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作 者:田梦凡 高青青 易雅丽 国大亮[1] 刘玉璇[1] TIAN Mengfan;GAO Qingqing;YI Yali;GUO Daliang;LIU Yuxuan(Tianjin University of Traditional Chinese Medicine,Tianjin 301617,China)
机构地区:[1]天津中医药大学,天津301617
出 处:《中医药导报》2024年第2期53-58,共6页Guiding Journal of Traditional Chinese Medicine and Pharmacy
基 金:河北省重点研发计划项目(19227115D)。
摘 要:目的:优化超声辅助酶提取天麻中天麻素工艺并通过双水相萃取和大孔树脂进一步纯化,为精制天麻素提供工艺参考。方法:通过单因素试验考察和正交优化试验得到最佳超声辅助酶提取条件。通过双水相工艺考察得到最佳双水相萃取条件。通过大孔树脂工艺考察对大孔树脂型号进行筛选,对上样条件、洗脱条件进行优化。结果:超声辅助酶提取选择α-淀粉酶,最佳提取条件设定为料液比为1∶30,加酶量为0.8%,酶解时间为80 min,酶解温度为60℃,酶解pH值为5.5。最佳双水相萃取条件设定为乙醇体积分数为47.5%,硫酸铵质量分数为15.0%,萃取液浓度为0.2 g/mL,大孔树脂筛选型号为HPD100,最佳上样浓度为0.2 g/mL,径高比为1∶5,上样流速为3 BV/h,上样量为100 mL,最佳洗脱液体积分数为30.0%,洗脱流速为4 BV/h,洗脱液用量为230 mL。结论:本研究对超声辅助酶提取工艺优化结果较好,采用双水相体系和大孔树脂纯化,使天麻素纯度明显提高。且这一系列工艺稳定可靠,可为后续制剂及新药研发奠定基础。Objective:To optimize the ultrasonic-assisted enzyme extraction of gastrodin from Tianma(Gastrodia elata)and further purify it according to aqueous two-phase extraction system and macroporous resin,so as to provide process reference for refining high-purity gastrodin.Methods:The optimum conditions of ultrasonic-assisted enzyme extraction were obtained by single factor and orthogonal optimization.The optimum conditions of aqueous two-phase extraction were obtained by drawing the two-phase diagram and process investigation.The optimum conditions of macroporous resin were obtained by process investigation,with optimization of loading and elution conditions.Results:The appropriate conditions wereα-amylase enzymes,1:30 of feed liquid,0.8%of enzymatic quantity,80 min of enzymolysis time,60℃of enzymolysis temperature,and pH 5.5 for enzyme solution.The optimal conditions for aqueous two-phase extraction were ethanol volume fraction of 47.5%,ammonium sulfate mass fraction of 15.0%,extraction liquid concentration of 0.2 g/mL,and suitable for macroporous resin screening as HPD100.The optimal sampling conditions were sampling concentration of 0.2 g/mL,with diameter to height ratio of 1:5.The loading flow rate was 3 BV/h,and the loading volume was 100 mL.The optimal elution condition was the integral number of elution liquid 30.0%,with the elution flow rate of 4 BV/h,and the elution volume was 230 mL.Conclusion:In this study,the optimization results of the ultrasonic-assisted enzyme extraction process were good.The purity of gastrodin was greatly improved by aqueous two-phase system and macroporous resin purification.And this series of processes is stable and reliable,laying the foundation for subsequent preparations and new drug research and development.
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