Abstract: This study assessed the levels of four major mycotoxins (ochratoxin A, zearalenone, fumonisin B1+B2 and aflatoxin B1) in a total of twenty (20) samples consisting of five (5) samples each of Oryza sativa, Zea mays, Pennisetum glaucum and Triticum aestivum that were randomly purchased from different markets in Calabar, Cross River State. The four different food items were subjected to the same analytical procedures for extraction with 100ml solvent mixture containing water/ methanol (3:2) and 2g of sodium chloride.