Maize starch aerogel (MSA), a biocompatible and biodegradable support, was loaded with α-tocopherol (vitamin E) and menadione (vitamin K3), two poorly water-soluble vitamins using supercritical carbon dioxide adsorption. Adsorption experiments were carried out at 15MPa and 40 and 60°C. Adsorption equilibrium data were measured and represented as isotherms. Kinetic data, related to adsorption rates, showed that the adsorption process, for both vitamins, was best described by a pseudo second-order model.Vitamin/MSA composites were characterized using FT-IR spectroscopy, X-ray diffractometry and specific surface area determination. In order to study the properties of the adsorbed MSA, as a vitamin delivery system, in vitro dissolution tests were performed. These analyses showed that vitamin loading was about 95–98% with respect to the expected concentration, for both the cases. The dissolution rate in phosphate buffered saline solution (PBS) was largely improved: it was 3.5 times faster than the one of unprocessed vitamin in the case of menadione and about 16 times faster in the case of α-tocopherol.