离子液体固载型大孔树脂富集刺五加中异嗪皮啶的研究  

Study on the enrichment of isoxaziridin from Acanthopanax senticosus by macroporous resin immobilized with ionic liquid

作　　者：马春慧[1] 罗一贵 李俊含 黄永鑫 姜宁 郭文琪 MA Chunhui;LUO Yigui;LI Junhan;HUANG Yongxin;JIANG Ning;GUO Wenqi(Material Science and Engineering College,Northeast Forestry University,Harbin 150040,China)

机构地区：[1]东北林业大学材料科学与工程学院,哈尔滨150040

出　　处：《林业工程学报》2021年第6期117-122,共6页Journal of Forestry Engineering

基　　金：中央高校基本科研业务费专项资金(2572019BB02);东北林业大学大学生创新训练项目(201910225286)。

摘　　要：采用聚合法将多种离子液体固载于AB-8大孔吸附树脂表面,利用离子液体的酸碱性对刺五加根茎中的刺五加苷B1进行水解,并利用大孔树脂的孔结构吸附水解产物异嗪皮啶,再选择合适的溶剂进行洗脱,水解与富集一步完成。结果表明:在氮气环境下将氯甲基化的大孔树脂与不同质量分数的离子液体进行固载,经红外表征后确认离子液体成功固载于大孔树脂表面。同时探究了不同离子液体固载AB-8树脂后对于刺五加苷B1的水解效率与吸附量,选择[C 4 mim]HSO 4@AB-8为研究对象,水解率为169.63%(以增量计),最佳水解温度为348 K,水解240 min达到平衡,最大水解效率为97.01%。吸附温度为303 K,吸附120 min达到平衡,最大吸附量为101.2 mg/g。异嗪皮啶富集后经75%乙醇洗脱,回收率达到27.3%。由此可知,采用聚合法将[C 4 mim]HSO 4离子液体成功固载于AB-8大孔树脂表面,制备了兼具酸性催化位点的吸附材料,将其应用于水解刺五加苷B1,并同时富集水解产物异嗪皮啶,不仅提高了异嗪皮啶的纯度与回收率,而且节约了水解与吸附两步法所耗费的时间与成本。Acanthopanax senticosus is a traditional medicinal plant in Northeast of China,which contains a variety of medicinal active ingredients,such as flavonoids,polysaccharides and glycosides.Among them,A.senticosus glycosides B1 is a unique active component,which could treat the cardiovascular and cerebrovascular diseases,enhancing immunity and relieving fatigue.Isaziridin is the hydrolysis product of A.senticosus glycosides B1,which has better pharmacological activities than glycosides B1.The traditional hydrolysis methods with inorganic acid or base catalyst have the problems of low yield,high energy consumption and prone to secondary pollution.Therefore,separation of isaziridin from A.senticosus extracts in a greener and more energy-saving ways have become a new research topic.Ionic liquid is a green solvent that is a liquid at room temperature and can be designed with anion and cation structure.The ionic liquid can be immobilized on the macroporous resin,which is a stable and environmentally friendly substrate,to prepare a composite material to hydrolyze A.senticosus glycosides B1 and enrich isaziridin in one step.It was found that the AB-8 macroporous resin immobilized on 1-butyl-3-hydroxyimidazole hydrogen sulfate had the best actual aggregation effect([C 4mim]HSO 4@AB-8).In the natural environment of N 2,the chloromethylated AB-8 macroporous resin converges with the ionic liquid.The infrared analysis confirmed that the ionic liquid was successfully immobilized.In subsequent experiments,it was discovered that the optimal hydrolysis conditions were 240 min at 348 K,counting the hydrolysis increase amount of 169.63%(calculated as the increase amount of isoaziridin),and the hydrolysis efficiency was 97.3%.In the subsequent adsorption experiment,it was found that the adsorption equilibrium was reached after 120 min at 303 K,and the adsorption capacity was 102 mg/g.In addition,[C_(4)mim]HSO_(4)@AB-8 also showed excellent elution performance.When eluted with 75%volume fraction of ethanol,the recovery efficiency reache

关 键 词：离子液体 固载 大孔树脂 刺五加 异嗪皮啶 

分 类 号：TQ320.4[化学工程—合成树脂塑料工业]