基于磁纳米材料的土壤中多农药残留高通量分析技术研究  

High Throughput Analysis of Multiple Pesticides Residue in Soil Samples Using Magnetic Nanoparticles as Dispersive Adsorbent

作　　者：王娇[1] 齐沛沛[1] 刘真真[1] 孙宇涵 汪志威[1] 王祥云[1] 徐浩[1] 狄珊珊 王强[1] 王新全[1] WANG Jiao;QI Pei-Pei;LIU Zhen-Zhen;SUN Yu-Han;WANG Zhi-Wei;WANGXiang-Yun;XU Hao;DI Shan-Shan;WANG Qiang;WANG Xin-Quan(Institute of Quality and Standard of Agro-products,Zhejiang Academy of Agricultural Sciences,Hangzhou 310021,China)

机构地区：[1]浙江省农业科学院农产品质量标准研究所,杭州310021

出　　处：《分析化学》2019年第2期262-270,共9页Chinese Journal of Analytical Chemistry

基　　金：国家自然科学基金项目(No.31501556);公益性行业(农业)科技专项(No.201503107)资助~~

摘　　要：建立了土壤中43种农药及代谢物残留的高通量分析方法。土壤样品经乙腈超声萃取后,采用分散固相萃取法进一步对萃取液进行净化。选择修饰N-丙基乙二胺(PSA)的Fe_3O_4磁纳米材料和C_(18)为分散净化吸附剂,采用超高效液相色谱-串联质谱(UPLC-MS/MS)分析。优化实验结果表明,超声萃取时间为10 min、净化吸附剂Fe_3O_4-PSA用量为40 mg、C_(18)用量为30 mg时,农药的回收率最佳。除3-羟基克百威和水胺硫磷(5～250μg/L)外,各农药在2～250μg/L范围内呈良好线性关系,相关系数(R)均大于0.9700,检出限为0.1～1.0μg/L。在10、100和200μg/kg的添加浓度下,目标分析物在土壤中的回收率在74.1%～120.0%之间,相对标准偏差≤18.1%。本方法前处理过程简单,灵敏度高,净化效果好,适用于土壤中多农药残留分析。A simple and rapid sample pretreatment method was developed based on magnetic nanoparticles for multi-pesticides residue analysis in soil samples.The target analytes were extracted by acetonitrile under the assistance of ultra-sonication,followed by the purification of dispersive solid phase extraction.The magnetite(Fe3O4)nanoparticles modified with 3-(N,N-diethylamino)propyltrimethoxysilane(Fe3O4-PSA)and commercial C18 were selected as the cleanup adsorbents to remove the matrix interferences.The target analytes were further analyzed by ultra-high performance liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS).The factors influencing the recoveries of analytes,such as extraction time,amount of Fe3O4-PSA and C18,were optimized.The optimal extraction time was 10 min,and the amount of Fe3O4-PSA and C18 were 40 mg and 30 mg,respectively.The method showed good linearity in the concentration range from 2μg/L to 250μg/L except for 3-hydroxy-carbofuran and isocarbophos(5μg/L to 250μg/L).The limits of detection(LODs)ranged from 0.1μg/L to 1.0μg/L.The recoveries ranged from 74.1%to 120.0%at three spiked concentration levels with relative standard deviations of lower than 18.1%.The proposed method was rapid,simple,low-cost and effective for detection of trace multi-pesticides residue in soil.

关 键 词：土壤 磁分散固相萃取 液相色谱-串联质谱 多农药残留 

分 类 号：O657.63[理学—分析化学] X833[理学—化学]