U.S. pecan nuts are rich in oil and phenolic compounds with important biological functions. At present, the reports about simultaneous extraction of oil and phenolic compounds are limited, and the traditional procedure is complicated and the yield is low. In this study, a new emulsion formed by hydrophobic deep eutectic solvent (DES) and water was used as extractant for synchronous extraction of oil and phenolic components from U.S. pecans, and subsequently the two were recovered from the upper and lower phases based on the incompatibility of DES and water, respectively. The oil and phenolic compounds obtained by the optimization of extraction conditions were 615.29 mg/g and 82.11 mg/g, respectively, which were higher than those obtained by conventional methods. At the same time, the extraction mechanism is discussed through the extraction kinetics and thermodynamics. The extraction process conformed to the Fick’s second law, and it was an endothermic process. After directional recovery by macroporous resin and back-extraction, the effectiveness of the method was proved by the analysis of fatty acid composition of oil, spectral characterization of phenolic compounds and antioxidant activities.
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