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高速逆流色谱法从植物提取物中制备分离轴花素-3-葡萄糖苷、金丝桃苷和苦杏仁苷

PREPARATIVE SEPARATION OF AXIFOLIN-3-GLUCOSIDE, HYPEROSIDE AND AMYGDALIN FROM PLANT EXTRACTS BY HIGH-SPEED COUNTERCURRENT CHROMATOGRAPHY.

作者信息

Wei Yun, Xie Qianqian, Ito Yoichiro

机构信息

Analytical Chemistry Department, Faculty of Sciences, Beijing University of Chemical Technology, 15 Beisanhuan East Road, Chaoyang District, Beijing 100029, P. R. China.

出版信息

J Liq Chromatogr Relat Technol. 2009 Jan 1;32(7):1010-1022. doi: 10.1080/10826070902790983.

Abstract

High-speed countercurrent chromatography (HSCCC) was successfully used to isolate three bioactive compounds, i.e., amygdalin from bitter almond and taxifolin-3-glucoside and quercetin-3-galactoside (hyperoside) from water extract of Agrimonia pilosa Ledeb, respectively. From 1 g of the crude extract 65 mg of amygdalin was isolated at 97% purity using a two-phase solvent system composed of ethyl acetate-n-butanol-water (5:2:5, v/v) by preparative HSCCC. From a 400 mg amount of crude extract of Agrimonia pilosa Ledeb, 11 mg of taxifolin-3-glucoside and 8 mg of hyperoside were isolated at 96% purity using a two-phase solvent system composed of ethyl acetate-methanol-water (25:1:25, v/v) similarly by preparative HSCCC. The final structural identification was performed by MS, (1)H-NMR and (13)C-NMR Spectra.

摘要

高速逆流色谱法(HSCCC)成功用于分离三种生物活性化合物,即分别从苦杏仁中分离出苦杏仁苷,从龙牙草水提取物中分离出 taxifolin - 3 - 葡萄糖苷和槲皮素 - 3 - 半乳糖苷(金丝桃苷)。通过制备型HSCCC,使用由乙酸乙酯 - 正丁醇 - 水(5:2:5,v/v)组成的两相溶剂系统,从1 g粗提取物中分离出65 mg纯度为97%的苦杏仁苷。同样通过制备型HSCCC,使用由乙酸乙酯 - 甲醇 - 水(25:1:25,v/v)组成的两相溶剂系统,从400 mg龙牙草粗提取物中分离出11 mg纯度为96%的taxifolin - 3 - 葡萄糖苷和8 mg纯度为96%的金丝桃苷。最终的结构鉴定通过质谱、¹H - NMR和¹³C - NMR光谱进行。

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