A thermo-assisted deep eutectic solvent (DES) based on dispersive liquid-liquid microextraction followed by gas chromatography with flame ionization detection was developed for the analysis of five phthalate esters in different water samples. In the procedure involved, a DES composed of lidocaine, an amphiphilic amine, and oleic acid, was mixed with the sample assisted by ultrasound, and phase separation was achieved with increasing temperature. The heating of the extraction system induced the change of acid-base properties of the DES components. Thus, the formation of microdroplets of DES in the sample was provided, and two phases were separated. The structure of the upper hydrophobic layer was characterized by Fourier-transform infrared spectroscopy. Also, the amount of water in the DES phase was analyzed by mass spectrometer and Karl Fischer titration. Some critical variables on the extraction yield were assessed. The proposed method achieved 1.2-1.3 and 4.1-4.3 µg/L for limits of detection and limits of quantification, respectively. The intra-day and inter-day percentage relative standard deviations (n = 5) were determined to be in the range of 4.2-6.2% and 5.1-7.2%, respectively. Ultimately, this method analyzed the five phthalate esters in different water samples with high recoveries.
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