Mycotoxin sequestration materials are important tools to reduce mycotoxin illness and enable proper handling of mycotoxin-contaminated commodities. Three food-grade bentonite clays and four generally recognized as safe (GRAS) charcoal/biochar carbon materials that are marketed as feed additives and supplements were evaluated for their ability to sequester the mycotoxins aflatoxin B, ochratoxin A, and zearalenone. The surface area of the clays varied between 32.1 to 51.4 mg/g, and the surface area of the carbon-based materials varied from 1.7 to 1735 mg/g. In vitro, gastric fluid studies indicated that certain pine biochar and activated coconut charcoal could sequester high amounts (85+%) of the mycotoxins at 1 ppm levels or below. However, some biochar materials with lower surface area properties lacked binding capacity. The coconut shell charcoal and pine biochar utilize agricultural waste products in a manner that significantly reduces carbon emissions and provides valuable materials to minimize exposure to toxins found in food and feed.