Development and validation of a rapid and simple LC-MS/MS method for quantification of vemurafenib in human plasma: application to a human pharmacokinetic study

Ther Drug Monit. 2015 Feb;37(1):132-6. doi: 10.1097/FTD.0000000000000110.

Abstract

Background: Vemurafenib (Zelboraf) is a new tyrosine kinase inhibitor that selectively targets activated BRAF V600E gene and is indicated for the treatment of advanced BRAF mutation-positive melanoma. We developed a simple method for vemurafenib quantification using liquid chromatography-tandem mass spectrometry. A stability study of vemurafenib in human plasma was also performed.

Methods: (13)C(6)-vemurafenib was used as the internal standard. A single-step protein precipitation was used for plasma sample preparation. Chromatography was performed on an Acquity UPLC system (Waters) with chromatographic separation by the use of an Acquity UPLC BEH C18 column (2.1 × 50 mm, 1.7-mm particle size; Waters). Quantification was performed using the monitoring of multiple reactions of following transitions: m/z 488.2 → 381.0 for vemurafenib and m/z 494.2 → 387.0 for internal standard.

Results: This method was linear over the range from 1.0 to 100.0 mcg/mL. The lower limit of quantification was 0.1 mcg/mL for vemurafenib in plasma. Vemurafenib remained stable for 1 month at all levels tested, when stored indifferently at room temperature (20 °C), at +4 °C, or at -20 °C. This method was used successfully to perform a plasma pharmacokinetic study of vemurafenib in a patient after oral administration at a steady state.

Conclusions: This liquid chromatography-tandem mass spectrometry method for vemurafenib quantification in human plasma is simple, rapid, specific, sensitive, accurate, precise, and reliable.

Publication types

  • Validation Study

MeSH terms

  • Antineoplastic Agents / blood*
  • Antineoplastic Agents / pharmacokinetics*
  • Calibration
  • Chromatography, High Pressure Liquid
  • Humans
  • Indicators and Reagents
  • Indoles / blood*
  • Indoles / pharmacokinetics*
  • Protein Kinase Inhibitors / blood*
  • Protein Kinase Inhibitors / pharmacology*
  • Quality Control
  • Reference Standards
  • Reproducibility of Results
  • Sulfonamides / blood*
  • Sulfonamides / pharmacokinetics*
  • Tandem Mass Spectrometry
  • Vemurafenib

Substances

  • Antineoplastic Agents
  • Indicators and Reagents
  • Indoles
  • Protein Kinase Inhibitors
  • Sulfonamides
  • Vemurafenib