Wei Yun, Xie Qianqian, Ito Yoichiro
Analytical Chemistry Department, Faculty of Sciences, Beijing University of Chemical Technology, 15 Beisanhuan East Road, Chaoyang District, Beijing 100029, P. R. China.
J Liq Chromatogr Relat Technol. 2009 Jan 1;32(7):1010-1022. doi: 10.1080/10826070902790983.
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.
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。