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基于不完全分离分析策略,建立了NMR/LC-MS异相关谱(NMR/LC-MS HCS)方法对系列混合物样品的LC-MS和NMR谱数据的整合分析,发掘混合物图谱中来自同一组分的LC-MS和NMR谱数据间的内在相关性。以新疆维吾尔民族药用植物草棉(Gossypium herbaceam L.)花瓣的乙醇提取物(AB-8-2)为研究对象,以多通道组合闪式色谱技术为分离手段,不完全分离并获取了组分含量呈连续动态变化的系列混合物,运用NMR/LC-MS HCS方法对提取物中的黄酮苷类成分进行了同步结构分析研究。由于随组分浓度动态变化的多种谱学信号强度间具有强的正相关性,通过NMR/LC-MS HCS图可以获得系列提取物中同一组分的互补性的LC-MS和1H NMR谱数据,包括保留时间(Rt)、质荷比(m/z)和化学位移值(δ)等关键数据。以已解析的关键谱学信号为线索,引入LC-MS/MS谱和二维NMR谱进行综合分析,成功地从AB-8-2中鉴定出12个黄酮醇苷类化合物,其中还包括2组共流出的同分异构体。结果表明:通过该新型分析方法可以在离线的情况下通过“数学联用的方式”实现与在线LC-NMR-MS联用技术相似的分析功能,这种新型谱学分析方法可以简化复杂混合物的分离分析过程,实现结构复杂成分以及多组分无需完全分离的快速同步结构鉴定;尤其对于常规分离条件下难以获得单体的微量成分或极性相近组分群显示出独特的解析能力。
Based on incomplete segregation analysis strategy, the LC / MS and NMR spectral data of the mixture of samples were integrated and analyzed by NMR / LC-MS heterospatial correlation spectroscopy (NMR / LC-MS HCS) The inherent correlation between LC-MS and NMR spectral data. The ethanol extract of petals (Gossypium herbaceam L.) from Xinjiang Uyghur medicinal plant Gossypium herbaceam L. was taken as the research object, and the multi-channel combined flash chromatography was used as the separation method. The group A series of mixtures with continuous and dynamic changes in content were used to study the simultaneous structural analysis of the flavonoid glycosides in the extract using NMR / LC-MS HCS method. Due to the strong positive correlation between multiple signal intensities that vary dynamically with component concentrations, LC-MS and 1H NMR spectra of the same components in the series of extracts can be obtained by NMR / LC-MS HCS plot Data including key data such as retention time (Rt), mass-to-charge ratio (m / z), and chemical shift value (δ) Based on the resolved key spectroscopy signals, LC-MS / MS and 2D-NMR spectra were introduced for comprehensive analysis. Twelve flavonol glycosides were successfully identified from AB-8-2, including 2 Group outflow of the isomers. The results show that the new analytical method can be used to realize the similar analysis function with the on-line LC-NMR-MS combined technology through the method of “mathematical combination” under the condition of offline. The new method of spectral analysis can simplify the complex Mixture separation and analysis process to achieve the structure of complex components and multi-component without the need for complete separation of the rapid synchronization of structural identification; especially for conventional separation conditions is difficult to obtain the composition of the micro-components or polar similar groups show a unique analytic ability.