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以连翘植物的活性提取物为研究对象,基于不完全分离分析策略,以制备型HPLC技术为分离手段,获取含量呈连续动态变化的系列混合物,运用NMR/LC-MS平行动态谱学方法对提取物中苯乙醇苷类成分进行了同步结构分析研究。采用本方法可获取系列提取物样品中同一成分内在相关且互补的谱学信息,包括保留时间、质荷比(m/z)和化学位移值(δ)等关键数据,结合LC-MS/MS和二维NMR谱分析,成功鉴定出提取物中7种成分的结构,其中包括1个新的苯乙醇苷和1个结构极其罕见的二聚苯乙醇苷生物碱。结果表明,此种谱学分析方法可以简化复杂混合物的分离分析过程,实现结构复杂成分及多组分无需完全分离的快速同步结构鉴定;尤其对于分析极性相近的组分群及常规分离条件下难以获得的微量组分,显示出独特的解析能力。同时,本方法具有从复杂混合物中快速发现及鉴定新的活性成分或先导物的能力,可极大提高分析效率。
Taking the active extract of Forsythia suspensa plant as the research object, based on the incomplete separation and analysis method, preparative HPLC was used as the separation method to obtain a series of mixtures with continuous dynamic changes. By using NMR / LC-MS parallel kinetic spectroscopy The phenylethanoid glycosides of the extracts were analyzed by synchronous structural analysis. By using this method, we can obtain the relevant and complementary spectral information of the same components in the series of extracts, including key data such as retention time, mass-to-charge ratio (m / z) and chemical shift value (δ) And two-dimensional NMR spectroscopy, successfully identified seven components of the structure of the extract, including a new phenylethanoid glycosides and a structure of extremely rare diphenylethanolamine alkaloids. The results show that this method can simplify the separation and analysis of complex mixtures and realize the rapid identification of complex structures and complex components without the need for complete separation. Especially for the analysis of polar groups and difficult separation conditions The trace components obtained show a unique analytical ability. In the meantime, this method has the ability to rapidly discover and identify new active ingredients or precursors from complex mixtures, which can greatly improve the efficiency of the analysis.