Abstract: The composition of the volatile substances in the base wine of Wuyi red qu yellow rice wine was clarified, and the established method for the detection of volatile substances in the base wine of Wuyi red qu yellow rice wine was investigated. The volatile components in 10-year-old red qu yellow rice wine were analyzed by gas chromatography. The volatile substances in 10-year-old red qu yellow rice wine were analyzed by gas chromatography. A total of 48 volatile components were detected, including 22 esters, 5 alcohols, 5 acids and 3 aldehydes. The main components were phenylethanol, benzaldehyde, diethyl succinate, 2-hydracrylic acid ethyl, furfuraldehyde, 3-methyl-1-butanol, 2-octanone and 2-methyl-1-propyl alcohol. The results of the methodological investigation showed that the relative standard deviations of the relative retention time and the relative peak area of chromatographic peaks of the top 10 volatile substances in base wine were less than 0.2% and 5%, respectively, which could meet the detection requirements of volatile substances in the base wine of Wuyi red qu yellow rice wine.