In this work, microtubes with walls, containing Fe3O4 nanoparticles, obtained by “rolling up” of the interfacial films, were synthesized by the gas-solution interface technique (GSIT), using a mixture of aqueous solutions of FeCl2 and FeCl3 and gaseous ammonia. The synthesized microtubes were characterized by Scanning Electronic Microscopy (SEM), Energy-Dispersive X-ray spectroscopy (EDX), X-Ray Diffraction analysis (XRD) and magnetization measurements. It was established that under optimal synthetic conditions the microtube diameter ranged from 5 to 10 µm, the length was up to 120 µm and the thickness of walls was about 0.6 µm, the walls themselves being formed by nanoparticles with a size of about 10 nm. The reversible hysteresis behavior, the low coercive force, the low remanence magnetization and the approaching of Mr/Ms to zero, confirmed the superparamagnetic nature of the synthesized microtubes. A hypothesis on the formation of microtubes by the gas-solution interface technique was proposed.