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使用水/甲醇/氯仿三元体系进行均相液-液萃取以预富集多环芳烃。

Homogeneous liquid-liquid extraction for preconcentration of polycyclic aromatic hydrocarbons using a water/methanol/chloroform ternary component system.

作者信息

Tavakoli Laleh, Yamini Yadollah, Ebrahimzadeh Homeyra, Shariati Shahab

机构信息

Department of Chemistry, Faculty of Sciences, Tarbiat Modares University, PO Box 14115-175, Tehran, Iran.

出版信息

J Chromatogr A. 2008 Jul 4;1196-1197:133-8. doi: 10.1016/j.chroma.2008.04.036. Epub 2008 Apr 22.

Abstract

A fast and effective preconcentration method for the extraction of polycyclic aromatic hydrocarbons (PAHs) was developed using a homogeneous liquid-liquid extraction based on phase separation phenomenon in a ternary solvent (water/methanol/chloroform) system. The phase separation phenomenon occurred by salt addition. After centrifugation, the extracting solvent was sedimented in the bottom of the conical test tube. The PAHs were transferred into the sedimented phase during the phase separation step. The extracted PAHs were determined using gas chromatography-flame ionization detection. Several factors influencing the extraction efficiency were investigated and optimized. Optimal results were obtained at the following conditions: volume of the consolute solvent (methanol), 1.2 mL; volume of the extracting solvent (chloroform), 60 muL; volume of the sample, 2.5 mL; concentration of NaCl, 15% (w/v). Under the optimum conditions, the enrichment factors of 225-257, the extraction percent of 90-100%, the dynamic linear range of 0.1-400 microg L(-1), and the limits of detection of 0.02-0.18 microg L(-1) were obtained for the PAHs. Using internal standard, the relative standard deviations for 100 microg L(-1) of the PAHs in the water samples were obtained in the range of 4.2-10.3% (n=5). Finally, the proposed method was successfully applied for the extraction and determination of the PAHs in waste water samples.

摘要

基于三元溶剂(水/甲醇/氯仿)体系中的相分离现象,采用均相液-液萃取法开发了一种快速有效的多环芳烃(PAHs)预浓缩方法。加盐会引发相分离现象。离心后,萃取溶剂沉淀在锥形试管底部。在相分离步骤中,PAHs转移到沉淀相中。采用气相色谱-火焰离子化检测法测定萃取的PAHs。研究并优化了影响萃取效率的几个因素。在以下条件下获得了最佳结果:混溶溶剂(甲醇)体积为1.2 mL;萃取溶剂(氯仿)体积为60 μL;样品体积为2.5 mL;NaCl浓度为15%(w/v)。在最佳条件下,PAHs的富集因子为225 - 257,萃取率为90 - 100%,动态线性范围为0.1 - 400 μg L⁻¹,检测限为0.02 - 0.18 μg L⁻¹。使用内标法,水样中100 μg L⁻¹的PAHs的相对标准偏差在4.2 - 10.3%范围内(n = 5)。最后,该方法成功应用于废水样品中PAHs的萃取和测定。

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