Properly-dispersed diminished graphene oxide (RGO) nanostructures with uniform ornament of silver nanoparticles (AgNPs) on them have been ready by way of a hydrothermal course of adopted by the freeze-drying technique. The obtained graphene-layer-like construction with uniform distribution of AgNPs have then been utilized on the glassy carbon electrodes (GCE) to detect totally different focus of hydroquinone (HQ) and catechol (CC) of their combined options. Due to such well-dispersed construction and uniform distribution of AgNPs, the AgNPs/RGO/GCE illustrated enhanced simultaneous detection efficiency for HQ and CC. Within the HQ and CC combined resolution with pH of 6.0, the AgNPs/RGO/GCE electrode reveals a large linear vary of HQ (0.18–130 μM) and CC (0.07–120 μM), and correct restrict of detection (2.37 × 10−2 μM for HQ and 5.8 × 10−2 μM for CC). Thus, it’s believed that the AgNPs/RGO nanostructures reveals a terrific potential of making use of as doable probes for simultaneous detection of HQ and CC in actual setting.