The effects of modified atmosphere packaging (MAP) in combination with superchilling (−1.3 °C) on the physicochemical properties, flavor retention, and organoleptic evaluation of turbot samples were investigated during 27 days storage. Results showed that high-CO2 packaging (70% or 60% CO2) combined with superchilling could reduce the productions of off-flavor compounds, including total volatile basic nitrogen (TVB-N) and ATP-related compounds. Twenty-four volatile organic compounds were determined by gas chromatography–mass spectrometry (GC/MS) during storage, including eight alcohols, 11 aldehydes, and five ketones. The relative content of off-odor volatiles, such as 1-octen-3-ol, 1-penten-3-ol, (E)-2-octenal, octanal, and 2,3-octanedione, was also reduced by high-CO2 packaging during superchilling storage. Further, 60% CO2/10% O2/30% N2 with superchilling (−1.3 °C) could retard the water migration on the basis of the water holding capacity, low field NMR, and MRI results, and maintain the quality of turbot according to organoleptic evaluation results during storage