多壁碳纳米管分散固相萃取气相色谱法检测蔬菜中23种农药残留  

Detection of 23 pesticides in vegetables by multi-walled carbon nanotubes dispersive solid phase extraction combined with gas chromatography

作　　者：刘晓亮[1] 郭泽旺 黄璐璐[1] 封国君 王彦辉[1,2] 曾东强[1] 黄永禄[1] 

机构地区：[1]广西大学农药与环境毒理研究所,南宁530005 [2]广西农业科学院植物保护研究所,南宁530007

出　　处：《南方农业学报》2016年第3期401-406,共6页Journal of Southern Agriculture

基　　金：广西自然科学基金项目(2015GXNSFBA139062;2013GXNSFBA019049);国家现代农业产业技术体系广西创新团队建设项目[大宗蔬菜产业功能专家(nycytxgxcxtd-03-10)];广西大学科研基金项目(XJZ130368)

摘　　要：【目的】建立一种多壁碳纳米管（MWCNTs）分散固相萃取气相色谱法（GC）检测蔬菜中多种农药残留的分析方法,为气相色谱法快速检测蔬菜中农药残留提供一种新的材料和应用方法。【方法】采用分散固相萃取法,10.00 g样品用10 m L乙腈提取,加入1.00 g Na Cl和4.00 g无水Mg SO4液液分离,取1 m L乙腈提取液用150 mg无水Mg SO4和15 mg多壁碳纳米管进行分散固相净化,运用气相色谱微电子俘获检测器（GC-u ECD）进行分析检测,通过添加回收试验对方法进行考察,基质匹配标准液外标法定量对蔬菜中23种农药进行检测。【结果】在0.05~1.00 mg/kg添加范围内,23种农药的添加回收率为73.0%~98.4%,相对标准偏差（RSD,n=5）为1.3%~11.0%,方法的定量限（LOQ）为0.02~0.05 mg/kg。采用该方法对市场样品进行检测,无目标农药检出。【结论】多壁碳纳米管作为分散固相吸附剂与气相色谱联用,在回收率、检出限及精密度等方面均能满足农药残留分析的要求,且成本明显低于商品化基质分散吸附剂,可在蔬菜农药残留检测分析中推广应用。【 Objective 】 The multi- walled carbon nanotubes（ MWCNTs） dispersive solid phase extraction（d-SPE）method combined with gas chromatography was established to determine pesticide multi-residue in vegetables, in order to provide a new material and application method for rapid determination of pesticide residue in vegetables using gas chromatography. 【Method】The dispersive solid-phase extraction method was used to extract pesticide from samples. Firstly,10.00 g samples were treated with 10 m L acetonitrile, and then liquid-liquid separation was realized by adding 4.00 g anhydrous Mg SO4 plus 1.00 g Na Cl. After that, 1 m L acetonitrile extracts solution was purified by using 150 mg anhydrous Mg SO4 and 15 mg MWCNTs. the extracts were determined by gas chromatography with micro-electron capture detection（GC-u ECD）. Finally, the accuracy of this method were investigated based on recovery test, and then 23 kinds of pesticides in vegetables was determined by of matrix-matched external standard method. 【Result】When adding 0.05-1.00 mg/kg,the recoveries for 23 kinds of pesticides were 73.0%-98.4%, with relative standard deviation（RSD, n =5） of 1.3%-11.0%, and the limit of quantitation（LOQ） was 0.02-0.05 mg/kg. Using this method detect pesticides in market samples,and the target pesticides were not detected. 【Conclusion】MWCNTs as a d-SPE adsorbent combined with gas chromatography can meets requirements for pesticide residue analysis in some respects of recovery, LOQ and precision. Furthermore,this method has broad application prospect because low cost of MWCNTs is lower greatly than that of other commercial d-SPE adsorbents.

关 键 词：多壁碳纳米管 分散固相萃取 GC-u ECD 蔬菜 农药残留 

分 类 号：S481.8[农业科学—农药学]