文章摘要
丛景香,王绍艳,张伟,吴秀红,董永梅.异甘草素键合硅胶固定相的合成及应用[J].精细化工,2019,36(4):
异甘草素键合硅胶固定相的合成及应用
Synthesis and Application of Isoliquiritigenin Boned Silica Gel Stationary Phases
投稿时间:2018-07-18  修订日期:2018-11-27
DOI:
中文关键词: 异甘草素  固定相  合成  表征  分离机制
英文关键词: Isoliquiritigenin  stationary phase  application  synthesis  performance
基金项目:国家自然科学基金(21576127);辽宁省教育厅科研项目(2016HZPY03)
作者单位E-mail
丛景香 辽宁科技大学 congjingxiang@126.com 
王绍艳 辽宁科技大学  
张伟 辽宁科技大学  
吴秀红 辽宁科技大学  
董永梅 辽宁科技大学  
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中文摘要:
      异甘草素是重要的查尔酮类药物成分,具有平面共轭结构。以10 μm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%。两根色谱柱对标准样品混合物及中药提取物多组分样品均具有良好的分离能力。
英文摘要:
      Isoliquiritigenin is an important chalcone component with plane-conjugated structure. The 10 μm silica gel was used as the substrate and the isoliquiritigenin was used as the ligand. The new isoliquiritigenin bonded silica gel stationary phases (ISLSP-Ⅰ, ISLSP-Ⅱ) were synthesized by continuous liquid phase reaction and intermediate method, respectively. The synthesized stationary phases were characterized by FTIR spectrum 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, and the chromatographic performences of the stationary phases synthesized by the two methods were systematically evaluated. The results showed that the column efficiency of both and the peak shapes are good, and the retentions depend on mass transfer at higher flowrate for the test sample. In the methanol-water solvent, column 2 exhibited a certain reversed-phase chromatographic separation mechanism. The relative deviation of retention times do not exceed 0.9 % for test components after 6 months’ use, indicating that the stabilities of the synthesized stationary phases were good. The test results showed that the two columns have good separation abilities for the multi-component samples of standard mixtures and the Chinese medicine extracts.
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