高纯鬼臼毒素制备新工艺

以桃儿七为原料 ,甲醇作溶剂 ,70℃回流提取 3次 ,每次 2h。所得浸膏 ,用苯在 80℃加热回流溶解 ,过滤、浓缩、放置结晶 ,得浅黄色粗品。用无水乙醇溶解粗品 ,经活性炭脱色后 ,浓缩成树脂状 ,用苯悬浮溶解 ,弃去不溶物。采用二步结晶法 ,先用苯作溶剂 ,除去绝大部分杂质后 ,再用苯 乙醇〔V(苯 )∶V(乙醇 ) =2∶1〕为溶剂 ,重结晶 ,得白色针状溶剂加合物结晶 (熔点 92～ 93℃ ) ,12 5℃烘干 2h ,脱去溶剂分子后 ,即得精品鬼臼毒素 ,其质量分数 >96 % ,产率为 1 7%

A New Technology for Preparing Podophyllotoxin of High Purity

For perparation of podophyllotoxin of high purity from sinopodophyllum emodi Wall.by handy way,techniques of separation and purification of podophyllotoxin were studied.The raw material which was the smashed root of sinopodophyllum emodi Wall.was extracted under reflux 3 times (2 h each time) at 70 ℃ with methanol.After the raffinate was concentrated into extract,it was dissolved at 80 ℃ by refluxing with benzene and filtered.The concentrated filtered liquor was put for crystallization.The light yellow crude product was filtered and dissloved in absolute alcohol.After decoloration the solution was concentrated into resinous substance,which was suspended in benzene and the isoluble substances were discarded.Two step crystallization method was used.At the first step,benzene was used as solvent and most impurity was separated.At the second step,using benzene absolute alcohol 〔 V (C\-6H\-6)∶ V (CH\-3CH\-2OH)=2∶1〕 as solvent,white needles were obtained.The needles were transformed into refined podophyllotoxin by oven drying for 2 h at 125 ℃.Mass percentage of podophyllotoxin in the refined product was>96% and the total yield was 1 7%.