作者：杨敬坡^1,2, 王文军³, 陈晓轩^1,2, 郭延凯^1,2, 吴黎军⁴, 都泽铭^1,2

作者单位：1. 河北科技大学环境科学与工程学院, 河北 石家庄 050018;
2. 河北省污染防治生物技术实验室, 河北 石家庄 050018;
3. 保定学院汽车与电子工程学院, 河北 保定 071051;
4. 邯郸学院学工部, 河北 邯郸 056005

关键词：快速溶剂萃取;GC-MS/MS;土壤;甲霜灵;农药

摘要：

建立一种利用快速溶剂萃取（ASE）-气相色谱-三重四级杆质谱仪检测经济作物土壤中甲霜灵、嘧霉胺、戊唑醇等6种农药的分析方法。样品经研钵研细，利用ASE进行提取，提取液经氮吹浓缩后，上GC-MS/MS进行检测，外标法定量。6种农药质量浓度在0.05~5 μg/mL范围内线性关系良好，相关系数均大于0.995；检出限在0.005~0.023 μg/mL；加标回收率在81.2%~108.7%之间；重复性（n=6）相对标准偏差在3.26%~4.40%之间。实验表明该方法具有操作简单、检测速度快、检出限低等优点，适用于经济作物土壤中多种农药残留的分析检测。

Accelerated solvent extraction -GC-MS/MS method for the determination of 6 commonly used pesticide residues in the soil of economic crops, including metalaxyl, pyrimethanil and tebuconazole
YANG Jingpo^1,2, WANG Wenjun³, CHEN Xiaoxuan^1,2, GUO Yankai^1,2, WU Lijun⁴, DU Zeming^1,2
1. School of Environmental Science & Engineering, Hebei University of Science and Technology, Shijiazhuang 050018, China;
2. Pollution Prevention Biotechnology Laboratory of Hebei Province, Shijiazhuang 050018, China;
3. College of Automobile and Electronic Engineering, Baoding College, Baoding 071051, China;
4. Department of Student Affairs, Handan University, Handan 056005, China
Abstract: A ASE(accelerated solvent extraction)-GC/MS/MS method for determination of 6 common pesticides residuals such as pyrimethani, metalaxyl, thiamethoxam, et al in economic crop soil was established. Soil samples were grinded in mortar, then extracted by ASE, The exracted solution were dryed under nitrogen, then samples were analyzed by GC-MS/MS. External standard was used as quantitative method. The concentration of 6 pesticides showed good linear relationships in the range 0.05-5 μg/mL, the correlation coefficients were all above 0.995. The detection limits were bewteen 0.005 and 0.023 mg/kg, and the recoveries were ranged from 81.2% to 108.7%. The relative standard deviation(RSD)of Repeatability (n=6) were 3.26%-4.40%. This method was proved to be simple and quick treated, and with low detection, which can be used to determine pesticide residues in economic crop soil.
Keywords: ASE;GC-MS/MS;soil;metalaxyl;pesticide
2019, 45(2):72-77  收稿日期: 2018-10-12;收到修改稿日期: 2018-11-17
基金项目: 国家自然科学基金（41807157）；河北省科技支撑计划项目（15273610D）；河北科技大学16PT基金（2016PT43）；河北省社会科学发展研究课题民生调研专项（201701410）；河北省海洋局项目（HYJJDC201606）
作者简介: 杨敬坡(1978-),男,河北保定市人,高级实验师,硕士,研究方向为土壤修复
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