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Related Experiment Videos

Microflow NMR: concepts and capabilities.

Dean L Olson1, James A Norcross, Mark O'Neil-Johnson

  • 1Protasis/MRM Corporation, 101 Tomaras Avenue, Savoy, Illinois 61874, USA. dolson@microNMR.com

Analytical Chemistry
|May 18, 2004
PubMed
Summary
This summary is machine-generated.

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A new capillary microflow probe offers NMR sensitivity comparable to cryoprobes for limited samples. This advanced NMR probe enables rapid analysis of small sample volumes, improving mass sensitivity and spectral acquisition times.

Area of Science:

  • Analytical Chemistry
  • Spectroscopy
  • Nuclear Magnetic Resonance (NMR)

Background:

  • Analyzing volume- or mass-limited samples in NMR spectroscopy presents significant challenges.
  • Existing NMR probes may lack the sensitivity or efficiency required for trace analysis.
  • Development of specialized probes is crucial for advancing microscale NMR applications.

Purpose of the Study:

  • To identify key principles and parameters for selecting NMR probes for limited sample analysis.
  • To introduce and characterize a novel capillary-based microflow NMR probe.
  • To demonstrate the probe's capabilities for analyzing small quantities of complex molecules.

Main Methods:

  • Design and construction of a capillary microflow NMR probe with a 1.5 microL observe volume and fused silica flow path.

Related Experiment Videos

  • Integration of proton and carbon observe channels, deuterium lock, and z-gradient capability.
  • Evaluation of four sample injection modes: manual, manual-assisted, automated, and capillary HPLC.

    • Main Results:

    • The microflow probe achieved mass sensitivity comparable to cryoprobes with a significantly smaller observe volume (1.5 microL).
    • Successful acquisition of 1D proton spectra from 1 nmol of sucrose in 10 min.
    • Acquisition of heteronuclear multiple-quantum coherence (HMQC) spectra from 15 microg of sucrose in under 15 hours.
    • Rapid acquisition of various 2D NMR spectra (gCOSY, gHMQC, gHMBC) for the natural product muristerone A.

    Conclusions:

    • The capillary microflow NMR probe is highly effective for analyzing volume- and mass-limited samples.
    • The probe offers advantages in sensitivity, efficiency, and reduced sample dispersion.
    • The described injection modes provide flexibility for diverse analytical workflows in NMR spectroscopy.