In this study a simple extraction procedure was developed to minimize the sulfur interferences on the determination of butyltin in sediment samples based on extraction with tartaric acid solution.The optimal conditions were determined using an experimental design methodology and these were achieved using a solution of tartaric acid (0.5 M) with methanol (30 % v/v) for 12 hours in an orbital shaker.This protocol could be followed by a liquid-liquid extraction and this organic phase can be analyzed directly by gas chromatography with pulsed flame photometric detection (GC-PFPD) without any further cleanup due to interferences from elemental sulfur were completely eliminated.The accuracy of the procedure was verified analyzing two reference materials (CRM) (BCR-646, freshwater sediment and PACS-2, marine sediment) and comparing the results to the certified values, the optimized method produced satisfactory results certified values in the CRMs.Finally, harbour sediment samples were analyzed in order to evaluate the suitability of the method for organotin control in complex environmental samples containing high concentrations of sulfur compounds.