Analysis of a basic drug by on-line solid-phase extraction liquid chromatography/tandem mass spectrometry using a mixed mode sorbent

Rapid Commun Mass Spectrom. 2002;16(8):805-13. doi: 10.1002/rcm.639.

Abstract

Two on-line configurations using multiple 6- and 10-port valves were investigated for high-flow on-line extraction of a basic drug in rat plasma and human urine using a reversed-phase and a cation-exchange SPE sorbent. The first configuration studied was a single reversed-phase extraction cartridge (2.1 x 20 mm, 25 microm) using an optimized washing protocol. The results showed that up to 1.5 mL of sample (urine or plasma diluted 1:1) can be injected with limits of quantification (LOQs) as low as 100 pg/mL. The second configuration studied was the combination of a cation exchanger and a reversed-phase cartridge using at-column dilution. The results showed better LOQs than those obtained with the single cartridge at 10 pg/mL with the same injection volume. The mass spectrometer was operated in the multiple reaction monitoring (MRM) mode. All calibration curves gave an average of 5% relative standard deviation (RSD).

MeSH terms

  • Absorption
  • Adrenergic beta-Antagonists / analysis
  • Adrenergic beta-Antagonists / blood
  • Adrenergic beta-Antagonists / urine
  • Animals
  • Chromatography, Liquid
  • Humans
  • Indicators and Reagents
  • Mass Spectrometry
  • Pharmaceutical Preparations / analysis*
  • Propranolol / analysis
  • Propranolol / blood
  • Propranolol / urine
  • Rats
  • Spectrometry, Mass, Electrospray Ionization

Substances

  • Adrenergic beta-Antagonists
  • Indicators and Reagents
  • Pharmaceutical Preparations
  • Propranolol