Development of a pharmacodynamic assay based on PLCγ2 phosphorylation for quantifying spleen tyrosine kinase (SYK)-Bruton's tyrosine kinase (BTK) signaling

J Biomol Screen. 2013 Sep;18(8):890-8. doi: 10.1177/1087057113489881. Epub 2013 May 23.

Abstract

Spleen tyrosine kinase (SYK) and Bruton's tyrosine kinase (BTK) are key mediators in coupling cell surface receptors, such as the B-cell receptor (BCR), to downstream signaling events affecting diverse biological functions. There is therefore tremendous interest in the development of pharmacological inhibitors targeting the SYK-BTK axis for the treatment of inflammatory disorders and hematological malignancies. A good pharmacodynamic (PD) assay, ideally a blood-based assay that measures proximal events, is warranted for evaluation of such inhibitors. In platelets, collagen-induced activation of membrane glycoprotein GPVI is dependent on the SYK-BTK axis. Here, we report the development of a novel immunoassay that uses the dissociation-enhanced lanthanide fluorescent immunoassay (DELFIA) to measure GPVI-mediated phosphorylation of phospholipase C γ2 (PLCγ2), a direct substrate of SYK and BTK, in platelets. The assay was validated using SYK or BTK inhibitors and generated IC50 correlated with those from the BCR-induced B-cell activation assay. Furthermore, this assay showed good stability and uniformity over a period of 24 h in different donors. Interestingly, compound IC50 values using blood from patients with rheumatoid arthritis were slightly higher compared with those produced using samples from healthy donors. This novel platelet PLCγ2 phosphorylation-based immunoassay should serve as a promising PD assay for preclinical and clinical development of inhibitors targeting the SYK-BTK axis.

Keywords: BTK; PLCγ2; SYK; pharmacodynamic assay; platelets.

MeSH terms

  • Agammaglobulinaemia Tyrosine Kinase
  • Antigens, CD / analysis
  • Antigens, Differentiation, T-Lymphocyte / analysis
  • Arthritis, Rheumatoid / blood
  • Arthritis, Rheumatoid / metabolism
  • Blood Platelets / cytology
  • Blood Platelets / metabolism
  • Enzyme Assays / methods*
  • Hematologic Neoplasms / metabolism
  • Humans
  • Immunoassay / methods*
  • Inflammation / metabolism
  • Intracellular Signaling Peptides and Proteins / antagonists & inhibitors*
  • Intracellular Signaling Peptides and Proteins / metabolism
  • Lectins, C-Type / analysis
  • Phospholipase C gamma / metabolism*
  • Phosphorylation
  • Protein-Tyrosine Kinases / antagonists & inhibitors*
  • Protein-Tyrosine Kinases / metabolism
  • Signal Transduction
  • Syk Kinase

Substances

  • Antigens, CD
  • Antigens, Differentiation, T-Lymphocyte
  • CD69 antigen
  • Intracellular Signaling Peptides and Proteins
  • Lectins, C-Type
  • Protein-Tyrosine Kinases
  • Agammaglobulinaemia Tyrosine Kinase
  • BTK protein, human
  • SYK protein, human
  • Syk Kinase
  • Phospholipase C gamma