Extraction and quantification of nano- and microplastics from sediments and soils is challenging. Although no standard method has been established so far, flotation is commonly used to separate plastic from mineral material. The objective of this study was to test the efficiency of flotation for the extraction of nano- and microplastics from biosolids and soil. We spiked biosolids and soil samples with polystyrene nano- and microbeads (0.05, 1.0, 2.6, 4.8, and 100 μm diameter). Different extraction methods (w/ and w/o H2O2 digestion) were tested, and plastic beads were separated from mineral particles by flotation in a ZnCl2 solution. Plastic particles were quantified by UV-Vis spectrometry and gravimetrically. While large beads (100 μm) could be quantitatively extracted (∼100%) from both biosolids and soils, smaller beads had low extraction efficiencies (ranging from 5 to 80%, with an average of 20%). Except for the 100 μm beads, oxidation with H2O2 negatively impacted the extraction efficiencies. For the soil, extraction with water only, followed by flotation in a ZnCl2 solution, resulted in relatively high extraction efficiencies (>75%) for beads larger than 1 μm, but low efficiencies (<30%) for the 0.05 and 1.0 μm beads. Our results indicate that while flotation generally works to separate plastic nano- and microbeads in a solution, the challenge is to quantitatively extract nano- and microbeads from a biosolids or soil matrix. Samples high in organic matter content require removal of the organic matter, but the common method of H2O2 oxidation leads to poor extraction efficiencies for nano- and microbeads.