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再看一眼乙腈/水混合溶液中盐析辅助液液萃取的情况。

Another glimpse over the salting-out assisted liquid-liquid extraction in acetonitrile/water mixtures.

机构信息

REQUIMTE - Departamento de Química e Bioquímica, Faculdade de Ciências, Universidade do Porto, Rua do Campo Alegre no. 687, 4169-007 Porto, Portugal.

出版信息

J Chromatogr A. 2013 Sep 20;1308:58-62. doi: 10.1016/j.chroma.2013.08.014. Epub 2013 Aug 8.

DOI:10.1016/j.chroma.2013.08.014
PMID:23958692
Abstract

The use of the salting-out effect in analytical chemistry is very diverse and can be applied to increase the volatility of the analytes in headspace extractions, to cause the precipitation of proteins in biological samples or to improve the recoveries in liquid-liquid extractions. In the latter, the salting-out process can be used to create a phase separation between water-miscible organic solvents and water. Salting-out assisted liquid-liquid extraction (SALLE) is an advantageous sample preparation technique aiming HPLC-UV analysis when developing analytical methodologies. In fact, some new extraction methodologies like QuEChERS include the SALLE concept. This manuscript discusses another point of view over SALLE with particular emphasis over acetonitrile-water mixtures for HPLC-UV analysis; the influence of the salting-out agents, their concentration and the water-acetonitrile volume ratios were the studied parameters. α-dicarbonyl compounds and beer were used as test analytes and test samples, respectively. The influence of the studied parameters was characterized by the obtained phase separation volume ratio and the fraction of α-dicarbonyls extracted to the acetonitrile phase. Results allowed the distribution of salts within three groups according to the phase separation and their extractability: (1) chlorides and acetates, (2) carbonates and sulfates and (3) magnesium sulfate; of all tested salts, sodium chloride had the highest influence on the α-dicarbonyls fraction extracted.

摘要

盐析效应在分析化学中的应用非常多样化,可以用于增加顶空萃取中分析物的挥发性,使生物样品中的蛋白质沉淀,或提高液液萃取中的回收率。在后一种情况下,盐析过程可用于在水混溶性有机溶剂和水之间产生相分离。盐析辅助液液萃取(SALLE)是一种有利的样品制备技术,用于开发分析方法学中的 HPLC-UV 分析。事实上,一些新的提取方法,如 QuEChERS,包括 SALLE 概念。本文讨论了 SALLE 的另一个观点,特别强调用于 HPLC-UV 分析的乙腈-水混合物;研究了盐析剂、其浓度以及水-乙腈体积比等参数的影响。α-二羰基化合物和啤酒分别用作测试分析物和测试样品。通过获得的相分离体积比和α-二羰基化合物萃取到乙腈相的分数来表征研究参数的影响。结果表明,根据相分离和可提取性,盐可分为三组:(1)氯化物和醋酸盐,(2)碳酸盐和硫酸盐,(3)硫酸镁;在所测试的盐中,氯化钠对α-二羰基化合物的萃取分数影响最大。

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