Inverse detection and heteronuclear editing in 1H-15N correlation and 1H-1H double-quantum NMR spectroscopy in the solid state under fast MAS.
Signal enhancement in heteronuclear correlation spectra as well as signal selection in 1H experiments can be achieved through inverse, i.e., 1H, detection in the solid state under fast MAS conditions. Using recoupled polarization transfer (REPT), a heteronuclear 1H-15N single-quantum correlation (HSQC) experiment is presented whose symmetrical design allows the frequency dimensions to be easily interchanged. By observing the 15N dimension indirectly and detecting on 1H, the sensitivity is experimentally found to be increased by factors between 5 and 10 relative to conventional 15N detection. In addition, the inverse 1H-15N REPT-HSQC scheme can be readily used as a filter for the 1H signal. As an example, we present the combination of such a heteronuclear filter with a subsequent 1H-1H DQ experiment, yielding two-dimensional 15N-edited 1H-1H DQ MAS spectra. In this way, specific selection or suppression of 1H resonances is possible in solid-state MAS experiments, by use of which the resolution can be improved and information can be unravelled in 1H spectra.
Schnell
I
I
Max-Planck-Institut für Polymerforschung, Mainz, D-55021, Germany.
Langer
B
B
Söntjens
S H
SH
van Genderen
M H
MH
Sijbesma
R P
RP
Spiess
H W
HW