An NMR-based antagonist induced dissociation assay for targeting the ligand-protein and protein-protein interactions in competition binding experiments

J Med Chem. 2007 Sep 6;50(18):4382-7. doi: 10.1021/jm070365v. Epub 2007 Aug 16.

Abstract

We present an NMR-based antagonist induced dissociation assay (AIDA) for validation of inhibitor action on protein-protein interactions. As opposed to many standard NMR methods, AIDA directly validates the inhibitor potency in an in vitro NMR competition binding experiment. AIDA requires a large protein fragment (larger than 30 kDa) to bind to a small reporter protein (less than 20 kDa). We show here that a small fragment of a protein fused to glutathione S-transferase (GST) can effectively substitute the large protein component. We successfully used a GST-tagged N-terminal 73-residue p53 domain for binding studies with the human MDM2 protein. Other interactions we studied involved complexes of CDK2, cyclin A, p27, and the retinoblastoma protein. All these proteins play a key role in the cell division cycle, are associated with tumorigenesis, and are thus the subject of anticancer therapy strategies.

MeSH terms

  • Binding, Competitive
  • Cyclin A / chemistry*
  • Cyclin-Dependent Kinase 2 / chemistry*
  • Cyclin-Dependent Kinase Inhibitor p27 / chemistry*
  • Glutathione Transferase / chemistry
  • Glutathione Transferase / genetics
  • Humans
  • Ligands
  • Magnetic Resonance Spectroscopy
  • Nitrogen Isotopes
  • Protein Binding
  • Protein Structure, Tertiary
  • Proto-Oncogene Proteins c-mdm2 / chemistry*
  • Recombinant Fusion Proteins / chemistry
  • Recombinant Fusion Proteins / genetics
  • Retinoblastoma Protein / chemistry*
  • Tumor Suppressor Protein p53 / chemistry*
  • Tumor Suppressor Protein p53 / genetics

Substances

  • Cyclin A
  • Ligands
  • Nitrogen Isotopes
  • Recombinant Fusion Proteins
  • Retinoblastoma Protein
  • TP53 protein, human
  • Tumor Suppressor Protein p53
  • Cyclin-Dependent Kinase Inhibitor p27
  • MDM2 protein, human
  • Proto-Oncogene Proteins c-mdm2
  • Glutathione Transferase
  • Cyclin-Dependent Kinase 2