Optimization of the SPME parameters and its online coupling with HPLC for the analysis of tricyclic antidepressants in plasma samples

J Chromatogr Sci. 2006 Jul;44(6):340-6. doi: 10.1093/chromsci/44.6.340.

Abstract

Solid-phase microextraction (SPME)-liquid chromatography (LC) is used to analyze tricyclic antidepressant drugs desipramine, imipramine, nortriptyline, amitriptyline, and clomipramine (internal standard) in plasma samples. Extraction conditions are optimized using a 2(3) factorial design plus a central point to evaluate the influence of the time, temperature, and matrix pH. A Polydimethylsiloxane-divinylbenzene (60-mum film thickness) fiber is selected after the assessment of different types of coating. The chromatographic separation is realized using a C(18) column (150 x 4.6 mm, 5-microm particles), ammonium acetate buffer (0.05 mol/L, pH 5.50)-acetonitrile (55:45 v/v) with 0.1% of triethylamine as mobile phase and UV-vis detection at 214 nm. Among the factorial design conditions evaluated, the best results are obtained at a pH 11.0, temperature of 30 degrees C, and extraction time of 45 min. The proposed method, using a lab-made SPME-LC interface, allowed the determination of tricyclic antidepressants in in plasma at therapeutic concentration levels.

Publication types

  • Research Support, Non-U.S. Gov't

MeSH terms

  • Antidepressive Agents, Tricyclic / blood*
  • Chromatography, High Pressure Liquid / methods*
  • Dibenzazepines / blood*
  • Dimethylpolysiloxanes
  • Humans
  • Hydrogen-Ion Concentration
  • Polyvinyls
  • Solid Phase Microextraction / methods*
  • Temperature

Substances

  • Antidepressive Agents, Tricyclic
  • Dibenzazepines
  • Dimethylpolysiloxanes
  • Polyvinyls
  • poly(dimethylsiloxane-divinylbenzene)