Identification of chemical constituents in two traditional Chinese medicine formulae by liquid chromatography-mass spectrometry and off-line nuclear magnetic resonance
Identification of chemical constituents in two traditional Chinese medicine formulae by liquid chromatography-mass spectrometry and off-line nuclear magnetic resonance
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DOI：
10.1016/j.jpba.2015.09.007
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发表时间：
2016-01-05
影响因子：
3.4
通讯作者：
Cheng, Yiyu
中科院分区：
文献类型：
--
作者：
Wang, Shufang;Zhu, Yunxiang;Cheng, Yiyu
液相色谱-质谱联用技术在中药化学成分鉴定方面的研究越来越多。然而，一般来说，仅凭质谱数据无法区分异构体，未知化合物的结构也无法确定。本研究采用液相色谱-质谱引导半制备液相色谱制备微尺度异构体，并通过离线NMR分析确定其结构。应用该方法对栀子肝草脂汤（ZZGCCT）和栀子白皮汤（ZZBPT）两方进行了成分鉴别。通过LC-IT-MS， LC-Q-TOF-MS和NMR初步或明确鉴定了119个成分。其中有20个成分与对照品进行了明确的表征。此外，制备了21个无对照物质的成分，用于后续的1D-NMR和/或2D-NMR分析，并通过MS、1D-NMR和2D-NMR对其结构进行了明确的鉴定。两种三萜苷（化合物134和140）和一种黄酮类苷（化合物62a和62b）为新化合物。化合物125、129和62a、b为外显子。(C) 2015 Elsevier B.V.版权所有
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 by MS data, and the structures of unknown compounds cannot be confirmed. In this study, semi-preparative LC guided by LC-MS was used to prepare the isomers in microscale followed by off-line NMR analysis to confirm their structures. This approach was applied to identifying the constituents in two TCM formulae, Zhi-Zi-Gan-Cao-Chi-Tang (ZZGCCT) and Zhi-Zi-Bai-Pi-Tang (ZZBPT). A total number of 119 constituents were identified tentatively or unambiguously by LC-IT-MS, LC-Q-TOF-MS, and NMR. Among them, 20 constituents were characterized unambiguously by comparing with the reference substances. In addition, 21 constituents without reference substances were prepared for the following 1D-NMR and/or 2D-NMR analysis, and their structures were unambiguously identified by MS, 1D-NMR, and 2D-NMR. Two triterpenoid glycosides (compounds 134 and 140) and one flavonoid glycoside (compound 62a or 62b) were showed to be novel compounds. Compounds 125 and 129, as well as 62a,b, were epimers. (C) 2015 Elsevier B.V. All rights reserved.