藤黄中藤黄酸B的制备分离方法优选及结构确证

目的建立一种高效且重现性好的藤黄酸B的制备分离方法,并对分离产物进行结构确证。方法采用乙醇超声提取方式对藤黄药材进行初步提取,用中压制备色谱和高压制备色谱相结合的方式对藤黄乙醇提取物中藤黄酸B进行分离和纯化,并采用正交设计对提取和分离工艺进行优化。采用红外光谱、质谱、1 H-核磁共振谱、13C-核磁共振谱对分离得到的样品进行结构鉴定。结果优选的分离方法较其他方法简便且高效可控,分离得到的样品通过结构鉴定,确定为藤黄酸B且纯度可达到99%以上。结论所建立的藤黄酸B的提取分离方法具有高效、简便且重现性好的特点。同时,本研究提供了藤黄酸B相对完整的谱图信息,并确证了所分离藤黄酸B的结构。

Optimization of Extraction and Isolation of Morellic Acid in Garcinia hanburyi and Its Structure Confirmation

Objective To establish an efficient and repeatable method for isolation of morellic acid and to confirm the structure of isolated product. Methods Garcinia hanburyi was subjected to ethanol ultrasonic extraction, and the ethanol extract was treated by a combination of medium-pressure preparative chromatography and high-pressure preparative chromatography to isolate and purify morellic acid. An orthogonal design was used to optimize the extraction and isolation process. Also, infrared spectrometry, mass spectrometry, 1H-nuclear magnetic resonance (NMR), and 13C-NMR were used for the structural identification of isolated sample. Results The optimized isolation method was simple and controllable. The isolated sample was structurally identified as morellic acid with a purity over 99%. Conclusion The established extraction and isolation method for morellic acid is efficient, simple, and repeatable. This study also provides relatively full spectral information on morellic acid and confirms the structure of isolated morellic acid.