第 46 卷第 2 期 Vol. 46 No. 2 2016 年 4 月 Apr 2016

所属栏目：分析与测试 乙螨唑在柑橘和土壤中的残留检测方法研究

刘 晴1，彭秧锡1*，欧晓明1，2，3，梁 骥2，3，张贵群2，3，付启明2，3，金晨钟1 （1. 湖南人文科技学院 农田杂草防控技术与应用协同创新中心，湖南 娄底 417000；2. 湖南化工研究院有限公司 国家农药创制工程技术研究中心，湖南 长沙 410014；3. 湖南省农用化学品重点实验室，湖南 长沙 410014）

摘　要：乙螨唑是登记用于防治柑橘害螨的二苯基噁唑啉类杀螨剂。为了评价其在柑橘生态系统中的归趋，采用气相色谱仪-氮磷检测器（GC-NPD）建立了乙螨唑在柑橘全果、果皮、果肉及土壤中的残留检测分析方法。样品在醋酸钠缓冲液中采用乙腈进行提取，经盐析后浓缩，GC-NPD检测。结果表明，添加水平为0.1～5.0 mg／kg时，乙螨唑在柑橘全果、果皮、果肉及土壤中的平均添加回收率为93.4%～101.2%，相对标准偏差为1.6%～4.5%。乙螨唑在柑橘中的最小检出量（LOD）为0.4 ng，最低检测浓度（LOQ）为0.1 mg／kg，说明该方法的准确度和精密度符合国家农药残留检测分析要求。

关键词：气相色谱-氮磷检测器；乙螨唑；残留；柑橘；土壤

中图分类号：O657.7+1　　文献标识码：A　　文章编号：1009-9212（2015）06-0068-05

Determination of Etoxazole Residue in Citrus and Soil by GC-NPD

LIU Qin1, PENG Yang-xi1*, OU Xiao-ming1，2，3, LIANG Ji2，3, ZHANG Gui-qun2，3, FU Qi-ming2，3, JIN Chen-zhong1 (1. Collaborative Innovation Center for Field Weeds Control and Application，Hunan University of Humanities, Science and Technology，Loudi 417000，China; 2. National Engineering Research Center for Agrochemicals, Hunan Research Institute of Chemical Industry Co.,Ltd., Changsha 410014, China; 3. Hunan Province Key Laboratory for Agrochemicals，Changsha 410014，China)

Abstract：Etoxazole is an acaricide belonging to the diphenyloxazoline group of chemicals which is registered for control of the mites in crops such as citrus through inhibition of chitin biosynthesis and by causing adults to lay sterile eggs. In order to evaluate the fate of etoxazole in citrus ecosystem，a method for the determination of etoxazole residue in the whole orange，peel，pulp and soil was established using gas chromatography with nitrogen phosphorus detector（GC-NPD）. The samples were extracted with acetonitrile in the sodium acetate buffer solution，concentrated after salting out and determinated by GC-NPD. The results showed that the average recoveries of etoxazole in the whole orange，peel，pulp and soil were from 93.4% to 101.2%，and the relative standard deviations were from 1.6% to 4.5% when the spiked levels ranged from 0.1 mg／kg to 5.0 mg／kg. LOD and LOQ of the method was 0.4 ng and 0.1 mg／kg，respectively，indicating that the method meet with the requirement for residue test guideline.

Key words：GC-NPD；etoxazole；residue；citrus；soil

基金项目： 湖南省科技计划项目（2015JC3062）资助。

作者简介： 刘 晴（1990-），女，湖南益阳人，硕士研究生，主要从事农药残留化学研究。

联 系 人： 彭秧锡，教授，主要从事分析化学和材料化学的教学与科研工作研究。

收稿日期： 2015-12-2