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Sensitive capillary GC‐MS‐SIM determination of selective serotonin reuptake inhibitors: Reliability evaluation by validation and robustness study
Author(s) -
Berzas Nevado Juan José,
Villaseñor Llerena María Jesús,
Guiberteau Cabanillas Carmen,
Rodríguez Robledo Virginia,
Buitrago Sierra
Publication year - 2006
Publication title -
journal of separation science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.72
H-Index - 102
eISSN - 1615-9314
pISSN - 1615-9306
DOI - 10.1002/jssc.200500119
Subject(s) - chromatography , chemistry , citalopram , fluvoxamine , fractional factorial design , factorial experiment , sertraline , fluoxetine , antidepressant , serotonin , mathematics , receptor , hippocampus , neuroscience , biology , biochemistry , statistics
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.