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超临界CO2萃取-柱色谱分离联用制备冬凌草甲素新工艺的研究
New method for preparing oridonin by supercritical CO2 fluid extraction and column chromatography
【摘要】 目的建立冬凌草甲素的提取和分离新工艺。方法用正交实验优化超临界CO2萃取冬凌草甲素的工艺条件,并进行 中试放大实验,用HPLC测定冬凌草甲素的含量。将萃取所得产物用硅胶柱色谱进一步分离,用红外光谱,紫外光谱和核磁共 振光谱等手段鉴定所得结晶。结果超临界CO2萃取的最佳工艺务件为压力38.5 MPa,温度40℃,夹带剂用量1.5 mL·g-1。 柱色谱进一步分离可制备高纯度冬凌草甲素。结论超临界CO2萃取与柱色谱分离技术联用使冬凌草甲素的制备工艺大大 简化,效果理想,可向工业化方向发展。
【Abstract】 OBJECTIVE To establish a new method for the extraction and separation of oridonin.METHODS Orthogonal experiment was applied to optimize the process parameters of the supercritical CO2 fluid extraction. The extraction was analyzed by HPLC, and was separated by column chromatography ulteriorly. The crystal was identified by IR spectrum, UV spectrum, NMR,et al.RESULTS The optimized conditions were as follows: pressure 38.5 MPa, temperature 40℃, modifier 1.5 mL·g-1. Oridonin was purified by the further separation of column chromatography. CONCLUSION Supercritical CO2 fluid extraction follows by column chromatography simplified the preparation of oridonin. The investigation are satisfied and provids a new thought for the industrial production of oridonin.
【Key words】 supercritical CO2 fluid extraction; orthogonal experiment; oridonin; column chromatography;
- 【文献出处】 中国药学杂志 ,Chinese Pharmaceutical Journal , 编辑部邮箱 ,2005年23期
- 【分类号】TQ461
- 【被引频次】22
- 【下载频次】416