Study on a New Open Tubular Capillary Liquid Chromatography(OTCLC) System Based on Micro-Phase Separation of Mixed Solvents

基于混合溶剂微相分离的新型开管毛细管液相色谱（OTCLC）系统研究

基本信息

批准号：
15350046
负责人：
TABATA Masaaki
金额：
$ 8.06万
依托单位：
Saga University
依托单位国家：
日本
项目类别：
Grant-in-Aid for Scientific Research (B)
财政年份：
2003
资助国家：
日本
起止时间：
2003 至 2004
项目状态：
已结题

项目摘要

The proposed open tubular capillary liquid chromatography(OTCLC) system utilizes the recent discoveries of "microheterogeneity" in some organic-water mixed solvents and salting-out phase separation phenomena observed in these mixed solvents. For example, acetonitrile is miscible with water at any ratio ; heterogeneities, however, have been observed at a molecular level in its water mixtures. When an acetonitrile-water mixture of suitable salt concentration is pumped into such a capillary micro-phase separation is likely happening in the vicinity of the capillary wall, in a water-enriched aqueous phase attached to the capillary inner wall. In other words, a liquid membrane that has considerably different properties from the mobile phase is dynamically formed on the inner wall of the capillary.When a mixture of analytes is injected into the capillary, participation of the analytes occurs between the mobile phase and the liquid membrane, providing the separation power of the proposed chromatograpy system.Chromatographs clearly demonstrated the ability of separating neutral compounds from charged compounds by the OTCLC system. Moreover, it was also possible to separate compounds of similar molecular structure but different charges. The elution orders can readily be explained by the retention mechanism. p-Nitroaniline is effectively extracted to the upper (acetonitrile-enriched) phase while 2,7-NDS remains in the lower (water-enriched) phase, confirming the elution order observed. The high concentration of acetonitrile content in the mobile phase slightly increased the elution time of 1-naphthol but significantly increased the elution time of 2,6-naphtalene disulfonic acid. More interestingly, at the absence of NaCl, no separation in both cases (AN/aq 9/1 and AN/aq 8/2) were observed, demonstrating the necessity of additional electrolyte for the micro-phase separation in the capillary tubing.

拟议的开放管状毛细血管液相色谱（OTCLC）系统利用了一些在这些混合溶剂中观察到的有机水混合溶剂和盐水分离现象的最新发现。例如，乙腈在任何比例上都与水混溶。然而，在其水混合物中的分子水平上观察到了异质性。当将合适的盐浓度的乙腈 - 水混合物泵入这种毛细管微相分离中时，可能会在毛细管壁附近发生，在含水含水的水相中附着在毛细血管内壁上。换句话说，在毛细管的内壁上动态形成了与流动相的液体膜，当将分析物的混合物注入到毛细管中时，分析物的参与是流动相和液体膜之间的参与，从而从质拟疗法的分离能力中出现。 OTCLC系统。此外，还可以分离相似分子结构但不同电荷的化合物。洗脱订单可以通过保留机制很容易解释。有效地将硝基苯胺提取到上部（乙腈富集）相，而2,7-ND仍处于下部（富含水的）相处，证实观察到的洗脱顺序。流动阶段中高浓度的乙腈含量稍微增加了1-萘醇的洗脱时间，但显着增加了2,6-萘二烯二硫酸的洗脱时间。更有趣的是，在没有NaCl的情况下，观察到两种情况下都没有分离（AN/AQ 9/1和AN/AQ 8/2），这表明在毛细管中需要额外的电解质进行微相分离。