Determination of sec-O-glucosylhamaudol in rat plasma by gradient elution liquid chromatography-mass spectrometry

J Chromatogr B Analyt Technol Biomed Life Sci. 2014 Jan 1:944:35-8. doi: 10.1016/j.jchromb.2013.11.001. Epub 2013 Nov 15.

Abstract

Sec-O-glucosylhamaudol is one of the major bioactive compounds of the Saposhnikoviae Radix. A simple and selective liquid chromatography-mass spectrometry (LC-MS) method for determination of sec-O-glucosylhamaudol in rat plasma was developed. After addition of carbamazepine as internal standard (IS), protein precipitation with acetonitrile-methanol (9:1, v/v) was used as sample preparation. Chromatographic separation was achieved on a Zorbax SB-C18 (2.1mm×150mm, 5μm) column with acetonitrile-0.1% formic acid in water as mobile phase with gradient elution. Electrospray ionization (ESI) source was applied and operated in positive ion mode; selective ion monitoring (SIM) mode was used for quantification using target fragment ions m/z 439 for sec-O-glucosylhamaudol and m/z 237 for the IS. Calibration plots were linear over the range of 50-8000ng/mL for sec-O-glucosylhamaudol in rat plasma. Mean recovery of sec-O-glucosylhamaudol in plasma was in the range of 74.8-83.7%. Intra-day and inter-day precision were both <15%. This method was successfully applied in pharmacokinetic study after intravenous administration of 2.5mg/kg sec-O-glucosylhamaudol in rats.

Keywords: LC–MS; Pharmacokinetics; Rat plasma; Sec-O-glucosylhamaudol.

MeSH terms

  • Animals
  • Carbamazepine
  • Chromatography, Liquid / methods*
  • Chromones / blood*
  • Chromones / chemistry
  • Chromones / pharmacokinetics
  • Linear Models
  • Male
  • Mass Spectrometry / methods*
  • Rats
  • Rats, Sprague-Dawley
  • Reproducibility of Results
  • Sensitivity and Specificity

Substances

  • Chromones
  • Carbamazepine