A new and fast microextraction technique termed vortex-assisted supramolecular solvent microextraction (VASUSME) has been developed. The method was based on the microextraction of endocrine disrupting compounds (EDCs), including bisphenol-A (BPA), 2,4-dichlorophenol (2,4-DCP), bisphenol-AF (BPAF) and tetrabromobisphenol-A (TBBPA) in 10 mL sample with 500 μL of a supramolecular solvent (SUPRASs), and then detection by high-performance liquid chromatography (HPLC). In the VASUSME procedure, dispersion of microvolumes of a low density extraction solvent into the aqueous sample is achieved by vortex mixing, a mild emulsification procedure. Under the optimum conditions, the repeatability of the proposed method was found to be good. The relative standard deviations (RSD, n = 5) were 3.98–5.64%. The limits of detection (LOD) were in the range of 0.14–0.32 ng mL−1 and the limits of quantification (LOQ) were in the range of 0.41–1.02 ng mL−1. All correlation coefficients of the calibration curves were higher than 0.998. Recoveries of the EDCs spiked into samples of liquid foods and their packaging materials were in the range of 91% to 105.1%. The VASSUSME method was successfully applied to the analysis of BPA, 2,4-DCP, BPAF and TBBPA in samples of liquid foods and their packaging materials. Moreover, the method is simple, sensitive and environmentally-friendly and consumes much less solvent than traditional methods.
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