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基于应用低密度有机溶剂的超声辅助乳化微萃取方法,随后采用气相色谱分析法测定水样中的多环芳烃。

Ultrasound-assisted emulsification microextraction method based on applying low density organic solvents followed by gas chromatography analysis for the determination of polycyclic aromatic hydrocarbons in water samples.

作者信息

Saleh Abolfazl, Yamini Yadollah, Faraji Mohammad, Rezaee Mohammad, Ghambarian Mahnaz

机构信息

Department of Chemistry, Tarbiat Modares University, P.O. Box 14115-175, Tehran, Iran.

出版信息

J Chromatogr A. 2009 Sep 25;1216(39):6673-9. doi: 10.1016/j.chroma.2009.08.001. Epub 2009 Aug 7.

DOI:10.1016/j.chroma.2009.08.001
PMID:19674752
Abstract

In this study, a fast, simple and efficient ultrasound-assisted emulsification microextraction (USAEME) method was successfully developed based on applying low density organic solvents. Fourteen microliters of toluene was injected slowly into a 12 mL home-designed centrifuge glass vial containing an aqueous sample that was located inside the ultrasonic water bath. The formed emulsion was centrifuged and 2 microL of separated toluene (about 4 microL) was injected into a gas chromatographic system equipped with a flame ionization detector (GC-FID) for analysis. Some polycyclic aromatic hydrocarbons (PAHs) were selected as model compounds for developing the method and evaluating its performance and to compare the efficiency of the proposed method with previously reported techniques. Several factors influencing the emulsification, extraction and collection efficiency such as the nature and volume of organic solvent, emulsification-extraction temperature, ionic strength and equilibrium and centrifugation times were investigated and optimized. Under the optimum conditions, preconcentration factors (PFs) in a range of 1776-2714 were obtained. The performance of the proposed method was studied in terms of linear dynamic range (LDRs from 0.05 to 100 microg L(-1)), linearity (R(2) > or = 0.994), precision (repeatability: RSD% < or = 7.9, reproducibility: RSD% < or = 14.6) and extraction percents (59.2-90.5%). Limits of detection (LODs) in the range of 0.02-0.05 microg L(-1) were obtained for different PAHs. The applicability of the proposed method was evaluated by the extraction and determination of PAHs from several natural water samples.

摘要

在本研究中,基于使用低密度有机溶剂成功开发了一种快速、简单且高效的超声辅助乳化微萃取(USAEME)方法。将14微升甲苯缓慢注入一个12毫升自行设计的离心玻璃小瓶中,该小瓶中装有置于超声水浴内的水样。将形成的乳液离心,然后将2微升分离出的甲苯(约4微升)注入配备火焰离子化检测器(GC-FID)的气相色谱系统进行分析。选择了一些多环芳烃(PAHs)作为模型化合物来开发该方法并评估其性能,以及将所提出方法的效率与先前报道的技术进行比较。研究并优化了影响乳化、萃取和收集效率的几个因素,如有机溶剂的性质和体积、乳化-萃取温度、离子强度以及平衡和离心时间。在最佳条件下,获得了1776 - 2714范围内的预富集因子(PFs)。从线性动态范围(LDRs为0.05至100微克/升(-1))、线性度(R(2)≥0.994)、精密度(重复性:RSD%≤7.9,再现性:RSD%≤14.6)和萃取率(59.2 - 90.5%)方面研究了所提出方法的性能。对于不同的PAHs,检测限(LODs)在0.02 - 0.05微克/升(-1)范围内。通过从几个天然水样中萃取和测定PAHs来评估所提出方法的适用性。

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