Different techniques for extracting polyaromatic hydrocarbons (PAHs) from coal tar pitch for their quantitative determination by gas chromatography-mass spectrometry are compared. It has been found that the ultrasonic treatment of a sample allowed the quantitative extraction of PAHs from coal tar pitch. The results of the quantitative determination of PAHs in samples of coal tar pitch obtained by Soxhlet extraction and liquid-liquid extraction with ultrasonic treatment agree within the experimental error range.