Abstract: In order to study the dynamic changes of tropical TVB-N components in different aquatic product, the head/space solid phase micro extraction-gas chromatography/mass spectrometer (HS/SPME-GC/MS) was developed for the total volatile basic nitrogen (TVB-N) components firstly, then dynamic changes of the four TVB-N components in Scophthalmus maximus and Penaeus vannamei during 4℃ storage were determined. Extracting with 85 μm Carboxen/Polydimethylsiloxane (CAR/PDMS) fiber at 40℃ for 5 mins, ammonia (NH₃), methylamine (MA), dimethylamine (DMA) and trimethylamine (TMA) were demonstrated satisfactory analytical efficiency:a good linear relationship was observed (R² > 0.999) within a certain range, the relative standard deviation (RSD) was 2.21%~5.64%, the average recovery ratio of Scophthalmus maximus was 86.20%~98.60% and of Penaeus vannamei was 78.27%~108.78%, the method detection limit was 0.1~1 mg/100 mg and the instrument detection limit was 0.003~0.029 mg/100 mg. In compassion to other methods, it was demonstrated more simple, rapid and accurate.MA and DMA were not detected in Scophthalmus maximus and Penaeus vannamei. In Scophthalmus maximus, the content of TMA changed significantly (p < 0.05) on the seventh day, and reached 23.94 mg/100 g on the thirteenth day. In Penaeus vannamei, the content of NH₃ changed significantly (p < 0.05), and reached 39.59 mg/100 g on the sixth day. These results could help further understand the dynamic changes of TVB-N components and their relation with the quality of different aquatic products during refrigerated storage.