磁性石墨烯固相萃取-毛细管电泳联用测定水样中三嗪类农药残留  

Determination of Triazine Pesticides in Water Samples by Capillary Electrophoresis Coupled with Solid Phase Extraction Based on Magnetic Graphene Nanocomposite

作　　者：李亚珍[1] 李兆乾[1] 朱华玲[1] 王卫平[1] 

机构地区：[1]浙江师范大学化学与生命科学学院,金华321004

出　　处：《分析化学》2015年第12期1882-1887,共6页Chinese Journal of Analytical Chemistry

基　　金：国家自然科学基金资助项目(No.21305128)~~

摘　　要：以磁性石墨烯（G/Fe_3O_4）为固相萃取吸附剂,考察其对三嗪类农药的萃取富集性能,并结合毛细管电泳技术,建立了环境水样中三嗪类农药的分析方法。在最佳萃取条件下,即样品溶液pH=7.0,20.0 mg G/Fe_3O_4作为吸附剂,0.5 mL丙酮为洗脱液,萃取时间20 min,磁性石墨烯对三嗪类农药具有较好的富集作用。4种三嗪类农药的峰面积和浓度在5-500μg/L范围内呈良好的线性关系,线性相关系数大于0.9909,检出限（S/N=3）低于3.12μg/L。日内和日间相对标准偏差（n=5）分别在2.7%~12.7%和7.7%~14.0%之间。将本方法用于河水和自来水水样分析,平均加标回收率在70.4%~117.3%之间,相对标准偏差（n=3）小于11.5%。In this study,magnetic solid-phase extraction（MSPE） combined with capillary electrophoresis was developed for the simultaneous determination of four triazine pesticides in aqueous solution.The obtained magnetic nanocomposite（graphene/Fe_3O_4,G/Fe_3O_4） as adsorbent for MSPE endowed the method with good enrichment for triazine pesticides.The MSPE conditions such as pH of sample solution,amount of adsorbent,extraction time and elutent were investigated.Under the optimal MSPE conditions including 20 mg of adsorbent（G/Fe_3O_4）,0.5 mL of acetone as eluent and 20 min of extraction time in pH 7.0 solution,good linearities were obtained for the analytes between peak area and concentration in the range of 5-500 μg/L with correlation coefficients greater than 0.9909.Detection limits were less than 3.12 μg/L.The relative standard deviations（RSDs） for both intra-and inter-day analysis（n =5） were in the range of 2.7%-12.7%and 7.7%-14.0%,respectively.The established method was applied to analyze the water samples（river water and tap water）,and the mean recoveries of standard addition experiment were between 70.4%and117.3%for all analytes（RSDs less than 11.5%）.

关 键 词：磁性石墨烯 固相萃取 毛细管电泳 三嗪类农药 

分 类 号：X839.2[环境科学与工程—环境工程] O657.8[理学—分析化学]