Sensitivity-enhanced static 15N NMR of solids by 1h indirect detection

Journal of Magnetic Resonance
M Hong, S Yamaguchi

Abstract

A method for enhancing the sensitivity of 15N spectra of nonspinning solids through 1H indirect detection is introduced. By sampling the 1H signals in the windows of a pulsed spin-lock sequence, high-sensitivity 1H spectra can be obtained in two-dimensional (2D) spectra whose indirect dimension yields the 15N chemical shift pattern. By sacrificing the 1H chemical shift information, sensitivity gains of 1.8 to 2.5 for the 15N spectra were achieved experimentally. A similar sensitivity enhancement was also obtained for 2D (15)N-(1)H dipolar and 15N chemical shift correlation spectroscopy, by means of a 3D 1H/15N-1H/15N correlation experiment. We demonstrate this technique, termed PRINS for proton indirectly detected nitrogen static NMR, on a crystalline model compound with long 1H T(1rho) and on a 25-kDa protein with short 1H T(1rho). This 1H indirect detection approach should be useful for enhancing the sensitivity of 15N NMR of oriented membrane peptides. It can also be used to facilitate the empirical optimization of 15N-detected experiments where the inherent sensitivity of the sample is low.

References

Nov 18, 1998·Current Opinion in Structural Biology·F M Marassi, S J Opella

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Citations

Feb 13, 2008·The Journal of Chemical Physics·Chin H Wu, Stanley J Opella
Nov 6, 2007·Journal of Magnetic Resonance·Chin H Wu, Stanley J Opella
Oct 4, 2005·Journal of Magnetic Resonance·Jun AshidaJean-Paul Amoureux
Sep 5, 2001·Journal of Magnetic Resonance·A K Khitrin, B M Fung
May 31, 2002·Journal of Magnetic Resonance·Satoru Yamaguchi, Mei Hong
May 31, 2002·Journal of Magnetic Resonance·Aneta T Petkova, Robert Tycko
May 24, 2017·Physical Chemistry Chemical Physics : PCCP·Mark C ButlerKarl T Mueller
May 26, 2017·Angewandte Chemie·Jasmine Viger-GravelLyndon Emsley
Nov 5, 2019·The Journal of Physical Chemistry. a·Yasunari KusakaHironori Kaji
Jul 24, 2020·The Journal of Physical Chemistry. B·Martin D GelenterMei Hong
Sep 13, 2002·Journal of the American Chemical Society·Ingo Schnell, Kay Saalwächter

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