摘要
采用Qu ECh ERS前处理方法联合高效液相色谱串联二级质谱(HPLC-MS/MS)和气相色谱串联质谱(GC-MS),建立了测定土壤中110种农药残留的方法。通过调整加入水中的乙酸含量对Qu ECh ERS方法进行优化,结果表明加入1%的乙酸提高了农药的回收率。基于农药的极性、热稳定性、挥发性等特性差异,分别采用HPLC-MS/MS测定其中的43种农药和GC-MS测定另外的67种农药。采用内标法测定回收率,内标为阿特拉津-d5、磺酰磺隆、1,3-二甲基-2-硝基苯、磷酸三苯酯、苝-d12。在3个添加水平(10、20、50μg·kg^(-1))下,由HPLC-MS/MS测定的43种农药的平均回收率范围为59.1%~129.4%,相对标准偏差(RSD)在0.3%~15%之间;由GC-MS测定的67种农药的平均回收率范围为44.9%~168.1%,RSD在0.5%~20%之间。方法的检出限范围为0.01~5.00μg·kg^(-1)。采用该方法检测某土壤样品,共检出农药68种,其中主要包括烟嘧磺隆、炔苯酰草胺、乙氧氟草醚、灭菌丹、烯酰吗啉、高效氯氟氰菊酯和部分有机磷、有机氯农药等,结果表明该方法简单有效、检测灵敏度高,可用于土壤中农药多残留的检测。
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 characteristics 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 50 μg·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 from0.01 to 5.00 μg·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.
出处
《农业环境科学学报》
CAS
CSCD
北大核心
2017年第8期1680-1688,共9页
Journal of Agro-Environment Science
基金
公益性行业(农业)科研专项(201503107)
国家自然科学基金项目(21477013)~~
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
QuEChERS
high performance liquid chromatography tandem mass spectrometry
gas chromatography tandem mass spectrometry
pesticide residues
soil
