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Title: Biomolecular complex viewed by dynamic nuclear polarization solid-state NMR spectroscopy

Journal Article · · Biochemical Society Transactions
DOI:https://doi.org/10.1042/bst20191084· OSTI ID:1878627
 [1];  [1];  [1];  [2];  [3]; ORCiD logo [1]
  1. Louisiana State Univ., Baton Rouge, LA (United States)
  2. National High Magnetic Field Lab., Tallahassee, FL (United States)
  3. Louisiana State Univ. Health Sciences Center, New Orleans, LA (United States)

Solid-state nuclear magnetic resonance (ssNMR) is an indispensable tool for elucidating the structure and dynamics of insoluble and non-crystalline biomolecules. The recent advances in the sensitivity-enhancing technique magic-angle spinning dynamic nuclear polarization (MAS-DNP) have substantially expanded the territory of ssNMR investigations and enabled the detection of polymer interfaces in a cellular environment. This article highlights the emerging MAS-DNP approaches and their applications to the analysis of biomolecular composites and intact cells to determine the folding pathway and ligand binding of proteins, the structural polymorphism of low-populated biopolymers, as well as the physical interactions between carbohydrates, proteins, and lignin. Furthermore, these structural features provide an atomic-level understanding of many cellular processes, promoting the development of better biomaterials and inhibitors. It is anticipated that the capabilities of MAS-DNP in biomolecular and biomaterial research will be further enlarged by the rapid development of instrumentation and methodology.

Research Organization:
Louisiana State Univ., Baton Rouge, LA (United States). Center for Lignocellulose Structure and Formation
Sponsoring Organization:
USDOE Office of Science (SC), Basic Energy Sciences (BES); National Institutes of Health (NIH); National Science Foundation (NSF)
Grant/Contract Number:
SC0001090; AI149289; NSF/DMR-1644779
OSTI ID:
1878627
Journal Information:
Biochemical Society Transactions, Vol. 48, Issue 3; ISSN 0300-5127
Publisher:
Portland PressCopyright Statement
Country of Publication:
United States
Language:
English

References (98)

Structure and Dynamics of Membrane Proteins by Magic Angle Spinning Solid-State NMR journal June 2009
RNA structure determination by solid-state NMR spectroscopy journal May 2015
Emerging Structural Understanding of Amyloid Fibrils by Solid-State NMR journal October 2017
Protein Structure Determination by Magic-Angle Spinning Solid-State NMR, and Insights into the Formation, Structure, and Stability of Amyloid Fibrils journal May 2013
Structure and Dynamics of Membrane Proteins from Solid-State NMR journal May 2018
Magic-angle-spinning NMR spectroscopy applied to small molecules and peptides in lipid bilayers journal October 2007
Solid-state NMR spectroscopy as a tool for drug design: from membrane-embedded targets to amyloid fibrils journal October 2007
DNP-Enhanced MAS NMR: A Tool to Snapshot Conformational Ensembles of α-Synuclein in Different States journal April 2018
Lignin-polysaccharide interactions in plant secondary cell walls revealed by solid-state NMR journal January 2019
Molecular architecture of fungal cell walls revealed by solid-state NMR journal July 2018
Sensitivity-enhanced solid-state NMR detection of expansin's target in plant cell walls journal September 2013
Sensitivity-Enhanced NMR Reveals Alterations in Protein Structure by Cellular Milieus journal October 2015
Dynamic Nuclear Polarization Nuclear Magnetic Resonance in Human Cells Using Fluorescent Polarizing Agents journal April 2018
Efficient assignment and NMR analysis of an intact virus using sequential side-chain correlations and DNP sensitization journal May 2017
Theoretical aspects of Magic Angle Spinning - Dynamic Nuclear Polarization journal September 2015
High Frequency Dynamic Nuclear Polarization journal April 2013
Dynamic Nuclear Polarization Surface Enhanced NMR Spectroscopy journal March 2013
Stability of nitroxide biradical TOTAPOL in biological samples journal June 2019
Low-temperature dynamic nuclear polarization at 9.4T with a 30mW microwave source journal June 2010
Efficient DNP NMR of membrane proteins: sample preparation protocols, sensitivity, and radical location journal February 2016
Preparation of Fungal and Plant Materials for Structural Elucidation Using Dynamic Nuclear Polarization Solid-State NMR
  • Kirui, Alex; Dickwella Widanage, Malitha C.; Mentink-Vigier, Frederic
  • Journal of Visualized Experiments, Issue 144 https://doi.org/10.3791/59152
journal January 2019
Optimization of an absolute sensitivity in a glassy matrix during DNP-enhanced multidimensional solid-state NMR experiments journal February 2014
TOTAPOL: A Biradical Polarizing Agent for Dynamic Nuclear Polarization Experiments in Aqueous Media journal September 2006
Highly Efficient, Water-Soluble Polarizing Agents for Dynamic Nuclear Polarization at High Frequency journal August 2013
Computationally Assisted Design of Polarizing Agents for Dynamic Nuclear Polarization Enhanced NMR: The AsymPol Family journal August 2018
Neurotoxin II Bound to Acetylcholine Receptors in Native Membranes Studied by Dynamic Nuclear Polarization NMR journal December 2011
Fast and accurate MAS–DNP simulations of large spin ensembles journal January 2017
A Method for Dynamic Nuclear Polarization Enhancement of Membrane Proteins journal December 2014
Selective high-resolution DNP-enhanced NMR of biomolecular binding sites journal January 2019
Matrix-Free DNP-Enhanced NMR Spectroscopy of Liposomes Using a Lipid-Anchored Biradical journal February 2015
Targetable Tetrazine‐Based Dynamic Nuclear Polarization Agents for Biological Systems journal January 2020
Dynamic Nuclear Polarization/Solid-State NMR Spectroscopy of Membrane Polypeptides: Free-Radical Optimization for Matrix-Free Lipid Bilayer Samples journal June 2017
De novo design of a transmembrane Zn 2+ -transporting four-helix bundle journal December 2014
Using chemical shift perturbation to characterise ligand binding journal August 2013
Polyphenol/Peptide Binding and Precipitation journal March 2002
Determining Cholesterol Binding to Membrane Proteins by Cholesterol 13 C Labeling in Yeast and Dynamic Nuclear Polarization NMR journal October 2018
Cholesterol-binding site of the influenza M2 protein in lipid bilayers from solid-state NMR journal November 2017
Influenza Virus A M2 Protein Generates Negative Gaussian Membrane Curvature Necessary for Budding and Scission journal September 2013
NMR Determination of Protein Partitioning into Membrane Domains with Different Curvatures and Application to the Influenza M2 Peptide journal February 2012
Investigation of the Curvature Induction and Membrane Localization of the Influenza Virus M2 Protein Using Static and Off-Magic-Angle Spinning Solid-State Nuclear Magnetic Resonance of Oriented Bicelles journal March 2015
Influenza Virus M2 Protein Mediates ESCRT-Independent Membrane Scission journal September 2010
Molecular Rationale for Improved Dynamic Nuclear Polarization of Biomembranes journal August 2016
Biomolecular DNP-Supported NMR Spectroscopy using Site-Directed Spin Labeling journal July 2015
Dynamic nuclear polarization of membrane proteins: covalently bound spin-labels at protein–protein interfaces journal April 2015
Cysteine-Specific Labeling of Proteins with a Nitroxide Biradical for Dynamic Nuclear Polarization NMR journal July 2015
Selective Protein Hyperpolarization in Cell Lysates Using Targeted Dynamic Nuclear Polarization journal June 2016
Protein Structure Determination with Paramagnetic Solid-State NMR Spectroscopy journal March 2013
Paramagnet induced signal quenching in MAS–DNP experiments in frozen homogeneous solutions journal March 2014
NMR Signal Quenching from Bound Biradical Affinity Reagents in DNP Samples journal November 2017
Relaxation-compensated difference spin diffusion NMR for detecting 13C–13C long-range correlations in proteins and polysaccharides journal December 2014
The Target of β-Expansin EXPB1 in Maize Cell Walls from Binding and Solid-State NMR Studies journal October 2016
Probing a cell-embedded megadalton protein complex by DNP-supported solid-state NMR journal May 2015
Combining DNP NMR with segmental and specific labeling to study a yeast prion protein strain that is not parallel in-register journal March 2017
DNP‐Supported Solid‐State NMR Spectroscopy of Proteins Inside Mammalian Cells journal July 2019
Observing an Antisense Drug Complex in Intact Human Cells by in‐Cell NMR Spectroscopy journal July 2019
Wall Structure and Wall Loosening. A Look Backwards and Forwards: Fig. 1. journal January 2001
Hidden Killers: Human Fungal Infections journal December 2012
From the surface to the inner layer of the fungal cell wall journal February 1997
Spectral Snapshots of Bacterial Cell-Wall Composition and the Influence of Antibiotics by Whole-Cell NMR journal March 2015
Whole cell solid-state NMR study of Chlamydomonas reinhardtii microalgae journal January 2018
Solid-state NMR Reveals the Carbon-based Molecular Architecture of Cryptococcus neoformans Fungal Eumelanins in the Cell Wall journal March 2015
Molecular architecture of softwood revealed by solid-state NMR journal October 2019
Folding of xylan onto cellulose fibrils in plant cell walls revealed by solid-state NMR journal December 2016
Structure and Dynamics of Brachypodium Primary Cell Wall Polysaccharides from Two-Dimensional 13 C Solid-State Nuclear Magnetic Resonance Spectroscopy journal April 2014
Cellulose Structural Polymorphism in Plant Primary Cell Walls Investigated by High-Field 2D Solid-State NMR Spectroscopy and Density Functional Theory Calculations journal May 2016
Gradients in Wall Mechanics and Polysaccharides along Growing Inflorescence Stems journal October 2017
Effects of Pectin Molecular Weight Changes on the Structure, Dynamics, and Polysaccharide Interactions of Primary Cell Walls of Arabidopsis thaliana : Insights from Solid-State NMR journal August 2017
Phosphoethanolamine cellulose: A naturally produced chemically modified cellulose journal January 2018
Bacterial cell wall composition and the influence of antibiotics by cell-wall and whole-cell NMR journal October 2015
Solid-state NMR of plant and fungal cell walls: A critical review journal June 2020
Cellulose-Pectin Spatial Contacts Are Inherent to Never-Dried Arabidopsis Primary Cell Walls: Evidence from Solid-State Nuclear Magnetic Resonance journal June 2015
Multidimensional solid-state NMR spectroscopy of plant cell walls journal September 2016
Atomic resolution of cotton cellulose structure enabled by dynamic nuclear polarization solid-state NMR journal November 2018
Rapid Natural-Abundance 2D 13 C- 13 C Correlation Spectroscopy Using Dynamic Nuclear Polarization Enhanced Solid-State NMR and Matrix-Free Sample Preparation journal October 2012
Matrix-free dynamic nuclear polarization enables solid-state NMR 13C–13C correlation spectroscopy of proteins at natural isotopic abundance journal January 2013
Solid-State NMR on Bacterial Cells: Selective Cell Wall Signal Enhancement and Resolution Improvement using Dynamic Nuclear Polarization journal February 2013
Two-dimensional magic angle spinning NMR investigation of naturally occurring chitins: Precise1H and13C resonance assignment of ?- and ?-chitin journal January 2004
Hydrogen Bonding Structure and Stability of?-Chitin Studied by13C Solid-State NMR journal February 2005
Revisit of α-Chitin Crystal Structure Using High Resolution X-ray Diffraction Data journal May 2009
Exhaustive crystal structure search and crystal modeling of β-chitin journal March 2007
15 N− 15 N Proton Assisted Recoupling in Magic Angle Spinning NMR journal April 2009
Proton assisted recoupling and protein structure determination journal December 2008
Proton-Assisted Recoupling (PAR) in Peptides and Proteins journal November 2017
A quasi-optical and corrugated waveguide microwave transmission system for simultaneous dynamic nuclear polarization NMR on two separate 14.1 T spectrometers journal April 2018
Topology of Pretreated Wood Fibers Using Dynamic Nuclear Polarization journal November 2019
Atomic-Level Structure Characterization of Biomass Pre- and Post-Lignin Treatment by Dynamic Nuclear Polarization-Enhanced Solid-State NMR journal January 2017
Dynamic regulation of HIV-1 capsid interaction with the restriction factor TRIM5α identified by magic-angle spinning NMR and molecular dynamics simulations journal October 2018
Dynamic Nuclear Polarization Enhanced MAS NMR Spectroscopy for Structural Analysis of HIV-1 Protein Assemblies journal January 2016
Chemical Shifts for the Unusual DNA Structure in Pf1 Bacteriophage from Dynamic-Nuclear-Polarization-Enhanced Solid-State NMR Spectroscopy journal December 2011
Structural description of surfaces and interfaces in biominerals by DNP SENS journal October 2019
Detection of nucleic acids and other low abundance components in native bone and osteosarcoma extracellular matrix by isotope enrichment and DNP-enhanced NMR journal January 2019
Essential but sparse collagen hydroxylysyl post-translational modifications detected by DNP NMR journal January 2018
19 F Dynamic Nuclear Polarization at Fast Magic Angle Spinning for NMR of HIV-1 Capsid Protein Assemblies journal March 2019
Dynamic Nuclear Polarization-Enhanced Biomolecular NMR Spectroscopy at High Magnetic Field with Fast Magic-Angle Spinning journal April 2018
Natural Isotopic Abundance 13 C and 15 N Multidimensional Solid-State NMR Enabled by Dynamic Nuclear Polarization journal July 2019
Structural Fingerprinting of Protein Aggregates by Dynamic Nuclear Polarization-Enhanced Solid-State NMR at Natural Isotopic Abundance journal October 2018
Welcoming natural isotopic abundance in solid-state NMR: probing π-stacking and supramolecular structure of organic nanoassemblies using DNP journal January 2017
CCMRD: a solid-state NMR database for complex carbohydrates journal March 2020