| 王艳艳，杨帆，王凤丽，冯秋芳，王东旭，曾坤，谷贵章.EMR-Lipid/MWCNTs-OH改进的QuEChERS法
结合UHPLC-MS/MS测定食用植物油中
54种农药及代谢物残留[J].中国油脂,2026,51(8):.[WANG Yanyan, YANG Fan, WANG Fengli, FENG Qiufang,
WANG Dongxu, ZENG Kun, GU Guizhang.Determination of 54 pesticides and metabolites in edible vegetable oils by UHPLC-MS/MS with EMR-Lipid/MWCNTs-OH modified QuEChERS[J].China Oils and Fats,2026,51(8):.] |
| EMR-Lipid/MWCNTs-OH改进的QuEChERS法
结合UHPLC-MS/MS测定食用植物油中
54种农药及代谢物残留 |
| Determination of 54 pesticides and metabolites in edible vegetable oils by UHPLC-MS/MS with EMR-Lipid/MWCNTs-OH modified QuEChERS |
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投稿时间：2025-12-19 修订日期：2026-03-23 录用日期：2026-01-12
出版日期：
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| DOI：10.19902/j.cnki.zgyz.1003-7969.250528 |
| 中文关键词: 增强型脂质去除吸附剂 羟基化多壁碳纳米管 QuEChERS 超高效液相色谱-串联质谱 食用植物油 农药及代谢物 |
| 英文关键词:EMR-Lipid MWCNTs-OH QuEChERS UHPLC-MS/MS edible vegetable oil pesticides and metabolites |
| 基金项目:浙江省市场监督管理局科研计划项目（ZC2023078） |
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| 中文摘要: |
| 为有效消除基质干扰，实现食用植物油中多种农药残留的同时测定，以增强型脂质去除吸附剂（EMR-Lipid）与羟基化多壁碳纳米管（MWCNTs-OH）改进的QuEChERS为前处理方法，结合超高效液相色谱-串联质谱（UHPLC-MS/MS），建立同时测定食用植物油中54种农药及代谢物残留的分析方法。样品用1%氨水-乙腈溶液提取，提取液依次经EMR-Lipid和MWCNTs-OH净化，采用ZORBAX Eclipse Plus C18色谱柱分离，以1.0 mmol/L甲酸铵-水溶液（含0.01%甲酸）和1.0 mmol/L甲酸铵-甲醇溶液（含0.01%甲酸）进行梯度洗脱，气体辅助电喷雾离子源正离子模式扫描，多反应监测模式检测，外标法定量。结果表明：54种农药及代谢物在2～500 ng/mL质量浓度范围内线性关系良好，决定系数均大于0.998，方法检出限为0.002～0.005 mg/kg，定量限为0.005～0.018 mg/kg；在0.05、0.30、1.50 mg/kg 3个加标水平下，54种农药及代谢物平均回收率为70.4%～109.8%，相对标准偏差为0.4%～8.9%。该方法操作简单、分析快速、灵敏度和准确度高，适用于食用植物油中多种农药及代谢物残留的快速同时检测。 |
| 英文摘要: |
| To effectively eliminate matrix interference and enable the simultaneous determination of multiple pesticide residues in edible vegetable oils, an analytical method was established using a QuEChERS pretreatment modified with enhanced matrix removal lipid (EMR-Lipid) and hydroxylated multi-walled carbon nanotubes (MWCNTs-OH), combined with ultrahigh performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) for the simultaneous determination of residues of 54 pesticides and their metabolites in edible vegetable oils. Samples were extracted with 1% ammonia in acetonitrile. The extract was successively purified with EMR-Lipid and MWCNTs-OH. Separation was performed on a ZORBAX Eclipse Plus C18 column using gradient elution with 1.0 mmol/L ammonium formate in water (containing 0.01% formic acid) and 1.0 mmol/L ammonium formate in methanol (containing 0.01% formic acid). Detection was carried out using gas-assisted electrospray ionization in positive ion mode with multiple reaction monitoring (MRM), and quantification was performed by the external standard method. The results showed that the 54 pesticides and their metabolites exhibited good linearity in the mass concentration range of 2-500 ng/mL, with coefficients of determination greater than 0.998. The limits of detection ranged from 0.002 mg/kg to 0.005 mg/kg, and the limits of quantification ranged from 0005 mg/kg to 0.018 mg/kg. At three spiked levels of 0.05, 0.30 mg/kg and 1.50 mg/kg, the average recoveries of the 54 pesticides and their metabolites ranged from 70.4% to 109.8%, with relative standard deviations of 0.4%-8.9%. The method is simple to operate, rapid, and offers high sensitivity and accuracy, making it suitable for the rapid simultaneous determination of multiple pesticides and metabolite residues in edible vegetable oils. |
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