This study evaluates the feasibility of near-infrared (NIR) spectroscopy combined with chemometrics as a fast and efficient technique to predict the polysaccharide content and antioxidant activity of Poria cocos. The reference values of polysaccharide content were determined by the phenol-sulfuric acid method, and the antioxidant activities were determined by the DPPH scavenge assay, FRAP scavenge assay and ABTS scavenge assay, respectively. The partial least squares regression algorithm was used to relate the spectra to the reference values. Various methods for spectra pretreatment and variable selection were optimized to improve the predictability and stability of the models. As a result, the best models yielded very satisfying results, of which the values of coefficients of determination were all >0.94, and the values of residual predictive deviation were all >4. Such results confirmed that the present method is robust and applicable, and thus has good potential for rapid quality evaluation of Poria cocos.