高等学校化学学报 ›› 2009, Vol. 30 ›› Issue (8): 1533.

• 研究论文 • 上一篇    下一篇

电喷雾萃取电离质谱快速测定牙膏胶体中的二甘醇

丁健桦1,2, 杨水平1, 刘清3, 吴转璋1, 陈焕文1,2, 任玉林2, 郑健3, 刘清珺3   

  1. 1. 吉林大学化学学院, 长春 130012;
    2. 东华理工大学化学生物与材料科学学院, 抚州 344000;
    3. 北京市理化分析测试中心, 北京 100089
  • 收稿日期:2009-02-25 出版日期:2009-08-10 发布日期:2009-08-10
  • 通讯作者: 陈焕文, 男, 博士, 教授, 博士生导师, 主要从事分析化学和分析仪器研究. E-mail: chw8868@gmail.com
  • 基金资助:

    国家自然科学基金(批准号: 20505003)和北京市财政项目(批准号: XM-00001783050811002)资助.

Rapid Quantitative Detection of Toxic Diethylene Glycol in Toothpaste by Extractive Electrospray Ionization Ion Trap Mass Spectrometry

DING Jian-Hua1,2, YANG Shui-Ping1, LIU Qing3, WU Zhuan-Zhang1, CHEN Huan-Wen1,2*, REN Yu-Lin2, ZHENG Jian3, LIU Qing-Jun3   

  1. 1. College of Chemistry, Jilin University, Changchun 130012, China;
    2. College of Chemistry, Biology and Material Science, East China Institute of Technology, Fuzhou 344000, China;
    3. Beijing Center for Physical and Chemical Analysis, Beijing 100089, China
  • Received:2009-02-25 Online:2009-08-10 Published:2009-08-10
  • Contact: CHEN Huan-Wen. E-mail: chw8868@gmail.com
  • Supported by:

    国家自然科学基金(批准号: 20505003)和北京市财政项目(批准号: XM-00001783050811002)资助.

摘要:

将自行研制的电喷雾萃取电离源(EESI)和LTQ XL质谱仪耦合, 建立了选择性离子化快速测定牙膏胶状纳米级复杂基质样品中微量二甘醇的EESI-MS方法. 实验结果表明, 二甘醇与NH4+, Na+和K+离子在一级质谱中形成特征非共价配合物, 其它大量组分如纳米粒子及胶质等对测定无干扰. 该方法的样品消耗量约0.1 g, 灵敏度高, 单个样品的分析时间不到2 min, 可用于牙膏胶体中低含量二甘醇的选择性快速测定.

关键词: 电喷雾萃取电离; 质谱; 牙膏; 二甘醇; 快速测定; 分子-离子反应

Abstract:

Using ammonium acetate methanol solution(10 μmol/L) as the spray solvent, a novel method based on reactive extractive electrospray ionization(EESI) ion trap mass spectrometry was developed for the rapid determination of diethylene glycol(DEG) in toothpaste products, which are typical colloidal complex samples containing nano-scale particles in matrices. Under the optimized working conditions, DEG formed non-covalently bound complexes with NH4+, Na+ and K+ rather than the protonated molecules in the mass spectrum. About 0.1 g of the toothpaste products were required for direct sensitive analysis with EESI-MS, the whole procedure was completed within less than 2 min. Furthermore, the qualitative demonstration and quantitative analysis of DEG of the paste products was also done by the EESI-MS and EESI-MS/MS spectra. This method can be used for the rapid and selective determination of low-level DEG in toothpaste products, and it is a useful method for the rapid determination of low-level components in the viscous nano-materials.

Key words: Extractive electrospray ionization; Mass spectrometry; Toothpaste; Diethylene glycol; Rapid detection; Ion/molecule reaction

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