Carboxymethyl chitosan dialdehyde starch Schiff base (CMCDAS) and its metal complexes were synthesized by corn starch (St), sodium periodate, carboxymethyl chitosan and metal ions (copper, zinc, nickel, silver), and were characterized by Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), thermogravimetric analyzer (TGA), energy dispersive spectroscopy (EDS) and X-ray powder diffraction (XRD). The antibacterial activities of CMCDAS against E. coli and S. aureus increased according with its increasing nitrogen content, and the best minimum inhibitory concentrations (MIC) to E. coli and S. aureus were 30 mg/mL, respectively. Furthermore, the minimum inhibitory concentrations (MIC) of the metal Complexes (copper, nickel, silver, and zinc) against S. aureus were 7.50 mg/mL, 30 mg/mL, 30 mg/mL, and 1.88 mg/mL, respectively; and against E. coli were 7.50 mg/mL, 15 mg/mL, 15 mg/mL, and 0.94 mg/mL, respectively.