Optimization of solid-phase extraction and liquid chromatography-tandem mass spectrometry for simultaneous determination of capilliposide B and its active metabolite in rat urine and feces: Overcoming nonspecific binding

J Pharm Biomed Anal. 2016 Nov 30:131:6-12. doi: 10.1016/j.jpba.2016.08.003. Epub 2016 Aug 4.

Abstract

Capilliposide B, a novel oleanane triterpenoid saponin isolated from Lysimachia capillipes Hemsl, showed significant anti-tumor activities in recent studies. To characterize the excretion of Capilliposide B, a reliable liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed and validated for simultaneous determination of Capilliposide B and its active metabolite, Capilliposide A in rat urine and feces. Sample preparation using a solid-phase extraction procedure was optimized by acidification of samples at various degrees, providing extensive sample clean-up with a high extraction recovery. In addition, rat urinary samples were pretreated with CHAPS, an anti-adsorptive agent, for overcoming nonspecific analytes adsorption during sample storage and process. The method validation was conducted over the curve range of 10.0-5000ng/ml for both analytes. The intra- and inter-day precision and accuracy of the QC samples showed ≤11.0% RSD and -10.4-12.8% relative error. The method was successfully applied to an excretion study of Capilliposide B following intravenous administration.

Keywords: Capilliposide B; Excretion; LC–MS/MS; Nonspecific binding.

MeSH terms

  • Animals
  • Chromatography, Liquid / methods
  • Feces / chemistry*
  • Female
  • Male
  • Protein Binding / physiology
  • Rats
  • Rats, Sprague-Dawley
  • Saponins / analysis*
  • Saponins / metabolism*
  • Saponins / urine
  • Solid Phase Extraction / methods*
  • Tandem Mass Spectrometry / methods*
  • Triterpenes / analysis*
  • Triterpenes / metabolism*
  • Triterpenes / urine

Substances

  • Saponins
  • Triterpenes
  • capilliposide B