☆ 4.3 Article

Coherence transfer between spy nuclei and nitrogen-14 in solids

JOURNAL OF MAGNETIC RESONANCE (2008)

Journal

JOURNAL OF MAGNETIC RESONANCE

Volume 190, Issue 1, Pages 160-164

Publisher

ACADEMIC PRESS INC ELSEVIER SCIENCE

DOI: 10.1016/j.jmr.2007.10.008

Keywords

solid-state NMR; magic angle spinning (MAS); nitrogen-14 NMR; quadrupolar parameters; HSQC; HMQC; amino acids

Categories

Biochemical Research Methods Physics, Atomic, Molecular & Chemical Spectroscopy

Ask authors/readers for more resources

Protocol

Community support

Reagent

Community support

Abstract

Coherence transfer from 'spy nuclei' such as H-1 or C-13 (S=1/2) was used to excite single- or double-quantum coherences of N-14 nuclei (I=1) while the S spins were aligned along the static field, in the manner of heteronuclear single-quantum correlation (HSQC) spectroscopy. For samples spinning at the magic angle, coherence transfer can be achieved through a combination of scalar couplings J(I,S) and second-order quadrupole - dipole cross-terms, also known as residual dipolar splittings (RDS). The second-order quadrupolar powder patterns in the two-dimensional spectra allow one to determine the quadrupolar parameters of N-14 in amino acids. (c) 2007 Elsevier Inc. All rights reserved.

Authors

I am an author on this paper

Click your name to claim this paper and add it to your profile.

Reviews

Primary Rating

4.3

Not enough ratings

Secondary Ratings

Novelty

-

Significance

-

Scientific rigor

-

Rate this paper

Recommended

Article Biochemistry & Molecular Biology

Determination of Histidine Protonation States in Proteins by Fast Magic Angle Spinning NMR

Roman Zadorozhnyi, Sucharita Sarkar, Caitlin M. Quinn, Kaneil K. Zadrozny, Barbie K. Ganser-Pornillos, Owen Pornillos, Angela M. Gronenborn, Tatyana Polenova

Summary: Histidine residues in proteins play crucial structural and functional roles, such as metal-binding and enzyme catalysis. This study introduces a fast MAS NMR approach to determine the protonation and tautomeric states of His at frequencies of 40-62 kHz, using H-1 detection and TEDOR-based filters in 2D heteronuclear correlation experiments. The approach is demonstrated using microcrystalline assemblies of HIV-1 CA(CTD)-SP1 protein.

FRONTIERS IN MOLECULAR BIOSCIENCES (2021)

Add to Collection

Article Chemistry, Physical

Racing toward Fast and Effective 17O Isotopic Labeling and Nuclear Magnetic Resonance Spectroscopy of N-Formyl-MLF-OH and Associated Building Blocks

Michelle Ha, Serge Nader, Shane Pawsey, Jochem Struppe, Martine Monette, Sheref S. Mansy, Job Boekhoven, Vladimir K. Michaelis

Summary: Solid-state H-1, C-13, and N-15 nuclear magnetic resonance (NMR) spectroscopy has been essential in studying complex molecules and biomolecules, while oxygen-17 (O-17) NMR is a challenging yet ideal method for studying hydrogen bonding. By improving labeling procedures, a cost-effective O-17 labeling method has been developed, overcoming a key barrier in biomolecular studies. Additionally, advancements in NMR development for sensitivity enhancement techniques are showcased for future research.

JOURNAL OF PHYSICAL CHEMISTRY B (2021)

Add to Collection

Article Biochemical Research Methods

Half-integer-spin quadrupolar nuclei in magic-angle spinning paramagnetic NMR: The case of NaMnO2

Jose P. Carvalho, Wassilios Papawassiliou, Andrew J. Pell

Summary: This article presents a combination of solid-state NMR methods for extracting the 23Na shift and quadrupolar parameters in the structurally complex NaMnO2 Na-ion cathode material. By combining multiple experiments, the shift and quadrupolar parameters for observed Na environments were determined and showed agreement with theoretical models.

JOURNAL OF MAGNETIC RESONANCE (2022)

Add to Collection

Article Chemistry, Physical

Residue-Specific High-Resolution 17O Solid-State Nuclear Magnetic Resonance of Peptides: Multidimensional Indirect 1H Detection and Magic-Angle Spinning

Ivan Hung, Eric G. Keeler, Wenping Mao, Peter L. Gor'kov, Robert G. Griffin, Zhehong Gan

Summary: This study addresses the challenges of low sensitivity, low resolution, and large quadrupolar couplings in the NMR study of oxygen by employing efficient isotopic labeling, high magnetic fields, fast sample spinning, and H-1 detection. Oxygen sites specific to each amino acid residue are observed through multidimensional experiments. The use of cross-polarization at high sample spinning frequencies enables efficient C-13<->O-17 polarization transfer. Results show that using O-17 for initial polarization provides better sensitivity per unit time compared to H-1.

JOURNAL OF PHYSICAL CHEMISTRY LETTERS (2022)

Add to Collection

Article Biochemistry & Molecular Biology

Protein structural dynamics by Magic-Angle Spinning NMR

Marta Bonaccorsi, Tanguy Le Marchand, Guido Pintacuda

Summary: Magic-Angle Spinning Nuclear Magnetic Resonance (MAS NMR) is a rapidly developing technique that complements solution NMR, X-ray crystallography, and electron microscopy for the biophysical characterization of microcrystalline, poorly crystalline or disordered protein samples. MAS NMR is ideal for investigating both structures and dynamics, and has been increasingly applied in structural biology research in recent years to describe conformational dynamics in various systems.

CURRENT OPINION IN STRUCTURAL BIOLOGY (2021)

Add to Collection

Article Chemistry, Physical

Network Modifier Effects in Multiple Network Former Glasses: NMR Results on the System 70 SiO2-7.5 P2O5-(22.5-x)Al2O3-xNa(2)O (0 & LE; x & LE; 17.5)

Millena Logrado, Randall E. Youngman, Bruce G. Aitken, Hellmut Eckert

Summary: The modification of the glass structure in the SiO2-P2O5-Al2O3 system by Na2O was studied using Ramanspectroscopy and multinuclear solid state NMR. The results showed that the structure of these glasses is dominated by bonding between anionic aluminum and cationic phosphate units. The replacement of alumina by sodium oxide leads to structural changes, while the silica component remains unchanged.

JOURNAL OF PHYSICAL CHEMISTRY C (2023)

Add to Collection

Article Chemistry, Physical

Atomic-Level Structure of Mesoporous Hexagonal Boron Nitride Determined by High-Resolution Solid-State Multinuclear Magnetic Resonance Spectroscopy and Density Functional Theory Calculations

Rick W. Dorn, Patrick M. Heintz, Ivan Hung, Kuizhi Chen, Jin-Su Oh, Tae-Hoon Kim, Lin Zhou, Zhehong Gan, Wenyu Huang, Aaron J. Rossini

Summary: In this study, high-resolution solid-state NMR spectroscopy and plane-wave density-functional theory (DFT) calculations were used to describe the atomic-level structure of mesoporous hexagonal boron nitride (p-BN). The results revealed the presence of various B and N signals in p-BN and provided a detailed characterization of the pore and edge/defect sites within the material. This is of great importance for the design and development of next-generation p-BN-based materials.

CHEMISTRY OF MATERIALS (2022)

Add to Collection

Article Chemistry, Analytical

High-resolution magic-angle spinning NMR metabolic profiling with spatially localized spectroscopy under slow sample spinning

Alan Wong

Summary: High-Resolution Magic-Angle Spinning (HRMAS) NMR spectroscopy is considered an essential technique in metabolomics for assessing the biochemical composition of tissue samples. HRMAS localized profiling shows promise for spatial resolution of metabolic profiles within the sampling tissues.

ANALYTICAL METHODS (2023)

Add to Collection

Review Chemistry, Physical

Field and magic angle spinning frequency dependence of proton resonances in rotating solids

Kai Xue, Riddhiman Sarkar, Zdenek Tosner, Bernd Reif

Summary: Proton detection in solid state NMR is continuously advancing, and current achievements include the necessity of deuteration for optimal spectral quality, the superiority of 13CH3 isotopomers for methyl groups at high MAS frequencies, and the sensitivity enhancement with increased static magnetic field.

PROGRESS IN NUCLEAR MAGNETIC RESONANCE SPECTROSCOPY (2022)

Add to Collection

Article Biochemical Research Methods

Windowed cross polarization at 55 kHz magic-angle spinning

Evgeny Nimerovsky, Stefan Becker, Loren B. Andreas

Summary: In this study, we investigate the windowed sequence for cross polarization (wCP) and find that it has additional matching conditions compared to traditional cross polarization. By considering the flip angle of the pulse, we observe a striking similarity between wCP and CP transfer conditions. Using spin-1/2 formalism and average Hamiltonian theory, we derive an analytical approximation that matches these observed transfer conditions. Data recorded at spectrometers with different external magnetic fields show that these transfers and the selectivity of CP are related to flip angle (average nutation).

JOURNAL OF MAGNETIC RESONANCE (2023)

Add to Collection

Article Chemistry, Physical

Sign determination of dipolar couplings in liquid crystals by off-magic-angle sample spinning

Debashis Majhi, Boris B. Kharkov, Sergey Dvinskikh

Summary: Dipolar NMR spectroscopy is a powerful analytical tool for studying structural and dynamic properties of solids at the molecular level. An approach to determine the signs of dipolar couplings in liquid crystals is presented, where sign information can be directly obtained from one-dimensional NMR spectra in samples spinning slightly off the magic angle. This method can be used to develop an experimental strategy for sign-sensitive measurements of heteronuclear dipolar couplings in anisotropic soft materials.

CHEMICAL PHYSICS LETTERS (2021)

Add to Collection

Article Biochemistry & Molecular Biology

Histone H3 core domain in chromatin with different DNA linker lengths studied by 1H-Detected solid-state NMR spectroscopy

Sean T. Smrt, Nicole Gonzalez Salguero, Justin K. Thomas, Mohamad Zandian, Michael G. Poirier, Christopher P. Jaroniec

Summary: Chromatin, a dynamic protein-DNA complex that regulates eukaryotic genome accessibility and essential functions. Solid-state NMR techniques were used to investigate the conformational dynamics of histone H3 tails in nucleosome arrays with different DNA linker lengths. The chemical shifts and line broadening of certain residues at the H3-nucleosomal DNA interface varied in arrays with short DNA linkers compared to arrays with longer linkers, indicating increased nucleosome packing heterogeneity and structural strain.

FRONTIERS IN MOLECULAR BIOSCIENCES (2023)

Add to Collection

Article Biochemistry & Molecular Biology

Proton Detected Solid-State NMR of Membrane Proteins at 28 Tesla (1.2 GHz) and 100 kHz Magic-Angle Spinning

Evgeny Nimerovsky, Kumar Tekwani Movellan, Xizhou Cecily Zhang, Marcel C. Forster, Eszter Najbauer, Kai Xue, Riza Dervisoglu, Karin Giller, Christian Griesinger, Stefan Becker, Loren B. Andreas

Summary: The available magnetic field strength for high resolution NMR in persistent superconducting magnets has recently improved, leading to increased proton resonance frequency and improved resolution for some membrane proteins in MAS NMR spectra.

BIOMOLECULES (2021)

Add to Collection

Article Biochemical Research Methods

Stable magic angle spinning with Low-Cost 3D-Printed parts

Ke Xu, Oliver Pecher, Marco Braun, Joern Schmedt auf der Gunne

Summary: A 3D-printed double-bearing magic angle spinning system was developed for high-performance MAS experiments with different rotor sizes, also allowing the design of inserts to isolate samples from humidity.

JOURNAL OF MAGNETIC RESONANCE (2021)

Add to Collection

Article Chemistry, Multidisciplinary

On the use of radio-frequency offsets for improving double-quantum homonuclear dipolar recoupling of half-integer-spin quadrupolar nuclei

Nghia Tuan Duong, Daniel Lee, Frederic Mentink-Vigier, Olivier Lafon, Gael De Paepe

Summary: This study evaluates the performance of several homonuclear dipolar recoupling sequences for Al-27 nuclei and finds that BR2(2)(1) outperforms other sequences in terms of double-quantum transfer efficiency and bandwidth. The analytical approximation of BR2(2)(1) clarifies the interplay between radio-frequency offsets and double-quantum efficiency, providing insights for improving recoupling schemes for quadrupolar nuclei.

MAGNETIC RESONANCE IN CHEMISTRY (2021)

Add to Collection

Article Chemistry, Multidisciplinary

Characterising the role of water in sildenafil citrate by NMR crystallography

Anuji Abraham, David C. Apperley, Stephen J. Byard, Andrew J. Ilott, Andrew J. Robbins, Vadim Zorin, Robin K. Harris, Paul Hodgkinson

CRYSTENGCOMM (2016)

Add to Collection

Article Chemistry, Medicinal

Correlation of Phosphorus Cross-Linking to Hydration Rates in Sodium Starch Glycolate Tablet Disintegrants Using MRI

Anuji Abraham, Dolapo Olusanmi, Andrew J. Ilott, David Good, Denette Murphy, Daniel Mcnamara, Alexej Jerschow, Rao V. Mantri

JOURNAL OF PHARMACEUTICAL SCIENCES (2016)

Add to Collection

Article Chemistry, Multidisciplinary

NMR crystallography - Three polymorphs of phenobarbital

Anuji Abraham, David C. Apperley, Thomas Gelbrich, Robin K. Harris, Ulrich J. Griesser

CANADIAN JOURNAL OF CHEMISTRY-REVUE CANADIENNE DE CHIMIE (2011)

Add to Collection

Article Biochemical Research Methods

Line-narrowing in proton-detected nitrogen-14 NMR

Simone Cavadini, Veronika Vitzthum, Simone Ulzega, Anuji Abraham, Geoffrey Bodenhausen

JOURNAL OF MAGNETIC RESONANCE (2010)

Add to Collection

Article Chemistry, Medicinal

A multi-technique approach to the study of structural stability and desolvation of two unusual channel hydrate solvates of finasteride

Stephen Byard, Anuji Abraham, Paul J. T. Boulton, Robin K. Harris, Paul Hodgkinson

JOURNAL OF PHARMACEUTICAL SCIENCES (2012)

Add to Collection

Article Chemistry, Physical

1H MAS NMR Study of Cysteine-Coated Gold Nanoparticles

Anuji Abraham, Andrew J. Ilott, Joel Miller, Terry Gullion

JOURNAL OF PHYSICAL CHEMISTRY B (2012)

Add to Collection

Article Chemistry, Physical

Solid-State NMR Study of Cysteine on Gold Nanoparticles

Anuji Abraham, Eugene Mihaliuk, Bharath Kumar, Justin Legleiter, Terry Gullion

JOURNAL OF PHYSICAL CHEMISTRY C (2010)

Add to Collection

Article Chemistry, Physical

L-Cysteine Interaction with Au55 Nanoparticle

Jessica A. Carr, Hong Wang, Anuji Abraham, Terry Gullion, James P. Lewis

JOURNAL OF PHYSICAL CHEMISTRY C (2012)

Add to Collection

Article Medicine, Research & Experimental

Understanding API-Polymer Proximities in Amorphous Stabilized Composite Drug Products Using Fluorine-Carbon 2D HETCOR Solid-State NMR

Anuji Abraham, George Crull

MOLECULAR PHARMACEUTICS (2014)

Add to Collection

Article Chemistry, Physical

TRAPDOR double-resonance and high-resolution MAS NMR for structural and template studies in zeolite ZSM-5

Anuji Abraham, Roel Prins, Jeroen A. van Bokhoven, Ernst R. H. van Eck, Arno P. M. Kentgens

SOLID STATE NUCLEAR MAGNETIC RESONANCE (2009)

Add to Collection

Article Chemistry, Multidisciplinary

A nondestructive and noninvasive method to determine water content in lyophilized proteins using low-field time-domain NMR

Anuji Abraham, Omar Elkassabany, Mary E. Krause, Andrew Ott

MAGNETIC RESONANCE IN CHEMISTRY (2019)

Add to Collection

Article Chemistry, Multidisciplinary

Solid state nuclear magnetic resonance studies of hydroxypropylmethylcellulose acetyl succinate polymer, a useful carrier in pharmaceutical solid dispersions

Andrea Pugliese, Lucy E. Hawarden, Anuji Abraham, Michael Tobyn, Frederic Blanc

MAGNETIC RESONANCE IN CHEMISTRY (2020)

Add to Collection

Article Chemistry, Physical

Fast understanding of phases and phase separation in liquid crystal drug delivery systems using deuterium solid-state NMR

Anuji Abraham, Eric Chan, Hyunsoo Park

SOLID STATE NUCLEAR MAGNETIC RESONANCE (2020)

Add to Collection

Editorial Material Chemistry, Multidisciplinary

Advances of solid-state NMR spectroscopy in material sciences

Anuji Abraham, Elodie Salager, Damodaran Krishnan, Yongchao Su

MAGNETIC RESONANCE IN CHEMISTRY (2020)

Add to Collection

No Data Available

© Peeref 2019-2024. All rights reserved.