Gel time of prepreg is an important quality determinant in the manufacturing process of Copper Clad Laminate (CCL). Prepreg consists of a glass fiber reinforcement impregnated to a predetermined level with a resin matrix. In this work, near infrared spectroscopy associated with partial least squares (PLS) regression has been applied to analyse the gel time of prepreg samples in the manufacturing process. A total of 250 prepreg samples were randomly divided into a calibration set and a validation prediction set with a ratio of 4:1. The values of Root Mean Square Error of leave-one-out Cross-Validation (RMSECV) and the coefficient of determination (R2) of the calibration model was 2.95 s and 0.92 respectively, with eight PLS factors used. The results of the paired t-test revealed that there was no significant difference between the NIR method and the reference method. The analytical result showed that, NIR spectroscopy was a rapid, nondestructive, and accurate method for real-time prediction of prepreg quality in the CCL manufacturing process.