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.

Quantification of Tricyclic and Nontricyclic Antidepressants in Spiked Plasma and Urine Samples Using Microextraction in Packed Syringe and Analysis by LC and GC-MS

“…A number of LC-UV methods for determining antidepressants and their metabolites have been developed and reviewed [24][25][26][27][28][29][30][31][32][33]. For sample preparation prior to LC-UV analysis of antidepressants in biological fluids, either liquid-liquid extraction [34,35] or solid-phase extraction [36,37] was used.…”

Development and validation of an HPLC method for the determination of benzodiazepines and tricyclic antidepressants in biological fluids after sequential SPE

“…Some of these drugs have been determined in serum by direct on-column injection [46], automated online SPE [30], SPME [47,48], online dialysis [30], direct LC analysis using restricted access extraction materials [49], supported liquid membrane technique [50], column switching techniques [51,52] as well as liquid phase microextraction [53,54]. However, only a limited number of methods applicable to the simultaneous determination of both classes of drugs in biological fluids [5] or in two-component tablet formulations [55] exist.…”

Quantification of nortriptyline in plasma by HPLC and fluorescence detection

“…Nevertheless, this fact should not affect the analytical determination of NT concentrations in plasma samples if calibration curves are prepared in blank plasma. The literature available on HPLC methods for the analysis of NT in plasma samples using conventional detectors shows that practically all of these methods are based on UV detection [6][7][8][10][11][12][14][15][16]. Due to the relatively low therapeutic window of NT concentrations for the treatment of depression (50-150 ng/ml) [23] or for smoking cessation (≥40 ng/ml) [22], plasma or serum samples containing NT have to be concentrate before if an HPLC equipped with a UV detector is used for the quantification of this drug at the indicated concentration values.…”

“…Several HPLC analytical methods for NT analysis in plasma samples have been published, but, in general, these methods involve excessively large plasma samples (0.5-1 ml) for their application to small laboratory animals such as rats [6][7][8][9][10][11][12][13][14][15][16], use long concentration processes or expensive equipment (liquid chromatography-tandem mass spectrometry) [17][18][19][20].…”