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基于LC-MS/MS技术的三种维医药成分分析及其质量标准研究
赛那瓦尔·芒思尔
学位类型博士
导师阿吉艾克拜尔·艾萨
2017-06-03
学位授予单位中国科学院大学
学位授予地点北京
学位专业有机化学
关键词Uplc/qtof-ms/ms 新疆玫瑰花 榅桲子 对叶大戟 维吾尔药 液相指纹图谱 质量标准
摘要

本论文通过液质联用技术(LC-MS/MS)对常用维药材玫瑰花、对叶大戟和榅桲子开展了化学成分分析,确定了这三种药材的主要成份和微量成分,建立了药材质量标准及指纹图谱,为这三种维药创新药物的研发和质量控制提供科学与理论基础,具体研究结果如下:1.玫瑰花玫瑰花(Rosa rugosa Thunb)是蔷薇科蔷薇属植物玫瑰的干燥花蕾,具有活血、调经、止痛等作用。本论文首先采用HPLC/QTOF-MS/MS技术对其中的主要成分和微量成分进行了分析,共鉴定出包括有机酸、黄酮和多酚类等90个化合物,其中15个化合物在此植物属中首次发现。根据特征碎片和裂解规律,鉴定9个食子酸鞣(gallotannin)、19个鞣花酸鞣质(ellagotannin)、2个黄酮苷元和52个黄酮-O-苷。通过对di-O-galloyl-HHDP-glucose和hydrogalloyl-galloy-HHDP-glucose特征碎片的研究,总结出这类化合物的裂解规律:这类化合物特征碎片离子由m/z 633, 483, 331, 313, 300.99, 169和125。分子离子峰m/z 785和767,有两种裂解途径:1)分别两次失去两个没食子醛基得m/z 633, 613, 465特征碎片,然后六元糖基裂解得m/z300.99特征碎片鞣花酸基。2)[M-302 Da]-丢失HHDP基团,得m/z 483, 169和125特征碎片峰,其次六元糖基裂解失去170 Da和152 Da,得到的m/z 331和313碎片离子,此研究为这类化合物的质谱解析指明了方向。基于超高压液相(UPLC)建立同时检测玫瑰花药材中没食子酸、鞣花酸、金丝桃苷、黄芪苷和山奈酚-3-O-β-D-槐糖苷等指标成份的含量测定方法,此法为定量分析提供了一种可靠,快速简单的方法。完成了10批次新疆不同地区产的玫瑰花药材进行水分,总灰分和浸出物等检查,其结果完全符合2015年版《中国药典》中玫瑰花药材中规定的量。建立的玫瑰花指纹图谱中检测出23个特征峰,特征吸收峰占总峰面积的65%。将共有特征峰与标准化合物的保留时间进行比较,指认出10个化合物。10批玫瑰花药材整个色谱图与标准指纹图谱之间相似度都高于0.9。此研究对新疆玫瑰花药材化学成分研究和质量控制提供科学依据。2,对叶大戟对叶大戟(Euphorbia sororia A. Schrenk)是大戟科大戟属一年生草本植物,有消散寒气、开通阻滞、燥湿开胃、健脑益智等功效。首先使用UPLC/QTOF- MS/MS技术对主要成分和微量成分进行了分析,共鉴定27个化合物,其中6个化合物在此植物中首次发现。通过7个绿原酸类化合物、3个黄酮苷元和13个黄酮-O-苷,2个豆甾醇衍生物的特征碎片离子总结出这类成分的裂解规律。基于超高压液相(UPLC)建立对叶大戟药材山奈酚-3-O-半乳葡萄糖苷作为指标的含量测定方法并进行了系统方法学考察。对8批次新疆不同产的对叶大戟药材进行水分和总灰分等检查,限定水分和总灰分分别小于5%和11%。建立的对叶大戟指纹图谱检测出25个共有峰,其在整个色谱峰面积中占53%。8批对叶大戟药材整个色谱图与标准指纹图谱之间相似度都高于0.9。此研究为新疆对叶大戟药材化学成分研究和质量控制提供科学依据。3.榅桲子榅桲子(Cydonia oblonga Mill)是为蔷薇科植物榅桲 Cydonia oblonga Mill. 的干燥种子。首先UPLC/QTOF-MS/MS技术对新疆榅桲子主要成分和微量成分进行分析,共鉴定了20个化合物。其中4个化合物在此植物中首次发现。通过包括11个有机酸,3个黄酮苷元和9个黄酮-O-苷的特征碎片离子总结出这类成分的裂解规律。其中4个化合物在此植物中首次发现。应用高效压液相(HPLC)建立榅桲子药材以苦杏仁苷作为指标含量测定的方法并系统进行方法学考察。对8批新疆不同地区产榅桲子进行水分,和总灰分等检查。其完全符合《中华人民共和国卫生部药品标准》(维吾尔药分册)中榅桲子药材规定的量。建立的榅桲子指纹图谱检测出24个特征共有峰,其在整个色谱中覆盖超过83%的总面积。通过跟标准化合物保留时间进行比较指认6个化合物。8批次榅桲子整个色谱图与标准指纹图谱之间的相似度均高于0.89。此研究可作新疆榅桲子药材化学成分研究和评估质量提供理论依据。

其他摘要

In this study, LC-MS was used to investigate the main components and trace components of the methanol extraction of Rosa rugosa Thunb, Euphorbia sororia A. Schrenk and Cydonia oblongaMill. Then establish the quality standard and fingerprint of those plants.1. Rosa rugosa ThunbRose (Rosa rugosa Thunb) is the dry flower of the Rosaceae rose. The plant can promote the blood circulation, regulate the menstrual function and relieve pain. In our study, we used the HPLC/QTOF-MS/MS to identify major and trace components, and identified 90 compounds in methanol extraction. Main components were organic acid, flavonoid and phenolic acid, among them 9 gallotannins and 19 ellagotannins are identified from the plant. The fragmentation rules of di-O - galloyl-HHDP-glucose, Hydrogalloyl-galloy-HHDP-glucose and characteristic fragment ions are summarized. And identified 2 flavonoid aglycones and 52 flavonoid glycosides, among them 15 compounds are identified for the first time from this plant. For the fingerprint analysis, 23 characteristic fingerprint peaks were applied to evaluate the similarity among 10 batches of R. rugosa, and they showed good similarity. For the quantitative determination, 10 components of the 10 batches of R. rugosa were successfully determined. The method developed in this study will provide an important reference to establish the quality control method for other related traditional Chinese medicinal preparations.2. Euphorbia sororia A. SchrenkA. (Euphorbia sororia Schrenk) is an annual herbaceous plant of euphorbia, used to cure dissipate cold, open block, dampness appetizer and have brain puzzle effect. Firstly, UPLC/QTOF-MS/MS was used to identify the components in the roots of Euphorbia sororia A. Schrenk, as a result 40 components were identified, including 11 organic acids, 3 flavonoid aglycones, and the total flavonoid glycosides of the 27 -O-. 6 compounds were identified for the first time from this plant. Take the kaempferol -3-O- galactose glucoside as control index, study the methodology and RSD less than 2.4%. According to the 2015 edition of Chinese "Pharmacopoeia", the water ash and total ash was tested, and the content 5%, and 11% respectively. 8 batches of Euphorbia sororia were analyzed, and showed that those plants have 25 common peaks, common peaks cover more than 53% of the total area in the whole chromatogram. The similarity between 8 batches of plants chromatograms and the standard fingerprint was higher than 0.9. This study provides the quality control of the raw materials of Euphorbia.3. Cydonia oblonga MillQuince (Cydonia oblonga Mill) is the son of dry seeds for Rosaceae quince Cydonia Mill. oblonga. UPLC/QTOF-MS/MS was used to identify the sub components of quince, and identified 20 components, including 11 organic acids, 3 flavonoid aglycones, and the total flavonoid glycosides of the 9 -O-. 6 compounds were identified for the first time from this plant. The amygdalin was control index, used the UHPLC to study the methodology, and the repeatability, precision, reproducibility and recovery rate were all less than 3% RSD. According to the results of water measurement, with reference to the Ministry of health, People's Republic of China pharmaceutical standards (Uighur Medicine fascicle) moisture content shall not exceed 8%, so the total amount of raw materials shall not be less than 1.5%. In order to standardize the fingerprint, 8 batches of samples were analyzed, and detected 23 common peaks, the common peaks were covering more than 83% of the total area in the whole chromatogram. 6 compounds were identified by comparing the retention time of the characteristic peaks with the UV spectra of the standard compounds. The similarity between the 8 batches of the entire chromatogram and quince substandard fingerprints were higher than 0.89.

文献类型学位论文
条目标识符http://ir.xjipc.cas.cn/handle/365002/4982
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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赛那瓦尔·芒思尔. 基于LC-MS/MS技术的三种维医药成分分析及其质量标准研究[D]. 北京. 中国科学院大学,2017.
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