Simultaneous qualitative analysis of fourteen sulpha drugs and their individual quantitative determinations have been performed by gas-liquid chromatography on solutions of dimethylformamide dialkylacetal derivatives of the drugs in acetone. Linear calibration curves were obtained for each sulpha drug under appropriate conditions. The structures of the above derivatives are assumed to be N1-methyl, N4-acetal sulphonamides, which can be detected with an electron capture detector with highly sensitive response. Columns used were 10% OV-101, 5% XE-60 and 5% OV-225.