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管花肉苁蓉提取物及其化学对照品的制备及质量研究
艾买提江.阿衣甫别克
学位类型博士
导师阿吉
2010-06-01
学位授予单位中国科学院研究生院
学位授予地点北京
学位专业有机化学
关键词管花肉苁蓉 苯乙醇苷提取物 化学标准物质 质量分析 制备工艺
摘要管花肉苁蓉 Cistanche tubulosa (Schrenk) R. Wight 为列当科中种子繁殖的多年生寄生草本植物,常寄生于柽柳属(Tamarix)植物的根部,在我国主要分布于新疆、内蒙古等具有大陆性气候的温暖荒漠地域。该植物是历史悠久的民间常用药材,现代药理学研究表明,它具有抗氧化与抗自由基、免疫调节、促进记忆力、神经保护、抗衰老、抗肿瘤等药理活性。其中的苯乙醇苷和多糖等化学成分在抗帕金森病、抗老年性痴呆、抗衰老和免疫调节等方面的研究更加受到重视。 20世纪90年代开始,随着人们不断对管花肉苁蓉的深入研究与开发利用,其野生植物资源受到了严重的威胁,已经成为我国珍稀濒危野生保护植物。近年来,国内学者对其进行了系统的保护生物学研究,在新疆区域内建立了规范化的管花肉苁蓉寄主柽柳的种植资源基地。目前,由于在新疆南部区域的人工栽培规模的扩展,资源有不断增加的趋势,为我国市场上中药肉苁蓉的主流基源植物。但是,随着中药现代化发展中规范化步伐的加快、标准化要求的不断提高和物质基础的完善,管花肉苁蓉药材资源的质量稳定性和可控性、利用效率和产业的持续发展等药材资源保护、开发和可持续利用面临着更大的压力,这些问题的关键在于缺乏管花肉苁蓉种质资源的质量评价(或控制)标准及其指标成分、中间产品(如标准提取物)制备工艺的技术标准与可比性,从而导致药材资源的供应与产业现代化、市场需求的矛盾日益突出。因此,本论文致力于继承传统中药材—管花肉苁蓉,以药理活性为出发点,综合运用多种制备色谱分离技术,对管花肉苁蓉及其粗提取物进行化学成分研究,分得12个化合物,用波谱学分析手段,确定了化合物结构,如:松果菊苷(1)、毛蕊花糖苷(2)、异麦角甾苷(3)、2'-乙酰基初麦角甾苷(4)、管花苷 A(5)、cistanoside C1/C2 (6)等含量均为 95.0 %以上。采用Melannoma mouse 皮肤瘤细胞株 KML筛选体外抗癌活性,结果表明echinacoside、 acteoside、 isoacteoside、cistanoside C1/C2等化合物对增殖有拮抗作用。在此基础上,采用HPLC法,对管花肉苁蓉药材进行指纹图谱研究,10 批药材的相似度均在 0.923 以上,又建立了简便、快速和准确的含量测定方法。基于中药提取动力学理论与方法,采用有机溶剂提取法,对新疆产管花肉苁蓉中苯乙醇苷化合物进行提取工艺研究,确定了最佳的提取工艺条件,即:固液比为1:16,乙醇浓度为 50 %,提取温度为60 ℃。接着又采用多种大孔吸附树脂,详细考察静态、动态吸附和解吸动力学过程,建立了富集管花肉苁蓉中苯乙醇苷的分离纯化制备工艺条件,即:每 1 g AB-8 大孔树脂对松果菊苷和毛蕊花糖苷的最佳吸附量分别为 79.8 mg 和 8.6 mg;吸附体积流速为 2 BV·h-1,以 50 %的乙醇溶液为解吸剂,洗脱体积流速 2 BV·h-1。同时,依照前述分离纯化工艺条件重复操作,结果得到管花肉苁蓉提取,其按干燥品计算,每1 g 管花肉苁蓉提取物含松果菊苷和毛蕊花糖苷的总量50.7%以上。以管花肉苁蓉药材与其提取物作为原料资源,通过半制备HPLC和HSCCC与柱色谱相结合,分离,纯化制备了 5种苯乙醇苷化学标准物质,含量均在 97.3 %以上,为新疆特色植物资源的深入开发提供科学依据。
其他摘要Cistanche tubulosa (Schrenk) R. Wight is a wild perennial herb of the Orobanchaceae family that usually parasitizes the roots of Tamarix chinensis, Tamarix taklamakanensis, etc. It is widely distributed in deserts in Autonomous Regions of Xinjiang and Inner Mongolia, China. The plant is frequently used in Traditional Chinese Medicine (TCM). Pharmacological studies have shown its pharmacological activity in scavenging free oxygen radicals, anti-decrepitude, improving the learning-memory, immunoregulation, neuroprotection, anti-aging, antitumor, etc. Some of chemical compositions, such as Cistanche polysaccharide and phenylethanoid glycosides (PeGs) are mainly researched for effectiveness in curing Parkinson's disease as well as senile dementia. Since 1990, with the in-depth study, development and utilization, C. tubulosa has suffered a serious threat and become a rare and endangered wild plant. In recent years, domestic scholars has conduct a systematic research of the conservation biology for C. tubulosa, and built a standardized cultivation production bases in Autonomous Regions of . At present, due to the expansion of cultivated area in southern Xinjiang, C. tubulosa has become the main source of Cistanche plants in the Chinese market. However, enormous challenges have been brought to the medicinal resource protection, development, and sustainable use of C. tubulosa by the development of modernization in the TCM standardization and further continuously standards research improving. Therefore, this thesis elaborated the studies on chemical constituents with pharmacological activities. During the phytochemical investigation, 12 compounds were isolated from this plant by different means, such as column chromatography (CC), low and medium pressure liquid chromatography (LPLC, MPLC), with different solid-phase including silica gel, reversed-phase C18 silica gel, and sephadex LH-20 as well. These compounds were identified based on MS, 1D and 2D NMR spectral data , such as echinacoside , acteoside , isoacteoside , 2'-acetylacteoside , tubuloside A , cistanoside C1/C2 . In the in vitro assays, echinacoside, acteoside, isoacteoside and cistanoside C1/C2 showed cytotoxic activities against Melannoma mouse skin tumor cell line proliferation KML. These compounds (1 ~ 6) were isolated from the crude extracts of C. tubulosa, and their contents were no less than 95.0%. On this basis, we studied the fingerprint of C. tubulosa by HPLC means, and the similarity of 10 batches was more than 0.923. We established a simple, rapid and accurate method for the determination. Based on the extraction dynamics theory and method of traditional Chinese medicine, the phenyletanoid glycoside compounds were extracted by organic solvent extraction from Xinjiang produced C. tubulodsa, and we determined the optimal extraction conditions as follows: solid to liquid ratio of 1:16, 50% ethanol for extraction solution, 60℃ for extraction temperature. Then the purification process of PeGs was studied by screening static state, dynamic state adsorption and desorption kinesics process of 20 kinds of macro porous resins. AB-8 resin offered the best adsorption and desorption capacity and obtained the optimum parameters as follows: sample flow rate : 2 BV·h-1,desorption agent: 50 % ethanol, elution flow rate : 2 BV·h-1. The maximum adsorption of echinacoside and acteoside on AB-8 resin were 79.8 mg/g and 8.6 mg/g. Then we get the product with echinacoside and acteoside by above optimized extraction and purification process, and their total content was more than 50.7%. Moreover, five kinds of chemical standard substances of PeGs were separated by HSCCC and Prep-HPLC means from C. tubulodsa extracts, and their purities were above 97.3 %. The results in this study may provide scientific references for developing local special plants resources in Xinjiang.
文献类型学位论文
条目标识符http://ir.xjipc.cas.cn/handle/365002/4453
专题资源化学研究室
作者单位中国科学院新疆理化技术研究所
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艾买提江.阿衣甫别克. 管花肉苁蓉提取物及其化学对照品的制备及质量研究[D]. 北京. 中国科学院研究生院,2010.
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