Interlayer reconstruction-induced dimensional leap: 2D Vitabrid to 3D VitaMOF

Stabilizing chemically labile bioactive molecules remains a fundamental challenge in functional materials and therapeutic formulations. Here, we report a solvent-directed interlayer reconstruction strategy that enables controlled dimensional transformation of zinc-ascorbate nanohybrids via coordination reorganization. By tuning the ethanol-water ratio during co-precipitation, two distinct zinc-ascorbate architectures are obtained: a layered ascorbic acid-zinc basic salt (AA-ZBS), which is here referred to as two-dimensional Vitabrid (2D-Vitabrid) intercalate at low ethanol content, and a porous ascorbic acid-metal-organic framework (AA-MOF), which is here referred to as three-dimensional VitaMOF (3D VitaMOF) at intermediate ethanol levels. Powder X-ray diffraction (PXRD) and Fourier transform infrared (FT-IR) spectroscopy analyses reveal that this transformation is governed by solvent-mediated Zn-ascorbate coordination dynamics. An optimal ethanol window (∼60-70%) promotes hydrolysis-assisted recoordination and framework maturation, whereas complete dehydration (100% ethanol) disrupts structural ordering and yields poorly defined phases. The optimized 3D framework exhibits a significantly enhanced surface area (553.95 ± 34.68 m² g^-1) compared to its 2D counterpart, enabling improved ascorbate loading and stabilization. Both nanohybrids show high biocompatibility (∼80% viability in CCD-986sk fibroblasts) while exhibiting potent cytotoxicity against melanoma (SK-MEL-28, WM-266-4) and squamous carcinoma (A431) cells, with IC₅₀ values of 0.01-0.06 mM, outperforming free ascorbic acid. These findings establish solvent-programmed dimensional reconstruction as a generalizable strategy for stabilizing labile bioactives and engineering high-performance nanohybrid systems.