Abstract: Physicochemical characteristics of amylose and amylopectin fractions from retrograded maize starch were investigated by visible spectra, IR spectra, X-ray diffraction and SEM. The maximum visible absorbent wavelengths of maize amylose and amylopectin with iodine affinity were 548.0nm and 452.9nm, 578.9nm respectively. X-ray diffraction showed diffraction peaks for amylose and amylopectin fractions of retrograded maize starch were at 2θ of 17.1°, 22.4°, 23.9° and 17.0°, 19.5°, 22.0°, 23.8° respectively. Interaction between amylose and amylopectin had great effects on the diffraction pattern of maize starch. More lipids probably combined with amylopectin, not with amylose. The results of SEM showed that some kinds of layered structure existed in maize amylopectin fraction of retrograded maize starch.