Experimental aspects of proton NMR spectroscopy in solids using phase-modulated homonuclear dipolar decoupling.
In this paper we demonstrate experimentally that the continuously phase-modulated homonuclear decoupling sequence DUMBO-1 is suitable for high-resolution proton NMR spectroscopy of rigid solids. Over a wide range of experimental conditions, we show on the model sample L-alanine as well as on small peptides that proton linewidths of less than 0.5 ppm can be obtained under DUMBO-1 decoupling. In particular the DUMBO-1 sequence yields well resolved proton spectra both at slow and fast MAS. The DUMBO-1 decoupling scheme can in principle be inserted in any multi-nuclear or multi-dimensional solid-state NMR experiment which requires a high-resolution 1H dimension. An example is provided with the 13C-1H MAS-J-HMQC experiment.
Lesage
Anne
A
UMR-5532 CNRS/ENS, Laboratoire de Recherche Conventionné du CEA (23V), Ecole Normale Supérieure de Lyon, 69364 Lyon, France.
Sakellariou
Dimitris
D
Hediger
Sabine
S
Eléna
Bénédicte
B
Charmont
Patrick
P
Steuernagel
Stefan
S
Emsley
Lyndon
L
D000409:Alanine / Q000737:chemistry; D000465:Algorithms; D002244:Carbon; D002247:Carbon Isotopes; D003461:Crystallography / Q000379:methods; D016572:Cyclosporine / Q000737:chemistry; D004151:Dipeptides / Q000737:chemistry; D009682:Magnetic Resonance Spectroscopy / Q000379:methods*; D008280:Magnetics; D019906:Nuclear Magnetic Resonance, Biomolecular / Q000295:instrumentation / Q000379:methods*; D011208:Powders; D011487:Protein Conformation; D011506:Proteins / Q000737:chemistry*; D011522:Protons; D011786:Quality Control; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D012815:Signal Processing, Computer-Assisted; D013113:Spin Labels
D002247:Carbon Isotopes; D004151:Dipeptides; D011208:Powders; D011506:Proteins; D011522:Protons; D013113:Spin Labels; C038047:alanylaspartic acid; D002244:Carbon; D016572:Cyclosporine; D000409:Alanine