A simple method for the determination of plasma and tissue triglycerides is described. This procedure involves the extraction and saponification of triglycerides, the oxidation of the glycerol moiety to formaldehyde, and the conversion of formaldehyde to a yellow-colored compound, 3,5 diacetyl-1-4 dihydrolulidine, the intensity of which is determined spectrophotometrically. The recoveries of triglycerides added to plasma and tissues have been satisfactory. Plasma samples obtained from normal human subjects are found to have triglycerides in the range 83-200 mg./100 ml. From the standpoint of sensitivity, simplicity, and time required, this technic is believed to be an improvement over previously described procedures for triglyceride determination.