【作者】 史剑美；

【导师】 吴天星； 潘远江；

【作者基本信息】 浙江大学 ， 化学， 2010， 硕士

【摘要】 麒麟竭又名血竭(Dragon’s Blood),是我国传统名贵中药,具有着活血化淤,止血定痛,生肌敛疮,补血之功效,常用于内外诸科及妇科的各种血症。本文应用高速逆流色谱法(HSCCC)分离制备了麒麟竭中的血竭素,同时利用液相色谱质谱联用技术(HPLC/ESI-MS~n)对麒麟竭主要活性成分进行了初步的分析研究。首先,利用逆流色谱法,以正己烷-乙酸乙酯-甲醇-水(2:3:2:3,v/v)为两相溶剂系统,对麒麟竭主要成分进行了分离制备,同时分离得到血竭素及其对应查尔酮结构的混合物。基于血竭素结构与其对应查尔酮结构在不同pH下可发生结构相互转换,实验通过对该混合物进行pH调控,使查尔酮结构全部转变为血竭素结构,从而建立了仅一步分离即可获得高纯度血竭素的逆流色谱制备新方法。其次,运用液质联用技术分析鉴定了麒麟竭中8个主要成分,经柱层析分离纯化,通过核磁共振,高分辨质谱分析确定了其中2个化合物的结构。通过这两个化合物在多级质谱中的特征碎裂规律,并结合文献对照推测了另外6个化合物的可能结构。此外,本文对血竭的资源分布及麒麟竭在我国的应用进行了简要的总结。更多还原

【Abstract】 Dragon’s Blood from Daemonorops draco (D. draco) is a renowned traditional Chinese medicine. Its therapeutic applications are meant to stimulate blood circulation, control bleeding, heal wounds, promote tissue regeneration, and enrich blood. This study employed high-speed counter-current chromatography (HSCCC) to purify dracorhodin from the crude extract of D. draco. Afterward, high-performance liquid chromatography was combined with electrospray ion trap mass spectrometry (HPLC/ESI-MS~n) to investigate the major bioactive compounds in this crude extract. First, the purification procedure was performed using a two-phase solvent system composed of n-hexane/ethyl acetate/methanol/water (2:3:2:3, v/v) and a mixture of dracorhodin and its corresponding chalcone was obtained together. Since the transformation between these two compounds can be interconverted by pH changes, dracorhodin was obtained at very high purity by involving pH modulation to the isolated mixture. Thus, an HSCCC method was successfully established for purification of dracorhodin directly from the extract of D. draco. Second, the structural elucidation of the major compounds in the crude extract of D. draco have been determined by HPLC/(+) ESI-MS~n. A total of eight compounds were investigated, two of which were isolated by column chromatography and identified by NMR and ESI-FTICR-MS. Then, the structures of the other six compounds were tentatively proposed based on their mass data compared with those of the two isolated compounds, as well as those found in literature.In addition, the distribution of Dragon’s Blood and the application of its resin from D. draco were summarized briefly in this thesis.更多还原