Eco-Friendly, Simple, Fast, and Sensitive UPLC-MS/MS Method for Determination of Pexidartinib in Plasma and Its Application to Metabolic Stability

Molecules. 2022 Jan 4;27(1):297. doi: 10.3390/molecules27010297.

Abstract

Pexidartinib is the first drug approved by the U.S. Food and Drug Administration specifically to treat the rare joint tumor tenosynovial giant cell tumor. In the current study, a validated, selective, and sensitive UPLC-MS/MS assay was developed for the quantitative determination of pexidartinib in plasma samples using gifitinib as an internal standard (IS). Pexidartinib and IS were extracted by liquid-liquid extraction using methyl tert-butyl ether and separated on an acquity BEH C18 column kept at 40 °C using a mobile phase of 0.1% formic acid in acetonitrile: 0.1% formic acid in de-ionized water (70:30). The flow rate was 0.25 mL/min. Multiple reaction monitoring (MRM) was operated in electrospray (ESI)-positive mode at the ion transition of 418.06 > 165.0 for the analyte and 447.09 > 128.0 for the IS. FDA guidance for bioanalytical method validation was followed in method validation. The linearity of the established UPLC-MS/MS assay ranged from 0.5 to 1000 ng/mL with r > 0.999 with a limit of quantitation of 0.5 ng/mL. Moreover, the metabolic stability of pexidartinib in liver microsomes was estimated.

Keywords: UPLC-MS/MS; gifitinib; metabolic stability; pexidartinib; tyrosine kinase inhibitor.

MeSH terms

  • Aminopyridines / chemistry
  • Aminopyridines / pharmacokinetics*
  • Antineoplastic Agents, Immunological / chemistry
  • Antineoplastic Agents, Immunological / pharmacokinetics*
  • Chromatography, High Pressure Liquid* / methods
  • Chromatography, High Pressure Liquid* / standards
  • Drug Monitoring / methods
  • Drug Monitoring / standards
  • Drug Stability
  • Molecular Structure
  • Protein Kinase Inhibitors / chemistry
  • Protein Kinase Inhibitors / pharmacokinetics*
  • Pyrroles / chemistry
  • Pyrroles / pharmacokinetics*
  • Reproducibility of Results
  • Sensitivity and Specificity
  • Tandem Mass Spectrometry* / methods
  • Tandem Mass Spectrometry* / standards

Substances

  • Aminopyridines
  • Antineoplastic Agents, Immunological
  • Protein Kinase Inhibitors
  • Pyrroles
  • pexidartinib