制备型高效液相色谱法从牛胆汁中制备牛磺胆酸钠

Preparation of Taurocholate Sodium from Ox Gall by Preparative HPLC

建立了制备型液相色谱法从牛胆汁中制备牛磺胆酸钠。将牛胆汁用75%乙醇浸泡,过滤,经硅胶柱色谱吸附,以二氯甲烷∶甲醇∶水(70∶30∶10)下层洗脱,得到牛磺胆酸钠混合物粗品。采用GRACE Adsorbosphere C18色谱柱分离纯化,以甲醇∶0.4%磷酸二氢钠水溶液(55∶45)为流动相,检测波长205 nm。根据色谱图收集柱后浓度较高的牛磺胆酸流出液,经脱盐和碱化处理后得到牛磺胆酸钠,纯度98.1%,回收率约60%。利用红外、核磁共振等光谱学方法确证结构。

A preparative HPLC method was established for the preparation of taurocholate sodium from ox gall. The ox gall was soaked in 75 % ethanol and then filtered. The filtrate was adsorbed on a silica gel column, and then eluted by the lower layer of dichloromethane ： methanol ： water （70 ： 30 ： 10）. The crude product of taurocholic acid was collected then separated and purified on a GRACE Adsorbosphere C18 column, with the mobile phase of methanol ： 0.4% sodium dihydrogen phosphate solution （55 ： 45）, at the detection wavelength of 205 nm. The high concentration fraction of taurocholic acid was collected according to the chromatogram. After alkalization and desalination, taurocholate sodium with the purity of 98.1% was obtained. The recovery rate was about 60 %. Its structure was identified by infrared spectrum and NMR.