大孔吸附树脂纯化延胡索总生物碱工艺研究|延胡索所含的生物碱
[摘要] 目的 研究大孔吸附树脂分离和纯化延胡索总生物碱的工艺条件。 方法 以总生物碱和延胡索乙素的吸附量和解吸率等为考察指标，对12种不同类型的树脂进行评价，并对优选出的大孔树脂纯化延胡索总生物碱时的工艺条件及参数进行研究。 结果 D141大孔吸附树脂的动态吸附分离效果最好，样液浓度为0.35 g生药/mL，径高比为1∶6，吸附流速为4 BV/h，除杂溶剂和体积为0.3% NaCl溶液7 BV+纯净水1 BV，洗脱溶剂为4 BV 60%乙醇+4 BV 90%乙醇，洗脱流速为5.5 BV/h。通过大孔吸附树脂分离纯化后，终产品中总生物碱的纯度为82.0%。 结论 该工艺合理、可行，适合工业生产。
[关键词] 延胡索；总生物碱；延胡索乙素；大孔吸附树脂；纯化
[中图分类号] R283.6 [文献标识码] A [文章编号] 1673-7210（2012）07（b）-0109-04
Study on purification process of total alkaloids from Corydalis yanhusuo by macroporous adsorption resin
LU Ziming1,2 LIU Wenjuan2 YU Xianghong2 YANG Zhiyun2 LIANG Junqing2 TU Pengfei1▲
1.State Key Laboratory of Natural and Biomimetic Drugs School of Pharmaceutical Sciences, Peking University, Beijing 100191, China; 2.Beijing Yiling Pharmaceutical Co., Ltd, Beijing 100027, China
[Abstract] Objective To investigate the process of isolation and purification of total alkaloids from Corydalis yanhusuo by macroporous adsorption resin. Methods The absorption amount and desorption ratio were taken as the investigation indexes to evaluated 12 kinds of resins. And the process and parameters of purification of total alkaloids from Corydalis yanhusuo by macroporous adsorption resin were studied. Results The dynamic adsorption and isolation effect of D141 type macroporous adsorption resin was the best, with the drug solution concentration was 0.35 g of medicinal material/mL, ratio of diameter and height was 1∶6, velocity of absorption was 4 BV/h, solvent and volume of removing impurities was 0.3%NaCl solution 7 BV + purified water 1 BV, solvent of elution was 4 BV 60% of alcohol +4 BV 90% of alcohol, velocity of elution was 5.5 BV/h. The purity of total alkaloids in the final product was 82.0% after isolation and purification by macroporous adsorption resin. Conclusion The process is rational, feasible and suitable for industrial production.
[Key words] Corydalis yanhusuo; Total alkaloids; Macroporous adsorption resin; Tetrahydropalmatine; Purification
延胡索为**科植物Corydalis yanhusuo W. T. Wang的干燥块茎，具有活血化瘀、理气止痛之功效[1]。现代药理学研究表明，延胡索具有抗溃疡、抑制胃酸分泌、解痉及增加冠状动脉血流量、抗心律失常等作用[2]。延胡索生物碱包括叔胺碱和季胺碱，是其主要活性成分。目前，大孔树脂在中草药有效成分的分离、富集中的应用越来越受到人们的重视[3]。本文旨在优选出一种适合纯化延胡索总生物碱的大孔树脂，并对优选出的大孔树脂纯化延胡索总生物碱时的工艺条件及参数进行研究。
1 仪器与材料
UV-2550紫外分光光度计（日本岛津公司）；Agilent 1100 Series 高效液相色谱仪（美国安捷伦公司）；Sartorius BS 110电子天平（德国赛多利斯公司）；延胡索药材（购于河北省安国以岭饮片有限公司，经鉴定，符合《中国药典》2010年版一部标准，批号：070902）；延胡索乙素对照品（中国药品生物制品检定所，批号：0726-200208）；大孔吸附树脂NKA-9（南开大学）；HPD600、HPD500、HPD-450、HPD-400A、HPD-400、HPD100A（沧州宝恩吸附材料科技有限公司）；AB-8、D101、DM-130、D-100、D141（中蓝晨光化工研究院物资公司）。95%乙醇（药用规格，天津市科密欧化学试剂有限公司）；水为纯化水，其他试剂均为分析纯（北京化工厂）。