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1、广东药学院 硕士学位论文 蒲黄总黄酮提取分离与固体分散片制备的研究 姓名：柴洪帆 申请学位级别：硕士 专业：药剂学 指导教师：高崇凯 20090501 广东药学院硕士研究生学位论文 I 中文摘要中文摘要 蒲黄 （Pollen Typhae） ， 为香蒲科 （Typhaceae） 植物水烛香蒲 （Typha angustifolia L.） 、东方香蒲（Typha orientalis Presl.）或同属植物的干燥花粉，是一味经典中 药，有凉血止血，活血祛癖，止痛，利尿等功效。黄酮类成分是其主要有效成分， 被认为对血液系统、心血管系统疾病的治疗有较好疗效。本课题首先研究了含量 测定标准及蒲黄总
2、黄酮的提取纯化工艺。 将大孔吸附树脂技术应用到对大类成分 的纯化工艺中，取了较满意的效果，并对蒲黄总黄酮进一步进行了剂型开发，主 要内容和结果如下： 对从蒲黄中提取纯化总黄酮的工艺条件进行了优化。 在单因素试验的基础上 采用 L9(34)正交试验确定了乙醇回流法提取总黄酮的最佳工艺参数：乙醇浓度 70%，提取温度 80C，料液比为 1:12，提取时间 2h，进行 3 次提取。 确定了碱溶酸沉除杂的最佳工艺条件为：调节 pH 为 23，冷冻静置 12h， 溶液恢复至室温后 2000r/min 离心 30min，取上层溶液，调节 pH 为 1011，冷冻 静置 12h，溶液恢复至室温后 2000r
3、/min 离心 30min，取下层沉淀。继续探讨了 大孔吸附树脂法纯化蒲黄总黄酮的工艺， 研究结果表明 AB-8 型大孔吸附树脂适 合于蒲黄总黄酮的纯化， 纯化工艺条件为： 上样量 1.5 倍树脂体积， 上柱样品 pH 值约为 6， 浓度为 2mg/ml， 以 2ml/min 的速度流过树脂， 待吸附平衡后， 用 5BV 的蒸馏水淋洗树脂，然后用 50%的乙醇溶液以 2ml/min 的流速进行洗脱，收集 4BV 的洗脱液，其干燥品中的黄酮纯度可达 39%左右。 本研究制备了蒲黄黄酮固体分散体，考察了提取物与聚乙烯吡咯烷酮 K30(PVPK30)不同比例对黄酮的溶出速率的影响，得出以 PVPk3
4、0 为载体，提取 物和 PVPK30比例为 1：3 时，采用溶剂法制备固体分散体的溶出速率最好。并进 一步考察了加入泊洛沙姆 188(poloxame188)，与 PVPK30作为联合载体对黄酮的 溶出速率的影响，得到当三者比例为 1：3：1 时黄酮的溶出速率最快。固体分散 体、 物理混合物及蒲黄提取物的溶出速率比较结果显示蒲黄黄酮固体分散体的溶 出速率最好。固体分散体的红外光谱分析结果以及 X 射线衍射(X-ray)分析结果 显示黄酮以无定型状态分散在载体中。 广东药学院硕士研究生学位论文 II 蒲黄总黄酮固体分散体片的制备研究中， 选择了交联聚乙烯吡咯烷酮(PVPP) 作为崩解剂。 以固体
5、分散片的崩解时间和 10min 溶出度为考察指标， 采用均匀设 计法进行处方设计，预测结果与处方验证结果得出的黄酮固体分散体片(400mg) 最佳处方为：蒲黄黄酮固体分散体 250mg，交联聚乙烯吡咯烷酮 PVPP46mg，微 晶纤维素 20mg，硬脂酸镁 4mg，乳糖 80mg。制备的蒲黄黄酮固分散体片外观完 整光洁，色泽均匀，崩解时间为 6 秒，10 分钟的溶出度为 90%以上。 关健词关健词：蒲黄总黄酮；固体分散体；聚乙烯吡咯烷酮 K30；泊洛沙姆 188； 分散片 广东药学院硕士研究生学位论文 i 英文摘要英文摘要 ABSTRACT Puhuang is a common used C
6、hinese herb with long history in traditional chinese medicine，which originates from the pollen of Typha angustifolia L., Typha orientalis Presl. and the other plants of the genus Typha. It has the effects of cooling blood, promoting blood circulation and relieving pains, it is often presumed to have
7、 better therapeutic effect on hematological system and cardiovascular system. The object of this paper is to study the extraction and purification of total flavonoids in puhuang and to establish the quantity standard. In second part, applying the maropotous resin techniques to the process of purific
8、ation, had obtained satisfied results. The major contents and results of the researches were as follows. The extraction technology for total flavonoids in puhuang was systematically studied with single factor experiment and orthogonal design. The optimum technological conditions were attained as fol
9、low: extracted temperature at 80C with 70% ethanol, the ratio of materiel to solvent was 1:12, and extracted for 2 times, 2h for each time. The two methods of purication with alkali-solution acid-isolation and maropotous resin techniques were studied in this paper, and the results of single factor e
10、xperiments showed that, when after two times of alkali-solution with pH 23 and acid-isolation with pH 1011，the effect of purification was better. Every time after alkali-solution or andacid-isolation purification, the solution needed to refrigerate for 12h, stay to room temperature, then centrifuge
11、30min under 2000r/min. The purification of total flavonoids by using the method of macroporous resin was experimented. The results indicated that AB-8 maropotous resin mostly fitted for the separation of total flavonoids. The condition of adsorption and desorption was to determined: the adsorption r
12、atio of flavonoids was 1.5BV of the resin; the best pH and concentration of the sample were pH 6 and 2mg/ml; the amount of distilled water was 5BV of the resin; the eluting agent was 15% ethanol(4 times the volume of the resin) 广东药学院硕士研究生学位论文 ii by velocity of 2ml/min. The total flavonoids solid dis
13、persion was prepared in the study，the influence of different ratio of PVPk30 and poloxame 188 was considered. Moreover, the dissolution rate of flavonoids was highest when drug: PVPk30: poloxame 188= 1:3:1. The infrared spectrum (IR) test and the X-ray test showed that flavonoids dispersed in carrie
14、rs in amorphism. The flavonoids solid dispersion tablets were prepared in the different disintegrating agent, the results showed that the tablet with PVPP had best disintegration time. In the uniform design test, disintegration time and dissolution rate at 10 min(D10) of flavonoids solid dispersion
15、tablet were considered as inspection items to optimize preparation prescription, and concluded that the optimizing of solid dispersion tablet was flavonoids solid dispersion 250mg, PVPP 46mg, CMC 20mg, lactose 80mg, magnesium stearate 4mg.The tablets had good appearance, the disintegration time was
16、6 second, the D10 was above 90%. As a result, the flavonoids solid dispersion tablet reached the purpose of increasing the dissolution rate in vitro. Keyword: puhuang total flavonoids; solid dispersion; PVPK30; poloxame188; solid dispersion tablet 广东药学院学位论文原创性声明广东药学院学位论文原创性声明 本人郑重声明： 本人所呈交的学位论文，系我个人在导师的指导下 进行研究工作所取得的成果。 除文中已特别加以标注和致谢的地方外， 不 包含其它个人或机构已经发表或撰写过的研究成果。 对本研究做出贡献的 其它个人和集体， 均已在文中明确说明和致谢。 本人充分意识到本声明的 法律结果完全由本人承担。 学位论文作者签名： 日 期： 年 月 日 学位论文使用授权的声明学位论文使用授权的声明 本人完全了解广东药学院有关
