目录
中文摘要 (1)
英文摘要 (2)
引言 (4)
正文 (5)
1.1.1 实验原理 (5)
1.1.2 仪器、试剂和药材 (5)
1.1.3 实验方法 (6)
1.1.4 实验结果 (6)
健康之路 性功能
1.1.5 讨论 (6)
1.2提取部位的选择 (8)
1.2.1 实验方法 (8)
1.2.2 实验结果 (8)
1.2.3 讨论 (8)
1.3提取溶剂的选择 (9)
1.3.1 实验方法 (10)
1.3.2 实验结果 (11)
1.3.3 讨论 (12)
2新棒状花椒酰胺的纯化工艺研究 (13)
2.1 提取 (13)
2.2 柱谱纯化 (14)
2.2.1 实验方法 (14)
2.3 制备薄层法纯化新棒状花椒酰胺 (14)
2.3.1 制备板的铺制 (14)
2.3.2 展开系统的确定 (14)
2.3.3 展开方式的选择 (14)
2.3.4 制备过程 (14)
2.4 制备高效液相法纯化新棒状花椒酰胺 (15)
2.4.1 实验仪器与试剂 (15)
2.4.2 谱条件的摸索 (15)
novellnetware2.4.3 制备过程 (16)
2.4.4 纯度检测 (17)
2.4.4.1 仪器与试药 (17)
2.4.4.2 薄层TLC检查纯度 (17)
2.4.4.3 面积归一化法检查纯度 (18)
3光谱数据 (20)
3.1 紫外光谱 (20)
3.2 红外光谱 (21)
4实验室制备新棒状花椒酰胺的应用 (21)
4.1 提取条件优化 (22)
4.1.1 仪器、试剂和药材 (22)
4.1.2 实验方法 (22)
4.1.2.1 样品准备 (22)
4.1.2.2 谱条件 (22)
4.1.3 实验结果 (22)
4.2不同产地、品种和部位两面针中新棒状花椒酰胺含量比较 (22)
4.2.1 药材准备 (22)
4.2.2 实验方法 (23)
4.2.2.1 样品准备及谱条件 (23)
谱纯
4.2.3 实验结果 (23)
4.2.4 讨论 (24)
结论 (25)
t10钢参考文献 (28)
综述 (30)
致谢 (38)
攻读学位期间发表的学术论文目录 (39)
作者声明 (40)
个人简历 (41)
中文摘要
目的：对从中药两面针中提取制备新棒状花椒酰胺(ne ohe rc uline)的工艺进行了研究。以本实验室分离的新棒状花椒酰胺，采用高效液相谱(HPLC)法测定和比较了采自广西金秀、南宁和钦州的两面针中活性成分新棒状花椒酰胺的含量。
十八大特邀代表方法：采用HPLC峰面积比较法比较了金秀和武鸣两面针根的皮部和除皮部位和分析纯、谱纯甲醇、二氯甲烷以及谱甲醇超声0.5小时、1小时、回流1小时、2小时对提取新棒状花椒酰胺的影响，结果表明谱纯甲醇超声1小时提取金秀产两面针根皮部的效果最好；用薄层法和高效液相法对制得的新棒状花椒酰胺进行了纯化，得到了纯度为82.58%的新棒状花椒酰胺；用U V、IR对制得的新棒状花椒酰
胺进行了表征和鉴定。以本实验室分离出的新棒状花椒酰胺为参比，采用HPLC峰面积比较法测定和比较了广西金秀、南宁和钦州产两面针地上部分和根部新棒状花椒酰胺的含量。
结果：用谱甲醇对金秀两面针根的皮部加热回流提取2小时作为提取方法，以硅胶柱层析结合制备高效液相作为纯化方法，制得了纯度为82.58%的新棒状花椒酰胺，并给出了流程图。在广西钦州、南宁和金秀三个产地两面针中新棒状花椒酰胺含量测定中，金秀两面针根的含量最高，为0.0867%。
结论：用硅胶柱层析法结合制备高效液相谱法制得了纯度为82.58%的新棒状花椒酰胺。
关键词：两面针；新棒状花椒酰胺；制备工艺；高效液相谱法
Research on the Extract and Purification Technique of
Neoherculine from Zanthoxylum nitidum (Roxb.) DC.
ABSTRACT
Objective:The dissertation made research on the preparation technique of neoherculine from Zanthoxylum nitidum (Roxb.) DC.. The comparison of the content of neoherculine in Zanthoxylum nitidum from Jinxiu, Qinzhou and Nanning in Guangxi province has been made using the self-prepared neoherculine.
Methods: The extracting effects of the bark or the leftover parts of the radix of Zanthoxylum nitidum from Jinxiu and Wuming, and dichloromethane, analytical pure methanol or chromatographic pure methanol on extraction efficiency of neoherculin have been compared by peak area and data points of HPLC chromatogram method, and results showed that using the bark of radix of Zanthoxylum nitidum from Jinxiu as the raw material, chromatographic pure methanol as solvent, ultrasonic extraction for 1 hour demonstrated the best effect; through silica gel column chromatography and Preparation HPLC, neoherculine has been prepared with purity of 82.58% and its structure were characterized and identified by UV and IR spectroscopic data. Taking the self-prepared neoherculine as reference material, the content of neoherculine in different parts of Zanthoxylum nitidum from Jinxiu, Nanning and Qinzhou have been measured and compared by HPLC method.
Results: With chromatographic pure methanol as extracting solvent, the bark of the radix of Zanthoxylum nitidum from Jinxiu was refluxed and extracted at 68℃,and the extract were purified by silica gel column chromatography and Preparation HPLC with C18reverse phase column, yielding a purity of 82.58%. The application part of self-prepared
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