2H-DNP-enhanced 2H–13C solid-state NMRcorrelation spectroscopy

Abstract

Perdeuteration of biological macromolecules for magic angle spinning solid-state NMR spectroscopy can yield high-resolution ²H–¹³C 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 ²H–¹³C 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 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 ²H–¹³C correlation spectra of U-[²H, ¹³C] proline.