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em meio ácido. A ordem de adição de reagentes foi avaliada e os parâmetros analíticos foram otimizados. As faixas lineares de concentração foram de 2,5-90 e de 5,0-50 mg L -1 para CPT e NAC, respectivamente. Os limites de detecção (3σ) foram calculados em 0,22 e 1,8 mg L -1 e desvios padrão relativos (N = 10) foram inferiores que 1,0 e 2,1% para CPT e NAC, respectivamente. O procedimento foi empregado para a determinação de CPT e NAC em diversas formulações farmacêuticas e os resultados concordaram com os obtidos pelos métodos de referência para 95% de confiabilidade aplicando teste-t pareado.A spectrophotometric flow analysis procedure to determine Captopril (CPT) and N-acetyl-L-cysteine (NAC) in pharmaceutical formulations was developed based on the reaction with iminoquinone radical produced from the N,N-dimethyl-p-phenilenediamene (DMPD) oxidation in acid medium. The reagents addition order was evaluated and analytical parameters were optimized. The linear concentrations ranges were 2.5-90 and 5.0-50 mg L -1 for CPT and NAC, respectively. Limits of detection (3σ) were calculated at 0.22 and 1.8 mg L -1 and the relative standard deviation (N = 10) were lower than 1.0 and 2.1% for CPT and NAC, respectively. The procedure was employed for CPT and NAC determination in diverse pharmaceutical formulations and by applying paired t-test the results were in agreement with those obtained by reference methods for 95% confidence level.