AbstractIntroductionWaste by‐products of the juice industry appear valuable for the circular economy concept, considering that the peel accounts for almost half of the total fruit weight. Therefore, the recovery of these highly valuable components from relevant biowaste has become a very interesting research topic.ObjectiveThe current study aims to develop an extraction process integrated with hydrophobic deep eutectic solvent (DES) based on statistical experimental design approach.Material and methodsHomogenizer‐assissted extraction (HAE) was used to recover the citrus extract rich in limonene (the main component of the volatile mixture) from lemon peels. Menthol‐based deep eutectic mixtures were accompanied by carboxylic acids (formic, acetic, and propionic acids). Optimization continued on the combination that gave the highest efficiency (in terms of limonene content) among the solvents prepared at different molar ratios (1/1, 1/2, and 2/1). Process parameters were analyzed to optimize the process through central composite design with response surface method (RSM). D‐Limonene yield was quantified with gas chromatography–mass spectrometry (GC‐MS) with solid‐phase microextraction (SPME) technique. The quality of the lemon peel extracts was also evaluated with respect to in vitro bioactivity assays (phenolic content and 2,2‐diphenyl‐1‐picrylhydrazyl [DPPH] free radical scavenging activity).ResultsThe maximum yield (3.80 mg‐limonene per g fresh sample) was achieved by 2 mg solid/30 mL DES, ~53 sec, and ~8500 rpm. Statistically most effective variable was identified as solid mass, followed by second powers of mixing speed and extraction time at p < 0.0001.