The autors have described the separation and identification of seven kinds of sulfonamides by means of the thin-layer chromatograghy and an example for the detection of sulfamonomethoxine sodium in the cadaveric blood. In the separation of these sulfonamides, the developers of chloroform-methanol system which consist of two or more kinds of polar and non-polar solvents, gave the satisfactory result. All these sulfonamides could be detected even in a very small quantities of 0.1 μg by using p-dimethylaminobenzaldehyde or diazo reagent and the color was very clear. As a result, both reagents would be expected to be available for the detecting reagent in the usual analysis of sulfonamides. From the blood (8 ml) of a man aged 52 who ”Daimeton” injection was intravenously received and suddenly died, sulfamonomethoxine sodium was separated and identified through the analysis coupled with the thin-layer chromatography and ultraviolet absorption spectrophotometry. The quantities of sulfamonomethoxine sodium determined about the remainder of blood extract after the qualititive analysis was approximately 3.0 mg.