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Divided-Evolution-Based Pulse Scheme for Quantifying Exchange Processes in Proteins: Powerful Complement to Relaxation Dispersion Experiments

Bouvignies, G; Hansen, DF; Vallurupalli, P; Kay, LE; (2011) Divided-Evolution-Based Pulse Scheme for Quantifying Exchange Processes in Proteins: Powerful Complement to Relaxation Dispersion Experiments. J AM CHEM SOC , 133 (6) 1935 - 1945. 10.1021/ja109589y.

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Abstract

A method for quantifying millisecond time scale exchange in proteins is presented based on scaling the rate of chemical exchange using a 2D N-15, H-1(N) experiment in which N-15 dwell times are separated by short spin-echo pulse trains. Unlike the popular Carr-Purcell-Meiboom-Gill (CPMG) experiment where the effects of a radio frequency field on measured transverse relaxation rates are quantified, the new approach measures peak positions in spectra that shift as the effective exchange time regime is varied. The utility of the method is established through an analysis of data recorded on an exchanging protein-ligand system for which the exchange parameters have been accurately determined using alternative approaches. Computations establish that a combined analysis of CPMG and peak shift profiles extends the time scale that can be studied to include exchanging systems with highly skewed populations and exchange rates as slow as 20 s(-1).

Type: Article
Title: Divided-Evolution-Based Pulse Scheme for Quantifying Exchange Processes in Proteins: Powerful Complement to Relaxation Dispersion Experiments
DOI: 10.1021/ja109589y
Keywords: CHARACTERIZING CHEMICAL-EXCHANGE, TIME-SCALE DYNAMICS, INVISIBLE EXCITED-STATES, NMR-SPECTROSCOPY, BIOLOGICAL MACROMOLECULES, SHIFTS, RESOLUTION, COUPLINGS, CATALYSIS, SEQUENCE
UCL classification: UCL > School of Life and Medical Sciences
UCL > School of Life and Medical Sciences > Faculty of Life Sciences
UCL > School of Life and Medical Sciences > Faculty of Life Sciences > Biosciences (Division of) > Structural and Molecular Biology
URI: http://discovery.ucl.ac.uk/id/eprint/1308577
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