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In this study, for the first time, a simple, inexpensive and sensitive method named emulsification liquid–liquid microextraction based on deep eutectic solvent (ELLME-DES) was used for the extraction of benzene, toluene, ethylbenzene (BTE) and seven polycyclic aromatic hydrocarbons (PAHs) from water samples. In a typical experiment, 100 μL of DES (as water-miscible extraction solvent) was added to 1.5 mL of sample solution containing target analytes. A homogeneous solution was formed immediately. Injection of 100 μL of THF (as emulsifier agent) into homogeneous solution provided a turbid state. After extraction, phase separation (aqueous phase/DES rich phase) was performed by centrifugation. DES rich phase was withdrawn by a micro-syringe and submitted to isocratic reverse-phase HPLC with UV detection. Under optimum conditions obtained by response surface methodology (RSM) and desirability …