超高效液相色谱—串联质谱法测定动物源性食品中百菌清及其代谢物4-羟基百菌清残留量
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(1. 湖南省产商品质量检验研究院 ,湖南 长沙 410007 ; 2. 食品安全监测与预警湖南省重点实验室 ,湖南 长沙 410007)

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刘小芳(1991—),女,湖南省产商品质量检验研究院工程师,硕士。E-mail:740954546@qq.com

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湖南省自然科学基金资助项目(编号:2023JJ60530)


Determination of chlorothalonil and its metabolite 4-hydroxychlorothalonil residues in animal-derived food by ultra-high performance liquid chromatography-tandem mass spectrometry
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(1. Hunan Provincial Institute of Product and Goods Quality Inspection , Changsha , Hunan 410007 , China ; 2. Hunan Provincial Key Laboratory of Food Safety Monitoring and Early Warning , Changsha , Hunan 410007 , China)

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    摘要:

    [目的]建立超高效液相色谱—串联质谱法同时测定动物源性食品中百菌清及其代谢物 4-羟基百菌清残留的检测方法。[方法]样品经 1%乙酸—乙腈溶液振荡提取,正己烷脱脂,基质分散固相萃取剂 (PSA、无水硫酸镁 )净化,通过Waters BEH C 18色谱柱分离,以乙腈— 0.1%甲酸水溶液为流动相进行梯度洗脱,采用大气压化学电离源 (APCI )负离子多反应监测模式 (MRM )进行测定,基质匹配外标法定量。[结果]百菌清及 4-羟基百菌清在 5~500 μg/L范围内线性关系良好,定量限均为 0.005 mg/kg,平均回收率分别为 69.3%~111.0%和65.3%~117.9%,相对标准偏差分别为 1.6%~10.8%和1.1%~9.0%。[结论]该方法前处理简单快速,灵敏度高,准确可靠,可用于动物源性食品中百菌清及其代谢物 4-羟基百菌清的同时测定。

    Abstract:

    [[Objective ]] To establish a method for simultaneous determination of chlorothalonil and its metabolite 4-hydroxychlorothalonil residues in animal -derived food by ultra -high performance liquid chromatography -tandem mass spectrometry.[[Methods ]] The samples were extracted by oscillating with acetonitrile solution of 1% acetic acid,defatted with n -hexane,purified by matrix dispersible solid phase extractant (PSA,anhydrous magnesium sulfate ),separated by Waters BEH C18 column under a gradient elution program using 0.1% formic acid aqueous solution and acetonitrile as the mobile phases.The anion multiple reaction monitoring model (MRM ) of atmospheric pressure chemical ionization source (APCI ) was used for the determination,and the matrix matching external standard method was used for quantitative determination.[[Results ]] The linear relationships of chlorothalonil and 4-hydroxychlorothalonil were good in the range of 5~500 μg/L,and the limits of quantitation were 0.005 mg/kg.The average recoveries of chlorothalonil and 4-hydroxychlorothalonil were 69.3%~111.0% and 65.3%~117.9%,respectively.The relative standard deviations of chlorothalonil and 4-hydroxychlorothalonil were 1.6%~10.8% and 1.1%~9.0%,respectively.[[Conclusion ]] The method is simple,rapid,sensitive,accurate and reliable for simultaneous determination of chlorothalonil and its metabolite 4-hydroxychlorothalonil in animal -derived food.

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刘小芳,李 政,何 浩,等.超高效液相色谱—串联质谱法测定动物源性食品中百菌清及其代谢物4-羟基百菌清残留量[J].食品与机械,2024,40(9):66-72.
LIU Xiaofang, LI Zheng, HE Hao, et al. Determination of chlorothalonil and its metabolite 4-hydroxychlorothalonil residues in animal-derived food by ultra-high performance liquid chromatography-tandem mass spectrometry[J]. Food & Machinery,2024,40(9):66-72.

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  • 收稿日期:2024-06-11
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  • 在线发布日期: 2025-02-18
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