Abstract:To investigate the changes in volatile compounds during the preparation of Double-Layer Steamed Milk Custard (DLSMC), the volatile substances at four key stages—raw material stage (group A), boiling stage (group B), cooling stage (group C), and steaming stage (group D)—were analyzed using electronic nose and headspace-gas chromatography-ion mobility spectrometry (HS-GC-IMS). The results showed that methyl compounds, alcohols, ketones, and aldehydes, were significantly different volatile components across the stages (P<0.01). A total of 38 compounds were identified by HS-GC-IMS, including esters, alcohols, ketones, aldehydes, ethers, acids, and pyrazine derivatives. Principal component analysis (PCA) and partial least squares discriminant analysis (PLS-DA) indicated that the boiling and steaming stages were the main stages for changes in volatile compounds. In the boiling stage (B group), the unpleasant flavor of 1-pentanol in the raw buffalo milk was significantly reduced (P<0.05), while the levels of 2-butanone, 2-butanol, dimethyl sulfide, and other compounds were significantly increased (P<0.05). In the steaming stage (group D), the levels of 2-pentanone, 2-heptanone, acetone, and diallyl disulfide significantly increased (P<0.05). Ultimately, the DLSMC exhibited flavor characteristics such as grassy, oily, fruity, milky, sweet, buttery, fruity, and roasted nut aromas.