Purification and functional characterization of the ligand-binding domain from the retinoic acid receptor alpha: evidence that sulfhydryl groups are involved in ligand-receptor interactions

Biochemistry. 1993 Nov 23;32(46):12428-36. doi: 10.1021/bi00097a022.

Abstract

The pGEX-2T expression vector was used to produce the ligand-binding domain from the human retinoic acid receptor alpha (hRAR alpha LBD) in Escherichia coli. The resulting fusion protein, containing the glutathione S-transferase separated from the truncated receptor (hRAR alpha 186-462) by a thrombin cleavage site, was purified with use of affinity chromatography on immobilized glutathione. A 90% homogeneity was obtained, with a specific activity of 100 pmol/mg and an overall 10% yield. Following purification and thrombin cleavage, a predominant monomeric (stokes radius = 2.3 nm, molecular mass of 32 kDa) [3H]retinoic acid hRAR alpha LBD complex was characterized by high-performance size-exclusion chromatography. The purified hRAR alpha LBD bound retinoic acid with an apparent Kd of 9 nM, a value close to the Kd of the full-length hRAR alpha expressed in COS cells. Kinetic studies at 0 degrees C demonstrate that the association of [3H]retinoic acid and [3H]CD367, a synthetic retinoid, to the overexpressed receptor was extremely rapid (complete in less than 3 min), whereas their dissociation from the receptor was slower, with half-lives of about 40 min at 0 degrees C. Experiments performed at various subzero temperatures allowed a more accurate assay of the association rate constant and indicate that the entropy of activation (delta Sa) is positive, which is characteristic of hydrophobic interactions. The ligand-binding activity was markedly decreased by pretreatment with various sulfhydryl modifying agents. 5,5'-Dithiobis(2-nitrobenzoic acid) (DTNB) appeared to be the most potent, whereas iodoacetamide was the least active. Furthermore, a series of N-alkylmaleimides was shown to inactivate the recombinant receptor.(ABSTRACT TRUNCATED AT 250 WORDS)

MeSH terms

  • Binding Sites
  • Humans
  • In Vitro Techniques
  • Kinetics
  • Ligands
  • Molecular Weight
  • Receptors, Retinoic Acid / chemistry*
  • Receptors, Retinoic Acid / isolation & purification
  • Receptors, Retinoic Acid / metabolism
  • Recombinant Fusion Proteins
  • Retinoic Acid Receptor alpha
  • Retinoids / metabolism
  • Sulfhydryl Reagents / pharmacology
  • Thrombin / pharmacology

Substances

  • Ligands
  • RARA protein, human
  • Receptors, Retinoic Acid
  • Recombinant Fusion Proteins
  • Retinoic Acid Receptor alpha
  • Retinoids
  • Sulfhydryl Reagents
  • Thrombin