Sensing of hydrazine, sulfite, and nitrite has attracted considerable attention in the chemical, pharmaceutical, agricultural, and food industries. The development of sensitive analytical methods for the detection and determination of hydrazine, sulfite, and nitrite is essential due to their importance in industry, food, water, and biological fluids and its toxicity. Numerous methods such as spectrophotometry, fluorimetry, and chromatography have been reported for the detection of hydrazine, sulfite, and nitrite. Among other analytical techniques, electrochemical sensors are embryonic in self-contained, compact, and low cost, with minimal power requirements. The electrochemical sensor also offers rapid response, high sensitivity, and selectivity providing quantitative analytical information.A three-dimensional amine-functionalized APS silicate sol–gel network-stabilized Au NPs-based electrochemical sensor platform is successfully developed in the absence of any other immobilized redox mediator/enzyme for hydrazine, sulfite, and nitrite. The fabricated electrocatalyst exhibits a large decrease in the electrochemical oxidation potential towards those analytes. Our experimental results reveal that the direct electrocatalytic performance of the Au NPs in APS silicate network is successfully utilized towards the detection of hydrazine, sulfite, and nitrite with low detection limits of 10 nM, 100 nM, and 1 μM, respectively, from the amperometric experimental evidences. This simple sensor platform concretes the tactic for the fabrication of Au NPs-based effective electrocatalytic platform for various environmental and food safety applications.This possesses major advantages of rapid response, low detection limits, high sensitivity and stability, capability of sensing multi-analytes for environment security, and food safety.I hope this writing would attract readers in the field of nanomaterial-based electrochemistry.