A rugged and accurate liquid chromatography-tandem mass spectrometry method for quantitative determination of BMS-790052 in plasma

J Chromatogr B Analyt Technol Biomed Life Sci. 2011 Jul 15;879(22):2064-72. doi: 10.1016/j.jchromb.2011.05.036. Epub 2011 May 30.

Abstract

To support toxicokinetic assessments, a liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed and validated for the quantification of BMS-790052 in rat, dog, monkey, rabbit and mouse K(2)EDTA plasma. The drug was isolated from buffered samples using ISOLUTE C8 96-well solid phase extraction (SPE) plates. Chromatographic separation was achieved on a Waters Atlantis dC18 analytical column (2.1 mm × 50 mm, 5 μm) with detection accomplished using an API 4000 tandem mass spectrometer in positive ion electrospray and multiple reaction monitoring (MRM) mode. The standard curves, which ranged from 5.00 to 2000 ng/mL for BMS-790052, were fitted to a 1/x(2) weighted linear regression model. The intra-assay precision (%CV) and inter-assay precision (%CV) were within 8.5%, and the assay accuracy (%Dev) was within ±7.1 for rat, dog, monkey, rabbit and mouse K(2)EDTA plasma. This accurate, precise, and selective SPE/LC-MS/MS method has been successfully applied to analyze several thousands of non-clinical study samples.

MeSH terms

  • Animals
  • Antiviral Agents / administration & dosage
  • Antiviral Agents / blood*
  • Antiviral Agents / pharmacokinetics
  • Carbamates
  • Chromatography, Liquid / methods*
  • Dogs
  • Drug Stability
  • Drugs, Investigational
  • Female
  • Haplorhini
  • Imidazoles / administration & dosage
  • Imidazoles / blood*
  • Imidazoles / pharmacokinetics
  • Linear Models
  • Male
  • Mice
  • Pyrrolidines
  • Rabbits
  • Rats
  • Reproducibility of Results
  • Sensitivity and Specificity
  • Tandem Mass Spectrometry / methods*
  • Valine / analogs & derivatives
  • Viral Nonstructural Proteins / antagonists & inhibitors*

Substances

  • Antiviral Agents
  • Carbamates
  • Drugs, Investigational
  • Imidazoles
  • Pyrrolidines
  • Viral Nonstructural Proteins
  • NS-5 protein, hepatitis C virus
  • Valine
  • daclatasvir