Dynamics of Non‐Volatile and Volatile Organic Components During Enzymatic Hydrolysis of Sulfited Sugarcane Syrup: Profiling Using <scp> ¹ H NMR </scp> , <scp>GC</scp> – <scp>MS</scp> , and <scp>GC</scp> – <scp>IMS</scp>

ABSTRACT To explore the changes in flavor compounds during the hydrolysis of sulfited sugarcane syrup (SS) by sucrase. This study characterized non‐volatile organic compounds (NVOCs) via nuclear magnetic resonance (NMR) spectroscopy. Volatile organic compounds (VOCs) were characterized using gas chromatography–mass spectrometry (GC–MS) and gas chromatography–ion mobility spectrometry (GC–IMS). About 14 NVOCs were identified, with 7 NVOCs, including sucrose, fructose, α‐glucose, and β‐glucose, showing significant dynamic changes. About 80 VOCs were identified by GC–MS. Pyrazines were the predominant compound in the SS, whereas pyrazines and acids became the major components in the hydrolyzed SS. Enzymatic hydrolysis significantly increased the overall VOCs content, particularly acids and aldehydes, while reducing unpleasant S‐containing compounds. Orthogonal partial least squares‐discriminant analysis (OPLS‐DA) revealed that 30 differential VOCs (Variable Importance in Projection, VIP &gt; 1) served as markers for distinguishing among the five syrup samples. Furthermore, three key differential aroma compounds (2,5‐dimethylpyrazine, dimethyl sulfide, and β‐damascenone) were identified by VIP and Odor Activity Value (OAV). Additionally, we detected 56 VOCs by GC–IMS. The fingerprint profiles and OPLS‐DA confirmed significant differences in VOCs during enzymatic hydrolysis. Overall, these findings offer new insights into the flavor chemistry of SS during enzymatic hydrolysis and a theoretical basis for optimizing flavored syrup processing.