Southern Shaanxi is one of China’s high-quality congou black tea production areas. However, the differences in geography, cultivation, and management techniques and production processes lead to uneven qualities of southern Shaanxi congou black tea in different production areas. This study used sensory analysis combined with gas chromatography–ion mobility spectrometry (GC-IMS) to determine southern Shaanxi congou black teas’ geographical origin and volatile fingerprints to prevent economic losses caused by fraudulent labeling. A total of 61 volatile compounds were identified and quantified by GC-IMS. Three main aroma types were found by sensory analysis coupled with significant difference analysis, and a clear correlation between volatile compounds, aroma type, and geographical origin was found by sensory and gallery plot analysis. The black tea with a green/grassy-roast aroma type was mainly distributed in production areas with an altitude of 400–800 m and 1-pentanol, cyclohexanone, 1-penten-3-one, 2-heptanone, dihydroactinidiolide and butyrolactone were the key aroma markers. The black teas produced in production areas with an altitude of 800–1000 m mainly presented strong honey and caramel-like aromas, and sotolone, furaneol, and phenylacetaldehyde played an important role. These results will be helpful for discriminating black tea from different tea production areas in southern Shaanxi.
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