Near infrared diffuse reflectance spectroscopy (NIDRS) calibrations of chemical composition in 62 kinds of steamed-flaking corn were developed by partial least squares (PLS) regression. The calibration models were constructed by the mean centre+first deviation+multivariate scattering calibration in the square regions (950～1 650 nm). Results showed that the R2VAL are 0.951 1, 0.903 2, 0.714 3 and 0.908 2 for CP, NDF, ADF and EE respectively. The SECV are 1.53, 1.89, 2.45 and 0.50 for CP, NDF, ADF and EE respectively. Therefore, the models could be used to predict the content of CP, NDF and EE in steamed-flaking corn and provide a fast and economical method for quality control of steamed-flaking corn.