Tuesday, July 31, 2012

High-Temperature Dynamic Nuclear Polarization Enhanced Magic-Angle-Spinning NMR

Akbey, Ü., A. Linden, and H. Oschkinat, High-Temperature Dynamic Nuclear Polarization Enhanced Magic-Angle-Spinning NMR. Appl. Magn. Reson., 2012. 43(1-2): p. 1-10.

Dynamic nuclear polarization (DNP) transfers electron spin-polarization to nuclear spins in close proximity, increasing sensitivity by two-to-three orders of magnitude. This enables nuclear magnetic resonance (NMR) experiments on samples with low concentrations of analyte. The requirement of using cryogenic temperatures in DNP-enhanced solid-state NMR (ssNMR) experiments may impair the resolution and hence limit its broad application to biological systems. In this work, we introduce a “High-Temperature DNP” approach, which aims at increasing spectral resolution by performing experiments at temperatures of around 180 K instead of ~100 K. By utilizing the extraordinary enhancements obtained on deuterated proteins, still sufficiently large DNP enhancements of 11–18 are obtained for proton and carbon, respectively. We recorded high sensitivity 2D 13 C– 13 C spectra in ~9 min with higher resolution than at 100 K, which has similar resolution to the one obtained at room temperature for some favorable residues.