Ji Wei, Cui Yulan, Chen Renjuan, Lin Xinren, Zhou Qingxin, Gan Chunji
College of Food Science, Fujian Agriculture and Forestry University, Fuzhou 350002, China.
Se Pu. 2010 Aug;28(8):813-6. doi: 10.3724/sp.j.1123.2010.00813.
Two rotenoids (rotenone and deguelin) were successfully isolated and purified from the roots of Derris by high-speed counter-current chromatography (HSCCC) with a two-phase solvent system composed of n-hexane-ethylacetate-methanol-water (7: 0. 25:5:3, v/v/v/v) on a preparative scale. The lower phase was used as the mobile phase and the upper phase was used as the stationary phase. The revolution speed was 850 r/min, the detection wavelength was set at 254 nm and the flow rate was 2.0 mL/min. Under the optimized conditions, within 2.5 h, 6.4 mg of rotenone with the purity of 96.60% and 23.4 mg of deguelin with the purity of 97.87% were obtained from 50 mg of the crude extract of the roots of Derris in a one-step elution. The results indicate that the rotenone and deguelin with high purities can be obtained by HSCCC, and the established method can provide the basic experimental material for the intensive study of rotenoids.
采用高速逆流色谱法(HSCCC),以正己烷 - 乙酸乙酯 - 甲醇 - 水(7:0.25:5:3,v/v/v/v)组成的两相溶剂系统,在制备规模上成功地从鱼藤根中分离并纯化出两种鱼藤酮类化合物(鱼藤酮和鱼藤素)。下层相用作流动相,上层相用作固定相。转速为850 r/min,检测波长设定为254 nm,流速为2.0 mL/min。在优化条件下,2.5小时内,从50 mg鱼藤根粗提物中一步洗脱得到纯度为96.60%的鱼藤酮6.4 mg和纯度为97.87%的鱼藤素23.4 mg。结果表明,通过高速逆流色谱法可获得高纯度的鱼藤酮和鱼藤素,所建立的方法可为鱼藤酮类化合物的深入研究提供基础实验材料。