This study was conducted to determine the effect of the homogenizing grade of sample on absorbance of near infrared reflectance spectrophotometer with which chemical compositions of food were rapidly and effectively analyzed. By the mathematical treatment of absorbance values standard error of prediction was reduced as follows. 1. The absorbance values of various samples ground for the same periods of time were calibrated before or after treatment with first or second derivative in an attempt to accurately predict the components of samples ground for the different periods of time. The standard error of prediction for moisture content were 1.478%, 0.658% and 0.580%, respectively, those for fat content 0.949%, 0.637% and 0.527%, respectively, and those for protein content 0.514%, 0.493% and 0.394%, respectively. Calibration of absorbance values after second derivative treatment showed the highest accuracy in predicting sample components. 2. The absorbance values of various samples ground for the different periods of time were calibrated before or after treatment with first or second derivative in order to accurately predict the components of samples ground for the different periods of time. The standard error of prediction for moisture content were 1.026%, 0.589% and 0.568%, respectively, and those for protein content 0.860%, 0.557% and 0.399%, respectively. The standard error of prediction were lower in the order of calibrations before and after first and second derivative treatments. As a result, calibration of absorbance values after second derivative treatment showed higher accuracy regardless of grinding time of samples.