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采用中空纤维微孔膜液液萃取和气相色谱-质谱联用技术测定环境水样中痕量多溴二苯醚

Determination of polybrominated diphenyl ethers at trace levels in environmental waters using hollow-fiber microporous membrane liquid-liquid extraction and gas chromatography-mass spectrometry.

作者信息

Fontanals Núria, Barri Thaer, Bergström Staffan, Jönsson Jan-Ake

机构信息

Department of Analytical Chemistry, University of Lund, P.O. Box 124, SE-22100 Lund, Sweden.

出版信息

J Chromatogr A. 2006 Nov 10;1133(1-2):41-8. doi: 10.1016/j.chroma.2006.08.026. Epub 2006 Sep 11.

Abstract

In this study, we present a simple and easy-to-use extraction method that is based on a hollow-fiber microporous membrane liquid-liquid extraction (HF-MMLLE), as an extraction technique, followed by gas chromatography-mass spectrometry (GC-MS) to determine a group of brominated flame retardants (BFRs), polybrominated diphenyl ethers (PBDEs), at trace levels in aqueous samples. The hollow-fiber membrane (HF) filled with organic solvent was immersed into the aqueous sample, spiked with the analytes at ng l(-1) level, and stirred for 60 min. The proposed method could attain enrichment factors (E(e)) up to 5200 times, after optimising parameters, such as organic solvent, stirring speed and extraction time, that affect the extraction. The HF-MMLLE-GC-MS method was successfully applied to the extraction of PBDEs from tap, river and leachate water samples with spike recoveries ranging from 85% to 110%. The method validation with reagent and leachate water samples provided good linearity, detection limits of 1.1 ng l(-1) or lower, both in reagent and leachate water, as well as satisfactory precision in terms of repeatability and reproducibility with values of % relative standard deviation (%RSD) lower than 8.6 and 16.9, respectively.

摘要

在本研究中,我们提出了一种基于中空纤维微孔膜液液萃取(HF-MMLLE)的简单易用的萃取方法,作为一种萃取技术,随后结合气相色谱-质谱联用(GC-MS)来测定水样中痕量水平的一组溴化阻燃剂(BFRs),即多溴二苯醚(PBDEs)。将填充有机溶剂的中空纤维膜(HF)浸入含有纳克/升(ng l⁻¹)水平分析物的水样中,并搅拌60分钟。在优化影响萃取的参数(如有机溶剂、搅拌速度和萃取时间)后,所提出的方法可实现高达5200倍的富集因子(E(e))。HF-MMLLE-GC-MS方法成功应用于从自来水、河水和渗滤液水样中萃取PBDEs,加标回收率在85%至110%之间。用试剂和渗滤液水样进行的方法验证提供了良好的线性关系,在试剂和渗滤液水中的检测限均为1.1 ng l⁻¹或更低,并且在重复性和再现性方面具有令人满意的精密度,相对标准偏差(%RSD)值分别低于8.6和16.9。

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