Colloidal suspensions of triglycerides are under investigation as potential drug carrier systems. The properties of the matrix lipids are altered in the nanoparticles compared to those of the bulk material. For instance, the metastable alpha-modification of the triglycerides usually transforms into the stable beta-polymorph quite rapidly in the colloidal particles. Recently, it was observed that the alpha-modification can be preserved for a considerable period of time in tristearin nanoparticles when the particles are stabilized with a blend of saturated long-chain phospholipids and the bile salt sodium glycocholate [Bunjes, H.; Koch, M. H. J. J. Controlled Release 2005, 107, 229-243]. As triglyceride nanoparticles in the alpha-modification may offer some advantages over those in the beta-form with regard to drug delivery applications, the structure of the corresponding dispersions was investigated in more detail with differential scanning calorimetry, X-ray diffraction, and electron microscopy. The electron microscopic investigations confirmed a platelet-like, layered structure for particles in the beta-modification and revealed a spheroidal shape with concentric layers for larger particles in the alpha-form. For the first time, not only was information on the internal structure of solid triglyceride nanoparticles obtained from freeze-fracture electron micrographs but also details were observed by cryoelectron microscopy.