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Biocompatible nanochannel and mesoporous structures of a three-dimensional (3D) periodicity, facilitating protein entrapment at native conformations, constitute organized protective media of interest for the fast developing fields of protein biochips and affinity biosensors. Three-dimensional periodic nanochannel structures possessing reactive chemical groups, surface-exposed to the aqueous phase, are formed here in self-assembled mixtures of a nonlamellar lipid glycerylmonooleate (MO) and a maleimide(triethylene glycol)ether lipid (MTEG) under physiological hydration conditions and are investigated by high-resolution time-resolved synchrotron X-ray diffraction in the interval from 3 to 96 °C. The mechanism of formation and the structural parameters of two nonlamellar cubic phases Q²²⁴ and Q²²⁹ (of space groups Pn3m and Im3m) are monitored. The structural phase behavior of the MO/MTEG-based …