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J Magn Reson. 2017 May;278:60-66. doi: 10.1016/j.jmr.2017.03.012. Epub 2017 Mar 22.

Solvent signal suppression for high-resolution MAS-DNP.

Author information

1
Univ. Grenoble Alpes, INAC, F-38000 Grenoble, France; CEA, INAC, F-38000 Grenoble, France.
2
Univ. Grenoble Alpes, INAC, F-38000 Grenoble, France; CEA, INAC, F-38000 Grenoble, France. Electronic address: gael.depaepe@cea.fr.

Abstract

Dynamic nuclear polarization (DNP) has become a powerful tool to substantially increase the sensitivity of high-field magic angle spinning (MAS) solid-state NMR experiments. The addition of dissolved hyperpolarizing agents usually results in the presence of solvent signals that can overlap and obscure those of interest from the analyte. Here, two methods are proposed to suppress DNP solvent signals: a Forced Echo Dephasing experiment (FEDex) and TRAnsfer of Populations in DOuble Resonance Echo Dephasing (TRAPDORED) NMR. These methods reintroduce a heteronuclear dipolar interaction that is specific to the solvent, thereby forcing a dephasing of recoupled solvent spins and leaving acquired NMR spectra free of associated resonance overlap with the analyte. The potency of these methods is demonstrated on sample types common to MAS-DNP experiments, namely a frozen solution (of l-proline) and a powdered solid (progesterone), both containing deuterated glycerol as a DNP solvent. The proposed methods are efficient, simple to implement, compatible with other NMR experiments, and extendable past spectral editing for just DNP solvents. The sensitivity gains from MAS-DNP in conjunction with FEDex or TRAPDORED then permits rapid and uninterrupted sample analysis.

KEYWORDS:

Dipolar dephasing; Dipolar recoupling; Dynamic nuclear polarization; Magic angle spinning; Solid-state NMR; Solvent suppression

PMID:
28365491
DOI:
10.1016/j.jmr.2017.03.012

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