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作 者:程悦[1] 严志勇[1] 卢嘉丽[1] 叶创兴[2] 王冬梅[1]
机构地区:[1]中山大学药学院,广东广州510006 [2]中山大学生命科学学院,广东广州510275
出 处:《中山大学学报(自然科学版)》2010年第3期65-69,共5页Acta Scientiarum Naturalium Universitatis Sunyatseni
基 金:中山大学张宏达科学研究基金资助项目
摘 要:应用高速逆流色谱法分离制备了苦茶中的苦茶碱。以正己烷-二氯甲烷-甲醇-水(体积比为1∶5∶4∶2)为两相溶剂系统,在主机转速800 r/min、流速2.0 mL/min、检测波长278 nm条件下进行分离制备。所得流分经高效液相色谱法检测,与对照品进行比较,并通过质谱、核磁共振氢谱、碳谱鉴定化合物的结构。结果表明,从2.22 g苦茶总生物碱提取物中分离得到了3个化合物,分别为可可碱5 mg,苦茶碱389 mg,咖啡碱41mg,纯度均在99%以上,系首次采用高速逆流色谱法对苦茶中的苦茶碱进行分离。该法具有简便、快速的优点。Theacrine was prepared,isolated and purified from Camellia assamica var.kucha by high-speed counter-current chromatography.A two-phase solvent system composed of hexane-dichloromethane-methanol-water(1∶5∶4∶2,v/v/v/v) was selected with comprehensive analysis of the settling time,the ratio of up and down phase's volume and the K value.Five mg of theobromine,389 mg of theacrine and 41 mg of caffeine with their purities over 99% were obtained from 2.22 g of the crude extract of Camellia assamica var.kucha under the condition of a flow rate of 2.0 mL/min,800 r/min and the detection wavelength of 278 nm.The obtained fractions were analyzed by high perform liquid chromatography,compared with standard substance and identified by MS,1H NMR and 13C NMR methods.Theacrine was the first time isolated from Camellia assamica var.kucha by HSCCC,which is a simple,rapid and effective method.
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