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<i>Huangjiu</i> is one of the oldest alcoholic beverages in the world. It is usually made by fermenting grains, and Qu is used as a saccharifying and fermenting agent. In this study, we identified differential carbonyl compounds in <i>Huangjiu</i> with varying sugar contents from different regions. First, we developed and validated a detection method for volatile carbonyl compounds in <i>Huangjiu</i>, and for optimal extraction, 5 mL of <i>Huangjiu</i> and 1.3 g/L of O-(2,3,4,5,6-pentafluorobenzyl)hydroxylamine hydrochloride (PFBHA) were incubated at 45 °C for 5 min before extracting the volatile carbonyl compounds at 45 °C for 35 min. Second, the targeted quantitative analysis of 50 carbonyl compounds in <i>Huangjiu</i> showed high levels of Strecker aldehydes and furans. Finally, orthogonal projections to latent structures discriminant analysis (OPLS-DA) was used to differentiate between <i>Huangjiu</i> with different sugar contents, raw materials, and region of origin. A total of 19 differential carbonyl compounds (VIP > 1, <i>p</i> < 0.05) were found in <i>Huangjiu</i> with different sugar contents (semidry and semisweet <i>Huangjiu</i>), and 20 differential carbonyl compounds (VIP > 1, <i>p</i> < 0.05) were found in different raw materials for <i>Huangjiu</i> production (rice and nonrice <i>Huangjiu</i>). A total of twenty-two and eight differential carbonyl compounds, with VIP > 1 and <i>p</i> < 0.05, were identified in semidry and semisweet <i>Huangjiu</i> from different regions (Zhejiang, Jiangsu, Shanghai, and Fujian), respectively.