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以丙烯胺-β-环糊精(Allylamine-β-CD)为功能单体,采用一步键合法制备毛细管电色谱手性整体柱,并考察了整体柱的制备条件。在毛细管电色谱(CEC)模式下,以苯丙氨酸为对象,考察了整体柱的分离能力,同时考察缓冲溶液pH,柱温,分离电压对拆分的影响。苯丙氨酸的拆分达到了基线分离,并在优化条件下,应用整体柱对盐酸去甲苯福林和愈创甘油醚对映体进行拆分,均达到基线分离。同时,以硫脲为电渗流标记物,测得整体柱的理论塔板数达87488板/m,并且可持续使用16 h,可间歇使用3个月以上,仍具有良好的柱效。
In this work, the chiral monolithic column was prepared by the one-step method using allylamine-β-CD as the functional monomer. The preparation conditions of the monolithic column were also investigated. In the capillary electrochromatography (CEC) mode, phenylalanine was used as a target to investigate the separation ability of the monolithic column. Meanwhile, the effect of buffer solution pH, column temperature and separation voltage on the resolution was investigated. The separation of phenylalanine reached the baseline separation, and under optimized conditions, enantioselective separation of phenylephrine hydrochloride and guaifenesin using monolithic columns was achieved. At the same time, using thiourea as the electroosmotic flow marker, the theoretical plate number of the monolithic column was 87488 plates / m, and the sustainable use of 16 h, can be intermittent use for more than 3 months, still has good column efficiency.