作者：赵生寿

作者单位：海东市循化县生态环境局，青海 海东 811100

关键词：ASE;GC-MS/MS;土壤;杀虫剂;氟环唑

摘要：

该文建立快速溶剂萃取（ASE）联合气相色谱三重四级杆质谱（GC-MS/MS）检测土壤中的氟环唑、乙螨唑、硅氟唑、烯丙苯噻唑和氟醚唑杀虫剂残留的分析方法。土壤样品经粉碎研细后，过100目筛网，取过筛后的土壤样品约15 g，上快速溶剂萃取仪（ASE）进行提取，提取液经氮吹至近干，加1 mL甲醇溶解残渣，0.45 µm滤膜过滤后进样气相色谱串联质谱仪（GC-MS/MS）分析。结果表明氟环唑、乙螨唑、硅氟唑、烯丙苯噻唑和氟醚唑在浓度0.01~5.0 μg/mL范围内线性关系良好；检出限在0.012~0.024 mg/kg之间；加标回收率在89.2%~104.9%之间；重复性RSD（n=6）在5.0%以内。实验证明，该方法具有简便、快速、重复性好、检测结果准确等优点，可以用于土壤中极微量三唑类杀虫剂残留的监测，为指导当地农药使用和环境保护提供技术参考。

Gas chromatography-tandem mass spectrometry method for determination of triazole pesticide residues in soil
ZHAO Shengshou
Ecological Environment Bureau of Xunhua County in Haidong, Haidong 811100, China
Abstract: To establish an accelerated solvent extraction(ASE) united gas chromatography - triple four-step mass spectrometry(GC-MS/MS) method for determination of epoxiconazole, etoxazole, silicon fluoride azole, probenazole and tetraconazole pesticide residues in soil. Soil samples were grinded and sieved by 100 mesh first, about 15 g sifted samples was weighed and extracted on accelerate solvent extractor. The extracted solution was flowed to near dry by nitrogen, the residues was dissolved by 1 mL methanol. Samples were filtered by 0.45 µm filter membrane analyzed on GC-MS/MS. Epoxiconazole, etoxazole, silicon fluoride azole, probenazole and tetraconazole showed good linear relationships in the concentration range 0.01-5.0 µg/mL. The detection limits were in the range 0.012-0.024 mg/kg and average recoveries were varied from 89.2% to 104.9%. Relative standard deviation(RSD) of repeatability was below 5%(n=6). The method was simple, rapid, accurate with good repeatability, and can be used to monitor small amounts of triazole pesticides in soil. It also provides technical reference for guiding local pesticide use and environmental protection.
Keywords: ASE;GC-MS/MS;soil;pesticide;epoxiconazole
2020, 46(8):69-73  收稿日期: 2020-01-15;收到修改稿日期: 2020-02-18
基金项目:
作者简介: 赵生寿（1989-），男，青海西宁市人，工程师，硕士，主要从事工作环境监测
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