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题名: Capillary liquid chromatography-microcoil H-1 nuclear magnetic resonance spectroscopy and liquid chromatography-ion trap mass spectrometry for on-line structure elucidation of isoflavones in Radix astragali
作者: Xiao, HB;  Krucker, M;  Putzbach, K;  Albert, K
关键词: capillary LC-NMR ;  natural products ;  Radix astragali ;  structure elucidation ;  HPLC-MS
刊名: JOURNAL OF CHROMATOGRAPHY A
发表日期: 2005-03-04
DOI: 10.1016/j.chroma.2005.01.015
卷: 1067, 期:1-2, 页:135-143
收录类别: SCI
文章类型: Article
WOS标题词: Science & Technology ;  Life Sciences & Biomedicine ;  Physical Sciences
类目[WOS]: Biochemical Research Methods ;  Chemistry, Analytical
研究领域[WOS]: Biochemistry & Molecular Biology ;  Chemistry
英文摘要: Miniaturization and hyphenation of chromatographic separation techniques to nuclear magnetic resonance spectroscopy is being increasingly demanded in the field of biomedical, drug metabolite and natural product analysis. Herein, capillary liquid chromatography was coupled on-line to microcoil H-1 nuclear magnetic resonance spectroscopy (capLC-NMR) equipped with a 1.5 mu L solenoidal probe for structure elucidation of isoflavones in Radix astragali. The extract was screened by HPLC-UV-MS as the preliminary step and four major peaks were identified tentatively by ion trap mass spectrometry molecular weights and characteristic fragments. Then, stopped-flow capLC-UV-NMR was performed using 33 mu g extract injected on-column. The four peaks were parked manually in the micro probe one by one and corresponding H-1 NMR spectra were recorded with good resolutions under the applied capLC-NMR conditions (120 and 220 ng injected on-column for peaks 2 and 4, respectively). All aromatic regions of H-1 NMR spectra correlated well to the characteristic signals of isoflavone aglycone protons. And the signal corresponding to the anomeric proton of the glucopyranoside of isoflavone glycoside was also obtained for peak 1. Therefore, these four peaks are determined as calycosin-7-O-beta-D-glucopyranoside (1), ononin (2), calycosin (3) and formononetin (4) unambiguously. The capLC-NMR results indicate that this hyphenated technique could be used for the determination of a great variety of natural products from small sample amounts, e.g., only 5 g R. astragali in this study. (c) 2005 Elsevier B.V. All rights reserved.
关键词[WOS]: SOLID-PHASE DISPERSION ;  RESOLUTION NMR-SPECTROSCOPY ;  NATURAL-PRODUCTS ;  IDENTIFICATION ;  HPLC ;  HYPHENATION ;  SEPARATION ;  ELECTROCHROMATOGRAPHY ;  CONSTITUENTS ;  COMBINATION
语种: 英语
WOS记录号: WOS:000227925800011
Citation statistics: 
内容类型: 期刊论文
URI标识: http://cas-ir.dicp.ac.cn/handle/321008/139759
Appears in Collections:中国科学院大连化学物理研究所_期刊论文

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作者单位: 1.Univ Tubingen, Inst Organ Chem, D-72076 Tubingen, Germany
2.Chinese Acad Sci, Dalian Inst Chem Phys, Dalian 116011, Peoples R China

Recommended Citation:
Xiao, HB,Krucker, M,Putzbach, K,et al. Capillary liquid chromatography-microcoil H-1 nuclear magnetic resonance spectroscopy and liquid chromatography-ion trap mass spectrometry for on-line structure elucidation of isoflavones in Radix astragali[J]. JOURNAL OF CHROMATOGRAPHY A,2005,1067(1-2):135-143.
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