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In this study, the electrospun fibers of chitosan (Ch)/poly (methyl methacrylate) (PMMA) (K1), Ch/PMMA (K2) containing 0.3 wt.% ibuprofen (Ibu) and Ch/PMMA (K3) containing 0.6 wt.% Ibu were obtained for the first time by electrospinning technique. The controlled release of ibuprofen from the K2 and K3 fiber surfaces was investigated by quartz crystal microbalance (QCM) system. The results of QCM were compared with the results of ultraviolet-visible (UV-Vis) absorption spectroscopy. The morphological characteristics of the biocompatible fibers were characterized by scanning electron microscopy with energy dispersive spectroscopy (SEM-EDS). It was observed that the best drug release mechanism from the drug release kinetics graphs was attributed to the K2 fiber structure obtained from the Ch/PMMA solution containing 0.3 wt.% Ibu and this was found to be the optimal drug concentration. [ABSTRACT FROM AUTHOR]