Rapid, sensitive and selective HPLC-MS/MS method for the quantification of topically applied besifloxacin in rabbit plasma and ocular tissues: Application to a pharmacokinetic study

J Pharm Biomed Anal. 2016 Jan 5:117:37-46. doi: 10.1016/j.jpba.2015.08.023. Epub 2015 Aug 22.

Abstract

Besifloxacin is a fourth-generation broad-spectrum fluoroquinolone registered for the topical treatment of bacterial conjunctivitis. In this study, a rapid, sensitive and selective liquid chromatography tandem mass spectrometry (LC-MS/MS) method was developed for quantification of besifloxacin in rabbit plasma and ocular tissues using nateglinide as the internal standard (IS). The analyte and IS were separated on a Sepax GP-Phenyl column by isocratic elution with methanol-acetonitrile-5 mM ammonium formate-formic acid (29:55:16:0.1, v/v/v/v) as the mobile phase at a flow rate of 1.2 mL/min, and the total run time was 3.0 min. An electrospray ionization (ESI) source was applied and operated in the positive ion mode; multiple reaction monitoring (MRM) mode was used for quantification, and the monitored transitions were 394.2→377.1 for besifloxacin and m/z 318.3→166.1 for the IS. The calibration curve was linear over the range of 0.103-206 ng/mL for plasma and 2.06-2060 ng/mL for tears, aqueous humor, conjunctiva and cornea with correlation coefficient (r) greater than 0.99. The lower limit of quantification (LLOQ) for besifloxacin was 0.103 ng/mL for plasma and 2.06 ng/mL for other ocular tissues with good accuracy and precision. Intra- and inter-batch precision were both lower than 15% and accuracy ranged from 85% to 115% at all QC levels. The method was successfully applied to the pharmacokinetic study of besifloxacin in rabbit plasma and ocular tissues after single and multiple topical administrations.

Keywords: Besifloxacin; Fluoroquinolone; LC–MS/MS; Ocular pharmacokinetics; Rabbit; Topical.

Publication types

  • Research Support, Non-U.S. Gov't

MeSH terms

  • Administration, Ophthalmic
  • Administration, Topical
  • Animals
  • Aqueous Humor / drug effects
  • Aqueous Humor / metabolism
  • Azepines / administration & dosage*
  • Azepines / blood*
  • Azepines / metabolism
  • Chromatography, High Pressure Liquid / methods
  • Chromatography, High Pressure Liquid / standards
  • Conjunctiva / drug effects
  • Conjunctiva / metabolism*
  • Cornea / drug effects
  • Cornea / metabolism*
  • Fluoroquinolones / administration & dosage*
  • Fluoroquinolones / blood*
  • Fluoroquinolones / metabolism
  • Male
  • Rabbits
  • Tandem Mass Spectrometry / methods
  • Tandem Mass Spectrometry / standards*
  • Time Factors

Substances

  • Azepines
  • Fluoroquinolones
  • besifloxacin