作者：陈阳

作者单位：河南省南阳生态环境监测中心，河南 南阳 473000

关键词：加速溶剂萃取;气相色谱质谱;土壤;农药

摘要：

建立一种全自动快速溶剂提取联合GC-MS/MS法同时测定农作物土壤中炭疽病5种常用农药（抑霉唑、咪鲜胺、醚菌酯、吡唑醚菌酯和己唑醇）微量残留的分析方法。随机采集农作物土壤样品，预处理后置快速溶剂萃取池中，按照设定的程序进行提取。提取液浓缩至近干，残渣用1 mL丙酮溶解，涡旋后，0.22 μm微孔滤膜过滤，进样气相色谱质谱系统（GC-MS/MS），多反应监测模式 (MRM)扫描，外标法定量。抑霉唑、咪鲜胺、醚菌酯、吡唑醚菌酯和己唑醇在0.05~5.0 μg/mL范围内呈良好的线性关系， 3个样品浓度加标回收率在89.6%~101.5%之间，重复性与精密度相对标准偏差均在5%以内(n=6)。实验结果证明，该方法自动化程度高、操作简便，定性定量结果准确，适用于土壤中农药残留的检测。

Simultaneous determination of five common anthrax pesticides in crop soil by automatic rapid solvent extraction combined with GC-MS/MS
CHEN Yang
Nanyang Ecological Environment Monitoring Center of Henan Province, Nanyang 473000, China
Abstract: To establish accelerated solvent extraction(ASE) method for detetermination of 5 anthrax pesticide residues (Imazali, prochloraz, kresoxim-methyl,pyraclostrobin and hexaconazole) in crop soil by gas chromatography- triple quadrupole mass spectrometry(GC-MS/MS). Random soil samples were collected, pre-treated and took to solvent extraction tank. Samples were extracted according to ASE procedure. The extracted solution was flowed to near dry, residues was volumned to 1 mL by acetone. Samples were filtered by 0.22 µm membrane filter and analyzed on GC-MS/MS by multi-response monitoring(MRM) mode, external standard was selected for quantitative analysis. The linear range of imazalil, prochloraz, kresoxim, pyraclostrobin and hexaconazole was 0.05-5.0 μg/mL. the recoveries of three samples were 89.6%-101.5%, and the relative standard deviations of repeatability and precision were within 5% (n = 6). The experimental results show that the method is highly automated, easy to operate, accurate in qualitative and quantitative determination, which is suitable for the detection of pesticide residues in soil.
Keywords: ASE;GC-MS/MS;soil;pesticides
2022, 48(4):73-76,109  收稿日期: 2020-12-03;收到修改稿日期: 2021-02-26
基金项目:
作者简介: 陈阳（1968-），女，河南南阳市人，高级工程师，从事环境监测分析工作
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