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In this study, an efficient and simple designed nanohybrid created for individual and simultaneous detection of ascorbic acid (AA), dopamine (DA) and uric acid (UA). This nanohybrid is a combination of chemical reduced graphene oxide (CRGO) and redox poly(para-phenylene) (Fc-ac-PP) modified in a lateral position with ferrrocenyl group CRGO/Fc-ac-PPP. The CRGO/Fc-ac-PPP nanohybrid demonstrated a synergistic effect resulting in a large conductivity, surface area and catalytic properties provided by the redox attached ferrocene. Moreover, this nanocomposite is able to detect individually as well as simultaneously AA, DA and UA in a co-existence system with defined and separated redox peaks oxidation. The linear response ranges for AA, DA and UA, when detected simultaneously, are 0.1–10000 μM, 0.0001–1000 μM and 0.1–10000 μM, respectively, and the detection limits (S/N = 3) are 0.046 μM, 0.2 nM and 0.013 μM, respectively. The proposed sensor shown satisfactory results when applied to real spiked urine samples for measuring the abnormal high or lowconcentration of AA, DA and UA in vivo.