The pufferfish Pleuranacanthus sceleratus (El-Karad) represents serious public health problems, because of its responsibility for many incidents in Egypt, especially in the Suez Gulf. In the present study, samples of this fish were collected monthly and the toxins were extracted from gonads, liver, digestive tract, muscles, and skin, then purified and identified using TLC and electrophoresis. The alkaline hydrolyzates of these toxins were also detected using UV absorption and GC-mass spectra of their trimethylsilyl derivatives.