[superscript 2]H-DNP-enhanced [superscript 2]H-[superscript 13]C solid-state NMR correlation spectroscopy

Abstract

Perdeuteration of biological macromolecules for magic angle spinning solid-state NMR spectroscopy can yield high-resolution [superscript 2]H–[superscript 13]C correlation spectra and the method is therefore of great interest for the structural biology community. Here we demonstrate that the combination of sample deuteration and dynamic nuclear polarization yields resolved [superscript 2]H–[superscript 13]C correlation spectra with a signal enhancement of ε ≥ 700 compared to a spectrum recorded with microwaves off and otherwise identical conditions. To our knowledge, this is the first time that [superscript 2]2H-DNP has been employed to enhance MAS-NMR spectra of a biologically relevant system. The DNP process is studied using several polarizing agents and the technique is applied to obtain [superscript 2]H–[superscript 13]C correlation spectra of U-[[superscript 2]H, [superscript 13]C] proline.