Polycyclic aromatic hydrocarbons (PAHs) are persistent organic pollutants that pose significant risks to both the environment and human health. This highlights the necessity for sensitive, reliable, and eco-friendly analytical methods for their detection. This study introduces an innovative green approach for PAH extraction utilizing two-dimensional mesoporous silica nanosheets (2D-MSNs) enhanced with deep eutectic solvents (DES). The synthesized 2D-MSN@DES composite was characterized using advanced techniques, including Fourier-transform infrared spectroscopy (FTIR), Brunauer–Emmett–Teller (BET) analysis, X-ray diffraction (XRD), and field emission scanning electron microscopy (FESEM). The material demonstrated a high surface area (705.4 m2/g), an appropriate pore size (∼8.38 nm), and excellent pore volume properties, making it suitable for micro-solid phase extraction (μ-SPE). Under optimized conditions—10 mg of adsorbent, a 5-min extraction time, 50 μL of hexane as the desorption solvent, a 3-min desorption time, a pH of 6.0, and 0.1 % NaCl—the method exhibited broad linearity (0.02–600 μg/L), low limits of detection (LOD), and quantification (LOQ), with intra- and inter-day relative standard deviations (RSDs) below 6.1 %. Analysis of real water samples from various sources, including tap water, agricultural water, hookah water, and refinery well water, revealed significant contamination in hookah and refinery water samples, particularly with acenaphthylene and pyrene. The proposed method was validated against existing techniques, demonstrating comparable or superior performance in terms of linearity, LOQ, recovery, and precision. A greenness assessment using the AGREE metric yielded a score of 0.75, indicating its sustainability despite minor limitations associated with hexane use and gas chromatography (GC). This hybrid approach, combining the advantages of 2D-MSNs and DES, provides a powerful platform for efficient PAH extraction, aligning with green chemistry