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QuEChERS法结合高效液相色谱-三重四级杆质谱同时测定植物源食品中9种新型农药残留
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刘逸丰(1999-),男,硕士研究生,研究方向:食品加工与安全,E-mail:liuyifengts@163.com 通讯作者:刘俊(1978-),男,正高级工程师,研究方向:食品安全,E-mail:47575290@qq.com

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国家重点研发计划项目(2022YFF1100804);四川省科技创新人才项目(2023JDRC0007)


Simultaneous Determination of Nine Pesticide Residues in Plant-derived Foods by QuEChERS Coupled with High-performance Liquid Chromatography-triple Quadrupole Mass Spectrometry
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    摘要:

    该研究是建立改良QuEChERS方法结合高效液相色谱-三重四级杆质谱(HPLC-MS/MS)同时检测植物源食品中伐虫脒盐酸盐、环溴虫酰胺、吡唑酰苯胺等九种新型农药残留,该九种农残在中国的植源性食品安全国家标准中,目前尚未设立相应的检测标准。然而,在出口到欧盟和日本的水果和蔬菜中,农残成为了重点检测对象。首先使用乙腈进行提取,接着利用硫酸镁(无水)和氯化钠进行水分去除,随后对上层液体进行150 mg N-丙基乙二胺(PSA)以及900 mg硫酸镁(无水)的净化处理,最终运用高效液相色谱-三重四级杆质谱技术进行检测。结果表明:九种农药物质在0.000 2~0.02 mg/L之间的线性关系良好,相关系数(r2)均超过0.998,检出限(S/N=3)为0.028~1.493 μg/kg,定量限(S/N=10)为0.093~4.975 μg/kg,在加标水平为5、10、20 μg/kg时,平均回收率为70.60%~108.75%,相对标准偏差(n=6)为1.35%~12.99%。结果全部都与欧盟、日本等国对果蔬中农药残留限量的标准相符合,可为我国植源性食品中该类农药的进口和出口检验提供可借鉴的方法。

    Abstract:

    An improved QuEChERS method was established and combined with high-performance liquid chromatography-triple quadrupole mass spectrometry (HPLC-MS/MS) for the simultaneous detection of nine new pesticide residues, including formetanate hydrochloride, cyclaniliprole, and pyflubumide, in plant-based foods. In the national standards of China for plant-based food safety, the detection standards for these nine pesticide residues are not yet established. However, when fruits and vegetables are exported to the European Union (EU) and Japan, pesticide residues are one of the main targets in food safety testing. Firstly, methyl cyanide is used for extraction, followed by water removal using magnesium sulfate (anhydrous) and sodium chloride. Subsequently, the supernatant is purified with 150 mg of N-propyl ethylenediamine and 900 mg of magnesium sulfate (anhydrous). Finally, HPLC-MS/MS is used for pesticide residue detection. The results suggest that all nine pesticide substances show good linear relationships at 0.000 2~0.02 mg/L, with correlation coefficients (r2) exceeding 0.998. The limit of detection (S/N=3) is 0.028~1.493 μg/kg, and the limit of quantification (S/N=10) is 0.093~4.975 μg/kg. At spiked levels of 5, 10, and 20 μg/kg, the average recovery rates are 70.60%~108.75%, and the relative standard deviations (n=6) are 1.35%~12.99%. The results all comply with the standards for pesticide residue limits in fruits and vegetables set by EU countries and Japan. This study offers a reference method for the import and export inspection of such pesticides in plant-based foods originating from China.

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刘逸丰,刘俊,张锐,孙千然,苟圆,李永丽,华燚. QuEChERS法结合高效液相色谱-三重四级杆质谱同时测定植物源食品中9种新型农药残留[J].现代食品科技,2025,41(7):351-358.

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  • 收稿日期:2024-04-26
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  • 在线发布日期: 2025-09-30
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