高速逆流色谱分离制备苦茶中的苦茶碱

 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∶〖KG-*2〗5∶〖KG-*2〗4∶〖KG-*2〗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41 mg，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。

Isolation and Preparation of Theacrine by High-Speed Counter-Current Chromatography from Camellia assamica var.kucha

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 13C NMR methods. Theacrine was the first time isolated from Camellia assamica var. kucha by HSCCC, which is a simple, rapid and effective method.