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第 36 卷第 4 期 精 细 化 工 Vol.36, No.4
201 9 年 4 月 FINE CHEMICALS Apr. 2019
中药现代化技术
异甘草素键合硅胶固定相的合成及应用
丛景香,王绍艳,张 伟,吴秀红,董永梅
(辽宁科技大学 化学工程学院,辽宁 鞍山 114051)
摘要: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。
关键词:异甘草素;固定相;表征;分离机制;中药现代化技术
中图分类号:TQ032 文献标识码:A 文章编号:1003-5214 (2019) 04-0658-06
Synthesis and Application of Isoliquiritigenin Bonded
Silica Gel Stationary Phases
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)
Abstract: 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.
Key words: isoliquiritigenin; stationary phase; characterization; separation mechanism; modernization
technology of traditional Chinese medicines
Foundation items: National Natural Science Foundation of China (21576127); Scientific Research Fund of
Liaoning Provincial Education Department (2016HZPY03)
液相色谱固定相是分离不同类型混合物的根 无机杂化材料等,制备方法主要有溶胶凝胶法、合
[1]
本。按材料性质,液相色谱固定相可分为天然高分 成法、聚合法等 。色谱固定相不断推陈出新,新
子材料、人工合成高分子材料、无机材料、有机- 型色谱固定相在分离效率、机械强度、使用寿命、
收稿日期:2018-07-18; 定用日期:2018-12-24; DOI: 10.13550/j.jxhg.20180530
基金项目:国家自然科学基金(21576127);辽宁省教育厅科研项目(2016HZPY03)
作者简介:丛景香(1979—),女,讲师,博士,E-mail:congjingxiang@126.com。