麻黄生物碱分离的过程优化
文献类型：学位论文
| 作者 | 廖小雪 |
| 学位类别 | 硕士 |
| 答辩日期 | 2004 |
| 授予单位 | 中国科学院过程工程研究所 |
| 授予地点 | 中国科学院过程工程研究所 |
| 导师 | 苏志国 |
| 关键词 | 麻黄 麻黄碱 伪麻黄碱 吸附层析 离子交换层析 差向异构体 浸煮 |
| 其他题名 | Process Optimization in Separation of Ephedrine Alkaloids from Ephedra |
| 中文摘要 | 本文探索了从麻黄草中浸提麻黄生物碱的条件，研究了用大孔吸附树脂吸附麻黄 生物碱并在此基础上初步选择了分离麻黄碱差向异构体的介质，对整个麻黄碱生产工 艺进行了初步的过程优化。利用正交法考察了从麻黄草浸提麻黄生物碱过程中添加剂用量、浸煮水量、浸煮 温度、浸煮时间对麻黄碱提取率的影响，确定了较优的条件，氯化钙量9g，液固比 例为10，温度100℃，时间30min。实验发现，加大草的粉碎度能提高浸煮效率，添 加二价离子也能在一定程度上促进有效成分的浸出，为了节省生产用水，提高麻黄碱 在水溶液中的浓度，采用了三级逆流浸煮工艺，整个过程耗时3小时，比原工艺节省 了大量时间，提取率基本与原工艺持平。考察了不同种类的树脂富集麻黄生物碱的性能，pH为碱性条件下大孔吸附树脂 LSA-8、LSA-20和FXD-1的静态吸附量较大，分别为26.42mg／g resin、21.20mg.g resin 和22．12mg／g resin，动态吸附容量则是FXD-1最大，达27.5mg/ml resin，以FXD-1 树脂作为吸附介质，研究了用吸附层析取代现有的二甲苯萃取麻黄生物碱的工艺，重 点考察了洗脱剂和操作条件对产品纯度和回收率的影响，发现在树脂吸附后的洗脱 中，0.08M草酸的洗脱率最高，达99.3％，纯化倍数大于20；在操作条件中，进料 量、料液在层析柱中的停留时间和pH值影响最大：进料量增大导致纯度和收率的下 降；料液在柱中的停留时间在20min时纯度较高，而洗脱率随停留时间减少却略有下 降；pH=10时吸附性能较好。用弱酸性洗脱剂代替强酸性洗脱剂，用草酸洗脱后直 接可以按两种物质在草酸中的溶解度不同得以分离，能够很好地与现有精制工艺相衔 接。pH为酸性条件下弱酸性吸附树脂110、LSD001的静态吸附容量较大，分别为达 12.33mg／g resin和16.56mg／g resin。在相应条件下的动态吸附一容量则是LSD001的动 态吸附容量较高，达48.5mg／ml resin，浸煮液可以不调pH直接进料，各种酸性洗脱 剂和碱性洗脱剂中氨水洗脱效果最好。在研究树脂吸附富集麻黄生物碱的同时，考察了几种介质对麻黄生物碱差向异构 体分离的可能性，其中SP FF对两种混合物没有分离效能，Source 30S对混合液的洗 脱分离有一定作用，但分离度不佳，需进一步选择洗脱剂。若分离度达到一定要求，则可以代替精制过程繁琐的分离步骤和反复结晶过程，有很好地应用前景。从成品盐酸麻黄碱制备了游离麻黄生物碱，从半成品草酸麻黄碱制备了硫酸麻黄 碱和硝酸麻黄碱，结果都符合美国药典（26版）要求。 |
| 英文摘要 | This thesis mainly focus on primary process optimization of producing natural ephedrine from Ephedra. The macro-porous adsorption resin was selected as a suitable resin for the separation of ephedrine alkaloids. A varies of extracting parameters including the type of addictives, the content of soaking water, soaking temperature and time were evaluated by orthogonal method. The optimized extracting condition was as following: 9g of CaChwas added as addictives, the ratio of water and raw material was 10, and boiled at 100°C for 30min. The digestion efficiency was improved by increasing the grinding of herb. The three-step counter current digestion procedure was involved to utilize water efficiently and further increase alkaloids concentration. The yield was enhanced and the running time was shortern to 3hr by the novel extraction method. A number of resins for the enrichment of ephedrine alkaloids were evaluated to select resins LSA-8, LSA-20 and FXD-1 as three of the best macro-porous resins with high static capacity of 26.42mg/g resin, 21.20mg/g resin and 22.12mg/g resin respectively at pH value of 10. Resin FXD-1 gets the highest dynamic adsorption capacity at 27.5mg/g resin and selected as proper adsorption medium. Adsorption chromatography for separating alkaloids was developed to replace conventional xylene extraction. The highest recovery of 99.3% and purification fold of 20 were obtained by selected 0.08M oxalic acid as an eluent at the condition of pH 10, 20min of retention time and. The weak cation ion-exchanger of 110 and LSD001 have higher static adsorption capacity of 12.33mg/g resin and 16.56mg/g resin respectively at the pH value of 4.0. However, the dynamic adsorption capacity of LSDOOl was 48.5mg/g resin, where ammonia was found out to be the best eluents with high recovery. Further more, ephedrine epimers was separated by several resins, and only one peak was detected under 254nm by SPFF resin, comparing two peaks by source 30S, but the resolution was still too low to separate the mixture completely. A further investigation of eluents selection should be carried out in the future. |
| 语种 | 中文 |
| 公开日期 | 2013-09-16 |
| 页码 | 83 |
| 源URL | [http://ir.ipe.ac.cn/handle/122111/1432]  |
| 专题 | 过程工程研究所_研究所（批量导入） |
| 推荐引用方式 GB/T 7714 | 廖小雪. 麻黄生物碱分离的过程优化[D]. 中国科学院过程工程研究所. 中国科学院过程工程研究所. 2004. |
入库方式： OAI收割
来源：过程工程研究所
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