3-O-Methyl- d -glucose mutarotation and proton exchange rates assessed by 13 C, 1 H NMR and by chemical exchange saturation transfer and spin lock measurements
3-O-Methyl- d -glucose mutarotation and proton exchange rates assessed by 13 C, 1 H NMR and by chemical exchange saturation transfer and spin lock measurements
3-O-Methyl-d-glucose (3OMG) was recently suggested as an agent to image tumors using chemical exchange saturation transfer (CEST) MRI. To characterize the properties of 3OMG in solution, the anomeric equilibrium and the mutarotation rates of 3OMG were studied by 1H and 13C NMR. This information is essential in designing the in vivo CEST experiments. At room temperature, the ratio of α and β 3OMG anomers at equilibrium was 1:1.4, and the time to reach 95% equilibrium was 6Â*h. The chemical exchange rates between the hydroxyl protons of 3OMG and water, measured by CEST and spin lock at pH 6.14 and a temperature of 4Â*°C, were in the range of 360â??670Â*sâ??1.
Probing conformational dynamics in biomolecules via chemical exchange saturation transfer: a primer
Probing conformational dynamics in biomolecules via chemical exchange saturation transfer: a primer
Abstract
Although Chemical Exchange Saturation Transfer (CEST) type NMR experiments have been used to study chemical exchange processes in molecules since the early 1960s, there has been renewed interest in the past several years in using this approach to study biomolecular conformational dynamics. The methodology is particularly powerful for the study of sparsely populated, transiently formed conformers that are recalcitrant to investigation using...
nmrlearner
Journal club
0
03-19-2017 10:38 PM
[NMR paper] Spin Saturation Transfer Difference NMR (SSTD NMR): A New Tool to Obtain Kinetic Parameters of Chemical Exchange Processes.
Spin Saturation Transfer Difference NMR (SSTD NMR): A New Tool to Obtain Kinetic Parameters of Chemical Exchange Processes.
Spin Saturation Transfer Difference NMR (SSTD NMR): A New Tool to Obtain Kinetic Parameters of Chemical Exchange Processes.
J Vis Exp. 2016 Nov 12;(117):
Authors: Quirós MT, Macdonald C, Angulo J, Muñoz MP
Abstract
This detailed protocol describes the new Spin Saturation Transfer Difference Nuclear Magnetic Resonance protocol (SSTD NMR), recently developed in our group to study processes of mutual-site...
nmrlearner
Journal club
0
12-04-2016 02:24 AM
[U. of Ottawa NMR Facility Blog] CEST - Chemical Exchange Saturation Transfer
CEST - Chemical Exchange Saturation Transfer
Chemical Exchange Saturation Transfer (CEST) is a technique where one resonance, in slow exchange with a second resonance, is saturated with a selective low power pulse followed by a hard non-selective 90° pulse. The intensity of the second resonance is then diminished due to the transfer of saturation from the first resonance as the result of chemical exchange. The figure below demonstrates this for a 25 mM solution of salicylic acid in H2O/D2O buffered at pH 7. ...
nmrlearner
News from NMR blogs
0
04-22-2016 08:45 PM
[NMR paper] Determination of pseudocontact shifts of low-populated excited states by NMR chemical exchange saturation transfer.
Determination of pseudocontact shifts of low-populated excited states by NMR chemical exchange saturation transfer.
Determination of pseudocontact shifts of low-populated excited states by NMR chemical exchange saturation transfer.
Phys Chem Chem Phys. 2016 Mar 22;
Authors: Ma RS, Li QF, Wang AD, Zhang JH, Liu ZJ, Wu JH, Su XC, Ruan K
Abstract
Despite the critical roles of excited states in protein functions, they remain intractable for most structural studies because of their notably low populations. Chemical shifts for...
nmrlearner
Journal club
0
03-24-2016 04:30 PM
[NMR paper] Rapid Determination of Fast Protein Dynamics from NMR Chemical Exchange Saturation Transfer Data.
Rapid Determination of Fast Protein Dynamics from NMR Chemical Exchange Saturation Transfer Data.
Related Articles Rapid Determination of Fast Protein Dynamics from NMR Chemical Exchange Saturation Transfer Data.
Angew Chem Int Ed Engl. 2016 Jan 28;
Authors: Gu Y, Hansen AL, Peng Y, Brüschweiler R
Abstract
Functional motions of (15) N-labeled proteins can be monitored by solution NMR spin relaxation experiments over a broad range of timescales. These experiments however typically take of the order of several days to a week per...
Characterizing Slow Chemical Exchange in Nucleic Acids by Carbon CEST and Low Spin-Lock Field R1? NMR Spectroscopy
Characterizing Slow Chemical Exchange in Nucleic Acids by Carbon CEST and Low Spin-Lock Field R1? NMR Spectroscopy
Bo Zhao, Alexandar L. Hansen and Qi Zhang
http://pubs.acs.org/appl/literatum/publisher/achs/journals/content/jacsat/0/jacsat.ahead-of-print/ja409835y/aop/images/medium/ja-2013-09835y_0005.gif
Journal of the American Chemical Society
DOI: 10.1021/ja409835y
http://feeds.feedburner.com/~ff/acs/jacsat?d=yIl2AUoC8zA
http://feeds.feedburner.com/~r/acs/jacsat/~4/iu74AOgzY6s
nmrlearner
Journal club
0
12-19-2013 05:34 AM
[NMR paper] Probing Slow Chemical Exchange at Carbonyl Sites in Proteins by Chemical Exchange Saturation Transfer NMR Spectroscopy.
Probing Slow Chemical Exchange at Carbonyl Sites in Proteins by Chemical Exchange Saturation Transfer NMR Spectroscopy.
Probing Slow Chemical Exchange at Carbonyl Sites in Proteins by Chemical Exchange Saturation Transfer NMR Spectroscopy.
Angew Chem Int Ed Engl. 2013 Feb 28;
Authors: Vallurupalli P, Kay LE
Abstract
Seeing the invisible: A 13 CO NMR chemical exchange saturation transfer (CEST) experiment for the study of "invisible" excited protein states with lifetimes on the order of 5-50 ms has been developed. The 13 CO chemical...