Jimo Huangjiu (Chinese yellow rice wine), with its unique burnt odor, serves as a representative of Huangjiu in northern China. To decode the key odorants in Jimo Huangjiu, the volatiles were captured by headspace solid-phase microextraction and solid-phase extraction combined with solvent-assisted flavor evaporation, and analyzed by gas chromatography–mass spectrometry/olfactometry. and comprehensive two-dimensional gas chromatography–time of flight mass spectrometry. A total of 72 odor-active regions were screened, of which 69 odorants were positively identified and quantitated. Thirty-three of them had odor activity value (OAV) ≥ 1. Aroma recombination experiment verified the quantitate results, and 10 odorants were confirmed as key odorants by odor omission text. To further investigate the perceptual interaction of important odorants, 45 binary odor mixtures consisting of 10 selected odorants with OAV ≥ 1 were prepared, resulting that synergies were more likely to occur in odor combinations with similar chemical structures and odor descriptions.
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