Donovan, K.J. and L. Frydman, HyperBIRD: A Sensitivity-Enhanced Approach to Collecting Homonuclear-Decoupled Proton NMR Spectra. Angew Chem Int Ed Engl, 2014: p. n/a-n/a.
Samples prepared following dissolution dynamic nuclear polarization (DNP) enable the detection of NMR spectra from low-gamma nuclei with outstanding sensitivity, yet have limited use for the enhancement of abundant species like 1 H nuclei. Small- and intermediate-sized molecules, however, show strong heteronuclear cross-relaxation effects: spontaneous processes with an inherent isotopic selectivity, whereby only the 13 C-bonded protons receive a polarization enhancement. These effects are here combined with a recently developed method that delivers homonuclear-decoupled 1 H spectra in natural abundance samples based on heteronuclear couplings to these same, 13 C-bonded nuclei. This results in the HyperBIRD methodology; a single-shot combination of these two effects that can simultaneously simplify and resolve complex, congested 1 H NMR spectra with many overlapping spin multiplets, while achieving 50-100 times sensitivity enhancements over conventional thermal counterparts.
[U. of Ottawa NMR Facility Blog] 1H Decoupled 1H NMR Spectra
1H Decoupled 1H NMR Spectra
13C NMR spectra acquired with 1H decoupling are particularly simple to interpret as every symmetrically unique carbon atom gives rise to a peak in the NMR spectrum. One is usually able to simply count the number of carbons in a molecule by counting the peaks in the 13C NMR spectrum. 1H NMR spectra, on the other hand, are complicated by homonuclear 1H - 1H coupling such that many 1H resonances are complex multiplets spread over a frequency range of some tens of Hz. Furthermore, multiplets often overlap complicating the interpretation of the data. ...
nmrlearner
News from NMR blogs
0
07-12-2014 04:28 AM
[NMR paper] Homonuclear decoupling for enhancing resolution and sensitivity in NOE and RDC measurements of peptides and proteins
Homonuclear decoupling for enhancing resolution and sensitivity in NOE and RDC measurements of peptides and proteins
Publication date: Available online 22 November 2013
Source:Journal of Magnetic Resonance</br>
Author(s): Jinfa Ying , Julien Roche , Ad Bax</br>
Application of band-selective homonuclear (BASH) 1H decoupling pulses during acquisition of the 1H free induction decay is shown to be an efficient procedure for removal of scalar and residual dipolar couplings between amide and aliphatic protons. BASH decoupling can be applied in both dimensions of a...
[NMR paper] Long-Observation-Window Band-Selective Homonuclear Decoupling: Increased Sensitivity and Resolution in Solid-State NMR Spectroscopy of Proteins
Long-Observation-Window Band-Selective Homonuclear Decoupling: Increased Sensitivity and Resolution in Solid-State NMR Spectroscopy of Proteins
Publication date: Available online 13 September 2013
Source:Journal of Magnetic Resonance</br>
Author(s): Jochem O. Struppe , Chen Yang , Yachong Wang , Roy V. Hernandez , Lisa M. Shamansky , Leonard J. Mueller</br>
Sensitivity and resolution are the two fundamental obstacles to extending solid-state nuclear magnetic resonance to even larger protein systems. Here, a novel long-observation-window band-selective...
nmrlearner
Journal club
0
09-13-2013 12:05 PM
[NMR paper] Proton-decoupled CPMG: a better experiment for measuring 15N R2 relaxation in disordered proteins
Proton-decoupled CPMG: a better experiment for measuring 15N R2 relaxation in disordered proteins
Publication date: Available online 23 August 2013
Source:Journal of Magnetic Resonance</br>
Author(s): Tairan Yuwen , Nikolai R. Skrynnikov</br>
15N R2 relaxation is one of the most informative experiments for characterization of intrinsically disordered proteins (IDPs). Small changes in nitrogen R2 rates are often used to determine how IDPs respond to various biologically relevant perturbations such as point mutations, posttranslational modifications, weak ligand...
nmrlearner
Journal club
0
08-24-2013 03:01 AM
[Question from NMRWiki Q&A forum] proton decoupled of 14N
proton decoupled of 14N
Hi everyone,
Has someone tried to run proton decoupled of 14N? How long should be the 14N decoupling pulse? I had some problems with the lock signal (lost it) when I tried the pulse sequence zgig (1H on the observed channel). When recording 1D 14N spectrum, the lock was fine (it had some small distortions, but was not lost). We have a DRX 400 MHz spectrometer, with Topspin 1.3 and a BBFO atma probe.Any suggestions on how to set up this experiment will be highly appreciated. Thanks a lot, alina
Check if somebody has answered this question on NMRWiki QA forum
nmrlearner
News from other NMR forums
0
08-05-2013 09:06 AM
Origin and removal of mixed-phase artifacts in gradient sensitivity enhanced heteronuclear single quantum correlation spectra
Origin and removal of mixed-phase artifacts in gradient sensitivity enhanced heteronuclear single quantum correlation spectra
Abstract Here we describe phasing anomalies observed in gradient sensitivity enhanced 15N-1H HSQC spectra, and analyze their origin. It is shown that, as a result of 15N off-resonance effects, dispersive contributions to the 1H signal become detectable, and lead to 15N-offset dependent phase errors. Strategies that effectively suppress these artifacts are presented.
Content Type Journal Article
Category Article
Pages 199-207
nmrlearner
Journal club
0
09-30-2011 08:01 PM
[NMR paper] Sensitivity-enhanced static 15N NMR of solids by 1h indirect detection.
Sensitivity-enhanced static 15N NMR of solids by 1h indirect detection.
Related Articles Sensitivity-enhanced static 15N NMR of solids by 1h indirect detection.
J Magn Reson. 2001 May;150(1):43-8
Authors: Hong M, Yamaguchi S
A method for enhancing the sensitivity of 15N spectra of nonspinning solids through 1H indirect detection is introduced. By sampling the 1H signals in the windows of a pulsed spin-lock sequence, high-sensitivity 1H spectra can be obtained in two-dimensional (2D) spectra whose indirect dimension yields the 15N chemical...
HyperBIRD: A Sensitivity-Enhanced Approach to Collecting Homonuclear-Decoupled Proton NMR Spectra
Linear Mode
