The application of submicro inverse-detection gradient (SMIDG) NMR probe technology at 600 MHz is demonstrated for the rapid acquisition of both 1 H-13 C and 1 H-15 N heteronuclear chemical shift correlation data. Using a 750 µg (ca 1.5 µmol, MW 505) sample of the complex spirononacyclic alkaloid cr
Inverse Detection and Heteronuclear Editing in 1H–15N Correlation and 1H–1H Double-Quantum NMR Spectroscopy in the Solid State under Fast MAS
✍ Scribed by Ingo Schnell; Benedikt Langer; Serge H.M. Söntjens; Marcel H.P. van Genderen; Rint P. Sijbesma; Hans Wolfgang Spiess
- Publisher
- Elsevier Science
- Year
- 2001
- Tongue
- English
- Weight
- 371 KB
- Volume
- 150
- Category
- Article
- ISSN
- 1090-7807
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✦ Synopsis
Signal enhancement in heteronuclear correlation spectra as well as signal selection in 1 H experiments can be achieved through inverse, i.e., 1 H, detection in the solid state under fast MAS conditions. Using recoupled polarization transfer (REPT), a heteronuclear 1 H-15 N single-quantum correlation (HSQC) experiment is presented whose symmetrical design allows the frequency dimensions to be easily interchanged. By observing the 15 N dimension indirectly and detecting on 1 H, the sensitivity is experimentally found to be increased by factors between 5 and 10 relative to conventional 15 N detection. In addition, the inverse 1 H-15 N REPT-HSQC scheme can be readily used as a filter for the 1 H signal. As an example, we present the combination of such a heteronuclear filter with a subsequent 1 H-1 H DQ experiment, yielding two-dimensional 15 N-edited 1 H-1 H DQ MAS spectra. In this way, specific selection or suppression of 1 H resonances is possible in solid-state MAS experiments, by use of which the resolution can be improved and information can be unravelled in 1 H spectra.
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