HYDROGEN EXCHANGE AND METAL BINDING OF PROTEINS MONITORED BY TIME-RESOLVED ROOM TEMPERATURE PHOSPHORESCENCE

P. Wolanin, C.J. Fischer, A. Gafni, D.G. Steel

This poster was presented at the 1999 Biophysical Society Meeting in Baltimore, MD

Abstract

This work extends our previous studies of the effect of hydrogen/deuterium (H/D) exchange on the room temperature phosphorescence (RTP) lifetime from the core tryptophan (W109) of E. Coli  alkaline phosphatase (AP) [Schlyer, et al,  Biochem. Biophys. Res. Comm., 223, 1996, 670-674].  The kinetics of the exchange can be observed through an increase in the RTP lifetime that we believe occurs due to deuteration of the indole-ring enamine . We believe that the exchange at W109 is governed by EX1 kinetics, a hypothesis supported by the absence of a pD dependent exchange rate.  This work shows that RTP detected H/D exchange can be monitored in other proteins, including liver alcohol dehydrogenase (LADH) and glucose-6-phosphate dehydrogenase (G6PDH). In addition, we explore the use of measurements of RTP lifetime and H/D exchange rates to probe the effects of different states of metal binding in AP on the protein's flexibility where metal binding to apo AP changes the energy of stabilization and the core flexibility.

Our initial hypothesis was that H/D exchange rates would monotonically increase in proteins as their RTP lifetimes decreased.  Our data shows this to be true when comparing the native conformations of AP, LADH, and G6PDH. This is consistent with the fact that long RTP lifetimes are only observed from tryptophans in a rigid environment, usually deeply buried in the protein, and that this lifetime reflects the protein's flexibility. However, it appears that AP with only Zn bound exchanges very rapidly, despite having a RTP lifetime of about 1.1 seconds.

Supported by NIA grant AGO9761, ONR Grant

Introduction