高速逆流色谱法从藏药唐古特大黄中分离制备三种二苯乙烯苷。
Preparative isolation and purification of three stilbene glycosides from the tibetan medicinal plant Rheum tanguticum maxim. Ex Balf. by high-speed counter-current chromatography.
机构信息
Key Laboratory of Adaptation and Evolution of Plateau Biota, Northwest Institute of Plateau Biology, Chinese Academy of Sciences, Xining 810001, China.
出版信息
Phytochem Anal. 2013 Feb;24(2):171-5. doi: 10.1002/pca.2397. Epub 2012 Aug 31.
INTRODUCTION
Stilbene glycosides are the primary constituents of Rheum tanguticum Maxim. ex Balf., to which different bioactivities has been attributed, including: anti-HIV, anti-oxidant, anti-tumour, anti-malarial, and anti-allergy activity. However, effective methods for the isolation and purification of stilbene glycosides, such as trans-rhapontin, cis-rhapontin and trans-desoxyrhaponticin, from this herb are not currently available.
OBJECTIVE
To develop an efficient method for the preparative isolation and purification of three stilbene glycosides from Rheum tanguticum Maxim. ex Balf. via high-speed counter-current chromatography (HSCCC).
METHODS
A solvent system composed of chloroform:n-butanol:methanol:water (4:1:3:2, v/v/v/v) was developed for the separation. The upper phase was used as the stationary phase, and the lower phase was used as the mobile phase. The flow rate was 1.8 mL/min. The apparatus was controlled at 800 rpm and 25 °C, and the effluent was monitored at 280 nm. Chemical constituents were analysed by high-performance liquid chromatography (HPLC), and their structures were identified by ¹H- and ¹³C-NMR.
RESULTS
Under the optimised conditions, 25.5 mg trans-rhapontin, 16.0 mg cis-rhapontin and 20.5 mg trans-desoxyrhaponticin were separated from 80 mg crude sample; the isolates had purities of 99.6, 97.2 and 99.2%, respectively.
CONCLUSION
A simple and efficient HSCCC method has been optimised for the preparative separation of stilbene glycosides from Rheum tanguticum Maxim. ex Balf.
简介
二苯乙烯苷是大黄（Rheum tanguticum Maxim. ex Balf.）的主要成分，具有多种生物活性，包括抗 HIV、抗氧化、抗肿瘤、抗疟疾和抗过敏活性。然而，从该植物中分离和纯化二苯乙烯苷（如反式白藜芦醇苷、顺式白藜芦醇苷和反式去氧白藜芦醇苷）的有效方法目前尚未报道。
目的
建立一种高效的高速逆流色谱（HSCCC）法，从大黄中分离和纯化三种二苯乙烯苷。
方法
开发了一种由氯仿：正丁醇：甲醇：水（4:1:3:2，v/v/v/v）组成的溶剂体系用于分离。上相为固定相，下相为流动相。流速为 1.8mL/min。仪器控制在 800rpm 和 25°C，流出液在 280nm 处监测。采用高效液相色谱（HPLC）分析化学成分，并用 ¹H-和 ¹³C-NMR 鉴定其结构。
结果
在优化条件下，从 80mg 粗样品中分离出 25.5mg 反式白藜芦醇苷、16.0mg 顺式白藜芦醇苷和 20.5mg 反式去氧白藜芦醇苷；分离物的纯度分别为 99.6%、97.2%和 99.2%。
结论
优化了从大黄中分离二苯乙烯苷的简单高效 HSCCC 方法。
Zotero 插件