摘要
本文开发了基于QuEChERS前处理结合气相色谱三重四极杆串联质谱检测土壤中227种农药残留的高通量方法.对QuEChERS前处理的提取方式、提取时间、缓冲盐、净化条件等参数进行了优化,在最优条件下进行了方法学考查.结果表明,227种农药在2—200μg·L-1的范围内,线性良好,绝大部分农药的线性相关系数大于0.99;农药回收率在70%—120%之间,相对标准偏差<20%.根据不同添加浓度下的准确度和精密度数据确定了本方法的定量限在2—20μg·kg-1之间,78.4%的农药定量限可低至2μg·kg-1.最后将方法用于实际样品的检测.该方法简单、快速、重现性好、灵敏度高,可满足土壤中农药残留的大批量快速筛查和准确定量分析.
Quick and high efficient multiresidue analysis method is critical for screening and moniotring of the pesticide residue in soil. In this study, a high throughput multiresidue method was developed based on QuEChERS sample preparation method combined with gas chromatography-triple quadrupole mass spectrometry. The extraction and clean-up procedures and parameters including extraction method, extraction time, buffer system, and clean-up adsorbent selection were thoroughly investigated and optimized. Most coefficients of determination(r2) were higher than 0.99 within the calibration linearity range of 2—200 μg·L-1. Most recoveries at six spiking levels were in the range of 70%—120% with RSDs<20% indicating satisfactory accuracy. The limits of quantification(LOQ) for the pesticides were determined based on recovery and accuracy results and ranged from 2 to 20 μg·kg-1, and for 78.4% of the pesticides the LOQs were 2 μg·kg-1. Finally, the proposed method was used in real sample analysis. This method was proved to be simple, sensitive and effective, which can be applied for large-scale pesticide screening and quantification in soils.
作者
贺泽英
张艳伟
王雯雯
吕美玲
徐亚平
HE Zeying;ZHANG Yanwei;WANG Wenwen;LYU Meiling;XU Yaping(Key Laboratory for Environmental Factors Control of Agro-product Quality Safety,National Reference Laboratory for Agricultural Testing P.R.China,Ministry of Agriculture,Agro-Environmental Protection Institute,Ministry of Agriculture and Rural Affairs,Tianjin,300191,China;Agilent Technologies(China)Company,Ltd.,Beijing,100102,China)
出处
《环境化学》
CAS
CSCD
北大核心
2020年第7期2022-2025,共4页
Environmental Chemistry
基金
国家重点研发计划(2016YFD0201203)资助
