Reverse-phase HPLC with refractive index and light scattering detectors in isocratic and gradient elution modes, respectively, was applied for the separation of the major triacylglycerols (TAG) in coffee lipids. Twelve TAG species could be identified and determined using a linear gradient of acetonitrile in dichloromethane: dichloroethane. The quantitative evaluation was based on the relative area percentages derived directly from a data-station. The procedure was applied to determine the TAG composition of three types of coffee beans harvested in two coffee producing areas in Brazil and dried by two commonly used procedures. No significant differences in the TAG compositions due to the type, origin and drying procedure were found.