Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)An alternative methodology for simultaneous analysis of ethambutol, isoniazid, rifampicin and pyrazinamide in pharmaceutical formulations by capillary zone electrophoresis under UV direct detection with an analysis time of 8.0 min is proposed. Background running was based on the effective mobility curve of the analytes and an optimum separation condition was achieved using a 3(3) Box-Behnken design, with Brij 35, Cu(2+) and acetic acid/sodium acetate buffer as factors. An electrolyte consisting of 50.0 mmol L(-1) of acetic acid/sodium acetate buffer:12.5 mmol L(-1) of CuSO(4), and standard and sample solutions prepared in 2.00 mmol L(-1) of Brij 35 and 12.5 mmol L(-1) of CuSO(4) were optimized. After evaluating validation parameters, the method was successfully applied to the analysis of samples in the form of tablets and sachets. (C) 2010 Elsevier By. All rights reserved.821333339Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)Fundação de Amparo à Pesquisa do Estado de Minas Gerais (FAPEMIG)Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)CNPq [476386/2007-1, 300593/2008-2]Fundacao de Amparo a Pesquisa do Estado de Minas Gerais of Brazil [FAPEMIG-CEX-APQ 1906-502/07, CEX APQ 01837/08]