A procedure for the analytical validation of a rapid supercritical fluid extraction amperometric screening method for controlling macrocyclic lactone mycotoxins in maize flour samples has been developed. The limit established by European legislation (0.2 mg kg-1), in reference to zearalenone (ZON) mycotoxin, was taken as the reference threshold to validate the proposed method. Natural ZON metabolites were also included in this study to characterize the final screening method. The objective was the reliable classification of samples as positive or negative samples. The cut-off level was fixed at a global concentration of mycotoxins of 0.17 mg kg-1. An expanded unreliability zone between 0.16 and 0.23 mg kg-1 characterized the screening method for classifying the samples. A set of 30 samples was used for the final demonstration of the reliability and usefulness of the method.
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