In order to ensure the effect of fresh treatment on the characteristics of flavors of sturgeon meat during refrigerated storage, this experiment used solid phase microextraction-gas chromatography-mass spectrometry combined with electronic nose and electronic tongue technology to analyze chilled sturgeon meat with the fresh-keeping treatment of slightly acidic oxidation water and ε-polylysine during refrigerated storage. The result showed that the electronic nose can analyze the volatile components from the whole, and the data sets of the volatile odor of chilled sturgeon meat in the two groups had no overlapping areas, and the difference was obvious. SPME-GC-MS qualitatively identified 46 volatile substances, including aldehydes, ketones, hydrocarbons and alcohols. Among them, the main volatile substances of the fresh-keeping treatment group were caproaldehyde, enanthaldehyde, benzaldehyde, capryl aldehyde, nonanal, capric aldehyde, 2,5-octanedione, hypnone and 3,5-octanedipine-2-ketone. Thus, the preservation treatment can delay the production of astringency and the decline of flavor of chilled sturgeon meat. The bitterness, astringency and salty taste of chilled sturgeon meat during chilled storage were found to be lower than those of the control group. The two groups of samples showed significant differences in bitterness, astringency, salty taste and umami after 6 days of storage. The research showed the preservation treatment played a role in slowing down the decline of flavor of chilled sturgeon meat during refrigerated storage, and provided a theoretical basis for the application of chilled sturgeon meat preservation.