Neste trabalho foi otimizada uma metodologia de rotina para quantificar e confirmar a presença de benzo(a)pireno (BaP) em cachaça. Foram avaliados três procedimentos de extração; um, utilizando extração em fase sólida (EFS) tanto para extração como para purificação e dois, empregando extração líquido-líquido, seguida de limpeza por cromatografia em coluna com sílica gel. O BaP foi quantificado por cromatografia líquida de alta eficiência (CLAE), com detecção por fluorescência e confirmação por cromatografia gasosa com detector de massas. The present study evaluated and optimized a routine method to quantify and confirm BaP in Brazilian sugar cane spirit (cachaça). Three extraction procedures were tested, one using SPE for extraction and clean-up, while two others were liquid-liquid partition extraction followed by silica gel chromatography clean-up. BaP was quantified by high performance liquid chromatography with fluorescence detection and confirmed by gas chromatography-mass spectrometry. HPLC detection and quantification limits were 0.03 and 0.10 μg L -1 , respectively. The recovery results ranged from 82.9 to 97.0% with coefficients of variation (CV) ranging from 0.5 to 4.9% at concentration levels of 0.1, 1.0 and 3.0 μg L -1 , which are in accordance with those described by other authors. The three procedures were appropriated to quantify BaP in cachaça, although SPE extraction is the cheapest, fastest and the least solvent-consuming. The levels of BaP contamination on twenty cachaça samples ranged from no detected (LOD < 0.03 μg L