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Effects of sample preparation conditions on biomolecular solid-state NMR lineshapes
Authors:David L. Jakeman  Dan J. Mitchell  Wendy A. Shuttleworth  Jeremy N.S. Evans
Affiliation:(1) Department of Biochemistry and Biophysics, Washington State University, Pullman, WA, 99163-4660, U.S.A
Abstract:Sample preparation conditions with the 46 kDa enzyme complex of 5-enolpyruvyl-shikimate-3-phosphate (EPSP) synthase, shikimate-3-phosphate (S3P) and glyphosate (GLP) have been examined in an attempt to reduce linewidths in solid-state NMR spectra. The linewidths of 13P resonances associated with enzyme bound S3P and GLP in the lyophilized ternary complex have been reduced to 150 ± 12 Hz and 125 ± 7 Hz respectively, by a variety of methods involving additives and freezing techniques.
Keywords:EPSP synthase  fast freezing  narrowing linewidths  13P NMR  solid-state NMR  trehalose
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