Microplastic (MP) is a class of compounds that includes different polymeric synthetic materials in the size range between 5mm and 1µm. These materials have already been found in all environmental matrices and have great polluting potential. In addition to presenting physical, chemical and biological risks to organisms at the base of the food chain, they compromise water quality. In Brazil, the occurrence, distribution, characterization and impacts of this new class of pollutants is still poorly studied, especially in freshwater. The main objective of this study was to investigate the occurrence of MPs at four points in the Tietê-SP river and to evaluate the presence and concentration of polychlorinated biphenyls (PCBs) sorbed to these particles and to macroplastics. The sampling points in the Tietê River include: Biritiba-Mirim (P1), Santana do Parnaíba (P2), Tietê (P3) and the Barra Bonita reservoir located in Anhembi, SP (P4). To determine the occurrence of MPs, about 200 liters of surface water were collected with an aluminum bucket and poured into a 0.106 and 5.6 mm granulometric sieves scheme. MPs were quantified and classified by color, size and morphology. The chemical identity of the polymers was determined by vibrational midinfrared spectroscopy with Fourier transform (FTIR). MPs concentrations ranged from 6.67 to 1530 particles m -3 , being higher in P2 and P3. For the analysis of sorbed PCBs, the MPs were collected through nets of plankton fixed at each sampling point, for 30 minutes or until clog. Macroplastics were collected in a similar way in P2 and P3, however, in P1 and P4, they were collected from the river banks. All extracts were analyzed by gas chromatography coupled with mass spectrometry. The parameters used for validation proved to be adequate for the proposed objective, being them linearity, sensitivity, precision, accuracy, robustness and limits of detection and quantification. The total concentrations of PCBs in MPs and macroplastics ranged from 20.53 to 133.12 ng g -1 and from 24.98 to 40.99 ng g -1 , respectively. We expect that the results found can elucidate the relationship between MPs and organic pollutants in freshwater and provide relevant information about the current scenario of MPs in the Tietê River and the possible chemical risks associated with the transport of PCBs through these particles.