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建立了虎杖药渣中白藜芦醇的含量测定方法和提取纯化工艺。以白藜芦醇含量为评价指标,采用正交试验优化提取工艺。以大孔吸附树脂、柱色谱及重结晶法分离并纯化提取物浸膏中的白藜芦醇。结果表明,最佳提取工艺为虎杖药渣用90%乙醇加热至85℃回流提取3次,每次料液比均为1∶10,提取时间分别为1.5、1和0.5 h。所得提取物浸膏用水溶解后经D101型大孔吸附树脂吸附富集、硅胶柱色谱纯化和丙酮重结晶,可获得纯度达99%的白藜芦醇。
A method for determination of resveratrol in Polygonum cuspidatum and extraction and purification process were established. Using resveratrol as evaluation index, the orthogonal experiment was used to optimize the extraction process. Resveratrol in extract extract was isolated and purified by macroporous adsorption resin, column chromatography and recrystallization. The results showed that the best extraction process was that Polygonum cuspidatum residue was heated to 85 ℃ with 90% ethanol for 3 times and refluxed for 3 times, the ratio of material to liquid was 1:10 and the extraction time was 1.5, 1 and 0.5 h respectively. The obtained extract was dissolved in water and adsorbed on D101 macroporous resin, purified by silica gel column chromatography and recrystallized from acetone to obtain resveratrol with a purity of 99%.