This study proposes a procedure for speciation of antimony by hydride generation atomic absorption spectrometry in pentavalent antimony drugs. The Sb III content was determined by selective generation of SbH 3 in medium with higher Sb V concentration using 4 to 20-fold lower citric acid solutions than recommended in the available literature. The multivariate optimization of the methods was performed through factorial design followed by a central composite design (CCD). The limit of detection

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... D) and limit of quantification (LOQ) were calculated at 0.15 and 0.05 µg L -1 and 0.48 and 0.17 µg L -1 , for total Sb and Sb III , respectively. The relative standard deviation (RSD) values ranged from 3.1 to 19.6% and 9.1 to 20.1%, while recovery ranged from 95.6 to 102.3% and 89.1 to 108.1%, for total Sb and Sb III , respectively. This method was applied for the analysis of meglumine antimoniate samples. Total Sb and Sb III concentrations ranged from 79.2 to 101.1 mg mL -1 and 0.08 to 0.41 mg mL -1 , respectively.