Qu Jing, Hu You-cai, Li Jian-bei, Wang Ying-hong, Zhang Jin-lan, Abliz Zeper, Yu Shi-shan, Liu Yun-bao
Key Laboratory of Bioactive Substances and Resources Utilization of Chinese Herbal Medicine, Ministry of Education, Institute of Materia Medica, Peking Union Medical College & Chinese Academy of Medical Sciences, Beijing, People's Republic of China.
Rapid Commun Mass Spectrom. 2008;22(6):755-65. doi: 10.1002/rcm.3419.
A combination of electrospray ionization tandem mass spectrometry with high-performance liquid chromatography (HPLC/ESI-MSn), and hyphenation of liquid chromatography to nuclear magnetic resonance spectroscopy (HPLC/NMR), have been extensively utilized for on-line analysis of natural products, analyzing metabolite and drug impurity. In our last paper, we reported an on-line analytical method for structural identification of trace alkaloids in the same class. However, the structural types of the constituents in plants were various, such as flavanoids, terpenoids and steroids. It is important to establish an effective analytical method for on-line structural identification of constituents with molecular diversity in extracts of plants. So, in the present study, the fragmentation patterns of some isolated stilbenes, phloroglucinols and flavanoids from Lysidice rhodostegia were investigated by ESI-MSn. Their fragmentation rules and UV characteristics are summarized, and the relationship between the spectral characteristics, rules and the structures is described. According to the fragmentation rules, NMR and UV spectral characteristics, 24 constituents of different types in the fractions from L. brevicalyx of the same genus were structurally characterized on the basis of HPLC/HRMS, HPLC-UV/ESI-MSn, HPLC/1H NMR and HPLC/1H-1H COSY rapidly. Of these, six (10, 13, 14, 16, 17 and 23) are new compounds and all of them are reported from L. brevicalyx for the first time. The aim is to develop an effective analytical method for on-line structural identification of natural products with molecular diversity in plants, and to guide the rapid and direct isolation of novel compounds by chemical screening.
电喷雾电离串联质谱与高效液相色谱联用（HPLC/ESI-MSn）以及液相色谱与核磁共振光谱联用（HPLC/NMR），已被广泛用于天然产物的在线分析、代谢物分析和药物杂质分析。在我们的上一篇论文中，我们报道了一种用于同一类痕量生物碱结构鉴定的在线分析方法。然而，植物中成分的结构类型多种多样，如黄酮类、萜类和甾体类。建立一种有效的分析方法用于在线鉴定植物提取物中具有分子多样性的成分的结构非常重要。因此，在本研究中，通过ESI-MSn研究了从短萼黄杞中分离得到的一些芪类、间苯三酚类和黄酮类化合物的裂解模式。总结了它们的裂解规律和紫外特征，并描述了光谱特征、规律与结构之间的关系。根据裂解规律、核磁共振和紫外光谱特征，基于HPLC/HRMS、HPLC-UV/ESI-MSn、HPLC/1H NMR和HPLC/1H-1H COSY快速对同一属短萼黄杞馏分中24种不同类型的成分进行了结构表征。其中，有6种（10、13、14、16、17和23）是新化合物，且均首次从短萼黄杞中报道。目的是开发一种有效的分析方法用于在线鉴定植物中具有分子多样性的天然产物的结构，并通过化学筛选指导新型化合物的快速直接分离。
