Three Kinds of hyponotics, barbital, phenobarbarbaital, and α-bromoisovarerylurea were administrated to rabbits orally. Urines collected from rabbits which had been given hyponotics were acidified with saturated tartaric acid and shaken with the equal volume of ethylene dichroride to urine for ten minutes. The extracting procedure was repeated three times. After centrifigation the organic layer was evaporated to dryness under vacum. The residue was dissolved in ethanol and spotted on the chromartoplate. After identification, unchanged hyponntics were determined by the algebraic method based on the relation between the weight of material and the size of a spot through the thin-layer chromatography. The unknown spots were scraped from the plates and spot-materials which were extracted with ether and acetone from silicagel, were examined by U. V. and I. R. absorption spectrophotpmeter.