Development and validation of a LC-MS/MS method for the quantification of the checkpoint kinase 1 inhibitor SRA737 in human plasma

Bioanalysis. 2017 Jul;9(13):1001-1010. doi: 10.4155/bio-2017-0043. Epub 2017 Jul 10.

Abstract

Aim: SRA737 is an orally active small-molecule inhibitor of checkpoint kinase 1 being investigated in an oncology setting. A HPLC-MS/MS method for quantifying plasma concentrations of SRA737 was validated.

Methods & results: Sample preparation involved protein precipitation with acetonitrile following addition of 13C15N-deuterated SRA737 as internal standard. A rapid and selective method was fully validated across a range of 5-20,000 ng/ml, exhibiting good sensitivity, overall precision (expressed as coefficient of variation) ≤8.0% and accuracy 96-102%. Consistently high recovery was observed, with no matrix effect and a lower limit of quantitation of 5 ng/ml.

Conclusion: A novel method for analyzing SRA737 in human plasma has been validated and is now being utilized for quantification of SRA737 in a Phase I trial.

Keywords: CCT245737; CHK1; LC–MS/MS; SRA737; cancer; pharmacokinetics; validation study.

Publication types

  • Validation Study

MeSH terms

  • Blood Chemical Analysis / methods*
  • Checkpoint Kinase 1 / antagonists & inhibitors*
  • Chromatography, High Pressure Liquid / methods*
  • Heterocyclic Compounds, 4 or More Rings / blood*
  • Heterocyclic Compounds, 4 or More Rings / pharmacology
  • Humans
  • Limit of Detection
  • Linear Models
  • Protein Kinase Inhibitors / blood*
  • Protein Kinase Inhibitors / pharmacology
  • Tandem Mass Spectrometry / methods*

Substances

  • Heterocyclic Compounds, 4 or More Rings
  • Protein Kinase Inhibitors
  • SRA737
  • Checkpoint Kinase 1