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Related Experiment Videos

Double-quantum filtered rotational-echo double resonance.

Shigeru Matsuoka1, Jacob Schaefer

  • 1Department of Chemistry, Washington University, St. Louis, MO 63130, USA.

Journal of Magnetic Resonance (San Diego, Calif. : 1997)
|September 30, 2006
PubMed
Summary
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This study introduces a double-quantum filter (DQF) to eliminate background noise in 13C{15N} rotational-echo double-resonance (REDOR) experiments, enabling precise measurements of metabolic processes like glycine metabolism in plants.

Area of Science:

  • Nuclear Magnetic Resonance Spectroscopy
  • Biophysical Chemistry
  • Metabolomics

Background:

  • Natural abundance 13C background signals complicate 13C{15N} rotational-echo double-resonance (REDOR) experiments.
  • Accurate quantitative measurements in biological systems require methods to suppress background interferences.

Purpose of the Study:

  • To develop and validate a double-quantum filter (DQF) for 13C{15N} REDOR experiments.
  • To enhance the sensitivity and accuracy of 13C{15N} REDOR by removing natural-abundance 13C signals.
  • To quantitatively measure metabolic pathways in biological samples using the DQF-REDOR technique.

Main Methods:

  • Utilized homonuclear scalar coupling of directly bonded 13C-13C pairs to create a DQF.
  • Coincident DQF scalar and REDOR dipolar evolution periods were employed to maximize sensitivity for weak 13C-15N dipolar couplings.

Related Experiment Videos

  • Applied 13C{15N} DQF-REDOR to a test sample of mixed recrystallized labeled alanines and to a single soybean leaf labeled with 13CO2.

    • Main Results:

    • The DQF effectively removed natural-abundance 13C background signals in 13C{15N} REDOR experiments.
    • Calculated and observed 13C{15N} DQF-REDOR dephasings showed excellent agreement for the alanine test sample.
    • Quantitative measurement of glycine metabolism in a soybean leaf was achieved with no discernible background interferences.

    Conclusions:

    • The developed 13C-13C DQF is a powerful tool for background suppression in 13C{15N} REDOR NMR.
    • This method significantly improves sensitivity and accuracy for studying metabolic processes in biological systems.
    • 13C{15N} DQF-REDOR enables precise, interference-free quantitative metabolic analysis.