Cereal Chem. 94(2):237-241The effect of complexation temperature (30, 60, and 90°C) on the gelatinization properties, glass transition, enzymatic hydrolysis, and crystalline structure of high-amylose corn starch-oleic acid (HACS-OA) complexes created by a dimethyl sulfoxide (DMSO)-based complexation method and of normal corn starch-oleic acid (NCS-OA) complexes created by an alkaline-based complexation method were investigated by using differential scanning calorimetry, thermogravimetric analysis, and X-ray diffractometry. The results indicated that the highest complex indices were found in the complexes created at 30 and 60°C with the DMSO-based complexation method and alkaline-based complexation method, respectively. The X-ray diffraction patterns of both HACS-OA complexes and NCS-OA complexes created at different complexation temperatures were the V-type pattern. For the complexes created by the two methods, both the melting temperature and the glass transition temperature increased obviously with increasing complexation temperature. Complexation temperature also influenced the enzymatic hydrolysis rate of starch-OA complexes. † Corresponding