Resolution enhancement in MAS solid-state NMR by application of 13C homonuclear scalar decoupling during acquisition

Journal of Magnetic Resonance

Volumn 172, Issue 1, 2005, Pages 56-62

  Chevelkov, Veniamin ^a,b   Chen, Zhongjing ^a,b   Bermel, Wolfgang ^c   Reif, Bernd ^a,d  

^a LEIBNIZ INSTITUT FÜR MOLEKULARE PHARMAKOLOGIE   (Germany)

^b TECHNICAL UNIVERSITY OF MUNICH   (Germany)

^c BRUKER BIOSPIN GMBH   (Germany)

^d CHARITÉ UNIVERSITÄTSMEDIZIN BERLIN   (Germany)

Author keywords

Adiabatic pulses NMR; High resolution MAS solid state NMR; Homonuclear scalar decoupling; Spectral resolution and sensitivity

Indexed keywords

CORRELATION METHODS; FREQUENCIES; LIGHT POLARIZATION; MAGNETIZATION; MEMBRANES; PHASE SHIFT; PROTEINS;

ADIABATIC PULSES; HIGH RESOLUTION MAS SOLID-STATE NMR; HOMONUCLEAR SCALAR DECOUPLING; SPECTRAL RESOLUTION AND SENSITIVITY;

NUCLEAR MAGNETIC RESONANCE;

ACETYLCYSTEINE; AMINO ACID; CARBON; LEUCINE; NITROGEN; PEPTIDE; VALINE;

ARTICLE; CHEMISTRY; METHODOLOGY; NUCLEAR MAGNETIC RESONANCE; SIGNAL PROCESSING;

ACETYLCYSTEINE; AMINO ACIDS; CARBON ISOTOPES; LEUCINE; NITROGEN ISOTOPES; NUCLEAR MAGNETIC RESONANCE, BIOMOLECULAR; PEPTIDES; SIGNAL PROCESSING, COMPUTER-ASSISTED; VALINE;

EID: 10444273907     PISSN: 10907807     EISSN: None     Source Type: Journal    
DOI: 10.1016/j.jmr.2004.09.017     Document Type: Article

References (37)

1. F. Castellani, B.J.v. Rossum, A. Diehl, K. Rehbein, H. Oschkinat, Structure of a protein determined by solid-state magic-angle spinning NMR spectroscopy, Nature 420 (2002) 98-102.
2. C.M. Rienstra, L. Tucker-Kellogg, C.P. Jaroniec, M. Hohwy, B. Reif, T. Lozano-Peres, B. Tidor, R.G. Griffin, De novo structure determination of peptides and proteins with high resolution solid state MAS NMR, Proc. Natl. Acad. Sci. USA 99 (2002) 10260-10265.
3. J. Pauli, B.J.v. Rossum, H. Forster, H.J.M.d. Groot, H. Oschkinat, Sample optimization and identification of signal patterns of amino acid side chains in 2D RFDR spectra of the alpha-spectrin SH3 domain, J. Magn. Reson. 143 (2000) 411-416.
4. M. Ernst, M.A. Meier, T. Tuherm, A. Samoson, B.H. Meier, Low-power high-resolution solid-state NMR of peptides and proteins, J. Am. Chem. Soc. 126 (2004) 4764-4765.
5. M. Ernst, A. Samoson, B.H. Meier, Low-power XiX decoupling in MAS NMR experiments, J. Magn. Reson. 163 (2003) 332-339.
6. A. Bielecki, A.C. Kolbert, M.H. Levitt, Frequency-switched pulse sequence - homonuclear decoupling and dilute spin NMR in solids, Chem. Phys. Lett. 155 (1989) 341-346.
7. E. Vinogradov, P.K. Madhu, S. Vega, High-resolution proton solid-state NMR spectroscopy by phase-modulated Lee-Goldburg experiment, Chem. Phys. Lett. 314 (1999) 443-450.
8. A.E. Bennett, C.M. Rienstra, M. Auger, K.V. Lakshmi, R.G. Griffin, Heteronuclear decoupling in rotating solids, J. Chem. Phys. Lett. 103 (1995) 6951-6958.
9. M. Rosay, J.C. Lansing, K.C. Haddad, W.W. Bachovchin, J. Herzfeld, R.J. Temkin, R.G. Griffin, High-frequency dynamic nuclear polarization in MAS spectra of membrane and soluble proteins, J. Am. Chem. Soc. 125 (2003) 13626-13627.
10. B. Reif, R.G. Griffin, H-1 detected H-1, N-15 correlation spectroscopy in rotating solids, J. Magn. Reson. 160 (2003) 78-83.
11. E.K. Paulson, C.R. Morcombe, V. Gaponenko, B. Dancheck, R.A. Byrd, K.W. Zilm, Sensitive high resolution inverse detection NMR spectroscopy of proteins in the solid state, J. Am. Chem. Soc. 125 (2003) 15831-15836.
12. V. Chevelkov, B.J.v. Rossum, F. Castellani, K. Rehbein, A. Diehl, M. Hohwy, S. Steuernagel, F. Engelke, H. Oschkinat, B. Reif, H-1 detection in MAS solid-state NMR spectroscopy of biomacromolecules employing pulsed field gradients for residual solvent suppression, J. Am. Chem. Soc. 125 (2003) 7788-7789.
13. A. McDermott, T. Polenova, A. Bockmann, K.W. Zilm, E.K. Paulsen, R.W. Martin, G.T. Montelione, Partial NMR assignments for uniformly (C-13, N-15)-enriched BPTI in the solid state, J. Biomol. NMR 16 (2000) 209-219.
14. J. Cavanagh, W. Fairbrother, A.G. Palmer, N.J. Skelton, Protein NMR Spectroscopy: Principles and Practice, Academic Press, New York, 1996, pp. 480-481.
15. M. Sattler, J. Schleucher, C. Griesinger, Heteronuclear multidimensional NMR experiments for the structure determination of proteins in solution employing pulsed field gradients, Prog. NMR Spectrosc. 34 (1999) 93-158.
16. D.M. LeMaster, D.M. Kushlan, Dynamical mapping of E. coli thioredoxin via C-13 NMR relaxation analysis, J. Am. Chem. Soc. 139 (1996) 9255-9264.
17. M. Hong, K. Jakes, Selective and extensive C-13 labeling of a membrane protein for solid-state NMR investigations, J. Biomol. NMR 14 (1999) 71-74.
18. R. Brüschweiler, C. Griesenger, O.W. Sorensen, R.R. Ernst, Combined use of hard and soft pulses for omega-1 decoupling in two-dimensional NMR-spectroscopy, J. Magn. Reson. 78 (1988) 178-185.
19. S.K. Straus, T. Bremi, R.R. Ernst, Resolution enhancement by homonuclear J decoupling in solid-state MAS NMR, Chem. Phys. Lett. 262 (1996) 709-715.
20. T.I. Igumenova, A.E. McDermott, Improvement of resolution in solid state NMR spectra with J-decoupling: an analysis of lineshape contribution in uniformly 13-C enriched amino acids and proteins, J. Magn. Reson, 164 (2003) 270-285.
21. L. Duma, S. Hediger, B. Brutscher, A. Boekmann, L. Emsley, Resolution enhancement in multidimensional solid-state NMR spectroscopy of proteins using spin-state selection, J. Am. Chem. Soc. 125 (2003) 11816-11817.
22. L. Duma, S. Hediger, A. Lesage, L. Emsley, Spin-state selection in solid-state NMR, J. Magn. Reson. 164 (2003) 187-195.
23. M.D. Sørensen, A. Meissner, O.W. Sørensen, C-13 natural abundance (SE)-E-3 and (SCT)-C-3 experiments for measurement of J coupling constants between C-13(alpha) or H-1(alpha) and other protons in a protein, J. Magn. Reson. 137 (1999) 237-242.
24. H. Matsuo, E. Kupce, H.J. Li, G. Wagner, Increased sensitivity in HNCA and HN(CO)CA experiments by selective C-beta decoupling, J. Magn. Reson. B 113 (1996) 91-96.
25. H. Matsuo, E. Kupce, G. Wagner, Resolution and sensitivity gain in HCCH-TOCSY experiments by homonuclear C-beta decoupling, J. Magn. Reson. B 113 (1996) 190-194.
26. W. Bermel, I. Bertini, I.C. Felli, R. Kummerle, R. Pierattelli, C-13 direct detection experiments on the paramagnetic oxidized monomeric copper, zinc superoxide dismutase, J. Am. Chem. Soc. 125 (2003) 16423-16429.
27. N.C. Nielsen, H. Bildsoe, H.J. Jakobsen, M.H. Levitt, Double-quantum homonuclear rotary resonance: efficient dipolar recovery in magic-angle spinning nuclear magnetic resonance, J. Chem. Phys. 101 (1994) 1805-1812.
28. T.G. Oas, R.G. Griffin, M.H. Levitt, Rotary resonance recoupling of dipolar interactions in solid-state nuclear magnetic resonance spectroscopy, J. Chem. Phys. 89 (1988) 692-695.
29. M.A. McCoy, L. Mueller, Selective shaped pulse decoupling in NMR-homonuclear [C-13] carbonyl decoupling, J. Am. Chem. Soc. 114 (1992) 2108-2112.
30. M.A. McCoy, L. Mueller, Selective decoupling, J. Magn. Reson. A 101 (1993) 122-130.
31. G.A. Morris, R. Freeman, Selective excitation in Fourier-transform nuclear magnetic resonance, J. Magn. Reson. 29 (1978) 433-462.
32. M.H. Levitt, R. Freeman, Composite pulse decoupling, J. Magn. Reson. 43 (1981) 502-507.
33. H. Cho, J. Baum, A. Pines, Iterative maps with multiple fixed-points for excitation of 2 level systems, J. Chem. Phys. 86 (1987) 3089-3106.
34. H.M. Cho, R. Tycko, A. Pines, J. Guckenheimer, Iterative maps for bistable excitation of 2-level systems, Phys. Rev. Lett. 56 (1986) 1905-1908.
35. F. Bloch, A. Siegert, Magnetic resonance for nonrotating fields, Phys. Rev. 57 (1940) 522-527.
36. M.L.d.l. Paz, K. Goldie, J. Zurdo, E. Lacroix, C.M. Dobson, A. Hoenger, L. Serrano, Proc. Natl. Acad. Sci. USA 99 (2002) 16052-16057.
37. R.R. Ernst, G. Bodenhausen, A. Wokaun, Principles of Nuclear Magnetic Resonance in One and Two Dimensions, Clarendon, Oxford, 1987.