This study aims to validate the preparation approach of novel biodegradable polymer-bioactive ceramic composites of poly (lactic acid) (PLA), chitosan (CS), and tricalcium phosphate (TCP) and evaluate their suitability for Guided Bone Regeneration (GBR). GBR is a dental surgical procedure that uses barrier membranes to direct the growth of new bone tissues. Resorbable membranes eliminate the need for a second surgery that patients with non-resorbable membranes need. Cryomilling, a solid-state, low-temperature blending process, facilitates bulk fabrication by eliminating difficulties such as high viscosity, insolubility and long processing times. It is a cost-effective technique to generate particles with high surface area to volume ratio, which provide a larger area for biological activity. Electrospinning was used to fabricate fibrous barrier membranes using the biocomposites prepared by cryomilling. X-Ray Diffraction (XRD) and Differential Scanning Calorimetry (DSC) were utilized to characterize the molecular structures, identify the glass transition and melting temperatures and to confirm the occurrence of homogeneous polymer-ceramic biocomposites. Scanning Electron Microscopy (SEM) was used to observe the morphology of the powder composites and the electrospun membranes. RAW 264.7 murine macrophages were used to evaluate the cytocompatibility of the biocomposites and quantitatively analyzed with CellTiter-Blueà ¯à ¿à ½ (CTBà ¯à ¿à ½) cell viability assay. Also, MG63 cells were seeded on electrospun membranes to quantify the capability of the biocomposites to encourage cell proliferation. Coherent anti-Stokes Raman Spectroscopy (CARS) and brightfield (BF) microscopy were used to analyze cell proliferation on the seeded membranes qualitatively. A 21- day in vitro degradation studies were performed and analyzed using Raman spectroscopy. CTBà ¯à ¿à ½ cell viability assay carried out on the electrospun membranes revealed that the cells are viable and

metabolically active both at 3 and at 7 days from cell seeding indicating the suitability of the material for GBR.