A near-infrared spectroscopy (NIR) technique has been applied for rapid and nondestructive quality determination of glass/epoxy prepreg. Abundant information related with resin and volatile was observed in the NIR spectra of the prepreg cloth. The partial least square (PLS) regression was used to develop the calibration models by utilizing several spectral pretreatments combined with different spectra ranges. Some unknown samples were analyzed by the NIR method. The mean absolute predicted errors were 0.32% and 0.214% for the resin content and the volatile content respectively. The results of the paired t-test revealed that there was no significant difference between the NIR method and standard method. The NIR method can be used to predict the resin and volatile content simultaneously within 30s. The study indicates that the NIR method is sufficiently for quality determination of glass/epoxy prepreg cloth.