Microplastics (MPs) are considered an important stratigraphic indicator, or ‘technofossils’, of the Anthropocene. Research on MP abundance in the environment has gained much attention but the lack of a standardized procedure has hindered the comparability of the results. The development of an effective and efficient method of MP extraction from the matrix is crucial for the proper identification and quantifying analysis of MPs in environmental samples. The procedures of density separation used currently have various limitations: high cost of reagents, limited solution density range, hazardous reagents, or a combination of the above. In this research, a procedure based on density separation with the use of potassium formate water solution (H2O/KCOOH) in controlled conditions was performed. Experimental sediment mixtures, spiked with polyethylene (PE), polystyrene (PS), polyurethane (PUR) and polyethylene terephthalate (PET) particles were prepared and an extraction procedure was tested in the context of a weight-based quantitative analysis of MPs. This article discusses the effectiveness and safety of the method. It additionally provides new information on the interactions between MP particles and the mineral matter of the sediment. Results were acquired with the use of instrumental methods, namely thermogravimetry (TG), Fourier Transform Infrared (FTIR) spectroscopy, Field Emission Scanning Electron microscopy and Energy Dispersive spectrometry (SEM/EDS), as well as X-ray fluorescence (XRF) analysis.