Abstract: Residual amounts of polycyclic aromatic hydrocarbons (PAH′s) in samples of water and soil were extracted by dispersive liquid phase micro-extraction (DLPME) with CS2 as extraction solvent and acetone as dispersant. The eluate was used for HPLC analysis, and the detectors of DAD and FLD were adopted in the determination. LiChrospher PAH column was used as stationary phase and mixed solutions of acetonitrile and water with different mixing ratio were used as mobile phase in the gradient elution. Under the optimized conditions, the enrichment factors between 220-560 were achieved, and 16 PAH′s in water samples were clearly separated. Values of detection limit (3S/N) found were in the range of 0.002-0.05 μg·L-1. Values of recovery found by standard addition method were in the range of 64%-108% with RSD′s (n=7) in the range of 2.0%-7.8%.