A microextraction pretreatment for powdered milk analysis, relying on the formation of a natural deep eutectic solvent is proposed. It relies on the in situ hydrolysis of milk fats (triglycerides) which yields fatty acids as precursors in the formation of the natural deep eutectic solvent. As a proof-of-concept, the innovation was applied to the determination of thirteen polycyclic aromatic hydrocarbons in powdered milk samples by HPLC with fluorometric detection. The alkaline hydrolysis of milk triglycerides minimized sample matrices interference through removal of proteins and fats, and led to formation of natural deep eutectic solvent precursors (fatty acids) directly from the sample components. Addition of only one precursor (terpenoid) was then required. Menthol and thymol (natural terpenoids) were investigated as deep eutectic solvent precursors for micro extraction of polycyclic aromatic hydrocarbons. Under the selected experimental conditions, limits of detection were estimated within the 0.002-0.09 mu g kg-1 range. The innovation provided satisfactory (70-91%) extraction of hydrophobic analytes from complex powdered milk matrices containing hydrophobic components (triglycerides) without the need for hazardous organic solvents. The RSD values were