Evaluation of hexamethyldisiloxane/ethyl isobutyrate/ethanol/water solvent system for liquid-liquid chromatography

IF 3.8 2区化学 Q1 BIOCHEMICAL RESEARCH METHODS Journal of Chromatography A Pub Date : 2025-03-13 DOI:10.1016/j.chroma.2025.465873

Kai Wang, Simon Vlad Luca, Mirjana Minceva

{"title":"Evaluation of hexamethyldisiloxane/ethyl isobutyrate/ethanol/water solvent system for liquid-liquid chromatography","authors":"Kai Wang, Simon Vlad Luca, Mirjana Minceva","doi":"10.1016/j.chroma.2025.465873","DOIUrl":null,"url":null,"abstract":"<div><div>The most commonly used solvent systems in liquid-liquid chromatography (LLC), such as heptane/ethyl acetate/methanol/water (ARIZONA) or its variant hexane/ethyl acetate/methanol/water (HEMWat), contain toxic petroleum-based solvents that raise serious risks to human health and environment. Therefore, there is a great need to find alternative, greener, and safer solvent systems for LLC applications. This work comprehensively evaluated an alternative biphasic solvent system, hexamethyldisiloxane/ethyl isobutyrate/ethanol/water (HMDSO/EIB/ethanol/water), by considering its thermodynamic properties, physical properties, and suitability for LLC applications. Compared with the HEMWat system, the HMDSO/EIB/ethanol/water system had a similar phase density difference, higher phase viscosity, and longer settling times. The distribution constants (<span><math><msub><mi>K</mi><mi>i</mi></msub></math></span>) of 12 test compounds with different polarities and chemical structural features representative of various classes of natural products were assessed in 16 compositions of the HMDSO/EIB/ethanol/water and HEMWat systems. System compositions with similar <span><math><msub><mi>K</mi><mi>i</mi></msub></math></span> values were identified for the two solvent systems. Since COSMO-RS provided good predictions of the <span><math><msub><mi>K</mi><mi>i</mi></msub></math></span> of the test compounds, its use can significantly reduce the process of finding an HMDSO/EIB/ethanol/water system composition for separating other components, using only their molecular structures as input. The results of countercurrent chromatography and centrifugal partition chromatography experiments showed comparable separation behaviors of selected compounds in both solvent systems, demonstrating that the HMDSO/EIB/ethanol/water system could be a viable, safer replacement for HEMWat and ARIZONA solvent systems in LLC.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1748 ","pages":"Article 465873"},"PeriodicalIF":3.8000,"publicationDate":"2025-03-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":null,"platform":"Semanticscholar","paperid":null,"PeriodicalName":"Journal of Chromatography A","FirstCategoryId":"1","ListUrlMain":"https://www.sciencedirect.com/science/article/pii/S0021967325002213","RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q1","JCRName":"BIOCHEMICAL RESEARCH METHODS","Score":null,"Total":0}

引用次数: 0

Abstract

The most commonly used solvent systems in liquid-liquid chromatography (LLC), such as heptane/ethyl acetate/methanol/water (ARIZONA) or its variant hexane/ethyl acetate/methanol/water (HEMWat), contain toxic petroleum-based solvents that raise serious risks to human health and environment. Therefore, there is a great need to find alternative, greener, and safer solvent systems for LLC applications. This work comprehensively evaluated an alternative biphasic solvent system, hexamethyldisiloxane/ethyl isobutyrate/ethanol/water (HMDSO/EIB/ethanol/water), by considering its thermodynamic properties, physical properties, and suitability for LLC applications. Compared with the HEMWat system, the HMDSO/EIB/ethanol/water system had a similar phase density difference, higher phase viscosity, and longer settling times. The distribution constants (

K_{i}

) of 12 test compounds with different polarities and chemical structural features representative of various classes of natural products were assessed in 16 compositions of the HMDSO/EIB/ethanol/water and HEMWat systems. System compositions with similar

K_{i}

values were identified for the two solvent systems. Since COSMO-RS provided good predictions of the

K_{i}

of the test compounds, its use can significantly reduce the process of finding an HMDSO/EIB/ethanol/water system composition for separating other components, using only their molecular structures as input. The results of countercurrent chromatography and centrifugal partition chromatography experiments showed comparable separation behaviors of selected compounds in both solvent systems, demonstrating that the HMDSO/EIB/ethanol/water system could be a viable, safer replacement for HEMWat and ARIZONA solvent systems in LLC.

查看原文

微信好友朋友圈 QQ好友复制链接

本刊更多论文

求助全文

约1分钟内获得全文去求助

来源期刊

Journal of Chromatography A 化学-分析化学

CiteScore

7.90

自引率

14.60%

发文量

742

审稿时长

45 days

期刊介绍： The Journal of Chromatography A provides a forum for the publication of original research and critical reviews on all aspects of fundamental and applied separation science. The scope of the journal includes chromatography and related techniques, electromigration techniques (e.g. electrophoresis, electrochromatography), hyphenated and other multi-dimensional techniques, sample preparation, and detection methods such as mass spectrometry. Contributions consist mainly of research papers dealing with the theory of separation methods, instrumental developments and analytical and preparative applications of general interest.