The detection of dopamine, an important neurotransmitter in the central nervous system, is relevant because low levels of dopamine can cause brain disorders. Here, a novel electrochemical platform made of a hydrogel–graphene oxide nanocomposite was employed to electrochemically determine simultaneously dopamine (DA) and ascorbic acid (AA). Unlike previous work, where the base electrode is modified, the active material (graphene oxide, GO) was dispersed in the hydrogel matrix, making an active nanocomposite where the electrochemical detection occurs. The GO, hydrogel and nanocomposite synthesis is described. Dynamic Light Scattering, UV-visible and FTIR spectroscopies showed that the synthesized GO nanoparticles present 480 nm of diagonal size and a few sheets in height. Moreover, the polymer swelling, the adsorption capacity and the release kinetic of DA and AA were evaluated. The nanocomposite showed lower swelling capacity, higher DA partition coefficient and faster DA release rate than in the hydrogel. The electrochemical measurement proved that both materials can be employed to determine DA and AA. Additionally, the nanocomposite platform allowed the simultaneous determination of both molecules showing two well separated anodic peaks. This result demonstrates the importance of the incorporation of the nanomaterial inside of the hydrogel and proves that the nanocomposite can be used as a platform in an electrochemical device to determinate DA using an unmodified glassy carbon electrode.