【作者】 韩笋；

【导师】 罗国安；

【作者基本信息】 华东理工大学 ， 分析化学， 2012， 硕士

【摘要】 淫羊藿属植物在中国约有40种,目前形成药材商品的主要有15种,为阐明不同品种淫羊藿之间化学成分的异同,更好地控制药材质量,本文运用液质联用技术建立了淫羊藿定性定量指纹图谱,并进行质量标准研究,对多个品种的淫羊藿样品进行比较研究。对5个药典品种的18批淫羊藿药材进行指纹图谱研究,并对4个非药典品种的5批药材、同一样品不同部位的指纹图谱进行比较研究,不同品种、不同部位的指纹图谱差异较大。通过HPLC-TOF-MS确定精确质量数及可能分子式,通过HPLC-TRAP-MSn得到三级碎片离子,推断裂解机理,与标准品或文献比对后,确定了18个化合物,除木兰花碱外,其余均为8-异戊烯基黄酮苷类化合物。以朝藿定A、B、C,淫羊藿苷及宝藿苷Ⅰ为定量指标,不同品种、批次及不同部位的样品含量差异较大。对5个药典品种的18批淫羊藿药材进行了TLC鉴别,水分、总灰分、酸不溶性灰分、醇浸物及总黄酮含量测定,为质量标准的建立提供参考依据,并对5批非药典品种进行了比较研究。以淫羊藿苷为内参,测定淫羊藿苷对朝藿定A、B、C的校正因子,用相对保留时间对目标峰定位,建立内参校正同时定量方法,与外标法测定结果相关性良好,校正因子适用于不同仪器和色谱柱。更多还原

【Abstract】 There are about 40 Epimedium species spread in China and 15 of them circulate in the crude drug markets. It’s difficult to distinguish different species only according to their physical appearances. In our study, qualitative and quantitative determination by HPLC coupled with TOF-MS and TRAP-MSn were applied to develop a specific and valid fingerprint analysis approach for comprehensive quality assessment of Yinyanghuo. Meanwhile, some physical and chemical tests were also carried out.18 samples of the 5 species belonged to Chinese Pharmacopoeia and 5 samples of other species, as well as root and stem samples were analysed. There were significant differences in HPLC fingerprint among different species, especially different parts of one sample. HPLC-TOF-MS was employed to get accurate molecular weight and possible formula, HPLC-TRAP-MSn was applied to analyse the fragmentation mechanism.18 compounds were identified compared with standard reference substance and literature, most of them were characteristic prenylated flavonoids. Meanwhile, the contents of five main flavonoids, epimedin A, epimedin B, epimedin C, icariin and baohuoside I were determined simultaneously.Epimedin A, epimedin C, icariin in samples was measured by TLC. Some physical and chemical tests such as content of H2O, total ash, acid-insoluble ash, EtOH extract and total flavonoids were also carried out to investigate the quality.Quantitative analysis of multi-components by internal reference (QAMIR) was taken out, with icariin as internal standard, the relative correction factors (RCF) of icariin to epimedin A, epimedin B, epimedin C were calculated and relative retention time were applied to target the 3 compounds. There were no significant differences between the quantitative results by external standard method and QAMIR method. The RCF was suitable on different instruments and columns.更多还原