Key Laboratory of Adaptation and Evolution of Plateau Biota, Northwest Institute of Plateau Biology, Chinese Academy of Sciences, Xining 810001, China.
Phytochem Anal. 2013 Feb;24(2):171-5. doi: 10.1002/pca.2397. Epub 2012 Aug 31.
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.
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).
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.
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.
A simple and efficient HSCCC method has been optimised for the preparative separation of stilbene glycosides from Rheum tanguticum Maxim. ex Balf.
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。
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。
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。
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%。
优化了从大黄中分离二苯乙烯苷的简单高效 HSCCC 方法。
