BackgroundDioscorea opposita Thunb. cv. Tiegun maturity (DM) is an important factor influencing its quality. However, there are few studies on the impact of harvest time on its maturation. In this study, a nuclear magnetic resonance (NMR)‐based metabolomics approach was applied to investigate the dynamic metabolic changes of Dioscorea opposita Thunb. cv. Tiegun at six different harvest stages of stage 1 (S1), stage 2 (S2), stage 3 (S3), stage 4 (S4), stage 5 (S5) and stage 6 (S6).ResultsPrincipal component analysis (PCA) showed distinct segregation of samples obtained from S1, S2, and S3 compared to those derived from S4, S5, and S6. Interestingly, these samples from the two periods were obtained before and after frost, indicating that frost descent might be important for DM. Eight differential metabolites responsible for good separation of different groups were identified by the PCA loading plot and partial least squares‐discriminant analysis (PLS‐DA). In addition, quantitative analysis of these metabolites using liquid chromatography–tandem mass spectrometry (LC–MS/MS) determined the effects of harvest time on these metabolite contents, two of which, sucrose and allantoin, were considered as potential biomarkers to determine DM.ConclusionThe work demonstrated that NMR‐based metabolomics approach could serve as powerful tool to identify differential metabolites during harvesting processes, which also offered a fresh insight for understanding the DM and the potential mechanism of quality formation.This article is protected by copyright. All rights reserved.