Published: Journal of Chromatographic Science, ISSN 0021-9665 Volume 44, Number 6, July 2006, pp.340-346

Optimization of the SPME Parameters and Its Online Coupling with HPLC for the Analysis of Tricyclic Antidepressants in Plasma Samples

Claudete Alves[1], Christian Fernandes[1], Alvaro José dos Santos Neto[1], José Carlos Rodrigues[1], Maria Eugênia Costa Queiroz[2], and Fernando Mauro Lanças[1],
[1]Universidade de São Paulo, Instituto de Química de São Carlos Av. Trabalhador Sãocarlense 400, Caixa Postal 780, CEP 13566-590, São Carlos (SP), Brazil and
[2]Universidade de São Paulo, Departamento de Química, Faculdade de Filosofia Ciências e Letras de Ribeirão Preto

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 23 factorial design plus a central point to evaluate the influence of the time, temperature, and matrix pH. A Polydimethylsiloxane­divinylbenzene (60-µm film thickness) fiber is selected after the assessment of different types of coating. The chromatographic separation is realized using a C18 column (150 ¥ 4.6 mm, 5-µm 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 UV­vis detection at 214 nm. Among the factorial design conditions evaluated, the best results are obtained at a pH 11.0, temperature of 30°C, and extraction time of 45 min. The proposed method, using a lab-made SPME­LC interface, allowed the determination of tricyclic antidepressants in in plasma at therapeutic concentration levels.

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