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采用液相色谱-多级质谱联用技术分离和测定均相脂肪醇聚氧乙烯醚

Separation and determination of homogenous fatty alcohol ethoxylates by liquid chromatography with mulitstage mass spectrometry.

作者信息

Zembrzuska Joanna, Budnik Irena, Lukaszewski Zenon

机构信息

Institute of Chemistry and Technical Electrochemistry, Poznan University of Technology, Poznan, Poland.

出版信息

J Sep Sci. 2014 Jul;37(13):1694-702. doi: 10.1002/jssc.201301391. Epub 2014 May 15.

DOI:10.1002/jssc.201301391
PMID:24737670
Abstract

Alcohol ethoxylates (AEs) are a significant component of a stream of surfactants directed to the aquatic environment. The aim of this work was the investigation of the dependence of the analytical signals of homogeneous AE homologues on liquid chromatography with tandem mass spectrometry conditions, as well as the separation of AEs from the water matrix and, on this basis, the development of an analytical procedure suitable for the determination of AEs in environmental samples. Homogeneous homologues containing dodecyl moiety and 2-9 oxyethylene subunits were investigated. The analytical signals of the investigated homologues were optimized in terms of concentration of ammonium acetate in the mobile phase (optimum 5 mM) and a column temperature (optimum 35°C) of the liquid chromatography with tandem mass spectrometry system. A separation of AEs from the water matrix by liquid-liquid extraction (ethyl acetate, chloroform) or solid-phase extraction (C18 , styrene divinylbenzene, H-RX) was investigated. In a model investigation, the best recoveries (>90%) were obtained with a styrene divinylbenzene cartridge eluted with a 1:1 mixture of chloroform and methanol. However, much worse recoveries were obtained from the river water sample. Better results were obtained for liquid-liquid extraction with ethyl acetate. Recoveries of 62-80% were obtained for homologues having 4-9 oxyethylene subunits, at the lowest spike.

摘要

脂肪醇聚氧乙烯醚(AEs)是排放到水生环境中的表面活性剂流的重要组成部分。这项工作的目的是研究均相AE同系物的分析信号与液相色谱-串联质谱条件之间的相关性,以及从水基质中分离AEs,并在此基础上开发一种适用于测定环境样品中AEs的分析方法。研究了含有十二烷基部分和2-9个氧乙烯亚基的均相同系物。在所研究的同系物的分析信号方面,对液相色谱-串联质谱系统的流动相中乙酸铵的浓度(最佳为5 mM)和柱温(最佳为35°C)进行了优化。研究了通过液-液萃取(乙酸乙酯、氯仿)或固相萃取(C18、苯乙烯-二乙烯基苯、H-RX)从水基质中分离AEs。在模型研究中,用氯仿和甲醇的1:1混合物洗脱的苯乙烯-二乙烯基苯柱获得了最佳回收率(>90%)。然而,从河水样品中获得的回收率要低得多。用乙酸乙酯进行液-液萃取获得了更好的结果。对于具有4-9个氧乙烯亚基的同系物,在最低加标水平下,回收率为62-80%。

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