The method of a biocompatible bottom-up for the synthesis of hierarchical biohybrid materials, was described. The ice-segregation-induced self-assembly (ISISA) process for the preparation of hierarchical biohybrid materials. A polymer such as ply(vinyl alcohol) (PVA) and an enzyme such as pig liver esterase (PLE), was used for the investigation. The nature of a material with the hierarchically organized structure should be ceramic rather than polymeric. The hybrid nature of the hierarchical material comes from the PVA incorporation of an enzyme such PLE into a hierarchical hybrid material, with full preservation of the enzyme activity. The hybrid nature of the hierarchical material comes from the PVA incorporation and is crucial for the preservation of the enzyme structure and activity. The results show that this hierarchical biohybrid material will be a sophisticated structure with up to six levels of spatial organization, which is the ternary structure of the esterase.

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