正相液相制备色谱分离纯化三七叶甙中人参皂甙单体Rb_3  

Isolation and Purification of Ginsenoide Rb_3 by HPLC Method

作　　者：韩金玉[1] 刘翀[1] 王华[1] 段衍泉[1] 

机构地区：[1]天津大学化工学院教育部绿色合成与转化重点实验室,天津300072

出　　处：《高校化学工程学报》2005年第2期192-196,共5页Journal of Chemical Engineering of Chinese Universities

基　　金：云南省省院省校科技合作项目(00YT06)。

摘　　要：以三七叶甙粗提物为原料,采用大孔吸附树脂法和正相液相制备色谱法建立了分离纯化三七叶甙中人参皂甙单体Rb3的制备工艺.首先采用D-101B大孔吸附树脂对原料进行精制,得到Rb3含量为50%的三七叶甙精制物.进而通过正相液相制备色谱柱(φ80mm×1000mm)分离纯化三七叶甙精制物,通过考察流动相组成、流速和上样量等因素对分离效果的影响,确定了适宜的工艺操作条件:流动相为正丁醇-乙酸乙酯-水溶液[体积比为2:1:1(上层)],流速为35～40mL.min-1,上样量为10g.在该工艺条件下得到了人参皂甙单体Rb3,纯度达95%.本方法简便、分离效率高、重复性好,为人参皂甙类新药的开发奠定了基础.A method combining the preparative macroporous resin adsorption and NP-HPLC (normal-phase high performance liquid chromatography) was developed to separate the individual ginsenoide Rb3 from crude extract of Panax notoginseng folium saponin. The enriched extract with 50% Rb3 was obtained by preparative adsorptive separation on D-101B macroporous resin, and then was further purified by NP-HPLC(φ80 mm×1000 mm). In order to optimize the chromatographic procedure, the influence of mobile phase composition, flow rate and sample load on the separation efficiency was studied experimentally. It is found that the suitable mobile phase and its composition is the upper phase of the mixing solvent of n-butanol-ethyl acetate-water with volumetric ratio of 2:1:1, and under the flow rate of 35-40 mL&middotmin-1 for 10 g sample load, the 95% enriched individual ginsennoide Rb3 can be obtained by NP-HPLC. The result shows that the method proposed is a convenient, high efficient and steady one.

关 键 词：人参皂甙Rb3 正相液相制备色谱 大孔吸附树脂 分离纯化 

分 类 号：TQ028.8[化学工程] Q946.83[生物学—植物学]