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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

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

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【作者】 徐芷怡陈梦婷侯锡爱刘丹

【Author】 XU Zhi-Yi;CHEN Meng-Ting;HOU Xi-Ai;LIU Dan;College of Science, China Agricultural University;

【通讯作者】 刘丹;

【机构】 中国农业大学理学院

【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R~2>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。

【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.

  • 【文献出处】 分析化学 ,Chinese Journal of Analytical Chemistry , 编辑部邮箱 ,2020年07期
  • 【分类号】O657.63;TS225.11
  • 【被引频次】15
  • 【下载频次】654
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