双胺型键合固定相的制备及评价

Synthesis, Characterization and Evaluation of a Novel Double-Amine Packing for Reversed-Phase High Performance Liquid Chromatography

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)与己二胺反应 ,然后再键合到硅胶上 ,最后与辛酰氯反应得到双胺型键合固定相 ,并用元素分析、1 3 C固体核磁、红外光谱进行了表征。用中性、酸性和碱性有机化合物为探测因子对其进行色谱评价。结果表明 :该固定相对含氮有机化合物的分离涉及疏水作用和离子排斥双重机理。

A novel double-amine packing (DABP) for reversed-phase high performance liquid chromatography (RP-HPLC) was synthesized by the reaction of hexyldiamine with β-(3,4-epoxycyclohexyl) ethyltrimethoxy silane, the intermediate product was coupled onto porous silica to get the intermediate product Ⅱ, then the product II was reacted with octanoyl chloride under catalytst. Characterization of the prepared packing was carried out with elemental analysis, solid-state 13C nuclear magnetic resonance and Fourier transform infrared(FT-IR). The chromatographic evaluation was carried out by using organic components including acidic, basic and neutral analytes as probe molecules. The results show that the separate mechanism of basic analytes on the DABP include shydrophobicity and ion repulse.