大孔树脂法分离纯化胆木中短小蛇根草苷

目的:考察不同型号大孔树脂分离纯化胆木提取液中短小蛇根草苷(Pum iloside,PML)的工艺条件及参数。方法:采用水煎法提取,HPLC法测定含量;以静态饱和吸附量、洗脱量、洗脱率为指标比较5种大孔树脂,并对AB-8树脂的吸附容量、洗脱溶剂、洗脱体积进行筛选;采用甲醇重结晶法纯化PML,并用波谱方法鉴定其化学结构。结果:5种树脂中,AB-8型树脂具有较好的吸附及洗脱参数,对PML的吸附容量为2.44 mg/g干树脂。适宜的工艺条件为:6倍柱体积蒸馏水洗脱后,再用4倍柱体积的30%乙醇以2 BV/h的流速洗脱,减压回收溶剂后过滤,沉淀甲醇重结晶。PML得率为75.1%,纯度>99.5%。结论:AB-8树脂附性能良好,适合胆木中PML的分离纯化。

Studies on the Separation and Purificaton of Pumiloside from Nauclea officinalis by Macroreticular Resin

Objective: To investigate the technological parameters and the process for separation and purification of pumiloside(PML) from Nauclea officinalis Pierrc ex Pitard by macroreticular resin.Methods: PML was extracted by hot water,and the content of PML was determinated by HPLC method.The static capacity absorption,static elution ratios of five types of resin were studied respectively,and were compared to evaluate their absorption and desorption effect to PML.And then the absorption capacity,elution solution and elution volume of the AB-8 resin were researched to set up the optimum separation process for PML.Finally, PML was recrysallized from MeOH and identified by spectra analysis.Results: The AB8 resin had the best absorptive and separative properties to PML.The dynamic absorption ratio was 2.44 mg/g.The applicable process was as follows: the water extracted solution of Nauclea officinalis flow through the resin column repeatedly,after being eluted with 6BV of distilled water,the resin column was eluted with 4BV 30% ethanol,the 30% ethanol fraction was combined and the solvent was recovered in vacuum.The precipitation was filtered and recrysallized from MeOH to give pure PML.The yield of PML was 75.1%,and the product purity was up to 99.5%.Conclusion: AB-8 resin shows better comprehensive absorption property. It can be used for separation and purification of PML from Nauclea officinalis successfully.