Simple and sensitive liquid chromatography-tandem mass spectrometry methods for quantification of tadalafil in rat plasma: application to pharmacokinetic study in rats

Arch Pharm Res. 2013 Apr;36(4):457-63. doi: 10.1007/s12272-013-0046-1. Epub 2013 Feb 23.

Abstract

A simple and sensitive liquid chromatography-tandem mass spectrometry method was developed and validated in rat plasma for quantification of tadalafil, a novel therapeutic agent for erectile dysfunction. Tadalafil and acebutolol (internal standard) were extracted by liquid-liquid extraction with tert-butyl methyl ether. The chromatographic separation was performed on a reverse phase C18 column with a mobile phase consisting of 0.1 % formic acid and acetonitrile (45:55, v/v) at a flow rate of 0.3 mL/min. The protonated analyte was quantitated by multiple reaction monitoring with a Waters Quattro micro™ API mass spectrometer. The calibration curve was linear over a concentration range of 2-2000 ng/mL, and the lower limit of quantification was 2 ng/mL with a precision (CV %) of 10.9 %. Acceptable intra-day and inter-day precision and accuracy were obtained at 3 concentration levels (3, 200, and 1500 ng/mL). Tadalafil was found to be stable in a battery of studies, including bench top, freeze-thaw, and autosampler conditions. The validated method was successfully used to determine tadalafil concentration in rat plasma samples after oral administration at a dose of 1 mg/kg.

Publication types

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

MeSH terms

  • Acetonitriles / chemistry
  • Administration, Oral
  • Animals
  • Calibration
  • Carbolines / administration & dosage
  • Carbolines / blood*
  • Carbolines / pharmacokinetics*
  • Chromatography, Reverse-Phase* / standards
  • Drug Stability
  • Formates / chemistry
  • Limit of Detection
  • Liquid-Liquid Extraction
  • Male
  • Methyl Ethers / chemistry
  • Phosphodiesterase 5 Inhibitors / administration & dosage
  • Phosphodiesterase 5 Inhibitors / blood*
  • Phosphodiesterase 5 Inhibitors / pharmacokinetics*
  • Rats
  • Rats, Sprague-Dawley
  • Reference Standards
  • Reproducibility of Results
  • Tadalafil
  • Tandem Mass Spectrometry* / standards

Substances

  • Acetonitriles
  • Carbolines
  • Formates
  • Methyl Ethers
  • Phosphodiesterase 5 Inhibitors
  • formic acid
  • methyl tert-butyl ether
  • Tadalafil
  • acetonitrile