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• DESs with low viscosity, density and melting point near room temperature were designed and used. • A centrifugation-free AA-LLME-SFDES method was developed. • Placket-burman design and central composite design were used for the method optimization. • This method was used for simultaneous analysis of bisphenols and PAHs in 15 tea infusions samples. • This method may be developed as a fully automated AA-LLME method. Deep eutectic solvents (DESs) are a new class of green "designer solvent"; its physicochemical properties can be easily tuned by adjusting DES′ constituents, chemical ratio and water content. In this study, three hydrophobic DESs with low viscosity, low density, and melting points close to room temperature were designed and synthesized. Based on these DESs, an air-assisted liquid–liquid microextraction technique was developed based on the solidification of floating DESs for the simultaneous determination of bisphenols and polycyclic aromatic hydrocarbons (PAHs) via HPLC. The microextraction parameters were optimized via the Plackett-Burman design and response surface methodologies. The method shows satisfactory linearity (R2 ≥ 0.9928), a low limit of detection (0.16–0.75 μg L−1) and satisfactory precision (≤2.3%), and was successfully applied for the simultaneous determination of bisphenols and PAHs from tea infusions with satisfactory recoveries (82.0–116.6%). This method is simple, rapid, economical, environmentally compatible, dispersive solvent-frees and centrifugation-free, and has promising applications in food safety. [ABSTRACT FROM AUTHOR]