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A convenient and rapid procedure involving methylation, silylation, and temperature-programmed gas-liquid chromatography (GLC) is described for analyzing unfractionated products from the hydrolysis of triglycerides with pancreatic lipase. The conditions employed for GLC were selected to provide maximum and rapid separation of silylated monoglycerides in which the acyl moieties differ in chain length or degree of substitution with oxygen-containing functional groups. Derivatives differing only in the number of double bonds present were not separated. In the GLC curves obtained, peaks representing methyl esters are generally readily distinguishable from those of other components. Therefore, the extent of lipolysis and the composition (with respect to chain length and substitution of acyl groups) of monoglycerides formed are determined simultaneously. The accuracy of the new method was demonstrated with standard mixtures and by comparison of results for several lipolysis products with data obtained by conventional procedures.