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目的:建立杉寄生药材中鞣花酸和3,3’-二甲氧基鞣花酸的提取分离及含量测定方法。方法:采用溶剂提取、硅胶柱色谱和重结晶等提取分离手段得到酚性化合物鞣花酸和3,3’-二甲氧基鞣花酸;建立其HPLC含量测定方法:采用Eclipse XDB-C18色谱柱(4.6 mm×250 mm,5μm),流动相甲醇-0.2%磷酸水溶液(47∶53),流速0.8 m L·min-1,检测波长254 nm,柱温25℃。结果:鞣花酸在0.030 6~0.551 2μg与峰面积呈良好的线性关系(r=0.999 8),平均回收率为101.25%,RSD0.9%;3,3’-二甲氧基鞣花酸在0.018 9~0.339 5μg与其峰面积呈良好的线性关系(r=0.999 8),平均回收率101.34%,RSD1.5%。结论:鞣花酸和3,3’-二甲氧基鞣花酸为首次从杉寄生药材中分得,并建立了其HPLC含量测定方法,该方法简便、快速、具有较好的稳定性和重复性,可用于上述2种化合物含量同时测定。
OBJECTIVE: To establish a method for the extraction, separation and determination of ellagic acid and 3,3’-dimethoxy-ellagic acid in Chinese fir parasiticus. Methods: Phenolic compounds ellagic acid and 3,3’-dimethoxy-ellagic acid were obtained by solvent extraction, silica gel column chromatography and recrystallization. HPLC method was established for the determination of its content by Eclipse XDB-C18 Column (4.6 mm × 250 mm, 5 μm), mobile phase methanol-0.2% phosphoric acid (47:53), flow rate 0.8 m L · min-1 and detection wavelength 254 nm at 25 ℃. Results: The ellagic acid showed a good linear relationship (r = 0.999 8) with the peak area of 0.030 6 ~ 0.551 2, the average recovery was 101.25% and the RSD was 0.9%. The ellagic acid In the range of 0.018 9 ~ 0.339 5μg and its peak area showed a good linear relationship (r = 0.999 8), the average recovery rate of 101.34%, RSD1.5%. CONCLUSION: Ellagic acid and 3,3’-dimethoxy-ellagic acid were separated from Cunninghamia lanceolata for the first time and their HPLC method was established. The method is simple, rapid and has good stability. Repeatability, can be used for simultaneous determination of the above two compounds.