Quantitative analysis of atractylenolide I in rat plasma by LC-MS/MS method and its application to pharmacokinetic study

J Pharm Biomed Anal. 2012 Jan 25:58:172-6. doi: 10.1016/j.jpba.2011.09.023. Epub 2011 Oct 1.

Abstract

A new high-performance liquid chromatography/tandem mass spectrometry (LC-MS/MS) was developed for quantitative analysis of atractylenolide I in rat plasma using buspirone as internal standard (I.S.). Rat plasma samples were deproteined with methanol and acetonitrile (1:1, v/v). Atractylenolide I and I.S. were separated on a Phenomenex Gemini C(18) column (50 mm × 2.0 mm, 5 μm) with gradient mobile phase at the flow rate of 0.4 ml/min. The detection was performed by positive ion electrospray ionization (ESI) in multiple reaction monitoring (MRM) mode. The linear calibration curve of atractylenolide I in rat plasma ranged 2.0-5000 ng/ml (R>0.9979). The limit of detection (LOD) and the limit of quantification (LOQ) were 0.6 ng/ml and 2.0 ng/ml, respectively. Both accuracy and precision of the assay were satisfactory. The recoveries of atractylenolide I and I.S. were 91.4% and 87.8%, respectively. This fully validated method was applied to a pharmacokinetic study of atractylenolide I in rats administered with 20 g/kg Atractylodis extract. The main pharmacokinetic parameters T(max) (the time to peak), C(max) (the concentration to peak), T(0.5) (the biological half time), and K(e) (the elimination rate constant) were 0.81 ± 0.11h, 7.99 ± 1.2 ng/ml, 1.94 ± 0.27 h, 0.365 ± 0.06/h, respectively.

Publication types

  • Research Support, Non-U.S. Gov't

MeSH terms

  • Acetonitriles / chemistry
  • Animals
  • Buspirone / analysis
  • Buspirone / chemistry
  • Calibration
  • Chromatography, High Pressure Liquid / methods*
  • Female
  • Lactones / blood*
  • Lactones / pharmacokinetics*
  • Limit of Detection
  • Male
  • Methanol / chemistry
  • Rats
  • Rats, Wistar
  • Reference Standards
  • Sesquiterpenes / blood*
  • Sesquiterpenes / pharmacokinetics*
  • Spectrometry, Mass, Electrospray Ionization / methods
  • Tandem Mass Spectrometry / methods*

Substances

  • Acetonitriles
  • Lactones
  • Sesquiterpenes
  • atractylenolide I
  • Buspirone
  • Methanol
  • acetonitrile