| 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. |
| 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 |
| 投稿时间：2016-12-26 |
| DOI：10.11654/jaes.2016-1657 |
| 中文关键词: 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 |
| 英文关键词: QuEChERS high performance liquid chromatography tandem mass spectrometry gas chromatography tandem mass spectrometry pesticide residues soil |
| 基金项目:公益性行业（农业）科研专项（201503107）；国家自然科学基金项目（21477013） |
| 作者 | 单位 | E-mail | | 蔡霖 | 大连理工大学环境学院, 工业生态与环境工程教育部重点实验室, 辽宁 大连 116024 | | | 席普宇 | 大连理工大学环境学院, 工业生态与环境工程教育部重点实验室, 辽宁 大连 116024 | | | 谢晴 | 大连理工大学环境学院, 工业生态与环境工程教育部重点实验室, 辽宁 大连 116024 | | | 李雪花 | 大连理工大学环境学院, 工业生态与环境工程教育部重点实验室, 辽宁 大连 116024 | | | 乔显亮 | 大连理工大学环境学院, 工业生态与环境工程教育部重点实验室, 辽宁 大连 116024 | | | 谢宏彬 | 大连理工大学环境学院, 工业生态与环境工程教育部重点实验室, 辽宁 大连 116024 | | | 陈景文 | 大连理工大学环境学院, 工业生态与环境工程教育部重点实验室, 辽宁 大连 116024 | | | 蔡喜运 | 大连理工大学环境学院, 工业生态与环境工程教育部重点实验室, 辽宁 大连 116024 | xiyuncai@dlut.edu.cn |
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| 中文摘要: |
| 采用QuEChERS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QuEChERS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、50 μg·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0.01~5.00 μg·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。 |
| 英文摘要: |
| 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 from 0.01 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. |
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