土壤中六种新烟碱类农药残留的分离及光谱研究  

Simultaneous Determination of 6 Neonicotinoid Residues in Soil Using DLLME-HPLC and UV

作　　者：孙宝利[1] 陕红[1] 李艳华[1] 曾娅玲[1] 申秀丽[1] 仝乘风[1] 

机构地区：[1]中国农业科学院农业环境与可持续发展研究所,农业部农业环境与气候变化重点开放实验室,北京100081

出　　处：《光谱学与光谱分析》2013年第9期2553-2557,共5页Spectroscopy and Spectral Analysis

基　　金：国家循环农业污染控制关键技术项目(2012BAD14BO2);国家自然科学基金项目(41201234)资助

摘　　要：建立了一种可同时检测土壤中吡虫啉、啶虫脒、噻虫嗪、噻虫啉、噻虫胺、烯啶虫胺六种新烟碱类农药残留的方法,该方法操作简单、成本低廉且重现性好,符合环境研究过程中实验量大、样品量多的特点。土壤样品经乙腈:二氯甲烷(2∶1φ)提取后,进一步用分散液液微萃取处理。分析方法采用Alltima TMC18色谱柱(4.6mm×250mm,5μm)分离,PDA检测器检测,外标法定量。六种农药在0.5～200μg·L-1浓度范围内线性关系良好,相关系数为0.998 2～0.999 9,检测限为0.000 5～0.003μg·mL-1(S/N=3)。以五种土壤为代表,在0.05,0.1,1.0mg·kg-1三个添加水平的平均加标回收率为55.3%～95.6%,相对标准偏差为1.4～7.0%。同时应用紫外分光光度法对净化效果进行考察,证明本实验所建立的方法具有明显的净化作用,因此满足土壤中六种新烟碱类农药残留检测的要求。A simple,cheap and rugged method was developed for simultaneous deter mination of 6neonicotinoid residues in soil,including imidacloprid,acetamiprid,thiamethoxam,thiacloprid,clothianidin and nitenpyram.The soil sample was produced by dispersive liquid-liquid micro-extraction（DLLME）after extracted by the mixed solution of acetonitrile and CH2Cl2（2∶1,φ）.The analytes were separated by HPLC with Alltima TMC18column（4.6mm×250mm,5μm）and detected by PDA at 260nm.External standard method was used for quantification.The results showed that good linearity was obtained with correlation coefficients between 0.998 2and 0.999 9in the range of 0.5～200μg·L^-1.The limits of detection（LODs）were in the range between 0.000 5and 0.003μg·mL^-1（S/N=3）.The method was validated with five soil samples spiked at three fortification levels（0.05,0.1,1.0mg·kg^-1）and recoveries were in the range of 55.3%～95.6% with RSD of 1.4%～7.0%.The effect of clean-up was evaluated by UV spectra and demonstrated that the method established is effective.In conclusion,this method is competent for the simultaneous analysis of 6neonicotinoid residues in soil.

关 键 词：HPLC 紫外光谱 分散液液微萃取 新烟碱类农药 土壤 

分 类 号：O657.7[理学—分析化学]