This chapter highlights the cutting-edge utilization of GO/ZnO hybrid nanocomposite in electrochemical analysis of environmental pollutants. We provide an overview of techniques employed for the preparation and modification of electrode surfaces using nanocomposites. Additionally, we present various instances of their application in environmental electrochemical sensors, specifically in the detection of formaldehyde. Furthermore, we discuss the current trends in the advantageous utilization of NC in the construction of electrochemical sensors for environmental monitoring, while also addressing the future challenges that lie ahead. It is worth noting that NPs exhibit promising potential in enhancing the competitiveness of electrochemical sensors in environmental monitoring. However, the majority of research efforts have primarily focused on developing methodologies for fabricating novel sensors, with limited studies conducted on optimizing the performance of these sensors and their applicability to real samples.