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Investigation on Retention Mechanism of Reversed-Phase Liquid Chromatography Using Peropyrene-type Polycyclic Aromatic Hydrocarbons.

哌芘型多环芳烃反相液相色谱保留机理的研究。

基本信息

批准号：
63550564
负责人：
JINNO Kiyokatsu
金额：
$ 1.47万
依托单位：
Toyohashi University of Technology
依托单位国家：
日本
项目类别：
Grant-in-Aid for General Scientific Research (C)
财政年份：
1988
资助国家：
日本
起止时间：
1988 至 1989
项目状态：
已结题

项目摘要

Polycyclic aromatic hydrocarbons (PAHs) have carcinogenic and/or mutagenic properties and therefore, it has been required to have a good analytical method. Generally in PAHs separation with reversed-phase liquid chromatography, which is seemed to be the most powerful and useful way, chemically bonded octadecylsilica (ODS) phases have been used as the representative stationary phase because of their capability and availability. In this investigation, different functional ODS phases have been synthesized in the laboratory and evaluated in their chromatographic performance, especially focusing on their ability of molecular planarity recognition for PAHs relating with their functionality and the retention mechanism has been interpreted by the consideration of molecular-molecular interaction between PAHs molecules and the stationary phase, of which structures have been confirmed by solid-state NMR spectrometry. After careful examinations, we have succeeded to design and synthesize two different types of stationary phases. One of them is dicoronylene and the other is multidentate phenyl bonded phases. The former can be useful to enhance the retention of planar PAHs and the latter can retain non-planar molecules longer than planar counterparts. The performance of those phases have been confirmed by chromatographic measurements. As the results, the investigations can open the new dimension to design novel stationary phases with enhanced selectivity of the separation, in which the theory induced from the interpretation of molecular-molecular interaction which plays an important role in liquid chromatography is basically used.

多环芳烃（PAHs）具有致癌和/或致突变特性，因此，需要有良好的分析方法。反相液相色谱法是目前分离多环芳烃的最有效的方法，而化学键合十八烷基硅胶（ODS）固定相由于其性能好、使用方便而被广泛用作多环芳烃的固定相。本研究在实验室合成了不同功能的ODS固定相，并对其色谱性能进行了评价，重点考察了ODS固定相对多环芳烃的平面识别能力，并从多环芳烃分子与固定相之间的分子-分子相互作用角度对ODS固定相的保留机理进行了解释。其结构已通过固态NMR光谱法确认。经过仔细的研究，我们成功地设计和合成了两种不同类型的固定相。其中一种是二亚戊基键合相，另一种是多齿苯基键合相。前者可用于提高平面多环芳烃的保留，后者可以保留非平面分子比平面对应物更长的时间。这些相的性能已通过色谱测量证实。研究结果表明，分子间相互作用理论在液相色谱中具有重要作用，该理论为设计具有更高分离选择性的新型固定相提供了新的思路。