Development of an intracellular quantitative assay to measure compound binding kinetics

Cell Chem Biol. 2022 Feb 17;29(2):287-299.e8. doi: 10.1016/j.chembiol.2021.07.018. Epub 2021 Sep 13.

Abstract

Contemporary drug discovery typically quantifies the effect of a molecule on a biological target using the equilibrium-derived measurements of IC50, EC50, or KD. Kinetic descriptors of drug binding are frequently linked with the effectiveness of a molecule in modulating a disease phenotype; however, these parameters are yet to be fully adopted in early drug discovery. Nanoluciferase bioluminescence resonance energy transfer (NanoBRET) can be used to measure interactions between fluorophore-conjugated probes and luciferase fused target proteins. Here, we describe an intracellular NanoBRET competition assay that can be used to quantify cellular kinetic rates of compound binding to nanoluciferase-fused bromodomain and extra-terminal (BET) proteins. Comparative rates are generated using a cell-free NanoBRET assay and by utilizing orthogonal recombinant protein-based methodologies. A screen of known pan-BET inhibitors is used to demonstrate the value of this approach in the investigation of kinetic selectivity between closely related proteins.

Keywords: BET proteins; BRD4; NanoBRET; SKR; bromodomain; k(off); k(on); kinetics; residence time; target engagement.

Publication types

  • Research Support, Non-U.S. Gov't

MeSH terms

  • Binding Sites
  • Bioluminescence Resonance Energy Transfer Techniques
  • Cells, Cultured
  • Female
  • Fluorescent Dyes / chemistry
  • Fluorescent Dyes / metabolism
  • HEK293 Cells
  • Humans
  • Kinetics
  • Luciferases / chemistry
  • Luciferases / metabolism*
  • Nerve Tissue Proteins / chemistry
  • Nerve Tissue Proteins / metabolism*
  • Receptors, Cell Surface / chemistry
  • Receptors, Cell Surface / metabolism*

Substances

  • DNER protein, human
  • Fluorescent Dyes
  • Nerve Tissue Proteins
  • Receptors, Cell Surface
  • Luciferases