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以四甲氧基硅烷(TMOS)为交联剂,氧氯化锆为原料,通过溶胶-凝胶技术制备磺丁基-β-环糊精氧化锆复合材料毛细管电色谱整体柱,并优化其实验条件。通过红外光谱(IR)、X射线衍射(XRD)及扫描电子显微镜(SEM)对整体柱固定相进行表征。整体柱内固定相分布均匀且与毛细管柱壁结合紧密,整体柱具有良好的通透性及稳定性。以硫脲为中性标记物,测定理论塔板数为7.9×104plates/m。以DL-组氨酸为考察物考察毛细管柱分离性能,其分离度为1.68。利用该整体柱对盐酸芬氟拉明对映体进行手性拆分,达到基线分离且分离度为1.51。
Using tetramethoxysilane (TMOS) as crosslinking agent and zirconium oxychloride as raw material, the monolithic column of sulfobutyl-β-cyclodextrin zirconium oxide composite was prepared by sol-gel technique and its Experimental conditions. The monolithic column was characterized by infrared spectroscopy (IR), X-ray diffraction (XRD) and scanning electron microscopy (SEM). The overall column stationary phase distribution and capillary column wall with close, the monolith has good permeability and stability. With thiourea as neutral marker, the theoretical plate number was determined as 7.9 × 104plates / m. The separation of capillary column was investigated with DL-histidine as the investigation material, the resolution was 1.68. Enantiomers of fenfluramine hydrochloride were chirally resolved using this monolithic column, achieving baseline resolution with a resolution of 1.51.