Radiation stability of CyMe4-BTPhen was examined in systems with three selected cyclohexanone-based diluents. Accelerated electrons were used as a source of ionizing radiation. The CyMe4-BTPhen radiation degradation identification and characterization of the degradation products were performed by high performance liquid chromatography (HPLC) and mass spectrometry (MS) analyses. Residual concentrations of tested ligand were determined. Moreover, extraction properties of the solvents irradiated at two different doses were compared with the extraction properties of non-irradiated solvents to estimate the influence of the presence of degradation products in the organic phase.