Literature DB >> 32217425

High-resolution Overhauser dynamic nuclear polarization enhanced proton NMR spectroscopy at low magnetic fields.

Timothy J Keller1, Alexander J Laut1, Jagadishwar Sirigiri1, Thorsten Maly2.   

Abstract

Dynamic nuclear polarization (DNP) has gained large interest due to its ability to increase signal intensities in nuclear magnetic resonance (NMR) experiments by several orders of magnitude. Currently, DNP is typically used to enhance high-field, solid-state NMR experiments. However, the method is also capable of dramatically increasing the observed signal intensities in solution-state NMR spectroscopy. In this work, we demonstrate the application of Overhauser dynamic nuclear polarization (ODNP) spectroscopy at an NMR frequency of 14.5 MHz (0.35 T) to observe DNP-enhanced high-resolution NMR spectra of small molecules in solutions. Using a compact hybrid magnet with integrated shim coils to improve the magnetic field homogeneity we are able to routinely obtain proton linewidths of less than 4 Hz and enhancement factors >30. The excellent field resolution allows us to perform chemical-shift resolved ODNP experiments on ethyl crotonate to observe proton J-coupling. Furthermore, recording high-resolution ODNP-enhanced NMR spectra of ethylene glycol allows us to characterize the microwave induced sample heating in-situ, by measuring the separation of the OH and CH2 proton peaks.
Copyright © 2020 Elsevier Inc. All rights reserved.

Entities:  

Keywords:  High-resolution NMR; Low-field NMR; Overhauser dynamic nuclear polarization

Year:  2020        PMID: 32217425      PMCID: PMC7172445          DOI: 10.1016/j.jmr.2020.106719

Source DB:  PubMed          Journal:  J Magn Reson        ISSN: 1090-7807            Impact factor:   2.229


  51 in total

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Authors:  Anne Lesage; Moreno Lelli; David Gajan; Marc A Caporini; Veronika Vitzthum; Pascal Miéville; Johan Alauzun; Arthur Roussey; Chloé Thieuleux; Ahmad Mehdi; Geoffrey Bodenhausen; Christophe Copéret; Lyndon Emsley
Journal:  J Am Chem Soc       Date:  2010-11-10       Impact factor: 15.419

2.  Theoretical aspects of dynamic nuclear polarization in the solid state - the solid effect.

Authors:  Yonatan Hovav; Akiva Feintuch; Shimon Vega
Journal:  J Magn Reson       Date:  2010-11-16       Impact factor: 2.229

3.  Hydration dynamics as an intrinsic ruler for refining protein structure at lipid membrane interfaces.

Authors:  Chi-Yuan Cheng; Jobin Varkey; Mark R Ambroso; Ralf Langen; Songi Han
Journal:  Proc Natl Acad Sci U S A       Date:  2013-09-30       Impact factor: 11.205

4.  One-thousand-fold enhancement of high field liquid nuclear magnetic resonance signals at room temperature.

Authors:  Guoquan Liu; Marcel Levien; Niels Karschin; Giacomo Parigi; Claudio Luchinat; Marina Bennati
Journal:  Nat Chem       Date:  2017-02-13       Impact factor: 24.427

5.  Computation of DNP coupling factors of a nitroxide radical in toluene: seamless combination of MD simulations and analytical calculations.

Authors:  Deniz Sezer
Journal:  Phys Chem Chem Phys       Date:  2012-11-22       Impact factor: 3.676

6.  Liquid state DNP for water accessibility measurements on spin-labeled membrane proteins at physiological temperatures.

Authors:  Andrin Doll; Enrica Bordignon; Benesh Joseph; René Tschaggelar; Gunnar Jeschke
Journal:  J Magn Reson       Date:  2012-06-16       Impact factor: 2.229

7.  Spin-labeled gel for the production of radical-free dynamic nuclear polarization enhanced molecules for NMR spectroscopy and imaging.

Authors:  Evan R McCarney; Songi Han
Journal:  J Magn Reson       Date:  2007-11-28       Impact factor: 2.229

Review 8.  Quantitative cw Overhauser effect dynamic nuclear polarization for the analysis of local water dynamics.

Authors:  John M Franck; Anna Pavlova; John A Scott; Songi Han
Journal:  Prog Nucl Magn Reson Spectrosc       Date:  2013-07-04       Impact factor: 9.795

9.  A new model for Overhauser enhanced nuclear magnetic resonance using nitroxide radicals.

Authors:  Brandon D Armstrong; Songi Han
Journal:  J Chem Phys       Date:  2007-09-14       Impact factor: 3.488

Review 10.  Overhauser Dynamic Nuclear Polarization for the Study of Hydration Dynamics, Explained.

Authors:  John M Franck; Songi Han
Journal:  Methods Enzymol       Date:  2018-12-11       Impact factor: 1.600

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  3 in total

1.  Overhauser dynamic nuclear polarization (ODNP)-enhanced two-dimensional proton NMR spectroscopy at low magnetic fields.

Authors:  Timothy J Keller; Thorsten Maly
Journal:  Magn Reson (Gott)       Date:  2021-04-12

2.  Microfluidic Overhauser DNP chip for signal-enhanced compact NMR.

Authors:  Sebastian Z Kiss; Neil MacKinnon; Jan G Korvink
Journal:  Sci Rep       Date:  2021-02-25       Impact factor: 4.379

3.  Functionalized Controlled Porous Glasses for Producing Radical-Free Hyperpolarized Liquids by Overhauser DNP.

Authors:  Raphael Kircher; Sarah Mross; Hans Hasse; Kerstin Münnemann
Journal:  Molecules       Date:  2022-09-28       Impact factor: 4.927

  3 in total

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