Development and validation of an LC-MS/MS method for the determination of SB-505124 in rat plasma: Application to pharmacokinetic study

J Pharm Biomed Anal. 2016 Jan 5:117:205-9. doi: 10.1016/j.jpba.2015.09.002. Epub 2015 Sep 3.

Abstract

A sensitive, selective and rapid liquid chromatography-electrospray ionization-tandem mass spectrometry (LC-MS/MS) method has been developed for the quantification of the novel transforming growth factor-β (TGF-β) inhibitor SB-505124 in rat plasma and then validated. Plasma samples were prepared by simple protein precipitation. Separation was performed on a Diamonsil ODS chromatography column using a mobile phase of acetonitrile and 0.1% (v/v) aqueous formic acid. SB-505124 and the internal standard doxorubicin were detected in the positive ion mode using multiple reaction monitoring of the transitions at m/z 336.2→320.1 and 544.2→397.2, respectively. Calibration curve was linear (r>0.9996) over a concentration range of 10-5000 ng/mL with the lower quantification limit of 10 ng/mL. Both intra- and inter-day precision were within 6.5% and trueness were not more than 3.1%. Extraction recovery and matrix effect were within acceptable limits. Stability tests showed that SB-505124 and the IS remained stable throughout the analytical procedure. The validated LC-MS/MS method was then used to analyze the pharmacokinetics of SB-505124 administered to rats intravenously (8 mg/kg) or orally (10 mg/kg). Oral bioavailability of SB-505124 was calculated as 76.4%, indicating the potential of SB-505124 as an orally administered drug.

Keywords: LC–MS/MS; Pharmacokinetic study; Rat plasma; SB-505124; Validation.

Publication types

  • Research Support, Non-U.S. Gov't
  • Validation Study

MeSH terms

  • Administration, Oral
  • Animals
  • Benzodioxoles / administration & dosage
  • Benzodioxoles / blood*
  • Benzodioxoles / pharmacokinetics*
  • Chromatography, Liquid / methods
  • Imidazoles / administration & dosage
  • Imidazoles / blood*
  • Imidazoles / pharmacokinetics*
  • Male
  • Pyridines / administration & dosage
  • Pyridines / blood*
  • Pyridines / pharmacokinetics*
  • Rats
  • Rats, Sprague-Dawley
  • Receptors, Transforming Growth Factor beta / antagonists & inhibitors*
  • Tandem Mass Spectrometry / methods*

Substances

  • 2-(5-benzo(1,3)dioxol-5-yl-2-tert-butyl-3H-imidazol-4-yl)-6-methylpyridine hydrochloride
  • Benzodioxoles
  • Imidazoles
  • Pyridines
  • Receptors, Transforming Growth Factor beta