Comparison of methods and optimisation of the analysis of fumonisins B1 and B2 in masa flour,an alkaline cooked corn product

A comparison study of different extraction and clean-up procedures for the liquid chromatographic analysis of fumonisins B₁ (FB₁) and B₂ (FB₂) in corn masa flour was performed. The procedures included extraction (heat or room temperature) with acidic conditions or EDTA-containing solvents, and clean-up by immunoaffinity or C18 solid-phase extraction columns. Thereafter an analytical method was optimised using extraction with an acidic mixture of methanol–acetonitrile–citrate/phosphate buffer, clean-up through the immunoaffinity column and determination of fumonisins by liquid chromatography with automated pre-column derivatisation with o-phthaldialdehyde reagent. Recovery experiments performed on yellow, white and blue masa flours at spiking levels of 400, 800 and 1200?µg?kg^?1 FB₁ and of 100, 200 and 300?µg?kg^?1 FB₂ gave overall mean recoveries of 99% (±6%) for FB₁ and 88% (±6%) for FB₂. Good recoveries (higher than 90% for both FB₁ and FB₂) were also obtained with corn tortilla chips. The limits of quantification of the method (signal-to-noise ratio of 10) were 25?µg?kg^?1 for FB₁ and 17?µg?kg^?1 for FB₂. The method was tested on different commercial corn masa flours as well as on white and yellow corn tortilla chips, showing fumonisin contamination levels (FB₁?+?FB₂) up to 1800?µg?kg^?1 (FB₁?+?FB₂) in masa flour and 960?µg?kg^?1 in tortilla chips. Over 30% of masa flours originating from Mexico exceeded the European Union maximum permitted level.