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基于LC-QTOF-MS技术对石榴皮多酚提取物的化学成分研究及药材资源的品质评价
热依木古丽·阿布都拉
Thesis Advisor刘照胜、阿吉艾克拜尔·艾萨
2017-06-03
Degree Grantor中国科学院大学
Place of Conferral北京
Degree Name博士
Degree Discipline有机化学
Keyword石榴皮 多酚, LC-Q/TOF-MS, 指纹图谱,资源评价
Abstract

石榴皮是石榴科植物石榴(Punica granatum L.)的干燥果皮,系多种维吾尔医和中医处方的组成部分,具有多种生物学活性和药理学作用。本研究以前期工作为基础,开展石榴皮多酚提取物的物质基础和药材资源品质研究,为石榴皮多酚提取方法的标准化及其与国际标准接轨提供依据。1. 石榴皮多酚提取物的物质基础和质量标准研究(1)采用液质联用质谱(LC-QTOF-MS)方法,对石榴皮多酚提取物的主要成分和微量成分进行结构分析,鉴别出50种多酚类化合物,包括35种水解鞣质和15种黄酮类,其中首次报道2种鞣质类和7种黄酮类成分;(2)以10批次石榴皮多酚提取物为原料进行超高效液相色谱(UPLC-PDA)指纹图谱研究,确认12个的特征峰,建立了石榴皮多酚的指纹图谱鉴别模式,继而确定了安石榴苷、鞣花酸、安石榴林、没食子儿茶素、柯里拉京、紫云英苷等7种石榴皮化学成分的含量;(3)在此基础上,首次建立了石榴皮多酚标准提取物的质量控制标准,其中制定提取物中安石榴苷含量不得低于30.0%,鞣花酸含量不得低于2.0%。2. 石榴皮药材资源品质的评价研究增设安石榴苷、安石榴林和鞣花酸三种鉴别项,优化了薄层色谱(TLC)方法;采用高效液相色谱(HPLC)建立了安石榴苷和鞣花酸的测定方法;以新疆产23批石榴皮药材为原料,建立了石榴皮药材UPLC-PDA指纹图谱;结合上述优化条件和指纹图谱相似度分析,对国内外石榴皮药材进行品质比较分析,发现新疆、陕西、四川、伊朗、乌兹别克斯坦等不同产地和品种石榴皮药材品质存在一定的差异,为石榴皮药材和提取物为原料的新药研发提供了科学依据。3. 石榴皮安石榴苷等指标成分的标准品研制对新疆石榴皮多酚进行溶剂提取、大孔吸附树脂富集、制备液相色谱纯化,获得了安石榴苷、安石榴林、鞣花酸等三种指标性成分,其HPLC纯度均为98%以上;按照天然产物国家标准样品制备技术要求,对上述三种化学成分进行结构确证、稳定性和均匀性研究,制定其有效期和不确定度,解决了民族药标准样品的缺乏问题,为完善药材、原料药和成药的质量控制标准提供了依据。

Other Abstract

Pomegranate (Punica granatum L.)peel is an important herbal medicine of prescriptions in traditional Uyghur medicine and Chinese medicine, and has multiple biological activities and pharmacological effects.In this work, we investigated the chemical composition of polyphenols extracted from the pomegranate peels and the material quality of pomegranate peels of different origins, to provide a standardized method for extraction of polyphenols from pomegranate peel, which meets the international standard. 1. Studies of chemical composition and quality standard of polyphenolic extracts from of the pomegranate peel(1) Fifty polyphenolic compounds, of which 35 hydrolyzable tannins and 15 flavonoids, were identified by chemical composition analysis of major and minor compounds in polyphenolic extracts from pomegranate peel using liquid chromatography coupled with tandem mass spectrometry (LC-QTOF-MS). Of these, 2 tannins and 7 flavonoids were reported for the first time in this study; (2) we analyzed the finger prints of 10 batches of polyphenolic extracts from pomegranate peels by ultra-high performance liquid chromatography (UPLC-PDA) and established finger print-based discrimination pattern for polyphenols from the pomegranate peel using 12 specific peaks. Accordingly, 7 compounds were identified and quantified in the polyphenolic extract, including punicalagin, ellagic acid, punicalin, gallocatechin,corilagin, and astragalin;(3) Based on these data, we established for the first time quality control standard for standardized extraction of polyphenols from pomegranate peel by setting punicalagin and ellagic acid contents of at least 30 and 2% of the extract, respectively. 2. The evaluation of the material quality of pomegranate peel from different sourcesWe optimized the quality of thin-layer chromatography (TLC) in the detection of polyphenols extracted from pomegranate peel by adding three compounds including punicalagin, punicalin and ellagic acid as additional discrimination profile; established a quantitative method for detection of punicalagin and ellagic acid by high-performance liquid chromatography; established a finger print for pomegranate material based on UPLC-PDA analysis of 23 batches of pomegranate material from different regions of Xinjiang China. Based on these methods, we comparatively analyzed the material quality of pomegranate peels from inside and outside of China, and found that the material quality of pomegranate peels was slightly different among different regions and pomegranate species. This may provide evidence for drug discovery based on pomegranate peel and its extracts. 3. Development of reference substance for quality control of pomegranate peel based on punicalaginBy solvent extraction, enrichmentwith macroporous resin and purification with preparative liquid chromatography, we obtained punicalagin, ellagic acid and punicalin as three characteristic compounds of polyphenols from the pomegranate peel with more than 98% purity estimated by HPLC. Subsequently, we analyzed these compounds for chemical identity, stability and homogeneity and defined the validity period and measurement uncertainty. These data may fill up a vacancy in traditional herbal medicine that lacks reference substances and provide evidence for improving the standard in quality control of medicinal material, bulk drug and patent herbal medicine.

Pages132
Document Type学位论文
Identifierhttp://ir.xjipc.cas.cn/handle/365002/7098
Collection资源化学研究室
Recommended Citation
GB/T 7714
热依木古丽·阿布都拉. 基于LC-QTOF-MS技术对石榴皮多酚提取物的化学成分研究及药材资源的品质评价[D]. 北京. 中国科学院大学,2017.
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