大学化学 >> 2022, Vol. 37 >> Issue (5): 2111066.doi: 10.3866/PKU.DXHX202111066

所属专题: 第2届全国大学生化学实验创新设计竞赛

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固相微萃取联用气相色谱-质谱法快速分析水中痕量苯系物

陈国胜, 王少涵, 陈月媚, 谢浩志, 肖华, 陈滔, 于禄丹, 李厚金, 朱芳(), 欧阳钢锋()   

  • 收稿日期:2021-11-24 录用日期:2021-12-07 发布日期:2022-04-06
  • 通讯作者: 朱芳,欧阳钢锋 E-mail:ceszhuf@mail.sysu.edu.cn;cesoygf@mail.sysu.edu.cn
  • 作者简介:欧阳钢锋, Email: cesoygf@mail.sysu.edu.cn
    朱芳, Email: ceszhuf@mail.sysu.edu.cn
  • 基金资助:
    广东省本科质量工程项目(2020);中山大学本科质量工程项目(2020);中山大学本科质量工程项目(2021);国家自然科学基金项目(22076222);国家自然科学基金项目(21737006);国家自然科学基金项目(22036003);广州市科技计划项目(201803030018)

Rapid Analysis of Trace BTEX in Water by Solid Phase Microextraction Coupled with Gas Chromatography-Mass Spectrometry

Guosheng Chen, Shaohan Wang, Yuemei Chen, Haozhi Xie, Hua Xiao, Tao Chen, Ludan Yu, Houjin Li, Fang Zhu(), Gangfeng Ouyang()   

  • Received:2021-11-24 Accepted:2021-12-07 Published:2022-04-06
  • Contact: Fang Zhu,Gangfeng Ouyang E-mail:ceszhuf@mail.sysu.edu.cn;cesoygf@mail.sysu.edu.cn

摘要:

样品前处理是分析检测的关键步骤,传统的样品前处理技术耗时、费力,且易对环境造成二次污染。固相微萃取(Solid phase microextraction, SPME)技术集采样、萃取、浓缩、进样于一体,萃取过程无需有机溶剂,是一种简单、快速、绿色环保的样品前处理技术。本项目采用SPME技术对水中苯系物进行萃取,优化SPME条件,并联用气相色谱-质谱(Gas chromatography-mass spectrometry,GC-MS)分析检测,建立水中苯系物的定量分析方法。实验结果表明,该方法对苯系物包括苯、甲苯、乙苯、二甲苯的检测具备良好的线性范围(均为100–10000 ng·L-1),且相关系数R2均大于0.9900。此外,该方法的检测限分别低至37.50、16.67、45.45、10.64 ng·L-1。将建立的方法用于实际水样中苯系物的检测,加标回收率在86.83%–114.8%之间,方法简便、高效,结果令人满意。本实验将先进的SPME技术引入本科教学实验,一方面融入思政元素,帮助学生牢固树立绿色环保理念,另一方面让学生掌握先进的样品前处理技术,感受前沿技术在化学领域带来的革命性创新。

关键词: 固相微萃取, 气相色谱-质谱, 苯系物,

Abstract:

Sample preparation is a critical step for target detection. However, the traditional sample preparation techniques usually experience limitations, including time-consuming and tedious workflows and environmentally harmful processes that give rise to secondary pollution. Solid-phase microextraction (SPME) technology integrates sampling, extraction, concentration, and sample injection into one step. It does not require organic solvents during the extraction process and is considered as a simple, fast, and environment-friendly sample pretreatment technique. In this study, SPME technology was used to extract BTEX from water samples. The SPME conditions were carefully optimized, and a BTEX quantitative detection method was established through coupling the SPME with gas chromatography-mass spectrometry (GC-MS). The results showed that this new SPME method possessed excellent linear ranges of 100–10000 ng·L-1 for benzene, toluene, ethylbenzene, and xylene, detection limits of 37.50, 16.67, 45.45 and 10.64 ng·L-1, respectively and linear correlation coefficients (R2) all higher than 0.99. Finally, the established SPME method was applied to real water samples for BTEX detection, obtaining recoveries of 86.83%–114.8%. The entire SPME workflow is simple and highly efficient, and the detection results are reliable. This work introduces the advanced SPME technology into undergraduate teaching experiments, thus incorporating ideological and political elements to lay the groundwork for green environmental protection for students. Furthermore, this experiment helps students learn advanced sample pretreatment technology and experience how the cutting-edge technology triggers revolutionary innovations within the field of analytical chemistry.

Key words: Solid phase microextraction, Gas chromatography-mass spectrometry, BTEX, Water

MSC2000: 

  • G64