Abstract: In order to explore the changes of physicochemical indexes and volatile components of giant salamander meat during cold storage (4 ℃, 0~8 d), the sensory evaluation, total volatile basic nitrogen (TVB-N) value and total bacterial count of giant salamander meat during cold storage were regularly determined, and headspace solid phase microextraction combined with gas chromatography-mass spectrometry (HS-SPME-GC-MS) was used to analyze the changes of volatile components in giant salamander meat. The results showed that the sensory quality of giant salamander meat decreased gradually with the extension of refrigeration time, while TVB-N and total bacterial count increased. Among them, the sensory quality of giant salamander meat was not acceptable on the 5th day, the TVB-N value exceeded the upper acceptable limit (30 mg/100 g) on the 7th day, and the total bacterial count exceeded the upper acceptable limit (6 lg CFU/g) on the 6th day. A total of 58 volatile substances in 7 categories were detected in giant salamander meat at different refrigerating times. Among them, the contents of 14 alcohols and 12 esters were relatively higher. With the extension of refrigeration time, the alcohol content decreased, while the ester content increased, and other compounds fluctuated slightly during refrigeration storage. Cluster analysis showed that the giant salamander meat with different refrigeration time could be clustered into four categories, namely, 0~4 d, 5 d, 6~7 d, and 8 d. Correlation analysis showed that hexyl caproate, ethyl 2-methylbutyrate, 2-heptanone, 2, 3-butanedione and linalool could be used as potential markers of corruption and deterioration of giant salamander meat during cold storage. This study provides a reference for the freshness evaluation and quality control of giant salamander meat during cold storage.