An analytical method using Raman spectroscopy was developed for the determination of amylose concentration in maize starches. FT-Raman spectra of four maize starches with amylose content varying from 3.3 to 66% were obtained. A Raman band at ≃1657 cm-1 correlated linearly with amylose concentration in the four maize starches, and a calibration curve for Raman band intensity versus amylose content was developed. The linear correlation of the I1657/I900 integrated areas with amylose content was r = 0.997. The Raman-based calibration curve allows fast and nondestructive determination of the amylose content in maize starches with minimal sample preparation.