Abstract: In this paper, volatile organic compounds (VOCs) of Penaeus merguiensis (De Man) Banana prawn during storage were sampled by the headspace solid phase micro-extraction (HSSPME) coupled with GC-MS detection. Prawn volatile profile characteristics at different storage phases were specified by chemometric methods and the relationship between volatile profile characteristics and the freshness of prawns were tentatively studied. 22 and 16 VOCs components were detected at fresh and deteriorated storage phases, respectively. In the PCA model prawn volatile profile characteristics showed different clustering rules at different storage phases and showed the transitional changing trends from fresh to deteriorated storage phases. Prawn volatile profile characteristics provide more precise alarming information for its spoilage during storage. The statistical and contrastive analysis using a common model showed that the top five volatiles contribute most to the difference of volatile profile characteristics during the prawn storage and can be considered as the potential alarming maker for the discrimination of prawn freshness.