应用高速逆流色谱一次性分离白豆蔻中5-羟基-3,7,4'-三甲氧基黄酮

One step separation of 5-hydroxy-3,7,4′-trimethoxyflavone in Amomum kravanh Pierre ex Gagnep by HSCCC

目的研究高速逆流色谱分离白豆蔻中黄酮醇类活性成分的方法。方法利用高速逆流色谱技术,采用正己烷-乙酸乙酯-甲醇-水作为两相溶剂系统,上相为固定相,下相为流动相,转速为900 r/min,体积流量为1.2 mL/min。结果一次性从白豆蔻黄酮醇类物质中分离得到5-羟基-3,7,4'-三甲氧基黄酮。通过EI-MS、1H-NMR和13C-NMR鉴定,HPLC检测分析,纯度达98%以上。结论利用高速逆流色谱技术可从白豆蔻中分离制备5-羟基-3,7,4'-三甲氧基黄酮,分离度好,产物纯度较高。

AIM To research separating the active component in Amonum kravanh Pierre ex Gagnep by high speed counter current chromatography（HSCCC）.METHODS 5-hydroxy-3,7,4′-trimethoxyflavone,one flavonol component of A.kravanh Pierre ex Gagnep,was one step separated by HSCCC.The solvents system used for HSCCC was composed of hexane-ethyl acetate-methanol-water（4∶4∶8∶4,v/v）,with a rotation speed at 900 r/min and a flow rate at 1.2 mL/min.And,the upper layer was used as the stationary phase,the sublayer was used as the mobile phase.RESULTS The chemical composition was confirmed by EI-MS,1H-NMR and 13C-NMR and its purity was analyzed by HPLC which was as high as 98%or above.CONCLUSION 5-hydroxy-3,7,4′-trimethoxyflavone is fit to be separated and prepared by HSCCC with good resolution and high purity.