The aim of this study was to explore the application of HS—SPME—GC/MS—AMDIS in the analysis of carp fish volatile substances. The volatile compounds in crucian carp fish were extracted by headspace solid phase micro extraction, and analyzed by using the gas phase chromatography-mass spectrometry combined with automatic mass spectral deconvolution and retention index, simultaneously compared with literature, to accurately determine the volatile compounds. The results showed that using this method 102 kinds of volatile compound was identified in the carp fish, including 18 kinds of benzene, 17 kinds of alcohols, 13 kinds of alkanes, 13 kinds of ketones, 12 kinds of naphthanes, 9 kinds of aldehyde, 4 kinds of indene, 3 kinds of esters, 3 kinds of acids, 2 kinds of phenols, 2 kinds of amine, 2 kinds of ether, 2 kinds of sulfur and a nitrogen. Comparing the present results with those obtained by using traditional methods, we can find that more volatile compounds in fish carp could be detected using the automatic mass spectral deconvolution and identification system, with higher credibility. Therefore, this may provide theoretical guidance for improving the quality of crucian carp and the satisfaction of consumer with better productions.