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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]

• Novel AA-LLME based on solidification of floating DES method was developed. • DESs with low viscosity, density and melting point near room temperature were used. • Central composite design was used for the method optimization. • This method is simple, low cost, centrifugal-free, and environment friendly. For this work, a novel air-assisted liquid-liquid microextraction based on solidification of floating deep eutectic solvent (AA-LLME-SFDES), coupled with a high performance liquid chromatography (HPLC) method was developed for the detection of benzophenone and salicylate ultraviolet filters in water samples. Three types of fatty acid-based hydrophobic deep eutectic solvents (DESs) with low viscosity, low-density, and melting point close to room temperature were prepared and employed as extraction solvents. This air-assisted liquid-liquid microextraction was carried out in a glass centrifuge tube. Subsequently, the glass tube was introduced into ice-water bath and held for 3 min, during which the upper DES phase was solidified. The water phase was easily extracted using a syringe equipped with a long needle, and later, the glass tube was removed from ice-water bath. The solidified DES phase was immediately melted at room temperature and used for HPLC analysis. The response surface methodology was employed to optimize some influencing parameters such as the volume of the extraction solvent, the pH value of sample solution, the number of extraction cycles, and the addition of salt. A quadratic model, namely a central composite design, was used to replace the conventional single factor analysis. It was found that under optimal conditions, the limits of determination and quantification were 0.045–0.54 µg L−1 and 0.15–2.0 µg L−1, respectively. The relative standard deviations for inter-day (n = 5) and intra-day (n = 5) precision were ≤ 4.2%, whereas the enrichment factors for the ultraviolet filters were obtained from 41 to 50. Furthermore, this novel method was successfully employed for the detection of benzophenone and salicylate ultraviolet filters from real water samples. The recoveries ranged from 87.5% to 105.8%, whereas the RSDs were lower than 3.6%. [ABSTRACT FROM AUTHOR]