Abstract This study was aimed to analyze the main volatile compounds and aroma profiles of the liquor that was made from Guanxi honey pomelo (Citrus grandix) juice. Brewing liquor is more bitter than distillation liquor. So we choose distillation liquor to study. To fulfill this aim, headspace solid phase micro-extraction (HP-SPME) coupled with gas chromatography-mass spectrometry (GC-MS) and gas chromatography-flame ionization detector-olfactory (GC-FID-O) were used to analyze the volatiles. As the result, 40 volatile components, including 8 alcohols, 14 esters, 10 terpenes and 8 others were identified from the liquor. The quantitative analysis showed that the main volatile components were ethyl caprate (744.73 μg/L), ethyl caproate (524.74 μg/L) and ethyl laurate (193.42 μg/L), respectively. Sensory evaluation showed fruit and citrus notes were the main odours of the liquor. The GC-Olfactory analysis indicated that d-limonene, ethyl valerate and ethyl caproate were the main aroma-active components. These results provide a experimental reference for future in-depth researches on the aroma of wine and liquor products from pomelo and other citrus fruits.