​A new green method of dispersive liquid-liquid micro-extraction (DLLME) assisted with a deep eutectic solvent (DES) was developed to determine emergent pharmaceuticals contaminants used for pain relieve (aspirin, ibuprofen and salicylic acid) over aqueous matrix. A DES was prepared over urea and Zinc-chloride on a proportion of 3,5:1 M, and was used as an extracting and dispersant phase. DES is characterized from its FT-IR spectroscopy in KBr pill, having a 2223,0 cm-1 band, its most highlighted featured signal; and a RMN spectroscopy, where signal move to lower field confirming DES formation. Analysis was made through high-resolution liquid chromatography with a diode arrangement detector (μHPLC-DAD). Method was lineal in the ranges of 0,50 ± 0,01 to 5,00 ± 0,01 mg/L of concentration for aspirin and salicylic acid, and also linear for ibuprofen: 1,00 ± 0,01 to 5,00 ± 0,01 mg/L; under correlation coefficients of > 0,9868. Effects of the elements possibly influencing the extraction performance, were studied by the DoE of Plackett-Burman and factorial 2k (k=2). Recovery percentages were between 17 to 35%, statistical analysis was done on Minitab 18. Present paper represents a breakthrough contribution applying this innovative deep eutectic solvents on DLLME.