Accelerated solvent extraction is an established technique to efficiently extract contaminants in solid and semisolid sample matrices with less solvent and time. Polyaromatic Hydrocarbons (PAHs) and Polychlorinated Biphenyls (PCBs) are considered toxic and carcinogenic, and therefore classified as persistent organic pollutants (POPs). Typically, PAHs and PCBs are extracted separately, using different solvent combinations. Our study demonstrates extraction of PAHs and PCBs using a single method from spiked mussel and from a soil spiked with a standard reference materials (SRMs).