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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
Xiao, HB; Krucker, M; Putzbach, K; Albert, K
KeywordCapillary Lc-nmr Natural Products Radix Astragali Structure Elucidation Hplc-ms
Source PublicationJOURNAL OF CHROMATOGRAPHY A
2005-03-04
DOI10.1016/j.chroma.2005.01.015
Volume1067Issue:1-2Pages:135-143
Indexed BySCI
SubtypeArticle
WOS HeadingsScience & Technology ; Life Sciences & Biomedicine ; Physical Sciences
WOS SubjectBiochemical Research Methods ; Chemistry, Analytical
WOS Research AreaBiochemistry & Molecular Biology ; Chemistry
WOS KeywordSOLID-PHASE DISPERSION ; RESOLUTION NMR-SPECTROSCOPY ; NATURAL-PRODUCTS ; IDENTIFICATION ; HPLC ; HYPHENATION ; SEPARATION ; ELECTROCHROMATOGRAPHY ; CONSTITUENTS ; COMBINATION
AbstractMiniaturization 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.
Language英语
WOS IDWOS:000227925800011
Citation statistics
Cited Times:50[WOS]   [WOS Record]     [Related Records in WOS]
Document Type期刊论文
Identifierhttp://cas-ir.dicp.ac.cn/handle/321008/139759
Collection中国科学院大连化学物理研究所
Affiliation1.Univ Tubingen, Inst Organ Chem, D-72076 Tubingen, Germany
2.Chinese Acad Sci, Dalian Inst Chem Phys, Dalian 116011, Peoples R China
Recommended Citation
GB/T 7714
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.
APA Xiao, HB,Krucker, M,Putzbach, K,&Albert, K.(2005).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.JOURNAL OF CHROMATOGRAPHY A,1067(1-2),135-143.
MLA Xiao, HB,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".JOURNAL OF CHROMATOGRAPHY A 1067.1-2(2005):135-143.
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