PMID- 28365491
OWN - NLM
STAT- PubMed-not-MEDLINE
LR  - 20191120
IS  - 1096-0856 (Electronic)
IS  - 1090-7807 (Linking)
VI  - 278
DP  - 2017 May
TI  - Solvent signal suppression for high-resolution MAS-DNP.
PG  - 60-66
LID - S1090-7807(17)30073-3 [pii]
LID - 10.1016/j.jmr.2017.03.012 [doi]
AB  - 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.
CI  - Copyright (c) 2017 Elsevier Inc. All rights reserved.
FAU - Lee, Daniel
AU  - Lee D
AD  - Univ. Grenoble Alpes, INAC, F-38000 Grenoble, France; CEA, INAC, F-38000 
      Grenoble, France.
FAU - Chaudhari, Sachin R
AU  - Chaudhari SR
AD  - Univ. Grenoble Alpes, INAC, F-38000 Grenoble, France; CEA, INAC, F-38000 
      Grenoble, France.
FAU - De Paepe, Gael
AU  - De Paepe G
AD  - Univ. Grenoble Alpes, INAC, F-38000 Grenoble, France; CEA, INAC, F-38000 
      Grenoble, France. Electronic address: gael.depaepe@cea.fr.
LA  - eng
PT  - Journal Article
PT  - Research Support, Non-U.S. Gov't
DEP - 20170322
PL  - United States
TA  - J Magn Reson
JT  - Journal of magnetic resonance (San Diego, Calif. : 1997)
JID - 9707935
OTO - NOTNLM
OT  - Dipolar dephasing
OT  - Dipolar recoupling
OT  - Dynamic nuclear polarization
OT  - Magic angle spinning
OT  - Solid-state NMR
OT  - Solvent suppression
EDAT- 2017/04/04 06:00
MHDA- 2017/04/04 06:01
CRDT- 2017/04/03 06:00
PHST- 2017/01/31 00:00 [received]
PHST- 2017/03/13 00:00 [revised]
PHST- 2017/03/20 00:00 [accepted]
PHST- 2017/04/04 06:00 [pubmed]
PHST- 2017/04/04 06:01 [medline]
PHST- 2017/04/03 06:00 [entrez]
AID - S1090-7807(17)30073-3 [pii]
AID - 10.1016/j.jmr.2017.03.012 [doi]
PST - ppublish
SO  - J Magn Reson. 2017 May;278:60-66. doi: 10.1016/j.jmr.2017.03.012. Epub 2017 Mar 
      22.