Modeling data from titration, amide H/D exchange, and mass spectrometry to obtain protein-ligand binding constants

J Am Soc Mass Spectrom. 2004 Mar;15(3):388-97. doi: 10.1016/j.jasms.2003.11.007.

Abstract

We recently reported a new method for quantification of protein-ligand interaction by mass spectrometry, titration and H/D exchange (PLIMSTEX) for determining the binding stoichiometry and affinity of a wide range of protein-ligand interactions. Here we describe the method for analyzing the PLIMSTEX titration curves and evaluate the effect of various models on the precision and accuracy for determining binding constants using H/D exchange and a titration. The titration data were fitted using a 1:n protein:ligand sequential binding model, where n is the number of binding sites for the same ligand. An ordinary differential equation was used for the first time in calculating the free ligand concentration from the total ligand concentration. A nonlinear least squares regression method was applied to minimize the error between the calculated and the experimentally measured deuterium shift by varying the unknown parameters. A resampling method and second-order statistics were used to evaluate the uncertainties of the fitting parameters. The interaction of intestinal fatty-acid-binding protein (IFABP) with a fatty-acid carboxylate and that of calmodulin with Ca(2+) are used as two tests. The modeling process described here not only is a new tool for analyzing H/D exchange data acquired by ESI-MS, but also possesses novel aspects in modeling experimental titration data to determine the affinity of ligand binding.

Publication types

  • Research Support, U.S. Gov't, P.H.S.

MeSH terms

  • Amides / chemistry*
  • Calcium / metabolism
  • Calmodulin / chemistry
  • Calmodulin / metabolism
  • Deuterium Exchange Measurement
  • Ligands
  • Models, Molecular
  • Proteins / chemistry*
  • Proteins / metabolism*
  • Spectrometry, Mass, Electrospray Ionization / methods*
  • Thermodynamics
  • Titrimetry

Substances

  • Amides
  • Calmodulin
  • Ligands
  • Proteins
  • Calcium