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Directly and indirectly detected through-bond heteronuclear correlation solid-state NMR spectroscopy under fast MAS

TitleDirectly and indirectly detected through-bond heteronuclear correlation solid-state NMR spectroscopy under fast MAS
Publication TypeJournal Article
Year of Publication2009
AuthorsMao KM, Pruski M
Journal TitleJournal of Magnetic Resonance
Volume201
Pages165-174
Date Published12/01
ISBN Number1090-7807
Accession NumberISI:000272006600007
Keywordsangle-spinning nmr, coal, decoupling sequences, fast mas, functionalized mesoporous silicas, hetcor, indirect detection, inept, j-coupling, nuclear-magnetic-resonance, peptide, pmlg, proton spectroscopy, rotating, sensitivity enhancement, solid-state nmr
Abstract

Two-dimensional through-bond H-1{C-13} Solid-state NMR experiments utilizing fast magic angle spinning (MAS) and homonuclear multipulse H-1 decoupling are presented. Remarkable efficiency of polarization transfer can be achieved at MAS rates exceeding 40 kHz, which is instrumental in these measurements. Schemes utilizing direct and indirect detection of heteronuclei are compared in terms of resolution and sensitivity. A simple procedure for optimization of H-1 homonuclear decoupling sequences under these conditions is proposed. The capabilities of these techniques were confirmed on two naturally abundant solids, tripeptide N-formyl-L-methionyl-L-leucyl-L-phenylalanine (f-MLF-OH) and brown coal. (C) 2009 Elsevier Inc. All rights reserved.
URL<Go to ISI>://000272006600007
DOI10.1016/J.Jmr.2009.09.004