Ferrocene (Fc) is an organometallic compound of sandwich structure. As the anticancer and excellent electrical activities, ferrocene and its derivatives have many applications in electrochemical monitoring [1-3]. Hydrogen peroxide (HP), with strong permeability and oxidation properties, is the product of many peroxidase catalyzed reaction, and it is widely used in medical and cosmetic fields, even for food bleaching by some illegal merchants which may cause healthy problem. In this study, the polyelectrolyte multilayer films containing ferrocene-derived polymer assembling by sol-gel process [4] was introduced to HP determination as a sensor.