Wang, Xiaoling, Bethany G. Caulkins, Gwladys Riviere, Leonard J. Mueller, Frederic Mentink-Vigier, and Joanna R. Long. “Direct Dynamic Nuclear Polarization of 15N and 13C Spins at 14.1 T Using a Trityl Radical and Magic Angle Spinning.” Solid State Nuclear Magnetic Resonance, April 2019, S0926204019300177.
https://doi.org/10.1016/j.ssnmr.2019.03.009.
We investigate solid-state dynamic nuclear polarization of 13C and 15N nuclei using monoradical trityl OX063 as a polarizing agent in a magnetic field of 14.1 T with magic angle spinning at ~100 K. We monitored the field dependence of direct 13C and 15N polarization for frozen [13C, 15N] urea and achieved maximum absolute enhancement factors of 240 and 470, respectively. The field profiles are consistent with polarization of 15N spins via either the solid effect or the cross effect, and polarization of 13C spins via a combination of cross effect and solid effect. For microcrystalline, 15Nenriched tryptophan synthase sample containing trityl radical, a 1500-fold increase in 15N signal was observed under microwave irradiation. These results show the promise of trityl radicals and their derivatives for direct polarization of low gamma, spin-½ nuclei at high magnetic fields and suggest a novel approach for selectively polarizing specific moieties or for polarizing systems which have low levels of protonation.