A rapid and effective procedure for the extraction and determination of 4-allylanisole (estragole), 4-allyl-1,3-benzodioxole (safrole) and 4-allyl-1,2-dimetoxybenzene (eugenol methyl ether) in food products was developed. These compounds were isolated from food matrices by employing a simultaneous distillation–extraction (SDE) technique with a Likens and Nickerson apparatus and using dichloromethane as extraction solvent. The method was validated by conducting recovery studies on fortified food products at several concentrations. Recoveries ranged between 94 and 105%. The analyses were performed by capillary gas-chromatography, the compounds identified by retention times and confirmed by GC/MS. The detection limits, determined both in standard solutions and in foods, were 10, 5 and 8 ng/ml for estragole, safrole and eugenol methyl ether, respectively and the calibration curves showed a good linearity for all the three compounds in the concentration range 0.5–25 ppm, with correlation coefficients ranging between 0.996 and 1.000. In a number of successive analyses, the estragole peak area repeatability (RSD) was 0.20 ng/ml, whereas for safrole resulted 0.33 ng/ml and for eugenol methyl ether 0.45 ng/ml. The estragole, safrole and eugenol methyl ether levels were measured in 42 samples, for a total of six product types, including “Pesto” sauce, tomato sauce containing basil, “Cola tasting” beverages, Bologna sausage (polony), Vienna sausage (wurstel) and fresh basil. The levels ranged from below the detection limit up to 19.30 mg/kg for estragole in “Pesto” sauce.