论文部分内容阅读
目的:建立了常规柱色谱结合高速逆流色谱法(HSCCC)分离纯化波棱瓜子中波棱芴酮的方法。方法:首先采用聚酰胺和硅胶柱色谱富集波棱芴酮,再用HSCCC进行分离制备,HSCCC最佳溶剂体系为石油醚-乙酸乙酯-甲醇-水(4∶9∶6∶8,V/V),上相为固定相,下相为流动相,从200mg富集物中一次分离得到80mg纯度为98.3%的波棱芴酮,所得产物经ESI-MS和NMR鉴定结构。结论:本方法所得产物纯度高,重现性好,适合于波棱芴酮的制备型分离。
OBJECTIVE: To establish a method for the separation and purification of boracic fluorenone from melon seeds by conventional column chromatography and high speed countercurrent chromatography (HSCCC). Methods: Polybene and silica gel column chromatography was used to enrich the wave fluorene ketones and then separated by HSCCC. The best solvent system of HSCCC was petroleum ether-ethyl acetate-methanol-water (4: 9: 6: 8, V / V). The upper phase was stationary phase and the lower phase was mobile phase. 80 mg of bergenofluorenone with purity of 98.3% was separated from 200 mg of concentrate at one time. The structure of the product was identified by ESI-MS and NMR. Conclusion: The product obtained by this method has high purity and good reproducibility. It is suitable for the preparative separation of boracrofluorenone.