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Liquid-liquid extraction (LLE) is the most commonly utilized technique for the extraction of odor-active esters (OAEs) in strong-aroma types of Baijiu (SAB). However, since the contents of different OAEs in SAB vary widely, it is still a puzzle to ensure that all OAEs to be thoroughly extracted by LLE without the problem of saturated adsorption. Herein, a novel approach of magnetic solid phase extraction (MSPE), based on the magnetic graphene oxide nanocomposite modified with polyacrylamide (GO/PAM/Fe3O4), was employed for the efficient extraction of six OAEs from SAB. Compared with LLE, GO/PAM/Fe3O4 exhibited highly selective recognition properties and larger adsorption capacities for OAEs (ranging from 13.68 to 39.06 mg/g), resulting in better extraction performances for OAEs. Coupled with GC–MS, six OAEs in real SAB were successfully determined, with recoveries ranged from 70.1 ∼ 90.0% and LODs at 0.08 ∼ 1.35 µg/L. Overall, the MSPE-GC/MS is a promising alternative for accurate determination of OAEs in SAB.