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Development of a Capillary Zone Electrophoretic method to determine six antidepressants in their pharmaceutical preparations. Experimental design for evaluating the ruggedness of method
Author(s) -
Rodríguez Flores Juana,
Berzas Nevado Juan J.,
Contento Salcedo Ana M.,
Cabello Díaz Maria P.
Publication year - 2004
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.200301646
Subject(s) - chromatography , fractional factorial design , capillary electrophoresis , chemistry , factorial experiment , detection limit , electrolyte , analyte , analytical chemistry (journal) , electrophoresis , resolution (logic) , central composite design , dosage form , matrix (chemical analysis) , response surface methodology , mathematics , electrode , statistics , artificial intelligence , computer science
A capillary zone electrophoresis method is proposed for the separation of six of the antidepressants most used for the treatment of mental illness (clomipramine, paroxetine, fluoxetine, citalopram, fluvoxamine, and trazodone). Optimum conditions for their separation were investigated. A background electrolyte solution consisting of 50 mM phosphate buffer adjusted to pH 2.0, hydrodynamic injection, and 25 kV as separation voltage were used. Relative standard deviations (RSD) were <0.38% and <2.93% for migration time and corrected peak area ( n = 24), respectively. Detection limits obtained for the six antidepressants ranged from 0.03 to 0.11 mg L –1 . Stability of the solutions, linear concentration range, accuracy, and precision were examined during validation of the method. A ruggedness test of this method was performed using the fractional factorial model of Plackett‐Burman, requiring in our case design of a matrix of 15 experiments, in which the influence of seven factors at three different levels was tested on different electrophoretic results: efficiency; resolution; and corrected peak area. Statistical evaluation of electrophoretic results was achieved by Youden and Steiner's method. The described method is rapid, sensitive, and rugged and it was tested for the pharmaceutical formulation analysis, giving recoveries between 95.6 and 99.1% with respect to the nominal content