A fast and simple method for analysis of 14 PAHs in grilled and smoked muscle foods using acetonitrile based-extraction was validated. The optimum amounts of magnesium sulfate and sodium chloride that promoted phase separation of acetonitrile extract containing PAHs from water phase were selected by Central Composite Design. Matrix-matched calibration curves were constructed by adding different concentrations of PAHs and then subjected to extraction followed by HPLC with fluorescent detection. An excellent linearity for all compounds applying weighed least squares linear regression procedure was achieved. LODs and LOQs were lower than 0.12 and 0.39 ng g−1 respectively. Validation was done according to International Conference on Harmonization recommendations for 14 PAHs. The criteria for 4 EU marker PAHs (benz[a]anthracene, chrysene, benzo[b]fluoranthene and benzo[a]pyrene) established by European Comission Regulation No. 836/2011 was also accomplished. Repeatability and reproducibility were lower than 8 and 13.3%, and the most of recoveries fall in the range of 80–110% in different grilled and smoked muscle foods. The proposed method is a robust tool for determination of PAHs in grilled and smoked muscle foods, being easy to perform in short time.