<p>Acrylonitrile and acrolein are prevalent toxic pollutants in industrial wastewater. These compounds pose significant environmental and health risks due to their toxicity, carcinogenicity, and potential to bioaccumulate. Effective monitoring is crucial due to their high toxicity (e.g., acrylonitrile's LD₅₀ of 78&#xa0;mg/kg in rats) and potential for bioaccumulation, yet current detection methods face sensitivity and interference challenges. This review focuses on environmental toxicology from acrylonitrile and acrolein, and integrats advanced detection techniques to mitigate risks by enabling monitoring. We evaluated spectroscopic, chromatographic, and sensor-based methods, assessing their detection limits (as low as 0.13 and 1.02&#xa0;μg/mL) and applicability in aquatic environments. The review synthesizes key findings on acrylonitrile and acrolein, including their sources, impacts, and detection performance, based on evaluated studies. Acrylonitrile and acrolein exhibits both acute toxicological effects and chronic risks, and show high toxicity to aquatic organisms. GC–MS offers high sensitivity and selectivity, while emerging sensors show promise for real-time monitoring but require further development to address interference and sensitivity issues. Acrylonitrile and acrolein pose significant environmental and health risks due to their toxicity, carcinogenicity, and potential for bioaccumulation. Effective monitoring is critical for mitigating impacts on ecosystems and human health, especially in industrial wastewater contexts. Current detection methods have trade-offs, and integrated approaches, combining chromatography for precision and sensors for real-time application, are recommended for comprehensive environmental surveillance. Future research should focus on optimizing sensor technologies to enhance sensitivity and field applicability, supporting regulatory compliance and public health protection.</p>