Tetrodotoxin (TTX) and a variety of paralytic shellfish poisons (PSPs) were extracted from toxic specimens of puffer and scallop, and quantitated by high-performance liquid chromatography with a fluorometric detection using o-phthalaldehyde. Fluorescence spectra for the TTX- and PSP-fluorophors in 0.05 M borate buffer (pH 10) showed maxima at 453 nm with 332-nm excitation. The fluorescence intensity per nM of TTX was found to be 3 and those of PSP to be 4-12. This fluorometric technique may be useful for the simultaneous quantitation of TTX and PSP in small volumes of toxin extracts.