In this work, zinc oxide-decorated graphene oxide (ZnO–rGO) was successfully synthesized with a fast reflux chemical procedure at 100 °C. An equal mass ratio of graphene oxide (GO) and zinc acetate was used as starting materials dissolved, respectively, in ultrapure distilled water and dimethylformamide (DMF). Particularly, pure GO was synthesized using Hummers modified protocol by varying the mass ratio of (graphite:potassium permanganate) as follows: 1:2, 1:3, and 1:4, which allow us to obtain six types of pure and decorated samples, named, respectively, GO1:2, GO1:3, GO1:4, ZnO–rGO1:2, ZnO–rGO1:3, and ZnO–rGO1:4 using reflux at 100 °C. X-ray diffraction, FTIR, and Raman spectroscopy spectra confirm the formation of wurzite ZnO in all ZnO-decorated samples with better reduction of GO in ZnO–rGO1:4, confirming that a higher degree of graphene oxidation allows better reduction during the decoration process with ZnO metal oxide. Antioxidant activity of pure and zinc oxide-decorated graphene oxide samples were compared using two different in vitro assays (DPPH radical and H2O2 scavenging activities). Considerable in vitro antioxidant activities in a concentration-dependent manner were recorded. Interestingly, pristine GO showed more elevated scavenging efficiency in DPPH tests while ZnO-decorated GO was relatively more efficient in H2O2 antioxidant assays.