QuEChERS-高效液相色谱-串联质谱法同时测定芝麻油中7种农药残留

引用本文: 徐芷怡, 陈梦婷, 侯锡爱, 刘丹. QuEChERS-高效液相色谱-串联质谱法同时测定芝麻油中7种农药残留[J]. 分析化学, 2020, 48(7): 928-936. doi: 10.19756/j.issn.0253-3820.191644 shu

Citation: XU Zhi-Yi, CHEN Meng-Ting, HOU Xi-Ai, LIU Dan. Simultaneous Determination of Seven Pesticide Residues in Sesame Oil Using QuEChERS-High Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, 2020, 48(7): 928-936. doi: 10.19756/j.issn.0253-3820.191644 shu

QuEChERS-高效液相色谱-串联质谱法同时测定芝麻油中7种农药残留

中国农业大学理学院, 北京 100193

摘要: 采用分散固相萃取QuEChERS前处理方法，结合高效液相色谱-串联质谱（HPLC-MS/MS），建立了精甲霜灵、丁草胺、乙草胺、异丙甲草胺、氟环唑、嘧菌酯、高效氟吡甲禾灵7种常用于油料作物的农药在芝麻油中的多残留分析方法。针对芝麻油基质的复杂性，对目标农药在芝麻油基质中的提取溶剂、净化剂种类进行筛选及优化，最终确定用10 mL乙腈涡旋提取一次，组合60 mg N-丙基乙二胺（PSA）和20 mg石墨化碳黑（GCB）去除芝麻油中脂肪、色素等干扰物，并利用HPLC-MS/MS进行定量分析。芝麻油中7种目标农药在0.001~10 mg/L浓度范围内呈良好线性关系，线性相关系数R²>0.99；7种目标农药在芝麻油中3个添加水平的平均回收率在86.9%~106.3%之间，RSD<5.2%，准确度、精密度和灵敏度均满足农药残留检测的要求。本研究建立的快速、简便、环保的方法适用于芝麻油中目标残留农药定量分析。

关键词:

English

Simultaneous Determination of Seven Pesticide Residues in Sesame Oil Using QuEChERS-High Performance Liquid Chromatography-Tandem Mass Spectrometry

College of Science, China Agricultural University, Beijing 100193, China
Received Date: 01 November 2019
Revised Date: 10 May 2020

Abstract: A method for determination of multi-residues of seven target pesticides in sesame oil was established by dispersive solid-phase extraction of quick easy cheap effective rugged and safe method (QuEChERS) and HPLC-MS/MS. Seven kinds of pesticides often used in oil crops such as metalaxyl-M, butachlor, acetochlor, metolachlor, epoxiconazole, azoxystrobin and haloxyfop-P-methyl were determined. Due to the complexity of sesame oil matrix, the types of extraction solvent and cleaning agent in sesame oil matrix were selected and optimized. Finally, 10 mL of acetonitrile extraction, 60 mg of PSA and 20 mg of GCB were selected to effectively remove fat, pigment, organic acids and other interference impurities in sesame oil. In the concentration range of 0.001-10 mg/L, the standard solution concentration of seven target pesticides in sesame oil matrix showed a good linear relationship with the corresponding chromatographic response value, and the correlation coefficients were all greater than 0.99. The average recoveries of the three added concentrations in sesame oil were between 86.9% and 106.3%, and the RSDs were less than 5.2%. The accuracy, precision and sensitivity all met the requirements of pesticide residue analysis. This method was fast, simple and environmentally friendly and suitable for quantitative analysis of target pesticide residues in sesame oil.

Key words:

Sesame oil
/ Pesticide residue
/ QuEChERS
/ High performance liquid chromatography-tandem mass spectrometry
/ Oil purification

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沈阳化工大学材料科学与工程学院沈阳 110142

QuEChERS-高效液相色谱-串联质谱法同时测定芝麻油中7种农药残留

English

Simultaneous Determination of Seven Pesticide Residues in Sesame Oil Using QuEChERS-High Performance Liquid Chromatography-Tandem Mass Spectrometry

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

QuEChERS-高效液相色谱-串联质谱法同时测定芝麻油中7种农药残留

English

Simultaneous Determination of Seven Pesticide Residues in Sesame Oil Using QuEChERS-High Performance Liquid Chromatography-Tandem Mass Spectrometry

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

CCS Chemistry：颜徐州、鲍哲南： 你的皮肤可能是一片SPMs

CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

CCS Chemistry：颜徐州、鲍哲南：你的皮肤可能是一片SPMs