色谱

色谱 ›› 2014, Vol. 32 ›› Issue (10): 1138-1143.DOI: 10.3724/SP.J.1123.2014.05040

• 研究论文 • 上一篇    下一篇

分散液液微萃取-在线衍生化-气相色谱-质谱联用法检测环境水样品中紫外吸收剂

李建1,2, 徐兰英1, 薛舒文2, 徐丽2   

  1. 1. 黄冈师范学院, 经济林木种质改良与资源综合利用湖北省重点实验室, 湖北 黄冈 438000;
    2. 华中科技大学同济药学院, 湖北 武汉 430030
  • 收稿日期:2014-05-30 发布日期:2014-09-29
  • 通讯作者: 徐丽，E-mail：xulpharm@mails.tjmu.edu.cn
  • 基金资助:

    教育部2012年度“新世纪优秀人才支持计划”项目（NCET-12-0213）；黄冈师范学院经济林木种质改良与资源综合利用湖北省重点实验室开放基金项目（2013000903）.

Determination of ultraviolet filters in environmental aqueous samples by dispersive liquid-liquid microextraction with online derivatization-gas chromatography-mass spectrometry

LI Jian1,2, XU Lanying1, XUE Shuwen2, XU Li2   

  1. 1. Hubei Key Laboratory of Economic Forest Germplasm Improvement and Resources Comprehensive Utilization, Huanggang Normal University, Huanggang 438000, China;
    2. Tongji School of Pharmacy, Huazhong University of Science and Technology, Wuhan 430030, China
  • Received:2014-05-30 Published:2014-09-29

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摘要：

建立了分散液液微萃取（dispersive liquid-liquid microextraction，DLLME）-在线衍生化-气相色谱-质谱（GC-MS）方法，将其用于环境水中6种二苯甲酮类紫外吸收剂（BPs）（二苯甲酮、2，4-二羟基二苯甲酮、2-羟基-4-甲氧基二苯甲酮、4-羟基二苯甲酮、2-羟基-4-辛氧基二苯甲酮、2，2'-二羟基-4，4'-二甲氧基二苯甲酮）的检测。系统优化了在线衍生化的条件（如进样口温度、不分流时间、衍生化试剂用量）以及DLLME萃取条件（如萃取剂种类、分散剂种类、萃取剂与分散剂比例、样品体积、样品溶液离子强度及pH值）等。在最优的条件下，所考察的6种BPs检出限为0.011~0.15 μg/L，重现性（RSD）为0.7%~16.6%。该方法结果准确可靠，操作简单，富集效果好，成本较低，环境友好，在实际样品检测中具有一定的应用前景。

关键词: 分散液液微萃取, 环境水样, 气相色谱-质谱, 在线衍生化, 紫外吸收剂

Abstract:

A method of dispersive liquid-liquid microextraction (DLLME) combined with online derivatization-gas chromatography-mass spectrometry (GC-MS) was developed for the determination of benzophenone-type ultraviolet (UV) filers (BPs) in environmental aqueous samples. It is found that the online derivatization was superior to the off-line derivatization with its simplicity, high reaction efficiency and less consumption of potential poisonous reagents. The influential factors for online derivatization, including the temperature of the injection port, the splitless time, the proportion of derivatization reagent and sample solution, were initially optimized. In addition, the influential factors for DLLME, including the type of the extractant and dispersing solvent, the proportion of the extractant and the dispersing solvent, the volume of sample solution, the pH and the salt concentration of the sample solution were individually optimized in detail. Under the optimized derivatization and DLLME conditions, the limits of detection for the six BPs, benzophenone, 2,4-dihydroxybenzophenone, oxybenzone, 4-hydroxybenzophenone, octabenzone and 2,2'-dihydroxy-4,4'-dimethoxybenzophenone, ranged from 0.011 to 0.15 μg/L. The intra-day and inter-day relative standard deviations varied from 0.7% to 16.6%. The method was applied to the analysis of lake and river water with good recoveries. It is cost effective, reliable, easy to operate, environment-friendly and promising in the real applications.

Key words: dispersive liquid-liquid microextraction (DLLME), environmental water samples, gas chromatography-mass spectrometry (GC-MS), online derivatization, ultraviolet filters (UV filers)

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