超高效液相色谱—串联质谱法同时测定茶饮料中15种有机磷酸酯和氨基甲酸酯农药残留
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1.北京市疾病预防控制中心,食物中毒诊断溯源技术北京市重点实验室,北京 100013;2.首都医科大学,燕京医学院,北京 101300;3.贵阳康养职业大学,医学技术系,贵州 贵阳 550081

作者简介:

姚凯 男 助理研究员 研究方向为食品中危害因子检测分析 E-mail:yaokaizz@163.com

通讯作者:

邵兵 男 研究员 研究方向为食品和环境危害物的前沿分析和健康效应研究 E-mail:shaobingch@sina.com

中图分类号:

R155

基金项目:

首都卫生发展科研专项项目(CFH 2022-1G-3013);高层次公共卫生技术人才培养计划(学科骨干-01-033)


Simultaneous determination of 15 kinds of organophosphate esters and carbamate pesticide residues in tea drinks by ultra-high-performance liquid chromatography tandem mass spectrometry
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1.Beijing Key Laboratory of Diagnostic and Traceability Technologies for Food Poisoning, Beijing Center for Disease Prevention and Control, Beijing 100013, China;2.Yanjing Medical College, Capital Medical University, Beijing 101300, China;3.Department of Medical Science and Technology, Guiyang Healthcare Vocational University, Guizhou Guiyang 550081, China

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    摘要:

    目的 建立茶饮料中的10种有机磷酸酯类农药和5种氨基甲酸酯类农药的超高效液相色谱-串联质谱分析方法。方法 提取液经150 mg MgSO4、25 mg乙二胺-N-丙基硅烷和2.5 mg石墨化碳黑净化后,4 ℃下14 000 r/min离心10 min后取上层清液,用等体积的超纯水进行稀释。选用Waters ACQUITY BEH C18(2.1 mm×100 mm,1.7 μm)色谱柱,以0.1%甲酸乙腈和0.1%甲酸水溶液作为流动相,梯度洗脱,多反应监测进行检测。结果 方法在5~160 μg/L范围内线性良好(R2>0.99),检出限和定量限分别为0.05~5 μg/L和0.15~15 μg/L。15种农药的平均回收率范围为71.2%~103.2%,日内相对标准偏差(n=6)为0.1%~13.8%,日间相对标准偏差(n=3)为0.4%~12.2%。基质效应为84.1%~114.3%,可被认为无基质效应。43份市售茶饮料中2份有乙酰甲胺磷检出,提示我们茶饮料中农药残留可能会造成人们健康风险上升。结论 该方法操作简单、快速、准确,适用于不同茶饮料中15种农药的测定。

    Abstract:

    Objective A QuEChERS ultra-high-performance liquid chromatography tandem mass spectrometry analytical method for the determination of 10 kinds of organophosphate esters pesticides and 5 kinds of carbamate pesticides in tea drinks was established.Methods The extraction solution was purified with 150 mg MgSO4, 25 mg Primary-secondary comine and 2.5 mg graphitized carbon black. After centrifugation at 14 000 r/min at 4℃ for 10 min and the supernatant was transferred, diluted with an equal volume of ultra-pure water. The pesticides were separated on a Waters ACQUITY BEH C18 (2.1 mm×100 mm, 1.7 μm) chromatographic column with gradient elution using 0.1% formate-acetonitrile and 0.1% formic acid aqueous solution. Pesticides were detected via multiple reaction monitoring mode.Results The method showed a good linear range of 5-160 μg/L (R2>0.99). The limits of detection and limits of quantification were 0.05-5 μg/L and 0.15-15 μg/L, respectively. Mean recoveries of 15 kinds of pesticides were 71.2%-103.2%. Intraday (n=6) and interday (n=3) relative standard deviations were 0.1%-13.8% and 0.4%-12.2%, respectively. Matrix effects were 84.1%-114.3%, and could be considered to have no matrix effect. Acephate was detected in 2 out of 43 commercial tea drinks, it suggests that pesticide residues in tea drinks may cause increased health risks for people.Conclusion The method was simple to operate, rapid, accurate, and suitable to detect fifteen kinds of pesticides in different tea drinks.

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姚凯,高子寒,张晶,戚燕,钟楠楠,邵兵.超高效液相色谱—串联质谱法同时测定茶饮料中15种有机磷酸酯和氨基甲酸酯农药残留[J].中国食品卫生杂志,2024,36(12):1349-1358.

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  • 收稿日期:2024-05-30
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  • 在线发布日期: 2025-03-19
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