This work reports the isolation and characterization of chitin from green algae using XRD, 13C CP/MAS NMR, FTIR and Microscopy. The XRD diffraction pattern confirmed orthorhombic structure of the crystalline polysaccharide, whereas the FTIR spectra revealed strong absorption bands at 896.9 cm-1 and 852 cm-1 typical of C–H axial and C–H equatorial vibrations within the anomeric center of the glucopyranosicyclic moiety. Another strong absorption band was observed at 1039.9 cm-1 and was assigned to C–O–C, C–O stretching bands. The purity and structure of the deacetylated chitin was confirmed using 13C NMR, showing overlapping peaks around 65 ppm assigned to both the sugar carbon at C2, as well as a methylene carbon at C6. An intense peak at 74 ppm is assigned to C3 and C5 with corresponding resonances at 81 and 104 ppm assigned to C4 and C1 respectively. Zeolite/Chitosan nanocomposites were synthesized by ionic cross-linking of chitosan with sodium tripolyphosphate. Chitosan nanoparticles and LTA of different concentrations were incubated with HeLa cancer cells to investigate their cytotoxicity effects. The exposure of the cells to chitosan nanoparticles resulted in a decreased in cell growth and this was concentration-dependent. Our results revealed the utility of locally available materials to produce new biodegradable nanoparticles to investigate their biological nanotoxicity.