An approach to incorporate a bioactive hydrophobic substance, C22H32N4O7 tetrapeptide (TP), into the structure of the hexagonal mesophases C12EO10/H2O and C12EO10/La(III)/H2O was proposed. Concentration and temperature ranges of mesophases in the C12EO10/H2O/TP and C12EO10/La(III)/H2O/TP systems were established. The analysis of the X-ray diffraction data revealed a change in the structural characteristics of mesophases in the presence of tetrapeptide. Formation of a denser packing of molecules in the mesophases with TP was detected. Based on the FTIR spectroscopy data, intermolecular changes in the systems were examined. Pulsed-gradient spin-echo NMR self-diffusion experiments were performed to characterize the structure of lyomesophases depending on system composition and temperature. The degree of hydration of water molecules in lyomesophases was analyzed. The data confirmed successful incorporation of tetrapeptide into the structure of lyomesophase and, therefore, the possibility of using hexagonal mesophases for both incapsulation and delivery of biomolecules.