title: Optimization of the SPME parameters and its online coupling with HPLC for the analysis of tricyclic antidepressants in plasma samples.
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.
authors.affiliation: Universidade de São Paulo, Instituto de Química de São Carlos Av. Trabalhador Sãocarlense 400, Caixa Postal 780, CEP 13566-590, São Carlos (SP), Brazil.
authors.forename: Claudete
authors.initials: C
authors.lastname: Alves
authors.forename: Christian
authors.initials: C
authors.lastname: Fernandes
authors.forename: Alvaro José
authors.initials: AJ
authors.lastname: Dos Santos Neto
authors.forename: José Carlos
authors.initials: JC
authors.lastname: Rodrigues
authors.forename: Maria Eugênia
authors.initials: ME
authors.lastname: Costa Queiroz
authors.forename: Fernando Mauro
authors.initials: FM
authors.lastname: Lanças
mesh_terms: D000929:Antidepressive Agents, Tricyclic / Q000097:blood*; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D003984:Dibenzazepines / Q000097:blood*; D004129:Dimethylpolysiloxanes; D006801:Humans; D006863:Hydrogen-Ion Concentration; D011145:Polyvinyls; D052617:Solid Phase Microextraction / Q000379:methods*; D013696:Temperature
chemical_list: D000929:Antidepressive Agents, Tricyclic; D003984:Dibenzazepines; D004129:Dimethylpolysiloxanes; D011145:Polyvinyls; C445089:poly(dimethylsiloxane-divinylbenzene)