Identification of chemical constituents in two traditional Chinese medicine formulae by liquid chromatography-mass spectrometry and off-line nuclear magnetic resonance.
作者： Shufang Wang , Yunxiang Zhu , Qing Shao , Yi Wang , Xiaohui Fan
DOI: 10.1016/J.JPBA.2015.09.007
关键词: Mass spectrometry 、 Chromatography 、 Chemical constituents 、 Tandem mass spectrometry 、 Glycoside 、 Epimer 、 Nuclear magnetic resonance spectroscopy 、 Chemistry 、 Liquid chromatography–mass spectrometry 、 Off line
摘要: There have been increasing works on identification of the chemical constituents in traditional Chinese medicines (TCMs) by liquid chromatography-mass spectrometry (LC-MS). However, isomers cannot be distinguished generally only MS data, and structures unknown compounds confirmed. In this study, semi-preparative LC guided LC-MS was used to prepare microscale followed off-line NMR analysis confirm their structures. This approach applied identifying two TCM formulae, Zhi-Zi-Gan-Cao-Chi-Tang (ZZGCCT) Zhi-Zi-Bai-Pi-Tang (ZZBPT). A total number 119 were identified tentatively or unambiguously LC-IT-MS, LC-Q-TOF-MS, NMR. Among them, 20 characterized comparing with reference substances. addition, 21 without substances prepared for following 1D-NMR and/or 2D-NMR analysis, MS, 1D-NMR, 2D-NMR. Two triterpenoid glycosides (compounds 134 140) one flavonoid glycoside (compound 62a 62b) showed novel compounds. Compounds 125 129, as well 62a,b, epimers.
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