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多通道过滤净化-液相色谱串联质谱法同时测定茶叶中 14 种农药残留量

Simultaneous determination of 14 pesticide residues in tea by multi-plug filtration cleanup combined with LC-MS/MS.

机构信息

Beijing Centre for Tea Qualify Supervision and Inspection, Beijing Academy of Food Sciences, Beijing, China.

China National Institute of Standardization, Beijing, China.

出版信息

J Environ Sci Health B. 2021;56(8):771-781. doi: 10.1080/03601234.2021.1944962. Epub 2021 Jun 30.

Abstract

A combined method of multi-plug filtration cleanup (m-PFC) and liquid chromatography-triple quadrupole mass spectrometry (LC-MS/MS) was established to simultaneously detect 14 pesticides in tea. The pesticides in water-soaked tea were extracted with acetonitrile. Cleanup of tea extract was performed using an m-PFC column packed with multiple cleanup materials: multi-walled carbon nano-tubes (MWCNTs), primary secondary amine (PSA) and anhydrous magnesium sulfate (MgSO). The cleanup effect of the column was evaluated based on the rates of removal of tea components that interfered with pesticide recovery, henceforth referred to as interference components. Results showed that 14 pesticides had strong linearity in the range of 5-500 μg L ( > 0.99). The quantitative limits were within the range of 3-50 μg kg. The average recoveries of 14 pesticides spiked into three different blank tea samples (green tea, black tea, oolong tea) at three levels of 0.05, 0.50 and 2.00 mg kg were in the range of 62.3-108.8% with relative standard deviations of 0.2-13.6%. The m-PFC method can greatly improve the efficiency of sample pretreatment. Furthermore, this work provides methodological guidance on how to select cleanup materials and allocate their proportions.

摘要

建立了一种多管过滤净化(m-PFC)和液相色谱-三重四极杆质谱(LC-MS/MS)联用的方法,用于同时检测茶叶中的 14 种农药。采用乙腈提取水浸茶中的农药。采用 m-PFC 柱对茶提取物进行净化,该柱填充有多种净化材料:多壁碳纳米管(MWCNTs)、初级二次胺(PSA)和无水硫酸镁(MgSO)。根据去除干扰农药回收的茶成分(以下简称干扰成分)的速率来评估柱的净化效果。结果表明,14 种农药在 5-500μg L 范围内具有很强的线性关系(>0.99)。定量限在 3-50μg kg 范围内。14 种农药在 0.05、0.50 和 2.00 mg kg 三个水平添加到三种不同空白茶样品(绿茶、红茶、乌龙茶)中的平均回收率在 62.3-108.8%范围内,相对标准偏差在 0.2-13.6%范围内。m-PFC 方法可以大大提高样品预处理的效率。此外,本工作为如何选择净化材料及其比例分配提供了方法学指导。

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