Polycyclic Aromatic Hydrocarbons (PAHs) are toxic and persistent environmental pollutants with significant carcinogenic and mutagenic risks. These contaminants accumulate in soil, water, and air due to industrial emissions, vehicle exhaust, and combustion processes, necessitating efficient extraction and quantification techniques. Deep eutectic solvents (DES), a class of green and biodegradable solvents, have emerged as promising extractive materials for PAH analysis due to their low toxicity, tunable physicochemical properties, and high extraction efficiency. In this study, hydrophobic DES are employed as extractive media for the preconcentration of PAHs through a microliquid-liquid extraction procedure. The extracted PAHs are subsequently analyzed using High-Performance Liquid Chromatography (HPLC), which offers high sensitivity by leveraging the hydrophobicity of the DES to effectively separate and concentrate the PAHs. The optimization of extraction conditions, including DES composition, extraction efficiency, and chromatographic parameters, will be investigated to improve recovery rates and detection limits. This methodology provides a sustainable and efficient approach for PAH monitoring in environmental samples, contributing to the advancement of green analytical techniques for contamination assessment.