异甘草素键合硅胶固定相的合成及应用  

Synthesis and Application of Isoliquiritigenin Bonded Silica Gel Stationary Phases

作　　者：丛景香[1] 王绍艳[1] 张伟[1] 吴秀红[1] 董永梅[1] CONG Jing-xiang;WANG Shao-yan;ZHANG Wei;WU Xiu-hong;DONG Yong-mei(School of Chemical Engineering, University of Science and Technology Liaoning, Anshan 114051, Liaoning, China)

机构地区：[1]辽宁科技大学化学工程学院,辽宁鞍山114051

出　　处：《精细化工》2019年第4期658-663,共6页Fine Chemicals

基　　金：国家自然科学基金(21576127);辽宁省教育厅科研项目(2016HZPY03)~~

摘　　要：以10μm硅胶为基质,异甘草素为配体,采用液相连续反应法及中间体法依次合成了异甘草素键合硅胶固定相ISLSP-Ⅰ和ISLSP-Ⅱ。采用FTIR及SEM对合成的固定相进行表征。将ISLSP-Ⅰ固定相填充于50 mm×10 mm i.d. 1号色谱柱中,将ISLSP-Ⅱ固定相填充于30 mm×10 mm i.d. 2号色谱柱中,系统评价了两种方法合成的固定相的色谱性能。结果表明:两根色谱柱的柱效及峰型均较好,大流速下测试组分的保留主要决定于传质阻力。在甲醇-水体系下,2号色谱柱表现出明显的反相色谱分离机制。合成的固定相稳定性良好,使用6个月后,测试组分在两根色谱柱上的保留时间相对偏差不超过0.9%。2号色谱柱对多组分标准样品及中药提取物均具有良好的分离能力。New isoliquiritigenin bonded silica gel stationary phases(ISLSP-Ⅰ, ISLSP-Ⅱ) were synthesized using 10 μm silica gel as the substrate and isoliquiritigenin as the ligand by continuous liquid phase reaction and intermediate method, respectively. The synthesized stationary phases were characterized by FTIR and SEM. The stationary phase ISLSP-Ⅰ was packed in a 50 mm × 10 mm i.d. column 1. The stationary phase ISLSP-Ⅱ was packed in a 30 mm × 10 mm i.d. column 2. Their chromatographic performances were systematically evaluated. The results showed that the column efficiency and peak shapes of these two chromatographic columns were good. The retention time of test components at large flowrate was mainly determined by mass transfer resistance. In the methanol and water mixed solvent, column 2 exhibited a certain reversed-phase chromatographic separation mechanism. For test components, the relative deviation of retention time on the two columns did not exceed 0.9% after 6 months of use, indicating that the synthesized stationary phases had good stability. In addition, the two columns had good separation abilities for the multi-components standard sample mixtures and the Chinese medicine extracts.

关 键 词：异甘草素 固定相 表征 分离机制 中药现代化技术 

分 类 号：TQ032[化学工程]