色谱

色谱 ›› 2012, Vol. 30 ›› Issue (02): 201-206.DOI: 10.3724/SP.J.1123.2011.10011

• 研究论文 • 上一篇    下一篇

基于轻质萃取剂的溶剂去乳化分散液-液微萃取-气相色谱法测定水样中多环芳烃

祝本琼, 陈浩, 李胜清*   

  1. 华中农业大学理学院化学系, 湖北 武汉 430070
  • 收稿日期:2011-10-11 修回日期:2011-12-23 出版日期:2012-02-28 发布日期:2012-03-22
  • 通讯作者: 李胜清,博士,副教授,研究方向为环境分析.
  • 基金资助:

    国家自然科学基金项目(20705009)、教育部新教师基金项目(20070504039)和中央高校基本科研业务费专项资金项目(2011PY128)

LLow-density solvent-based solvent demulsification dispersive liquid-liquid microextraction combined with gas chromatography for determination of polycyclic aromatic hydrocarbons in water samples

ZHU Benqiong, CHEN Hao, LI Shengqing*   

  1. Department of Chemistry, College of Science, Huazhong Agricultural University, Wuhan 430070, China
  • Received:2011-10-11 Revised:2011-12-23 Online:2012-02-28 Published:2012-03-22

PDF

514

被引次数

53

摘要： 以密度小于水的轻质溶剂为萃取剂,建立了无需离心步骤的溶剂去乳化分散液-液微萃取-气相色谱(SD-DLLME-GC)测定水样中多环芳烃的新方法。传统分散液-液微萃取技术一般采用密度大于水的有机溶剂为萃取剂,并需要通过离心步骤促进分相。而本方法以密度比水小的轻质溶剂甲苯为萃取剂,将其与丙酮(分散剂)混合并快速注入水样,获得雾化体系;然后注入乙腈作为去乳化剂,破坏该雾化体系,无需离心,溶液立即澄清、分相;取上层有机相(甲苯)进行GC分析。考察了萃取剂、分散剂、去乳化剂的种类及其体积等因素对萃取率的影响。以40 μL甲苯为萃取剂,500 μL丙酮为分散剂,800 μL乙腈为去乳化剂,方法在20～500 μg/L范围内呈现出良好的线性(r2=0.9942～0.9999),多环芳烃的检出限(S/N=3)为0.52～5.11 μg/L。用所建立的方法平行测定5份质量浓度为40 μg/L的多环芳烃标准水样,其含量的相对标准偏差为2.2%～13.6%。本法已成功用于实际水样中多环芳烃的分析,并测得其加标回收率为80.2%～115.1%。

关键词: 多环芳烃, 气相色谱, 轻质溶剂, 溶剂去乳化分散液-液微萃取, 水样

Abstract: A novel method of low-density solvent-based solvent demulsification dispersive liquid-liquid microextraction (SD-DLLME) was developed for the determination of eight polycyclic aromatic hydrocarbons (PAHs) in water samples by gas chromatography-flame ionization detection (GC-FID). Conventional DLLME methods usually employ organic solvents heavier than water as the extraction solvents and achieve the phase separation through centrifugation. On the contrary, in this proposed extraction procedure, a mixture of low-density extraction solvent (toluene) and dispersive solvent (acetone) was injected into the aqueous sample solution to form an emulsion. A demulsification solvent (acetonitrile) was then injected into the aqueous solution to break up the emulsion, which turned clear quickly and was separated into two layers. The upper layer (toluene) was collected and analyzed by GC. No centrifugation was required in this procedure. Factors affecting the extraction efficiency such as the type and volume of dispersive solvent, extraction solvent and de-emulsifier were investigated in detail. Under the optimized conditions, the proposed method provided a good linearity in the range of 20~500 μg/L (r2=0.9942 ~ 0.9999). The limits of detection (S/N=3) were in the range of 0.52~5.11 μg/L. The relative standard deviations (RSDs) for the determination of 40 μg/L PAHs were in the range of 2.2%~13.6% (n=5). The proposed method is fast, efficient and convenient. It has been successfully applied to the determination of PAHs in natural water samples with the spiked recoveries of 80.2%~115.1%.

Key words: polycyclic aromatic hydrocarbons, solvent demulsification dispersive liquid-liquid microextraction (SD-DLLME), water sample, gas chromatography (GC), low-density solvent