This paper describes a procedure for the isolation of 20 organic micro-pollutants among pesticides, drugs, recreational drugs, flame retardants from river sediments. After a solid-liquid extraction with a methanol:water (50:50, v/v) solution, the supernatant was diluted with water and cleaned up by stir-disc solid-phase extraction (SPE). The disc was made of buckypaper, a self-supporting entangled assembly of carbon nanotubes, which was used as a highly porous, two-sided, sorbent membrane. In the preliminary activation step, the membrane was oxidised for 2-hours with nitric acid to extend its extraction capability also to more polar compounds. All extracts were analysed by ultra-high-performance liquid chromatography-tandem mass spectrometry. A comparative investigation with commercial Strata-X Polymeric Reversed Phase SPE cartridges proved the effectiveness of the lab-made device. On the average, the analytes were recovered with yields around 69% (low spike level) and 80% (medium and high spike level), while only a couple of analytes exhibited values less than 50%. The relative standard deviation was always less than 20%. Limits of detections were in the range 0.02-9.9 ng g -1 . The validated method was then applied for the analysis of sediment samples from different sites of the River Turia basin in the area of Valencia (Spain), finding tris(2-chloroisopropyl)-phosphate in all sediments at a level ranging from 6.9 to 387.9 ng g -1 . Other compounds, such as pesticides and pharmaceuticals were more sporadically in these samples., Competing Interests: Declaration of Competing Interest Regarding the manuscript entitled “Multi-residue determination of organic micro-pollutants in river sediment by stir-disc solid phase extraction based on oxidized buckypaper” by P. Tomai, A. Gentili, S. Fanali, Yolanda Picó, the authors certify that there is no conflict of interest including any financial, personal or other relationships with other people or organizations regarding the material discussed., (Copyright © 2020. Published by Elsevier B.V.)