Identification of cardiac glycosides in fractions from Periploca forrestii by high-performance liquid chromatography/diode-array detection/electrospray ionization multi-stage tandem mass spectrometry and liquid chromatography/nuclear magnetic resonance

被引:15
作者
Li, Yong
Wu, Xianfu
Li, Jianbei
Wang, Yinghong [1 ]
Yu, Shishan
Lv, Haining
Qu, Jing
Abliz, Zeper
Liu, Jing
Liu, Yuanyan
Du, Dan
机构
[1] Peking Union Med Coll, Inst Mat Med, Minist Educ, Key Lab Bioact Subst & Resources Utilizat Chinese, Beijing 100050, Peoples R China
来源
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES | 2010年 / 878卷 / 3-4期
关键词
Periploca forrestii; Cardiac glycosides; High-performance liquid chromatography/diode-array detection/electrospray ionization tandem mass spectrometry; Liquid chromatography/nuclear magnetic resonance; Structural characterization; RAPID STRUCTURAL DETERMINATION; CANCER; CARDENOLIDES; SAPONINS; OLEANDER; EXTRACT;
D O I
10.1016/j.jchromb.2009.12.008
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
Cardiac glycosides are a class of naturally Occurring Compounds that are characterized by some interesting biological activities and are widely distributed in the plant kingdom and can also be found in some animals. There is an interest in the chemical characterization of these molecules due to their toxicity and their use in medicines. In the Study reported here, a combination of electrospray ionization tandem mass spectrometry with high-performance liquid chromatography equipped with diode-array detector (HPLC-DAD/ESI-MSn), and hyphenation to both liquid chromatography and nuclear magnetic resonance spectroscopy (HPLC/NMR) were utilized for the on-line analyses of cardiac glycosides from Periploca forrestii, The fragmentation patterns and H-1 NMR spectra of nine isolated cardiac glycosides were investigated: their fragmentation rules and H-1 NMR spectral characteristics were summarized and applied to the structural identification of similar constituents in fractions from P. forrestii. As a result, a total of nine trace cardiac glycosides were tentatively determined by analyses of accurate molecular masses, representative fragment ions and characteristic H-1 NMR signals provided by HPLC/high-resolution mass spectrometry (HRMS), HPLC-DAD/ESI-MSn and HPLC/H-1 NMR experiments, respectively. Of these. eight (2-9) are new Compounds and one (1) is reported from P.forrestii for the first time. Results of the present study can benefit the rapid identification and targeted isolation of new cardiac glycosides from crude plant extracts. (C) 2009 Elsevier B.V. All rights reserved.
引用
收藏
页码:381 / 390
页数:10
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