Here, we report hydrogen peroxide generation at 2-nitrophenyloctyl ether (NPOE)-water interface with decamethylferrocene as an electron donor. The progress of this reaction was detected by the observation of color change of the organic and aqueous phases in series of shake-flask experiments. The shape change of cyclic voltammograms recorded at carbon paste electrode with decamethylferrocene solution in NPOE also indicates (electro)catalytic reaction. Hydrogen peroxide was electrochemically detected at Pt microelectrode tip positioned in front of carbon paste electrode. For this purpose, scanning electrochemical microscopy (SECM) approach curves were recorded. Analogous experiments demonstrated the possibility of electrochemical regeneration of the electron donor. The (electro)catalytic effect of MoS2 on hydrogen peroxide generation was found by both shake-flask and SECM experiments.