大孔树脂柱层析法提取分离紫茎泽兰中β-榄香烯

Separation of β-elemene from Eupatorium adenophorum by Macroporous Resin Column Chromatography

[目的]提取分离恶性杂草植物紫茎泽兰中的β-榄香烯,鉴定其结构并测定含量。[方法]采用"水+乙二醇"蒸馏法从紫茎泽兰中提取挥发油后,分别以硅胶、银离子硅胶、D101大孔树脂和HP20大孔树脂作为层析介质,采用柱层析法从挥发油中分离得到β-榄香烯,对其分离效果进行鉴定,并用HPLC制备得到β-榄香烯纯品,通过IR、1H NMR、13C NMR和HRMS对其分子结构进行确认。[结果]紫茎泽兰挥发油中β-榄香烯的最佳分离方法为HP20大孔树脂层析法,所分离的主体产品的纯度可达63.1%,产率可达75.6%;经过"水+乙二醇"蒸馏、HP20大孔树脂柱层析和HPLC制备,紫茎泽兰干燥样品中提取分离得到的β-榄香烯的纯度为98.6%,总产率为36.5%。[结论]HP20大孔树脂层析法具有成本低廉、操作简便等优点,是紫茎泽兰挥发油中β-榄香烯的最佳分离方法。

[Objective] To extract β-elemene from worst weed Eupatorium adenophorum Spreng,identify its structure and determine its content.[Method] Having obtained volatile oil from E.adenophorum by ＂water＋ glycol＂ distillation,β-elemene was separated by column chromatography with slica,silver nitrate modified slica,D101 and HP20 macroporous resin respectively.The pure product of β-elemene was prepared by HPLC,and its molecular structure was validated by UV,IR,1H NMR,13C NMR and HRMS.[Result] The purity and yield of product was up to 63.1% and 75.6% respectively if using HP20 column chromatography,the optimal one for separation of β-elemene from E.adenophorum.Through three steps of ＂water＋ glycol＂ distillation,HP20 column chromatography and HPLC preparation,the β-elemene product with 98.6% purity and 36.5% yield could be obtained from E.adenophorum.[Conclusion] HP20 column chromatography is the most efficient way to separate β-elemene from E.adenophorum,which has the advantages of low cost and easy operation.