Document Detail


Hyphenation of capillary HPLC to microcoil (1)H NMR spectroscopy for the determination of tocopherol homologues.
MedLine Citation:
PMID:  15117207     Owner:  NLM     Status:  MEDLINE    
Abstract/OtherAbstract:
Highly selective reversed phases (C(30) phases) are self-packed in 250 microm inner diameter fused-silica capillaries and employed for capillary HPLC separation of shape-constrained natural compounds (tocopherol homologues, vitamin E). Miniaturized hyphenated systems such as capillary HPLC-ESI-MS (positive ionization mode) and, with special emphasis, continuous-flow capillary HPLC- NMR are used for structural determination of the separated compounds. Despite the small amount of sample available (1.33 microg of each tocopherol), the authors have been able to monitor the capillary HPLC separation under continuous-flow (1)H NMR conditions, thus allowing an immediate peak identification. Further structural assignment was carried out in the stopped-flow NMR mode as shown, for example, by a 2D (1)H,(1)H COSY NMR spectrum of alpha-tocopherol. We demonstrate in this paper the considerable potential of hyphenated capillary separations coupled to MS and NMR for the investigation of restricted amounts of sample.
Authors:
Manfred Krucker; Annette Lienau; Karsten Putzbach; Marc David Grynbaum; Paul Schuler; Klaus Albert
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Publication Detail:
Type:  Journal Article; Research Support, Non-U.S. Gov't    
Journal Detail:
Title:  Analytical chemistry     Volume:  76     ISSN:  0003-2700     ISO Abbreviation:  Anal. Chem.     Publication Date:  2004 May 
Date Detail:
Created Date:  2004-04-30     Completed Date:  2005-02-15     Revised Date:  2006-11-15    
Medline Journal Info:
Nlm Unique ID:  0370536     Medline TA:  Anal Chem     Country:  United States    
Other Details:
Languages:  eng     Pagination:  2623-8     Citation Subset:  IM    
Affiliation:
Institute of Organic Chemistry, University of Tübingen, Auf der Morgenstelle 18, D-72076 Tübingen, Germany.
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MeSH Terms
Descriptor/Qualifier:
Chromatography, High Pressure Liquid / instrumentation,  methods
Magnetic Resonance Spectroscopy / instrumentation,  methods*
Molecular Structure
Sensitivity and Specificity
Silicon Dioxide / chemistry
Spectrometry, Mass, Electrospray Ionization / methods
Tocopherols / analysis*,  chemistry
Chemical
Reg. No./Substance:
1406-66-2/Tocopherols; 7631-86-9/Silicon Dioxide

From MEDLINE®/PubMed®, a database of the U.S. National Library of Medicine


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