论文部分内容阅读
葛根素是葛根中黄酮类物质主要活性成分,该研究以葛根素粗品为原料,利用廉价易得的琼脂制备琼脂凝胶微球键合β-环糊精分离介质(AG-β-CD),结合AB-8大孔树脂进行前处理,以高回收率分离纯化得到高纯度的葛根素。以葛根素纯度和回收率以及相关杂质的色谱纯度为考察指标,对4种不同性质的大孔树脂ADS-7(强极性)、ADS-17(中极性)、ADS-21(极性)和AB-8(弱极性)进行分离效果筛选以及工艺优化,并对AG-β-CD纯化工艺优化和验证。结果表明,优选弱极性树脂AB-8作为葛根素粗品的前处理树脂效果最佳,通过8%乙醇洗脱15 BV后,葛根素纯度为87.68%的回收率达到89.66%;通过琼脂凝胶微球键合β-环糊精分离介质进行纯化,流动相15%乙醇,承载量(上样量与柱体积之比)1.33 g·L~(-1),上样浓度8 g·L~(-1),流速1 m L·min~(-1)时,葛根素纯度高于95%的回收率达到97%以上。
Puerarin is the main active ingredient of flavonoids in Pueraria lobata. In this study, the crude puerarin was used as raw material to prepare β-cyclodextrin-separating medium (AG-β-CD) Combined with AB-8 macroporous resin pretreatment, with high recovery of isolated and purified to obtain high-purity puerarin. According to the purity and recovery of puerarin and the chromatographic purity of the related impurities, four kinds of macroporous resin ADS-7 (strong polarity), ADS-17 (medium polarity), ADS-21 ) And AB-8 (weak polarity) to screen for separation effects and process optimization, and to optimize and validate the AG-β-CD purification process. The results showed that AB-8, a weakly polar resin, was the best pretreated resin for crude puerarin. After 15 BV was eluted with 8% ethanol, the recovery of puerarin reached 87.68% with a recovery of 89.66% Cyclosporine and β-cyclodextrin were separated and purified by mobile phase. The mobile phase consisted of 15% ethanol with the loading of 1.33 g · L -1 and loading concentration of 8 g · L ~ (-1), the recovery of puerarin with the purity higher than 95% reached more than 97% when the flow rate was 1 m L · min -1.