Determination of fluoxetine, fluvoxamine, and clomipramine in pharmaceutical formulations by capillary gas chromatography

A simple and fast capillary gas chromatographic method with flame ionization detection is proposed for the simultaneous determination of fluoxetine, fluvoxamine, and clomipramine without a prederivatization. The reported method is the first one that allows the determination of three selective serotonin reuptake inhibitors. Optimal conditions for the quantitative separation were investigated: column head pressure (80 kPa), injector and detector temperatures (260 and 250 degrees C), time and temperature for the splitless step (0.75 min and 60 degrees C), size of sample (2 microL), and oven temperature program, providing analysis times shorter than 10 min. Aspects such as the stability of the solutions, linearity, accuracy, and precision are examined in order to validate this method. Peak purity and detection and quantitation limits are also assessed using mass selective detection. The scope of the validated method is tested in the analysis of pharmaceutical preparations, with recoveries between 97.5 and 102.5% with regard to their nominal contents.