European Commission Regulation 882/2004/EC requires that official control laboratories for foodstuffs in the member states are certified according to UNI EN ISO/IEC 17025:2005 (general requirement for the competence of calibration and testing laboratories). This mandatory requirement has resulted in a continuous adaptation and development of analytical procedures. The aim of this study was to develop a method for semiquantitative screening of polychlorinated biphenyls in fish for human consumption. According to the Commission Decision 657/2002/CE, the detection capability, the precision, the selectivity-specificity, and applicability-ruggedness-stability were determined to validate the method. Moreover, trueness was verified. This procedure resulted in rapid execution, which allowed immediate and effective intervention by the local health authorities to protect the health of consumers. Finally, the procedure has been recognized by the Italian accrediting body, ACCREDIA.