Jin Wei, Tu Peng-Fei
School of Pharmaceutical Sciences, Peking University Health Science Center, Department of Natural Medicine, No. 38, Xueyuan Road, Beijing 100083, China.
J Chromatogr A. 2005 Oct 28;1092(2):241-5. doi: 10.1016/j.chroma.2005.08.009.
Preparative high-speed counter-current chromatography (HSCCC) was successfully used for isolation and purification of trans-3,5,4'-trihydroxystilbene-4'-O-beta-D-glucopyranoside (compound 1) and (+)catechin (compound 2) from Rheum tanguticum Maxim. ex Balf. by stepwise elution with a pair of two-phase solvent system composed of ethyl acetate-ethanol-water (25:1:25, v/v) and (5:1:5, v/v), and stepwise increasing the flow-rate of the mobile phase from 0.8 to 2.0 mlmin(-1) after 5 h. The preparative HSCCC separation was performed on 250 mg of crude extract yielding pure compound 1 (10.2 mg) and compound 2 (26.7 mg) all at purities of over 96% in a single run. The structures of the two compounds have been elucidated by means of spectroscopic methods including MS and 1H, 13C nuclear magnetic resonance spectroscopy.
制备型高速逆流色谱（HSCCC）成功用于从唐古特大黄中分离纯化反式-3,5,4'-三羟基二苯乙烯-4'-O-β-D-吡喃葡萄糖苷（化合物1）和（+）儿茶素（化合物2），采用由乙酸乙酯-乙醇-水（25:1:25，v/v）和（5:1:5，v/v）组成的两相溶剂系统进行梯度洗脱，并在5小时后将流动相流速从0.8逐步增加至2.0 mlmin⁻¹。在250 mg粗提取物上进行制备型HSCCC分离，单次运行即可得到纯度超过96%的纯化合物1（10.2 mg）和化合物2（26.7 mg）。通过包括质谱以及¹H、¹³C核磁共振光谱在内的光谱方法阐明了这两种化合物的结构。
