The use of rapid spectroscopic methods for quantitative analysis of glycoprotein production in a CHO cell fed-batch process is demonstrated. The research was conducted as part of a collaboration with Bristol-Myers Squibb in which unique access was provided to both samples and process information. The study focussed on the use of both Raman and Excitation Emission Matrix Fluorescence (EEMF) spectroscopies to analyse the various liquid samples of raw materials, media, and bioreactor broth. The spectral information was then processed and interpreted using a variety of chemometric (multi-variate analysis) techniques. Using these techniques it was possible to generate quantitative predictive models for process performance based on glycoprotein yield from measurements made on both feed media and samples extracted from bioreactors. Accurate predictions with relative errors of between <5% were obtained for samples extracted from the 100 to 5000L scale bioreactors.