The changes of volatile compounds in soy sauce during long‐term fermentation (12 months) were investigated using solid‐phase microextraction (SPME) and stir bar sorptive extraction (SBSE). A total of 144 and 129 compounds were identified in soy sauce with long‐term fermentation by SPME and SBSE, respectively. The contents of most compounds, such as acids, aldehydes, benzene and benzene derivatives, esters, lactones, pyrazines, pyrones, and pyrroles, showed a tendency to increase, whereas those of alcohols and ketones decreased according to long‐term fermentation. In addition, principal component analysis and partial least squares discriminant analysis were applied to discriminate soy sauce samples according to fermentation periods and determine key volatile compounds related to long‐term fermentation. The initial fermentation stages were mainly associated with some alcohols, ketones, and lactones, whereas the later stages were strongly associated with most esters, some phenols, benzene and benzene derivatives, and pyrroles. Moreover, the key volatile compounds associated with long‐term fermentation in soy sauce samples were ethyl 3‐methylbutanoate (ethyl isovalerate), ethyl pentanoate (ethyl valerate), 1‐octen‐3‐yl acetate, 3‐(methylthio)‐1‐propanol (methionol), ethyl benzoate, ethyl 2‐phenylacetate, 1‐(1H‐pyrrol‐2‐yl)ethanone (2‐acetylpyrrole), and 5‐pentyl‐2‐oxolanone (γ‐nonalactone). Practical Application This study investigated changes of volatile compounds in soy sauce during long‐term fermentation (12 months) using solid‐phase microextraction and stir bar sorptive extraction. In addition, the key volatile compounds associated with long‐term fermentation in soy sauce samples were determined. These results may help to predict the effective contributors related to long‐term fermentation of soy sauce and improve the quality of soy sauce during long‐term fermentation.
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