Short-and long-chain triacylglycerols (SLCT) are a family of lipids prepared by chemical or enzymatic interesterification of triacetin, tripropionin and/or tributyrin, and long-chain (C16!18) hydrogenated vegetable oils. In this study, a normal-phase cyanopropyl high-performance liquid chromatographic (HPLC) method was developed for the separation and quantification of SLCT. The method is capable of separating SLCT mixtures, free fatty acids and the neutral lipid classes of saturated long-chain triacylglycerols, diacylglycerols and monoacylglycerols. To characterize the specific SLCT classes, a normal-phase HPLC procedure using a non-modified silica column was developed to separate the SLCT into individual isomers based on total carbon number and position of fatty acids on the glycerol backbone. Online coupling with a mass detector (LC/MS) allowed the identification of the individual triacylglycerol structures.Original 0009-5893/99/04