摘要
目的:利用β-葡萄糖苷酶催化水解杜仲主要降压活性成分松脂醇二葡萄糖苷(PDG),制备其苷元(PDG-A)。方法:对水解反应时间、p H及温度等条件进行优化,并采用液相质谱联用和核磁共振波谱等手段对产物进行结构解析。结果:β-葡萄糖苷酶水解PDG的最佳条件为:水解时间6h,水解p H5,水解温度50℃,三次实验的PDG-A收率分别为98.52%、97.91%、98.69%;PDG的水解产物为PDG(M=682)水解掉2个葡萄糖基团(M=162)而成的苷元结构(M=358),结合1HNMR及13C-NMR确定其为苷元PDG-A。结论:β-葡萄糖苷酶催化水解PDG制备其苷元PDG-A的反应温和、转化率98%以上,此方法可以为大规模制备PDG-A提供理论指导。
Objective:Usingβ-glucosidase to prepare pinoresinol diglucoside aglycone(PDG-a)from pinoresinol diglucoside(PDG),an antihypertensive active components of Eucommia ulmoides Oliv.Methods:The reaction time,p H and temperature of the hydrolysis were optimized,and the structure of the product was analyzed by liquid mass spectrometry and NMR.Results:the optimal conditions of PDG hydrolysis byβ-glucosidase were as follows:hydrolysis time 6.17 h,hydrolysis p H 5.03,hydrolysis temperature 49℃.The hydrolysis rates of the three validation experiments were 98.52%,97.91%and 98.69%,respectively,which were consistent with the predicted value 98.72%.PDG(M=682)hydrolyzed two glucose groups(M=162)to form aglycone structure(M=358),which was identified as the aglycone of PDG by1 H-NMR and13 C-NMR.Conclusion:β-glucosidase can catalyze the hydrolysis of PDG into PDG-A with mild reaction and over 98%conversion rate.This method can provide theoretical guidance for large-scale preparation of PDG-A.
作者
刘洋
付冬梅
张良
张琳
祖元刚
Liu Yang(College of Forestry,Northeast Forestry University,Harbin Heilongjiang 150040)
出处
《黑龙江医药》
CAS
2021年第1期5-9,共5页
Heilongjiang Medicine journal
基金
中央高校基本科研业务费专项资金(编号:2572015CA06)
林业公益性行业科研专项(编号:201504701-205)。
