Tetrodotoxin (TTX) has been usually analyzed in marine and other sources by HPLC separation, followed by alkaline treatment and fluorescence assay. However, the applications of such methods were limited because of their tedious extraction and derivation procedures. A simpler, rapid LC-MS method, using selected ion-monitoring, has now been developed, and used to identify and quantitate TTX in a marine gastropod of the genus Nassarius, collected from Fijian province of China. The toxin was confirmed comparable to authentic TTX by MS and MSn. In addition, a moderate amount of TTX was detected in the Nassarius by this novel approach, suggesting that Nassarius would be a potential food poison source.