分散固相萃取技术结合超高效液相色谱-高分辨质谱法测定蜂蜜中三嗪类农药残留

何丽君; 陈豪; 翁淑琴; 郑婉玉; 严国鸿; 胡敏; 李德森

doi:10.13422/j.cnki.syfjx.2016220071

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分散固相萃取技术结合超高效液相色谱-高分辨质谱法测定蜂蜜中三嗪类农药残留

化学与分析 | 更新时间：2024-01-04

- 分散固相萃取技术结合超高效液相色谱-高分辨质谱法测定蜂蜜中三嗪类农药残留
- Simultaneous Determination of Triazine Pesticides in Honey by Using UHPLC-HRMS Combined with DSPE
- 中国实验方剂学杂志 2016年22卷第22期页码：71-76
- 作者机构：
- 作者简介：
- 基金信息：
  
  福建省科技厅社发处重点项目（2014Y0060）;全国中药特色技术传承人才培训项目（J20164811007）
- DOI：10.13422/j.cnki.syfjx.2016220071
  中图分类号： TS207.53;O657.63
- 纸质出版日期：2016
- 稿件说明：
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何丽君, 陈豪, 翁淑琴, 等. 分散固相萃取技术结合超高效液相色谱-高分辨质谱法测定蜂蜜中三嗪类农药残留[J]. 中国实验方剂学杂志, 2016,22(22):71-76.

HE Li-jun, CHEN Hao, WENG Shu-qin, et al. Simultaneous Determination of Triazine Pesticides in Honey by Using UHPLC-HRMS Combined with DSPE[J]. Chinese journal of experimental traditional medical formulae, 2016, 22(22): 71-76.
何丽君, 陈豪, 翁淑琴, 等. 分散固相萃取技术结合超高效液相色谱-高分辨质谱法测定蜂蜜中三嗪类农药残留[J]. 中国实验方剂学杂志, 2016,22(22):71-76. DOI： 10.13422/j.cnki.syfjx.2016220071.

HE Li-jun, CHEN Hao, WENG Shu-qin, et al. Simultaneous Determination of Triazine Pesticides in Honey by Using UHPLC-HRMS Combined with DSPE[J]. Chinese journal of experimental traditional medical formulae, 2016, 22(22): 71-76. DOI： 10.13422/j.cnki.syfjx.2016220071.

摘要

目的：采用分散固相萃取技术（DSPE），建立蜂蜜中21种三嗪类农药残留的同时测定分析方法。方法：用15%氯化钠水溶液溶解蜂蜜后，以1%甲酸乙腈进行盐析提取，提取液经DSPE净化后，采用超高效液相色谱-高分辨质谱（UHPLC-HRMS）进行外标法定量检测。结果： 21种三嗪类农药在各自浓度范围内具有较好的线性相关系数（r>0.999）。目标化合物在低、中、高3个浓度下的平均回收率为73.9%~110.4%（RSD 1.5%~9.6%），定量限（LOQ）为1~10 μg·kg-1。结论：该方法灵敏度高、准确性好，适合蜂蜜样品中21种三嗪类农药的快速准确定量分析。

Abstract

Objective: To develop a method for the simultaneous determination of 21 triazine pesticides in honey by using dispersive solid phase extraction (DSPE). Method: Honey samples were dissolved in 15% NaCl solution and extracted with 1% formic acid in acetonitrile by salting out method. The extracts were purified by DSPE procedure

and the quantitative analysis was operated by ultra high performance liquid chromatography-high resolution mass spectrometry (UHPLC-HRMS). Result: 21 traizine pesticides showed good linearity within their respective concentration range (r>0.999). The average recovery rates were 73.9%-110.4% (RSD 1.5%-9.6%) under low

middle and high concentrations

and the LOQs were from 1 to 10 μg·kg-1. Conclusion: The proposed method was sensitive and accurate

which was suitable for the rapid simultaneous determination of 21 triazine pesticide residues in honey.

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