Mycotoxins are toxic compounds produced by the metabolism of certain fungi that threaten the food and agricultural industry. Over hundreds of mycotoxins, one of the most common toxins, zearalenone (ZEN), has toxic effects on human and animal health due to its mutagenicity, treatogenicity, carcinogenicity, nephrotoxicity, immunotoxicity, and genotoxicity. In this work, attenuated internal reflection spectroscopic ellipsometry (AIR-SE) combined with the signal amplification via surface plasmon resonance conditions that were proved to be a highly sensitive analytical tool in bio-sensing was developed for the sensitive and selective ZEN detection in cereal products such as corn, wheat, rice, and oat. Combined with the oligonucleotide aptamer for ZEN recognition, our proposed method showed good performance with yielding 0.08 ng/mL LOD and 0.01-1000 ng/mL detection range. A mini-review was also introduced in, to compare various methods for ZEN detection.