杜仲中木脂素类化合物纯化工艺研究

Separation and Purification of the Liganas from Eucommia Ulmoide Oliver

对杜仲中木脂素类化合物松脂醇二葡萄糖甙(PDG)和丁香脂素二葡萄糖甙(SDG)进行分离纯化工艺研究。首先采用溶剂萃取法进行一次纯化,再采用大孔吸附树脂优化纯化工艺,最后采用硅胶柱色谱法同时分离、纯化杜仲中松脂醇二葡萄糖甙和丁香脂素二葡萄糖甙,采用反相高效液相色谱法跟踪检测纯度。纯化后得到两种晶体,经过UV、IR、MS和1HNMR定性分析确定为松脂醇二葡萄糖甙和丁香脂素二葡萄糖甙,其纯度分别为90.86%和91.73%,回收率分别为42.14%和47.17%。该纯化方法能获得高纯度的松脂醇二葡萄糖甙和丁香脂素二葡萄糖甙,操作简单、成本低。

A method for separation and purification of the lignans——pinoresinol diglucoside and syringaresinol diglucoside in Eucommia Ulmoide Oliver with solvent extraction-macroporous adsorption resin-silica gel column chromatography was established. Solvent extraction was choosen as the first purification. Then, the purification of S-8 macroporous adsorption resin was studied. The silica gel column chromatography was used to obtain two monomers of pinoresinol diglucoside and syringaresinol diglucoside. The purity of the product was deternmined by RP-HPLC detection. The two crystals were identified as PDG and SDG by UV,IR,MS and ^1H NMR. Their purity were 90.86% and 91.73%, and their recovery were 42.14% and 47.17% respectively. The high purity monomers of PDG and SDG can be obtained by this method, which is simple and of low cost.