This work describes a simple and environmental-friendly method for the simultaneous determination of five benzotriazole derivatives (BTRs) and four benzothiazole derivatives (BTs) that are frequently found in surface water. The target analytes were efficiently extracted from water samples using a “green” deep eutectic solvent (DES) as the extraction solvent based- ultrasound-assisted emulsification microextraction (DES-USAEME), and their determination were performed by ultrahigh-performance liquid chromatography and electrospray ionization (+)-quadrupole time-of-flight mass spectrometry (UHPLC-ESI(+)-QToF-MS). The DES was composed of a mixture of choline chloride and phenol (molar ratio 1:2). The DES-USAEME factors were optimized by a Box-Behnken Design coupled response surface methodology. The developed method was validated, providing limits of quantitation (LOQs; 02 μg L−1), high precisions (1–8%), and satisfactory mean spiked recoveries (72–104 %). Relatively high total concentrations of the target analytes were found in samples collected from a reservoir (47.2–101.3 μg L−1), which may have been released from tire-wear particles and scrap tires from buses and old tires that were strung alongside the shuttle boats to prevent the boats from coming into contact with each other or from impacting against the dock during docking. This is the first study on the occurrence of BTRs and BTs in reservoir samples.