制备色谱法分离纯化高良姜黄酮中高良姜素和山柰素

摘要

建立了制备型高效液相色谱（ Prep-HPLC）分离高良姜黄酮中高良姜素和山柰素的方法。高良姜黄酮经HPD-600树脂吸附洗脱纯化后，采用 Prep-HPLC分离高良姜黄酮中高良姜素和山柰素。制备色谱条件：流动相为甲醇-0.6％（v／v）乙酸水溶液（58∶42，v／v），柱温为常温，流速为7.0 mL／min，检测波长为360 nm，进样量为700μL，上样质量浓度为10.0 g／L。分离的单体由质谱和核磁共振氢谱、碳谱鉴定确证为高良姜素和山柰素，HPLC 外标法定量，纯度分别为99.5％和99.7％。该方法分离效果好、高效、低毒，可用于高良姜中高良姜素和山柰素的分离制备。%A method of the preparation of galangin and kaempferide from Alpinia officinarum Hance flavonoids using preparative high-performance liquid chromatography( Prep-HPLC)was established. After the Alpinia officinarum Hance flavonoids was purified by HPD-600 resin-based column chromatography,the flavonoid components were separated by Prep-HPLC on a Venusil XBP-C18 column(250 mm×21 mm,5. 0 μm). The mixture of methanol and 0. 6%(v/v)acetic acid solution(58∶42,v/v)was used as mobile phase at a flow rate of 7. 0 mL/min. The sample volume was 700 μL and the UV detection wavelength was 360 nm. With MS and NMR,the structures of component I and component II of the Alpinia officinarum Hance fla-vonoids were identified. The average relative molecular mass of the component I was 269,the same as galangin;and that of the component II was 299,the same as kaempferide. HPLC analy-sis showed that the purities of galangin and kaempferide were 99. 5% and 99. 7% respectively. The method is simple and of low toxicity. It can be applied to the separation and preparation of galangin and kaempferide.