Abstract
Total correlation spectroscopy (TOCSY) is a key experiment to assign nuclear magnetic resonance (NMR) spectra of complex molecules. Carbon-13 TOCSY experiments are essential to assign signals of protein side chains. However, the performance of carbon-13 TOCSY deteriorates at high magnetic fields since the necessarily limited radiofrequency irradiation fails to cover the broad range of carbon-13 frequencies. Here, we introduce a new concept to overcome the limitations of TOCSY using two-field NMR spectroscopy. In two-field TOCSY experiments, chemical shifts are labelled at high field but isotropic mixing is performed at a much lower magnetic field, where the frequency range of the spectrum is drastically reduced. We obtain complete correlations between all carbon-13 nuclei belonging to amino acids across the entire spectrum: aromatic, aliphatic and carboxylic. Two-field TOCSY should be a robust and general approach for the assignment of uniformly carbon-13 labelled molecules in high-field and ultra-high field NMR spectrometers beyond 1000 MHz.
PMID: 28485888 [PubMed - as supplied by publisher]
Combined zero-quantum and spin-diffusion mixing for efficient homonuclear correlation spectroscopy under fast MAS: broadband recoupling and detection of long-range correlations
Combined zero-quantum and spin-diffusion mixing for efficient homonuclear correlation spectroscopy under fast MAS: broadband recoupling and detection of long-range correlations
Abstract
Fast magic angle spinning (MAS) NMR spectroscopy is emerging as an essential analytical and structural biology technique. Large resolution and sensitivity enhancements observed under fast MAS conditions enable structural and dynamics analysis of challenging systems, such as large macromolecular assemblies and isotopically dilute samples, using only a fraction of...
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11-25-2014 07:13 AM
[NMR paper] Multiple acquisition/multiple observation separated local field/chemical shift correlation solid-state magic angle spinning NMR spectroscopy.
Multiple acquisition/multiple observation separated local field/chemical shift correlation solid-state magic angle spinning NMR spectroscopy.
Multiple acquisition/multiple observation separated local field/chemical shift correlation solid-state magic angle spinning NMR spectroscopy.
J Magn Reson. 2014 Jun 28;245C:98-104
Authors: Das BB, Opella SJ
Abstract
Multiple acquisition spectroscopy (MACSY) experiments that enable multiple free induction decays to be recorded during individual experiments are demonstrated. In...
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07-16-2014 10:46 AM
[NMR paper] Magnetic susceptibility to measure total protein concentration from NMR metabolite spectra: Demonstration on blood plasma.
Magnetic susceptibility to measure total protein concentration from NMR metabolite spectra: Demonstration on blood plasma.
http://www.bionmr.com//www.ncbi.nlm.nih.gov/corehtml/query/egifs/http:--media.wiley.com-assets-2250-98-WileyOnlineLibrary-Button_120x27px_FullText.gif Related Articles Magnetic susceptibility to measure total protein concentration from NMR metabolite spectra: Demonstration on blood plasma.
Magn Reson Med. 2014 Mar 17;
Authors: Jupin M, Michiels PJ, Girard FC, Wijmenga SS
Abstract
PURPOSE: Accurate metabolite and...
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03-19-2014 10:43 PM
[NMR paper] Identifying inter-residue resonances in crowded 2D (13)C- (13)C chemical shift correlation spectra of membrane proteins by solid-state MAS NMR difference spectroscopy.
Identifying inter-residue resonances in crowded 2D (13)C- (13)C chemical shift correlation spectra of membrane proteins by solid-state MAS NMR difference spectroscopy.
Identifying inter-residue resonances in crowded 2D (13)C- (13)C chemical shift correlation spectra of membrane proteins by solid-state MAS NMR difference spectroscopy.
J Biomol NMR. 2013 May 25;
Authors: Miao Y, Cross TA, Fu R
Abstract
The feasibility of using difference spectroscopy, i.e. subtraction of two correlation spectra at different mixing times, for substantially...
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05-28-2013 06:36 PM
High-resolution NMR field-cycling device for full-range relaxation and structural studies of biopolymers on a shared commercial instrument
High-resolution NMR field-cycling device for full-range relaxation and structural studies of biopolymers on a shared commercial instrument
Abstract Improvements are described in a shuttling field-cycling device (Redfield in Magn Reson Chem 41:753â??768, 2003), designed to allow widespread access to this useful technique by configuring it as a removable module to a commercial 500 MHz NMR instrument. The main improvements described here, leading to greater versatility, high reliability and simple construction, include: shuttling provided by a linear motor driven by an integrated-control...
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12-31-2011 10:40 AM
[NMR paper] 1H(C) and 1H(N) total NOE correlations in a single 3D NMR experiment. 15N and 13C tim
1H(C) and 1H(N) total NOE correlations in a single 3D NMR experiment. 15N and 13C time-sharing in t1 and t2 dimensions for simultaneous data acquisition.
Related Articles 1H(C) and 1H(N) total NOE correlations in a single 3D NMR experiment. 15N and 13C time-sharing in t1 and t2 dimensions for simultaneous data acquisition.
J Biomol NMR. 2003 Nov;27(3):193-203
Authors: Xia Y, Yee A, Arrowsmith CH, Gao X
Simultaneous data acquisition in time-sharing (TS) multi-dimensional NMR experiments has been shown an effective means to reduce experimental...
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11-24-2010 09:16 PM
Analytical Chemist, Spectroscopy | TOTAL Petrochemicals USA, Inc.
Analytical Chemist, Spectroscopy | TOTAL Petrochemicals USA, Inc.
US - Nationwide, Advanced degree or equivalent experience in Chemistry or related fieldUnderstanding and experience in NMR and FTIRExcellent communication skillsDemonstrated success in working as part of a team
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Full correlations across broad NMR spectra by two-field total correlation spectroscopy.
Linear Mode
