Homonuclear Zero-Quantum Recoupling in Fast Magic-Angle-Spinning NMR,

A. Brinkmann, J. Schmedt auf der Günne, and M. H. Levitt,
2nd Alpine Conference on Solid-State NMR, Chamonix-Mont Blanc, France (Sep. 2001), poster.

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Recently a new class of rotor-synchronized pulse sequences was described, which are characterized by three integers, called the symmetry numbers [1,2]. The symmetry theory of these pulse sequences [1,2] is used to design pulse sequences which implement zero-quantum homonuclear dipolar recoupling, while decoupling isotropic chemical shifts and chemical shift anisotropies in first order average Hamiltonian theory [3]. Supercycles and composite pulses are employed to improve the robustness of these sequences with respect to chemical shifts. We show that the RFDR sequence [4] may be explained using symmetry arguments.

One of the major applications of zero-quantum recoupling sequences is the homonuclear correlation spectroscopy of uniformly 13C-labelled peptides and proteins. We identify sequences which prove to be good candidates for operation at high spinning frequencies and magnetic fields. These sequences are compared with existing zero-quantum recoupling sequences by numerical simulations. The new sequences are demonstrated experimentally by obtaining longitudinal magnetization transfer curves for [2-13C, 15N]-glycine and by acquiring 2D homonuclear correlation spectra of [U-13C]-L-tyrosine.

  1. M. Carravetta, M. Edén, X. Zhao, A. Brinkmann, and M. H. Levitt, Symmetry Principles for the design of radiofrequency pulse sequences in the nuclear magnetic resonance of rotating solids, Chem. Phys. Lett. 321, 205-215, (2000). Abstract, Full text (PDF).
  2. A. Brinkmann, and M. H. Levitt, Symmetry principles in the nuclear magnetic resonance of spinning solids: Heteronuclear recoupling by generalized Hartmann-Hahn sequences, J. Chem. Phys. 115, 357-384, (2001). Abstract, Full text (PDF).
  3. A. Brinkmann, J. Schmedt auf der Günne, and M. H. Levitt, Homonuclear Zero-Quantum Recoupling in Fast Magic-Angle Spinning Nuclear Magnetic Resonance, J. Mag. Res. 156, 79-96, (2002). Abstract, Full text (PDF).
  4. A. E. Bennett, J. H. Ok, R. G. Griffin, and S. Vega, Chemical shift correlation spectroscopy in rotating solids: Radio frequency-driven dipolar recoupling and longitudinal exchange, J. Chem. Phys. 96, 8624-8627, (1992).
Dr. Andreas Brinkmann
Measurement Science and Standards
National Research Council
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