Estuaries are defined as a semi-enclosed water that serve as final receptors of organic matter. Emerging contaminants correspond, in most cases, to unregulated contaminants, which may be candidates for future regulation depending on research on their potential health efects and monitoring data regarding their occurrence. This is the case of the pharmaceuticals and personal care products (PPCPs) which the contamination origin is above all anthropogenic and continuously released in wastewater or directly in the environment (via human and animal excretion). They are more often persistent and bioaccumulable and the accurate assessment of PPCPs impact on the environment is as difficult as there is a multitude of input sources in environment. This work then aims to monitor PPCPs in the Piratininga lagoon which is located east of the Guanabara Bay, that is undergoing an accelerated process of residential and commercial expansion. In order to optimize time and cost, the sample extraction was defined based on tests of different methodologies, such as Solid Phase Extraction (SPE), a necessary step for extract purification. Identification and quantification were performed by gas chromatography coupled with mass spectrometry in Selected Ion Monitoring mode (SIM), combining sensitivity with high selectivity. For gas chromatography analysis, both methods, however, require prior derivatization to form a volatile compound. To assess the quality of the method, the linearity of the analytical curves was confirmed by the coefficient of determination (R2) value and by the F-test in the analysis of variance (ANOVA) of the regression. The homoscedasticity of the data was confirmed by the Breusch-Pagan test. The Limit of Detection (LOD) ranged from 0.11 to 0.52 ng g-1. Repeatability, expressed through the relative standard deviation (RSD), showed values below 30 percent. The average recovery of the analytes ranged from 59,8 percent to 100,7 percent. The validated method was applied to analyze sediment from Piratininga Lagoon and obtained results indicating a significant presence of the pharmaceuticals bisphenol A, beta-estradiol, and ibuprofen.