高速逆流色谱分离鬼臼中六个鬼臼毒素类化合物及其结构鉴定

采用制备型高速逆流色谱对鬼臼中鬼臼毒素类成分进行分离纯化。实验经优化获得的分离条件为：先用正己烷-乙酸乙酯-甲醇-水（2∶3.5∶2∶3.5,V/V）上相为固定相,下相为流动相洗脱48分钟后,换用正己烷-乙酸乙酯-甲醇-水（4∶5∶4∶5,V/V）下相进行洗脱;转速为1200r/min;流速为50mL/min;进样体积50mL;进样浓度20mg/mL;共收集到六种高纯度化合物,经鉴定为鬼臼毒素、山荷叶素、4’-去甲基鬼臼毒素、异苦鬼臼毒酮、4’-去甲基去氢鬼臼毒素和去氢鬼臼毒素。

Separation and Purification of Podophyllotoxin Lignans from the Chinese Herbal Medicine Dysosma Versipellis(Hance)M.Cheng by High Speed Counter-Current Chromatography

Preparative separation of podophyllotoxin lignans in Dysosma versipellis（Hance）M.Cheng was conducted by high speed counter-current chromatography（HSCCC）with a pair of two solvent systems consisting of n-hexane-ethyl acetate-methanol-water（2∶3.5∶2∶3.5,V/V）and（4∶5∶4∶5,V/V）.The optimized separation conditions were as follows：the upper phase of n-hexane-ethyl acetate-methanolwater（2∶3.5∶2∶3.5,V/V）was used as stationary phase,the lower phase was used as mobile phase at the first 48min,then the lower phase of n-hexane-ethyl acetate-methanol-water（4∶5∶4∶5,V/V）was used as mobile phase;rotation speed is 1200rpm;the flow rate is 50mL/min;sample volume is 50mL;sample concentration is 20mg/mL.Six compounds with high purity were collected and identified as podophyllotoxin,diphyllin,4′-demethylpodophyllotoxin,isopicropodophyllone,dehydropodophyllotoxin,4′demethyldehydropodophyllotoxin.