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Sensitive capillary GC-MS-SIM determination of selective serotonin reuptake inhibitors: reliability evaluation by validation and robustness study
Authors:Berzas Nevado Juan José  Villaseñor Llerena María Jesús  Guiberteau Cabanillas Carmen  Rodríguez Robledo Virginia  Buitrago Sierra
Affiliation:Regional Institute for Applied Scientific Research, Ciudad Real, Spain.
Abstract:A simple, fast, selective and very sensitive capillary GC-MS method for the simultaneous determination of five antidepressant drugs is described. Fluoxetine, fluvoxamine, citalopram, sertraline and paroxetine belong to the newest and most important drug group termed selective serotonin reuptake inhibitors. Imipramine was used in this method as an internal standard for quantification. Optimum parameters for GC separation were investigated, i.e., flow rate, column head pressure, injector temperature, injection splitless conditions and oven temperature program. MS detection was performed in SIM mode to increase the sensitivity. Stability of the solutions, linear concentration range, accuracy, precision, LOD, LOQ (3.6-41.5 mg/L) and specificity were examined in the presence of excipients for checking the reliability of this method. The robustness was evaluated with a matrix of 15 experiments (seven factors and three levels) using Plackett-Burman fractional factorial experimental design, and Youden and Steiner statistical treatment. The method was applied to the analysis of these antidepressants in nearly all their pharmaceutical formulations, obtaining recoveries between 98.1% and 102.7% with regard to the claimed values.
Keywords:Capillary gas chromatography  Pharmaceutical formulations  Selective serotonin reuptake inhibitors  Robustness  Validation
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