腐殖酸键合硅胶固相萃取-气相色谱法快速测定玉米油中拟除虫菊酯类农药残留

郑丹; 夏珍珍; 彭西甜; 夏虹; 谢光辉

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腐殖酸键合硅胶固相萃取-气相色谱法快速测定玉米油中拟除虫菊酯类农药残留
郑丹^1,2,夏珍珍^1,2,彭西甜^1,2*,夏虹^1,2,谢光辉³
1.湖北省农业科学院农业质量标准与检测技术研究所, 武汉 430064;2.农业农村部农产品质量安全风险评估实验室(武汉), 武汉 430064;3.中国农业大学农学院, 北京 100193

摘要:

为建立适用于玉米油中常见拟除虫菊酯类农药的快速分析方法，以腐殖酸键合硅胶作为固相萃取介质，建立固相萃取富集净化、气相色谱电子捕获检测器检测玉米油中氯氟氰菊酯、氟胺氰菊酯、氟氯氰菊酯、氰戊菊酯、溴氰菊酯、氟氰戊菊酯和氯氰菊酯7种拟除虫菊酯类农药的分析方法。结果表明，在优化好的条件下，上述7种农药在0.01~0.60 mg/L质量浓度范围内呈线性关系，R2>0.991 2。7种拟除虫菊酯类农药的方法检出限在0.001~0.005 mg/kg，均低于植物油中的最大残留限量。该方法较好地去除基质干扰，具有简单、快速和灵敏的特点，适用于玉米油中常见菊酯类农药的快速分析。

关键词: 腐殖酸固相萃取气相色谱玉米油拟除虫菊酯类农药

DOI：10.11841/j.issn.1007-4333.2021.02.05

分类号:

基金项目:国家自然科学基金(21607039)；湖北省重点研发计划(2020BBB078)；湖北省农业科学院青年拔尖人才培养计划(Q2018037)；湖北省农业科学院青年基金(2019 NKYJJ11)

Determination of pyrethroid pesticides in corn oil by humic acid-bonded silica solid-phase extraction coupled with gas chromatography

ZHENG Dan^1,2,XIA Zhenzhen^1,2,PENG Xitian^1,2*,XIA Hong^1,2,XIE Guanghui³

1.Institute of Agricultural Quality Standards and Testing Technology Research, Hubei Academy of Agricultural Sciences, Wuhan 430064, China;2.Laboratory of Quality & Safety Risk Assessment for Agr-products(Wuhan), Ministry of Agriculture and Rural Affairs, Wuhan 430064, China;3.College of Agronomy and Biotechnology, China Agricultural University, Beijing 100193, China

Abstract:

To establish a rapid detection system for the determination of pyrethroid pesticides in corn oil, taking humic acid-bonded silica as sorbent in solid-phase extraction, a method for the determination of 7 kinds of pyrethroid pesticides(cyhalothrin, cyfluthrin, flucythrinate, fenvalerate, tau-fluvalinate, cypermethrin and deltamethrin)was developed by combining dispersive solid phase extraction method and gas chromatography with electron capture detector(ECD). The result showed that: Under optimal extraction and purification conditions, good linearities of 7 pyrethroid pesticides were achieved within the range of 0. 01-0. 60 mg/L with correlation coefficients larger than 0. 991 2. The MDLs of the 7 pyrethroid pesticides were in the range of 0. 001 mg/kg to 0. 005 mg/kg, which were lower than the maximum residue limits in China. In conclusion, the method proposed in this study is simple, quick and sensitive, and is suitable for the regular analysis of pyrethroid residues in corn-oil samples.

Key words: humic acid solid-phase extraction(SPE) gas chromatography(GC) corn oil pyrethroid pesticides

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