An anaerobic digestion process, finalized to biogas production, is characterized by different steps involving the variation of some chemical and physical parameters related to the presence of specific biomasses as: pH, chemical oxygen demand (COD), volatile solids, nitrate (NO3−) and phosphate (PO3−). A correct process characterization requires a periodical sampling of the organic mixture in the reactor and a further analysis of the samples by traditional chemical-physical methods. Such an approach is discontinuous, time-consuming and expensive. A new analytical approach based on hyperspectral imaging in the NIR field (1000 to 1700 nm) is investigated and critically evaluated, with reference to the monitoring of wine waste anaerobic digestion process. The application of the proposed technique was addressed to identify and demonstrate the correlation existing, in terms of quality and reliability of the results, between "classical" chemical-physical parameters and spectral features of the digestate samples. Good results were obtained, ranging from a R2 = 0.68 and a RMSECV = 12.83 mg/l for nitrate to a R2 = 0.90 and a RMSECV = 5495.16 mg O2/l for COD. The proposed approach seems very useful in setting up innovative control strategies allowing for full, continuous control of the anaerobic digestion process.