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European intercomparison study for the determination of fumonisins in maize

Fumonisins are mycotoxins, occurring largely in maize and maize products, which cause animal diseases, such as equine leukoencephalomalacia, porcine pulmonary oedema and hepatocarcinomas in rats. The aim of this project is to rapidly raise the quality of European feed and food control laboratories to undertake regular monitoring of maize products as required to assess risks and to protect consumers and animals.
The project involved the following steps:
the preparation of a reference solution containing fumonisins FB1 and FB2;
the preparation of a batch of contaminated maize material together with its blank counterpart;
a preliminary study of the gamma irradiation conditions for sterilization of maize materials;
the control of the homogeneity and stability of the solution and the 2 maize materials;
an intercomparison study for fumonisins analysis in the above materials with the involvement of 24 European laboratories, most of which have national or international responsibilities for foodstuff and/or feedstuff control.

15 kGy gamma irradiation was required to efficiently sterilize maize materials. This process caused the decrease of fumonisins concentrations by about 20%.
The materials used in this intercomparison study were checked for homogeneity at the 95% confidence level, and no gradient due to the filling sequence and no instability were detected.
The intercomparison study generated overall data with very high precision (M + or - 1SD of 2.29 + or - 0.27 ug/g for FB1 and 1.25 + or - 0.17 ug/g for FB2 after correction for recoveries), but poor accuracy due to the low recoveries (mean = 70%) obtained by most participants. The following factors improving recoveries of fumonisins from maize have been identified: extraction mode; shaking for 30 minutes instead of blending for a few minutes; consecutive extractions; extraction with higher solvent to material ratio; SAX clean up instead of C18 clean up. The improved precision of the methods used in this study in comparison to the IUPAC study is clearly shown by the consistent decrease of both within laboratory (RSDl) and between laboratory (RSDr) relative standard deviations; the RSDr in particular dropped to about 0.50 and 0.33 for FB1 and FB2, respectively.
More intercomparison studies are necessary before carrying out a certification exercise in order to improve the accuracy of the analytical methods.

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Institute of Toxins and Mycotoxins
Viale Einaudi 51
70125 Bari
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