Fabbrocino, Serena (2015) MASS SPECTROMETRY APPROACHES FOR EVALUATION OF DIETARY EXPOSURE TO TOXIC CONTAMINANTS. [Tesi di dottorato]

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Abstract

The legislation on environmental contaminants in food and feed chain is constantly evolving. Some of these contaminants, such as mycotoxins, have already been the subject of official control of the food and feed chain, while others, such as cyanotoxins compounds, are not yet covered. Present work is based on the development of innovative techniques aimed at the implementation of confirmatory analytical methods for the control of substances present and of probable future inclusion in the Official monitoring plans, i.e. aflatoxin M1 in dairy products, T-2 and HT-2 toxins in feedingstuffs and microcystins and cylindrospermopsin in particular products such as dietary supplements. Regarding the mycotoxins, this work aims to focus on validation study of an analytical confirmatory method for the detection of T-2 and HT-2 toxins in feedingstuffs, as required by Commission Recommendation n 165 of 27 March 2013 with more rapid and reliable extraction methods based on QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) extraction kit coupled to detection in LC-MS/MS. The applicability of QuEChERS extraction method was also tested for the analysis of AFM1 in dairy products with final determination by LC-ESI-Ion Trap MS/MS. As to cyanotoxins, the Committee of Experts of the WHO defined a tolerable daily intake only for one of the up to 90 known microcystins, i.e. microcystin LR, although recent studies indicate that other congeners are eventually more toxic; here we present the development of a fully validated method for a rapid and reliable detection of these compounds in dietary supplements with ESI-Ion Trap MS/MS detection. So this work has allowed us to achieve several goals. Firstly, it has been provided an example, so far not present in the scientific literature, of application of the QuEChERS extraction analysis for a fully validated confirmatory method for T-2 and HT-2 determination in feedingstuffs, whose validity has been proved fullfilling European Legislation criteria requirements; moreover, for the confirmation of the presence of aflatoxin M1 in dairy products in compliance with the needs of a quick response, an analytical solution to laboratories appointed for Official Control was provided. Moreover, the development and validation of analytical methods for substances such as microcystins characterized by toxicity and evident presence in dietary supplements, which are not covered by national and European legislation allowed us to provide guidance to the regulation both for performance criteria and for safety levels. The presence in dietary supplements of another cyanotoxin, the cylindrospermopsin was also evidenced.

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