农业环境科学学报2017，Vol.36Issue(8)：1680-1688,9.DOI:10.11654/jaes.2016-1657
QuEChERS方法联合HPLC-MS/MS和GC-MS测定土壤中110种农药残留
Development of a multiresidue method for determination of 110 pesticide residues in soil using QuEChERS-HPLC-MS/MS and QuEChERS-GC-MS
摘要
Abstract
A method was established for the determination of 110 pesticides in soil using high performance liquid chromatography tandem mass spectrometry(HPLC-MS/MS)and gas chromatography tandem mass spectrometry(GC-MS)with modified QuEChERS(Quick, Easy, Cheap, Effective, Rugged, and Safe). Levels of acetic acid used in the QuEChERS procedure were optimized, and results indicated that higher recoveries were obtained when 1%acetic acid was added. Based on differences in polarity, thermostability, volatility, and other char-acteristics of pesticides, analysis of 43 pesticides was conducted via HPLC-MS/MS and the other 67 pesticides were analyzed using GC-MS. Five internal standards(atrazine-d5, sulfosulfuron, 1,3-dimethyl-2-nitrobenzene, triphenyl phosphate, and perylene-d12)were used for the method validation. The average recoveries of the 43 pesticides analyzed via HPLC-MS/MS at three spike levels(10, 20, and 50μg·kg-1) ranged from 59.1%to 129.4%with relative standard deviations(RSDs)between 0.3%and 15%;whereas the average recoveries of the 67 compounds analyzed using GC-MS ranged from 44.9%to 168.1%with RSDs of 0.5%~20%. The detection limits of the method ranged from 0.01 to 5.00μg·kg-1. The established method was used to determine pesticide resides in a soil sample, in which 68 pesticides were found, including nicosulfuron, propyzamide, oxyfluorfen, folpet, dimethomorph, lambda-cyhalothrin, some organophosphorus pesticides, and some organochlorine pesticides. Overall, the method is simple, efficient, and sensitive, and thus can be used for the simultaneous determination of pesticide residues in soil.关键词
QuEChERS/高效液相色谱串联质谱/气相色谱串联质谱/农药残留/土壤Key words
QuEChERS/high performance liquid chromatography tandem mass spectrometry/gas chromatography tandem mass spectrometry/pesticide residues/soil分类
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蔡霖,席普宇,谢晴,李雪花,乔显亮,谢宏彬,陈景文,蔡喜运..QuEChERS方法联合HPLC-MS/MS和GC-MS测定土壤中110种农药残留[J].农业环境科学学报,2017,36(8):1680-1688,9.基金项目
公益性行业(农业)科研专项(201503107) （农业）
国家自然科学基金项目(21477013) Project supported:The Special Scientific Fund for Agro-scientific Research in the Public Interest(201503107) （21477013）
National Natural Science Foundation of China(21477013) （21477013）
