Recebido em 31/08/2015; aceito em 04/02/2016; publicado na web em 15/04/2016 Pequi (Caryocar brasiliense Camb.), a typical fruit of the Brazilian Cerrado, is an important source of micronutrients and fatty acids. In this work, a new approach for the acid digestion (using H 2 SO 4 , HNO 3 and H 2 O 2 ) of pequi oil samples and the determination of Cu, Fe, Zn and Mn by flame atomic absorption spectrometry (F AAS) was employed. Capillary zone electrophoresis (CZE) was used for free fatty acid (FFA) determination after simple and fast extraction with heated ethanol. Good results regarding precision (RSD < 10%, in most cases), sensitivity and adequate LOD and LOQ values were obtained. The accuracy was evaluated using spike tests and the recoveries were from 97 to 107%. The analytes were investigated in four different pequi oil samples. Fe was the trace element with the highest concentration (from 1.99 to 10.3 mg/100 g), followed by Zn, Mn and Cu (1.15 to 3.19, 0.42 to 0.91 and 0.31 to 0.56 mg/100 g, respectively). The main FFA found were oleic acid and palmitic acid (1.61 to 10.7 and 0.82 to 2.69 g/100 g, respectively), while linoleic acid (0.50 g/100 g) was detected in only one sample. The pequi oil chemical composition showed good characteristics to be used as a food additive, in cosmetic formulations and for traditional medicine.