The procedure for the determination of polycyclic aromatic hydrocarbons (PAH) in agricultural products on the example of five crops (rapeseed, sunflower, flax, corn, soybeans) by gas chromatography mass spectrometry (GC-MS) was developed. It was showed the advantage of using binary mixtures of organic solvents "hexanedichloromethane" for PAH extraction. The time of Soxhlet extraction is from 6 to 8 hours at optimized conditions. The fractionation and purification of extracts by column chromatography on deactivated alumina was optimized. The article presents the optimization of sample injection in the programmed temperature vaporization (PTV) mode, parameters of gas chromatographic separation and mass spectrometric detection in determining 16 priority PAH in agricultural products. The recoveries, correctness and accuracy of the proposed method were checked by “spikes” with concentrations 0.5, 1.0, 2.5, 5.0 μg kg-1. The linearity of the method was determined by calibration curves obtained for three measurements of calibration solutions with concentrations of 0.5-100 ng mL-1. The effectiveness of the proposed combination of sample preparation and analysis by PTV-GC-MS was studied for linearity, accuracy, matrix effects and reproducibility. The method was validated by linearity, accuracy, matrix effect and reproducibility.