| Summary: | Gilthead sea bream (<i>Sparus aurata</i>) is one of the most important farmed Mediterranean fish species, and there is considerable interest for the development of suitable methods to assess its freshness. In the present work, gas chromatography–mass spectrometry-based metabolomics was employed to monitor the hydrophilic metabolites of sea bream during storage on ice for 19 days. Additionally, the quality changes were evaluated using two conventional methods: sensory evaluation according to European Union’s grading scheme and <i>K</i>-value, the most widely used chemical index of fish spoilage. With the application of chemometrics, the fish samples were successfully classified in the freshness categories, and a partial least squares regression model was built to predict <i>K</i>-value. A list of differential metabolites were found, which were distinguished according to their evolution profile as potential biomarkers of freshness and spoilage. Therefore, the results support the suitability of the proposed methodology to gain information on seafood quality.
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