新型烷基醚型键合固定相的制备及评价

 首次将一种新型硅烷偶联剂 β (3,4 环氧环己基 )乙基三甲氧基硅烷 (β ECTS)与辛醇反应 ,然后再键合到硅胶上 ,得到了醚型键合固定相 ,并用元素分析、13 C固体核磁、红外光谱等对其进行了表征。以甲醇 水简单的二元流动相体系 ,对该固定相进行了色谱评价。结果表明 ,该固定相具有较好的色谱性能 ,且在 pH 2 5～ 7 5时化学稳定性能良好 ,硅醇基效应得到了很好地抑制 ,可有效地用于碱性化合物的分离分析

Preparation and Evaluation of Alkyl Ether-Bonded Phase forReversed-Phase High Performance Liquid Chromatography

A new silane coupling agent, beta-(3,4-epoxycyclohexyl)ethyltrimethoxy silane, was for the firsty time used to react with octanol, then the intermediate product was coupled onto porous silica to obtain a novel bonded phase for reversed-phase high performance liquid chromatography (RP-HPLC). Characterization of prepared packing was carried out with elemental analysis, solid-state 13C nuclear magnetic resonance spectrometry (NMR), Fourier transform infrared(FT-IR) spectroscopy. Chromatographic evaluations were carried out by using a mixture of organic compounds and methanol-water as the binary mobile phase. The results showed that the stationary phase has excellent chromatographic properties and resist to hydrolysis at a pH value between 2.5 and 7.5. The silanophilic activity of the OEBP was weakened because of the existence of the cyclohexyl group in the packing. It can be efficiently used for the separation of basic compounds.