On-line pretreatment using methylcellulose-immobilized cation-exchange restricted access media for direct liquid chromatography/mass spectrometric determination of basic drugs in plasma

Rapid Commun Mass Spectrom. 2005;19(19):2827-32. doi: 10.1002/rcm.2130.

Abstract

A novel methylcellulose-immobilized restricted access media column with strong cation-exchange groups on an internal surface (MC-SCX) was evaluated for the direct injection analysis of basic polar drugs in plasma by column-switching liquid chromatography/mass spectrometry (LC/MS). Analytical conditions, including an automated pretreatment step and MS detection, were optimized for a series of basic drugs (doxepin, desipramine, imipramine, nortriptyline, amitriptyline, clomipramine). On-line pretreatment with the MC-SCX column followed by fast gradient analysis using a C18 column resulted in a total analysis cycle time of 7 min for each spiked plasma sample. More than 150 plasma samples spiked with target compounds were measured without compromising MS detection (relative standard deviations less than 11% for all compounds, and regression coefficients greater than 0.99).

Publication types

  • Evaluation Study

MeSH terms

  • Animals
  • Blood Chemical Analysis / methods*
  • Cation Exchange Resins / chemistry*
  • Chromatography, Liquid / methods*
  • Methylcellulose / chemistry*
  • Online Systems
  • Pharmaceutical Preparations / blood*
  • Rats
  • Reproducibility of Results
  • Sensitivity and Specificity
  • Solutions
  • Spectrometry, Mass, Electrospray Ionization / methods*

Substances

  • Cation Exchange Resins
  • Pharmaceutical Preparations
  • Solutions
  • Methylcellulose