A method was developed for determination of total antimony in hair samples from patients undergoing chemotherapy against Leishmaniasis based on the administration of pentavalent antimonial drugs. The method is based on microwave assisted digestion of the samples in a pressurized system, reduction of Sb 5+ to Sb 3+ with KI solution (10% w/v) in ascorbic acid (2%, w/v) and its subsequent determination by hydride generation atomic fluorescence spectrometry (HG-AFS). The proportions of each component (HCl, HNO 3 and water) used in the digestion were studied applying a constrained mixtures design. The optimal proportions found were 50% water, 25% HNO 3 and 25% HCl. Variables involved in the generation of antimony hydride were optimized using a Doehlert design revealing that good sensitivity is found when using 2.0% w/v NaBH 4 and 4.4 mol L -1 HCl. Under the optimum experimental conditions, the method allows the determination of antimony in hair samples with detection and quantification limits of 1.4 and 4.6 ng g -1 , respectively, and precision expressed as relative standard deviation (RSD) of 2.8% (n = 10 to 10.0 mg L -1 ). The developed method was applied in the analysis of hair samples from patients who take medication against Leishmaniasis.
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