Pyrene is one of the chemical compounds of polycyclic aromatic hydrocarbons (PAHs) that has been reported as toxic, carcinogenic, and mutagenic which commonly found in water, food, soil, and air. Therefore, a study of ultrasonic assisted dispersive liquid-liquid microextraction (USA-DLLME) was conducted to extract pyrene from polluted water. The analytical parameters such as volume of extractant solvent, volume of disperser solvent, sonication time, and centrifugation speed were optimized using response surface method (RSM). Gas chromatography-flame ionization detector was used to analyse the pyrene content. The extraction recovery obtained for validation on real water based on optimization are in the range of 14.8%-49.8%. The low value of extraction recovery must be due to unsuitable types of extraction solvent used. However, this study have achieved all the objectives based on the developed method.