Abstract: The individual compound isotopic composition determination of polycyclic aromatic hydrocarbons（PAHs） has become an important method in pollutant source identification and assessment of bioavailability of these pollutants. Accurate and precise determination of individual compound isotopic composition of PAHs depends on the sample pretreatment and instrument measurement.This review is focused on the sample pretreatment techniques including Soxhlet extraction, accelerated solvent extraction (ASE) and the sample purification techniques such as silica gel, alumina gel, SPE, GPC, HPLC and TLC. The recent development on GCCIRMS instrument measurement and data processing for the measurement of individual compound isotopic composition of PAHs such as column head pressure, sampling time, PTVLVI technique and isotope internal standard are also been presented.