SALATRIM 23CA is a member of the SALATRIM family of triacylglycerols developed by RJR Nabisco Co. It is an interesterification product of triacetin, tripropionin, and hydrogenated canola oil. To characterize this sample, a combination of reversed-phase high-performance liquid chromatography and high-temperature capillary gas chromatography (HTCGC) in sequence was used to separate the SALATRIM 23CA into individual components. An on-line coupling of HTCGC with positive chemical ionization mass spectrometry revealed the structure of the individual components. To obtain detailed quantitative information, a combination of a 5-m OV-1 capillary column and a 25-m methyl 65% phenyl silicone Al-clad column was used to determine the quantities of acylglycerols