The allyl isothiocyanate, capsaicin and dihydrocapsaicin as main components in self defense sprays were determined by gas chromatography-mass spectrometer (GC-MS). Although self defense spray was used to protect by myself, a social problem could be caused by the hazard of spray chemical due to use pungent liquid. To identify this, the pH of pungent liquid solutions, solubility to detergents, the existence of other materials and the types and amounts of pungent material in spray chemicals were investigated in this work. Finally, the amounts of allyl isothiocyanate, capsaicin and dihydrocapsaicin as pungent materials in them were determined by GC-MS. The pH of chemicals were about 5.7 as weak acid, the detergents can emulsify them with water well. And they did not contain fluorescent materials and hazard organic solvents. The pungent components in three real samples were only allyl isothiocyanate [47,600 mg/kg (47.6%)] in one sample, and mixtures with capsaicin [228 mg/kg~368 mg/kg (1.14%~1.84%)] and dihydrocapsaicin [224 mg/kg~414 mg/kg (1.12%~2.07%)] in the others, respectively.