胺型键合反相固定相的制备及评价

Preparation and Evaluation of Alkyl-amine Reversed Phase High Performance Liquid Chromatographic Packing

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)与辛胺反应 ,然后再键合到硅胶上 ,得到了胺型键合固定相 ,并用元素分析、1 3C固体核磁共振、红外光谱进行了表征。以甲醇和水为二元流动相 ,用包括碱性、酸性和中性有机化合物在内的混合物对该固定相进行评价 ,并考察了该填料的适用pH范围及水解稳定性。结果表明 ,该固定相具有较好的色谱性能 ,且在pH =2～ 8之间稳定性能良好 。

A new silane coupling agent-beta-(3,4-epoxycyclohexyl) ethyltrimethoxy silane was firstly used to react with octylamine, then the intermediate product was coupled onto porous silica to obtain a novel bonded phase for reversed-phase high performance liquid chromatography. Characterization of prepared packing was carried out with elemental analysis, solid-state C-13 nuclear magnetic resonance, Fourier transform infrared (FT-IR). Chromatographic evaluations were carried out by using a mixture of organic compounds including acidic, basic and neutral analytes and methanol-water as binary mobile phase. The results show that the stationary phase has excellent chromatographic properties and can resist stably on hydrolyzing between pH = 2 similar to 8. It can be efficiently used for the separation of basic compounds.