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Leon-Muez, D., Penalver-Duque, P., Ciudad, C., Munoz, M., Infante, O., Guemes Santos, S., Parrilla Giraldez, R., Serrano, L. 2020. First sampling of microplastics in streams and rivers of peninsular Spain. Ecosistemas 29(3):2087. https://doi.org/10.7818/ECOS.2087 During 2019 and 2020 a sampling campaign to identify microplastics was carried out in 157 streams and rivers in mainland Spain. The sampling was done by applying a sampling methodology developed by HyT, (Hombre y Territorio Association) within the framework of the LIBERA Project, and was concomitant with a pollutant monitoring in IBA (Important Bird and Biodiversity Areas) carried out by SEO/BirdLife. Samples were initially processed for the detection of microplastics under stereoscopic microscope and then, subjected to Fourier Transform Infrared Spectroscopy (FTIR) analysis, by the Microanalysis Service of the University of Seville. The results of this sampling campaign, the first to be carried out in Spain for the detection of these pollutants, showed that more than 70% of the samples presented microplastics, with a predominance of fibers, fragments and films. Among the samples analyzed with FTIR, a total of 33 different polymers have been identified. This work offers relevant data about this problem in rivers and streams of Spain.