RESUMO
Capillary electrophoresis (CE) with UV detection for the simultaneous and short-time analysis of clenbuterol, salbutamol, procaterol, fenoterol is described and validated. Optimized conditions were found to be a 10 mmoll(-1) borate buffer (pH 10.0), an separation voltage of 19 kV, and a separation temperature of 32 degrees C. Detection was set at 205 nm. Under the optimized conditions, analyses of the four analytes in pharmaceutical and human urine samples were carried out in approximately 1 min. The interference of the sample matrix was not observed. The LOD (limits of detection) defined at S/N of 3:1 was found between 0.5 and 2.0 mgl(-1) for the analytes. The linearity of the detector response was within the range from 2.0 to 30 mgl(-1) with correlation coefficient >0.996.
Assuntos
Agonistas Adrenérgicos beta/análise , Agonistas Adrenérgicos beta/urina , Preparações Farmacêuticas/química , Agonistas Adrenérgicos beta/química , Agonistas Adrenérgicos beta/isolamento & purificação , Albuterol/análise , Albuterol/química , Albuterol/isolamento & purificação , Albuterol/urina , Soluções Tampão , Clembuterol/análise , Clembuterol/química , Clembuterol/isolamento & purificação , Clembuterol/urina , Eletroforese Capilar , Fenoterol/análise , Fenoterol/química , Fenoterol/isolamento & purificação , Fenoterol/urina , Humanos , Concentração de Íons de Hidrogênio , Modelos Lineares , Procaterol/análise , Procaterol/química , Procaterol/isolamento & purificação , Procaterol/urina , Reprodutibilidade dos Testes , Sensibilidade e Especificidade , Temperatura , Fatores de Tempo , Raios UltravioletaRESUMO
This paper describes the methodological optimization and validation of a simple micellar electrokinetic chromatography for the rapid simultaneous separation of 2-methyl-4-isothiazolin-3-one, methylparaben, ethylparaben, propylparaben, and butylparaben. By using a 30 mM phosphate buffer (pH 7.2) containing 30 mM sodium dodecyl sulfate (SDS), an applied voltage of 10 kV and a separation temperature of 40 degrees C, a quantitative determination was achieved, resulting in an analysis time of approximately 4 min. Only dilution and filtration are needed before analysis. The parameters for validation, such as linear ranges, detection limits, accuracy, and precision, are also reported.