Research Article

A comparison of capillary-scale LC–NMR with alternative techniques: spectroscopic and practical considerations†

  1. Richard J. Lewis,
  2. Michael A. Bernstein,
  3. Sara J. Duncan,
  4. Chris J. Sleigh*

Article first published online: 27 JUL 2005

DOI: 10.1002/mrc.1614

Issue

Magnetic Resonance in Chemistry

Magnetic Resonance in Chemistry

Special Issue: Hyphenated NMR Techniques, Guest Editor: Professor Klaus Albert, University of Tübingen, Germany

Volume 43, Issue 9, pages 783–789, September 2005

Additional Information

How to Cite

Lewis, R. J., Bernstein, M. A., Duncan, S. J. and Sleigh, C. J. (2005), A comparison of capillary-scale LC–NMR with alternative techniques: spectroscopic and practical considerations. Magnetic Resonance in Chemistry, 43: 783–789. doi: 10.1002/mrc.1614

Author Information

  1. Department of Physical and Metabolic Science, AstraZeneca R & D Charnwood, Bakewell Road, Loughborough LE11 5RH, UK

*Department of Physical and Metabolic Science, AstraZeneca R & D Charnwood, Bakewell Road, Loughborough LE11 5RH, UK.

  1. †

    Presented as part of a special issue on Hyphenated NMR Techniques

Publication History

  1. Issue published online: 27 JUL 2005
  2. Article first published online: 27 JUL 2005
  3. Manuscript Accepted: 12 APR 2005
  4. Manuscript Revised: 4 APR 2005
  5. Manuscript Received: 29 SEP 2004

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Keywords:

  • NMR;
  • 1H NMR;
  • LC–NMR;
  • capillary LC;
  • cryoprobe;
  • solid-phase extraction;
  • off-line purification;
  • metabolite identification

Abstract

Experimental and practical details for the use of capillary LC (CapLC)–NMR are reported. The capillary NMR probe has high sensitivity and excellent flow characteristics and we found CapLC–NMR to be best suited to samples that are truly mass limited. CapLC–NMR relies on good capillary-scale chromatography where highly concentrated peaks with a volume closely matched to the NMR flow cell are achievable. Provided that the loading capacity of the capillary column is not limiting, the combination of high sensitivity and high solvent suppression quality makes CapLC–NMR an excellent choice. For many real samples, however, the loading is limiting and we found the combination of LC–SPE–MS–NMR with a cryoprobe enables more material to be purified for NMR analysis, while retaining sensitivity. Copyright © 2005 John Wiley & Sons, Ltd.

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