PCBs are a persistent organic pollutant (POP) and therefore are monitored in marine life including fish. Automated Solvent Extraction (ASE 350) technology, an automated extraction method, has been shown to produce good recoveries of naturally occurring PCBs from fish tissue samples, and is approved for use in U.S. EPA SW-846 Method 3545 for the extraction of PCBs, OCPs, BNAs, OPPs, herbicides, and dioxins and furans. ASE operates at elevated temperatures, thus increasing the efficiency of the extraction process. Here we demonstrate the extraction of PCBs in a raw fish tissue sample.