This study explores the innovative application of carbohydrate-based nanoparticles in aggressive colon cancer treatment. We synthesized Capecitabine (CTB) nanoparticles by conjugating them with potato starch and chitosan, utilizing the unique properties of these materials. CTB nanoparticles were meticulously fabricated through ultrasonication, hydrolysis with 0.1M NaOH, and ionotropic gelation. Characterization included drug loading, rheological studies, Surface-Enhanced Raman Spectroscopy (SERS), Fourier-Transform Infrared Spectroscopy (FTIR), Differential Scanning Calorimetry (DSC), X-ray Diffraction (XRD), and Thermogravimetric Analysis (TGA). Analysis of XRD and FTIR spectra revealed molecular disorder and crystallinity loss. Beyond physical characterization, we explored functional and antioxidant properties, showing promise with a mean particle size of 245±10.45nm, zeta potential +30.3±8.09 mV, leading efficacy 76.45±3.85%, and 92.25±5.78% drug release over 100 hours. Subsequently, we evaluated cytotoxicity against HT-29 cells in vitro and in vivo using N, N-dimethylhydrazine-induced male Balb/c mice. Capecitabine-loaded potato starch-chitosan (CTB-PS-CS) nanoparticles exhibited superior colon histology and lower tumour scores, highlighting their robust anticancer activity. CTB-PS-CS-NPs significantly reduced VEGD and CD31 compared to free CTB. We conducted various cellular assays, including tube-forming, wound-healing, crystal violet staining, and apoptosis studies, consistently demonstrating pronounced anticancer effects on HT-29 cells. Our study supports the enhanced anticancer activity of CTB-PS-CS-NPs, indicating their potential for assessing nanoparticle efficacy and compatibility across diverse cancer models.