Indole acids in urine and spinal fluid can be concentrated by continuous ether extraction at pH 4.2, converted to their tetramethylammonium salts, pyrolized into methyl esters at 340°C upon injection, and chromatographed on silicone liquid phase at 175°C. Urine can be analyzed for indoleacetic, indolepropionic, and 5-hydroxyindoleacetic acids. Spinal fluid contains less background material and gives better chromatograms than urine. 5-hydroxyindoleacetic, indoleacetic, indolepropionic, as well as vanilmandelic acids, can be analyzed in spinal fluid.