We　have　developed　a　new　class　of　organic–inorganic　hybrid　nanostructures　based　on　the　use　of　reduced　graphene　oxide　(rGO),　polyaniline,　and　a　nickel　metal　nanostructure.　It　was　applied　to　efficient　non-enzymatic　sensing　of　glucose　based　on　its　electrocatalytic　oxidation.　Scanning　electron　microscopy　and　energy-dispersive　X-Ray　were　employed　to　characterize　the　material.　It　is　shown　that　the　doped　polyaniline　plays　an　important　role　in　the　formation　of　the　hybrid　nanostructures.　Improved　analytical　performance　is　found　when　the　hybrid　nanostructures　were　placed　on　a　glassy　carbon　electrode　and　used　for　non-enzymatic　sensing　of　glucose　at　a　typical　working　potential　of　+450 mV　and　a　pH　value　of　13.　Features　include　a　fast　response　(~2 s),　high　sensitivity　(6,050 μA mM−1 cm−2),　a　linear　range　from　0.1 μM　to　1.0 mM,　and　a　low　detection　limit　(0.08 μM).　The　response　to　glucose　follows　a　Michaelis-Menten　kinetic　behavior,　and　the　KM　value　was　determined　to　be　0.241 μM.　Reproducibility　and　specificity　are　acceptable.　Fructose　and　maltose　do　not　interfere　significantly.　Importantly,　the　methodology　was　validated　and　evaluated　for　the　analysis　of　15　spiked　human　serum　specimens,　receiving　in　a　good　accordance　with　the　results　obtained　by　the　non-enzymatic　glucose　sensing　and　the　commercialized　personal　glucose　meter.　©　2014,　Springer-Verlag　Wien.