In this research the possibility of application of an innovative, simple, economical, selective ability and green (environmentally friendly) method of salting out and Vortex-Assisted dispersive liquid-liquid microextraction based on solidification of floating organic drop by using high performance liquid chromatography with containing UV for pre-concentration, the extraction and determination of polysiclic in water and solid samples followed by HPLC was studied. In this method three integrated and combined approaches have been adopted so as to maximize the advantages of the approach used while minimizing their disadvantages. The effects of experimental variables such as pH, the type and volume of dispersive extracting solvents (μl, pH), the volume of organic drop microextraction (extracting solvent), salt density (concentration), centrifuge condition (time), extraction time and temperature were examined, and the process of optimization was obtained by using a software based on Response Surface Methodology (RSM) and Box-Behnken design [as the experimental model] and Desirability Function (DF). This method has appropriate linear calibration between 0.2 to 800μg/L, and a significant limit of detection coefficient (r2> 9991) and low detection range (between 0.05 to 0.09 μg/L). The above method was also applied for the successful determination of polycyclic aromatic hydrocarbons in industrial was water, water and soil samples PAHs) and the percentage of recycling, repeatability and reproducibility, resulting in satisfactory results. Simplicity, being economical, quickness, proper repeatability, less consumption of organic solvent and efficient decomposition are of the principal advantages (merits) of the proposed method for the decomposition and determination of polycyclic aromatic hydrocarbons (PAHs) in water samples.