A number of recent advances in the field of magic-angle-spinning (MAS) solid-state NMR have enabled its application to a range of biological systems of ever increasing complexity. To retain biological relevance, these samples are increasingly studied in a hydrated state. At the same time, experimental feasibility requires the sample preparation process to attain a high sample concentration within the final MAS rotor. We discuss these considerations, and how they have led to a number of different approaches to MAS NMR sample preparation. We describe our experience of how custom-made (or commercially available) ultracentrifugal devices can facilitate a simple, fast and reliable sample preparation process. A number of groups have since adopted such tools, in some cases to prepare samples for sedimentation-style MAS NMR experiments. Here we argue for a more widespread adoption of their use for routine MAS NMR sample preparation.
[NMR paper] Preparation of Amyloid Fibrils for Magic-Angle Spinning Solid-State NMR Spectroscopy.
Preparation of Amyloid Fibrils for Magic-Angle Spinning Solid-State NMR Spectroscopy.
Related Articles Preparation of Amyloid Fibrils for Magic-Angle Spinning Solid-State NMR Spectroscopy.
Methods Mol Biol. 2016;1345:173-83
Authors: Tuttle MD, Courtney JM, Barclay AM, Rienstra CM
Abstract
Solid-state NMR spectroscopy (SSNMR) is an established and invaluable tool for the study of amyloid fibril structure with atomic-level detail. Optimization of the homogeneity and concentration of fibrils enhances the resolution and sensitivity...
[NMR paper] Experiments Optimized for Magic Angle Spinning and Oriented Sample Solid-State NMR of Proteins.
Experiments Optimized for Magic Angle Spinning and Oriented Sample Solid-State NMR of Proteins.
Related Articles Experiments Optimized for Magic Angle Spinning and Oriented Sample Solid-State NMR of Proteins.
J Phys Chem B. 2013 Sep 17;
Authors: Das BB, Lin EC, Opella SJ
Abstract
Structure determination by solid-state NMR of proteins is rapidly advancing as result of recent developments of samples, experimental methods, and calculations. There are a number of different solid-state NMR approaches that utilize stationary, aligned samples or...
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09-21-2013 06:50 PM
[NMR paper] Biomolecular magic-angle spinning solid-state NMR: recent methods and applications.
Biomolecular magic-angle spinning solid-state NMR: recent methods and applications.
Related Articles Biomolecular magic-angle spinning solid-state NMR: recent methods and applications.
Curr Opin Biotechnol. 2013 Mar 4;
Authors: Goldbourt A
Abstract
The link of structure and dynamics of biomolecules and their complexes to their function and to many cellular processes has driven the quest for their detailed characterization by a variety of biophysical techniques. Magic-angle spinning solid-state nuclear magnetic resonance spectroscopy...
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03-14-2013 10:05 PM
[NMR paper] On the use of ultracentrifugal devices for sedimented solute NMR.
On the use of ultracentrifugal devices for sedimented solute NMR.
http://www.ncbi.nlm.nih.gov/corehtml/query/egifs/http:--production.springer.de-OnlineResources-Logos-springerlink.gif Related Articles On the use of ultracentrifugal devices for sedimented solute NMR.
J Biomol NMR. 2012 Oct;54(2):123-7
Authors: Bertini I, Engelke F, Gonnelli L, Knott B, Luchinat C, Osen D, Ravera E
Abstract
We have recently proposed sedimented solute NMR (SedNMR) as a solid-state method to access biomolecules without the need of crystallization or other...
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02-13-2013 12:47 PM
On the use of ultracentrifugal devices for sedimented solute NMR
On the use of ultracentrifugal devices for sedimented solute NMR
Abstract We have recently proposed sedimented solute NMR (SedNMR) as a solid-state method to access biomolecules without the need of crystallization or other sample manipulation. The drawback of SedNMR is that samples are intrinsically diluted and this is detrimental for the signal intensity. Ultracentrifugal devices can be used to increase the amount of sample inside the rotor, overcoming the intrinsic sensitivity limitation of the method. We designed two different devices and we here report the directions for using...
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08-13-2012 04:40 AM
Magic Angle Spinning and Oriented Sample Solid-State NMR Structural Restraints Combine for Influenza A M2 Protein Functional Insights
Magic Angle Spinning and Oriented Sample Solid-State NMR Structural Restraints Combine for Influenza A M2 Protein Functional Insights
Thach V. Can, Mukesh Sharma, Ivan Hung, Peter L. Gor’kov, William W. Brey and Timothy A. Cross
http://pubs.acs.org/appl/literatum/publisher/achs/journals/content/jacsat/0/jacsat.ahead-of-print/ja3004039/aop/images/medium/ja-2012-004039_0004.gif
Journal of the American Chemical Society
DOI: 10.1021/ja3004039
http://feeds.feedburner.com/~ff/acs/jacsat?d=yIl2AUoC8zA
http://feeds.feedburner.com/~r/acs/jacsat/~4/xappAmN-wb8
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05-25-2012 07:14 PM
Workshop on Biomolecular NMR Sample Preparation - Wolfson College, Oxford
A wide range of talks on various aspects of biomolecular NMR sample preparation and protein expression can be found on the Wolfson College Website:
http://www.bioch.ox.ac.uk/nmrwolfson/
Topics include:
In vitro expression and selective protein labelling
Expression and selective modification of small peptides
Sample types for biological solid state NMR
Making nanocrystals, bicelles and nanodiscs for structural studies
On the use of ultracentrifugal devices for routine sample preparation in biomolecular magic-angle-spinning NMR
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