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以γ-(环氧丙氧)丙基键合硅胶为前体,于硅胶表面键合环氧基,在催化剂存在下以杯芳烃钠盐开环制备杯芳烃键合硅胶固定相.该方法反应条件温和,适用性强.将这个新方法首次用于制备对-叔丁基杯[8]芳烃电色谱键合固定相(C 8BS),采用加压电色谱初步评价其电色谱性能.研究结果表明,C 8BS电渗流(E lectrosm otic flow,EOF)较小,但通过控制键合反应及使用压力辅助电色谱可部分弥补上述不足.该固定相的EOF受流动相pH影响小(pH=3~8),同时大环配体屏蔽效应能有效地克服硅羟基引起的碱性化合物拖尾现象,这对电色谱分离具有重要意义.通过分步封尾研究EOF的来源发现,杯芳烃酚羟基对EOF有弱的贡献,这与报道的杯芳烃涂层具有径向电渗流调控能力相一致.
In this work, γ-glycidoxypropyl-bonded silica was used as the precursor, and the epoxy group was bonded to the surface of the silica gel to prepare the calixarene bonded silica stationary phase in the presence of a catalyst. Mild conditions and high applicability.This new method was first used to prepare p-tert-butylcalix [8] arene bonded chromatographic stationary phase (C 8BS), and its electrochromatographic properties were preliminary evaluated by electrocompression chromatography The results showed that the EOF of C 8BS was small, but this problem could be partially overcome by controlling the bonding reaction and using pressure-assisted electrochromatography.The EOF of the stationary phase was little affected by the pH of the mobile phase (pH = 3 ~ 8), while macrocyclic ligand shielding effect can effectively overcome the silanol-induced alkaline compound trailing phenomenon, which is of great significance for the separation of electrochromatography.Through step-by-step end-sealing study EOF sources found that calixarene phenolic hydroxyl Have a weak contribution to EOF, consistent with the reported radial infiltration control of calixarene coatings.