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高速逆流色谱法分离纯化龙胆碱性乙醇提取物中的龙胆碱
石垚, 王琳琳, 余河水, 赖青海, 丁辉, 张丽娟, 宋新波
天津中医药大学, 天津 300193
摘要:
[目的] 建立从龙胆碱性乙醇提取物中分离龙胆碱的高速逆流色谱(HSCCC)方法。[方法] 采用高速逆流色谱仪分离纯化龙胆碱性乙醇提取物中的龙胆碱,通过优化溶剂系统,以正己烷:乙酸乙酯:甲醇:水(5:5:4:6)为溶剂体系,上相为固定相,下相为流动相,仪器转速为850 r/min,流速为1.5 mL/min,温度为25 ℃,检测波长为280 nm.[结果] 龙胆碱性乙醇提取物经过D151弱酸性阳离子交换树脂富集(20%乙醇洗脱部分),再采用HSCCC技术进行分离纯化,制备得到的98.8%纯度的龙胆碱。[结论] 该方法稳定、回收率高,可高效地从龙胆碱性乙醇提取物中分离龙胆碱。
关键词:  龙胆  龙胆碱  高速逆流色谱
DOI:10.11656/j.issn.1673-9043.2016.01.12
分类号:
基金项目:天津市科技计划资助项目(12TXGCCX03800).
HSCCC separation and purification gentian alkaline ethanol extracts of gentian
SHI Yao, WANG Lin-lin, YU He-shui, LAI Qing-hai, DING Hui, ZHANG Li-juan, SONG Xin-bo
Tianjin University of Traditional Chinese Medicine, Tianjin 300193, China
Abstract:
[Objective] To establish the HSCCC method for separating the gentianine from the alkaline ethanol extracts of gentiana. [Methods] Separation and purification of gentianine by TBE300B HSCCC technology, through the optimization of the solvent system, with n-hexane : ethyl acetate : methanol : water (5:5:4:6) as the solvent system, the upper as stationary phase and the next phase as mobile phase, the rotational speed of the instrument was 850 r/min, the flow rate was 1.5 mL/min, the temperature was 25 ℃, the detection wavelength was 280 nm. [Results] The gentianine was obtained from the gentian alkaline ethanol extracts by D151 cation exchange resin combining with HSCCC, the content was above 98.8%. [Conclusion] The method is stable and has high results, it could be used to separate gentianine efficiently from alkaline ethanol extract of gentiana.
Key words:  Gentiana scabra Bunge  gentianine  HSCCC
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