BACKGROUNDCitrus peels, which are often discarded as waste in the food‐processing industry, are rich sources of polyphenols. The aim of the current study was to investigate the influence of an industrial freezing process along with blanching and cutting pretreatments on the in vitro gastrointestinal digestion stability of orange (Citrus sinensis L.) and lemon (Citrus limon L.) peel polyphenols. The major polyphenols were identified and quantified with ultra‐performance liquid chromatography‐electrospray tandem mass spectrometry (UPLC‐ESI‐MS/MS) and high performance liquid chromatography‐photodiode array detector (HPLC‐PDA), respectively.RESULTSThe results revealed that hesperidin and chlorogenic acid were the predominant flavonoid and phenolic acids in orange peels whereas, for lemon peels, eriocitrin and caffeic acid were the dominant flavonoid and phenolic acids, respectively. Blanching pretreatment enhanced the levels of major flavonoids in orange and lemon peels (by 39–82% and 54–146%, respectively) (P < 0.05) after in vitro gastrointestinal digestion. On the other hand, the application of cutting treatment after blanching significantly reduced the levels of flavonoids (23–62%) (P < 0.05); however, there was no statistically significant difference between the phenolic acid levels of cut and uncut citrus peels. Overall, the bioaccessibility of individual flavonoids and phenolic acids from frozen orange peels was generally slightly lower than that of untreated peels (9–34% and 9–49%, respectively). Nevertheless, frozen lemon peels contained higher bioaccessible flavonoids and phenolic acids in comparison with untreated peels (40–172% and 32–98%, respectively).CONCLUSIONThese results suggest that industrial freezing steps could largely preserve the bioaccessibility of polyphenols in orange and lemon peels. © 2023 The Authors. Journal of The Science of Food and Agriculture published by John Wiley & Sons Ltd on behalf of Society of Chemical Industry.