Inverse detection and heteronuclear editing in 1H-15N correlation and 1H-1H double-quantum NMR spectroscopy in the solid state under fast MAS

被引:60
作者
Schnell, I
Langer, B
Söntjens, SHM
van Genderen, MHP
Sijbesma, RP
Spiess, HW
机构
[1] Max Planck Inst Polymerforsch, D-55021 Mainz, Germany
[2] Eindhoven Univ Technol, Lab Macromol & Organ Chem, NL-5600 MB Eindhoven, Netherlands
关键词
inverse detection; heteronuclear editing; double-quantum MAS spectroscopy; heteronuclear correlation spectroscopy; recoupled polarization transfer;
D O I
10.1006/jmre.2001.2312
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
Signal enhancement in heteronuclear correlation spectra as well as signal selection in H-1 experiments can be achieved through inverse, i.e., H-1, detection in the solid state under fast MAS conditions. Using recoupled polarization transfer (REPT), a heteronuclear H-1-N-15 single-quantum correlation (HSQC) experiment is presented whose symmetrical design allows the frequency dimensions to be easily interchanged. By observing the N-15 dimension indirectly and detecting on H-1, the sensitivity is experimentally found to be increased by factors between 5 and 10 relative to conventional N-15 detection. In addition, the inverse H-1-N-15 REPT-HSQC scheme can be readily used as a filter for the H-1 signal. As an example, we present the combination of such a heteronuclear filter with a subsequent H-1-H-1 DQ experiment, yielding two-dimensional N-15-edited H-1-H-1 DQ MAS spectra. In this way, specific selection or suppression of H-1 resonances is possible in solid-state MAS experiments, by use of which the resolution can be improved and information can be unravelled in H-1 spectra. (C) 2001 Academic Press.
引用
收藏
页码:57 / 70
页数:14
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