) g,氟啶虫胺腈在全果、果肉、果皮和土壤中的最低检测浓度(LOQ)为0.05mg/kg。该方法杂质干扰少,准确性及灵敏度满足农药残留检测的基本要求,对检测硬件要求低,适用于柑橘和土壤中氟啶虫胺腈残留的分析。A method for determination of sulfoxaflor residue in citrus fruits and soil was established based on gas chromatography with electron capture detector （GC-ECD）. The sulfoxaflor residue in the whole orange, pulp and soil was extracted with acetonitrile, and the orange peel was extracted with acetonitrile-water solution （4 ： 1 ,V/V）,cleaned-up through the glass chromatography column filled orderly with anhydrous sodium sulfate, neutral aluminum oxide and anhydrous sodium sulfate from bottom to top, and determined by GC-ECD. Average spiked recoveries of sulfoxaflor in orange and soil samples were found in the range of 81. 3%-101. 2% at the spiked level from 0.05mg/kg to lmg/kg, with relative standard deviations （RSDs） of 0. 9%-4. 9%. The limit of detection （LOD） of sulfoxaflor was 5.0×10^-11g,and the limit of quantification （LOQ） of sulfoxaflor in samples was 0. 05mg/kg. The method was proved to meet the requirements of pesticide residue analysis on accuracy,sensitivity and precision,and to be suitable for the analysis of sulfoxaflor residue in citrus fruit and soil.

关 键 词：氟啶虫胺腈 气相色谱 柑橘 土壤 残留 

分 类 号：O657.71[理学—分析化学]