This work presents a greener approach for ultrasound-assisted (UA) dispersive liquid-liquid microextraction (DLLME) of carbonyl compounds from coffee samples, before GC-MS determination. This work aims to substitute the solvents used in the traditional DLLME procedures with greener alternatives and to decrease the volume of solvents used. Low-density solvents, 1-octanol and isooctane, were evaluated as the extraction solvent. Optimization of critical experimental parameters was conducted in two stages: an asymmetrical screening design 2