大学化学 >> 2024, Vol. 39 >> Issue (11): 296-303.doi: 10.12461/PKU.DXHX202402017

化学实验 上一篇    下一篇

分散固相萃取-液相色谱-三重四级杆质谱法分析水样中卤代醌类化合物

钟燕辉, 王冉, 林子俺   

  1. 福州大学化学学院, 福州 350108
  • 收稿日期:2024-02-03 录用日期:2024-04-15 发布日期:2024-11-09
  • 通讯作者: 林子俺 E-mail:zianlin@fzu.edu.cn
  • 基金资助:
    国家自然科学基金(22274021,22036001)；福建省自然科学基金(2022J01535)；福建省本科高校教育教学研究项目(FBJG20220268)；福州大学本科教育教学研究项目

Analysis of Halogenated Quinone Compounds in Environmental Water by Dispersive Solid-Phase Extraction with Liquid Chromatography-Triple Quadrupole Mass Spectrometry

Yanhui Zhong, Ran Wang, Zian Lin   

  1. College of Chemistry, Fuzhou University, Fuzhou 350108, China
  • Received:2024-02-03 Accepted:2024-04-15 Published:2024-11-09
  • Contact: Zian Lin E-mail:zianlin@fzu.edu.cn

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摘要： 本实验旨在通过分散固相萃取-液相色谱-三重四级杆质谱法分析环境水样中的卤代醌类化合物。实验选取了5种卤代醌类化合物作为目标物，采用阳离子共价有机骨架材料作为固相吸附剂，从水样中富集目标物。随后，使用液相色谱-三重四级杆质谱法对富集的化合物进行定性和定量分析。实验考察了吸附剂用量、富集时间、洗脱时间、洗脱溶剂种类、洗脱溶剂酸度和洗脱体积等条件对实验结果的影响，并建立了一种基于分散固相萃取的新方法。该方法在0.1-100 ng·L-1范围内显示出较好的线性关系(相关系数R2 ≥ 0.9924)，检出限可达到0.03-0.65 ng·L-1，并成功应用于分析自来水样品中卤代苯醌类化合物。通过这个实验，学生可以了解基本的样品前处理技术，并提高实验技能、研究和创新思维，增强解决问题的能力。

关键词: 分散固相萃取, 液相色谱-三重四级杆质谱, 卤代醌类化合物, 水

Abstract: This experiment aims to analyze halogenated quinone compounds in environmental water samples using dispersive solid-phase extraction (dSPE) combined with liquid chromatography-triple quadrupole mass spectrometry (LC-MS/MS). Five types of halogenated quinone compounds were used as analytes, and a cationic covalent organic framework material was employed as the solid-phase adsorbent to concentrate the target compounds from the water samples. Subsequently, the enriched compounds were subjected to qualitative and quantitative analysis by using LC-MS/MS. The experiment systematically examined the impact of various parameters on the experimental results, including the amount of the adsorbent, enrichment time, elution time, types of elution solvent, acidity of the elution solvent, and elution volume. A novel approach based on dSPE was developed. The method exhibited favorable linearity (with a correlation coefficient of R2 ≥ 0.9924) in the range of 0.1-100 ng·L-1, with detection limits ranging from 0.03-0.65 ng·L-1. The method was successfully applied to the analysis of halogenated quinone compounds in tap water samples. This experiment helps students understand fundamental sample preparation techniques and enhances their practical skills, research capabilities, and problem-solving abilities.

Key words: Dispersive solid-phase extraction, Liquid chromatography coupled-triple quadrupole mass spectrometry, Halogenated quinone compounds, Water