ABSTRACT The presence of mycotoxins in food is a significant concern due to their potential health risks. It is estimated that around 25% of global food production is contaminated with mycotoxins, which can be produced by certain types of fungi that infect crops during different stages of growth. As a result, it is crucial to monitor mycotoxins in food sources and develop effective methods for removal or reduction. One technique commonly used for detecting and separating mycotoxins is immunoaffinity chromatography (IAC). Traditionally, IAC uses antibodies covalently bonded to a solid support material, but this can lead to conformational changes and reduced affinity towards the analytes. To address these limitations, researchers have explored alternative methods for immobilising biomolecules, such as the sol-gel method, which involves encapsulating biomolecules within the pores of a glass matrix. This approach makes it easier to reuse the immunoaffinity columns and reduces the need for bacteriostatic agents, making the process more cost-effective and efficient. The results showed that sol-gel IAS was able to effectively separate these toxins from complex matrices, demonstrating its potential for widespread application in food safety monitoring. Additionally, the ability of sol-gel IAS to remove mycotoxins from environmental samples tested was highlighting its versatility and potential for broader applications beyond food safety. Finally, they demonstrated the compatibility of sol-gel IAS with high-performance liquid chromatography, enabling online coupling of the two techniques for improved efficiency and accuracy. The findings of this study suggest that sol-gel IAC is a promising method for the detection and separation of mycotoxins in various matrices, including food, environmental samples, and other biological fluids. Its advantages over traditional IAC methods make it an attractive option for large-scale analysis and monitoring of mycotoxins in diverse settings.