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Toxins 2019, 11(4), 222; https://doi.org/10.3390/toxins11040222

Development and Validation of a Liquid Chromatography High-Resolution Mass Spectrometry Method for the Simultaneous Determination of Mycotoxins and Phytoestrogens in Plant-Based Fish Feed and Exposed Fish

1
Toxinology Research Group, Norwegian Veterinary Institute, 0454 Oslo, Norway
2
Nofima—Norwegian Institute of Food, Fisheries and Aquaculture Research, 5141 Fyllingsdalen, Norway
3
Nofima—Norwegian Institute of Food, Fisheries and Aquaculture Research, 6600 Sunndalsøra, Norway
4
Faculty of Biosciences and Aquaculture, Nord University, 8049 Bodø, Norway
5
Chemistry Section, Norwegian Veterinary Institute, 0454 Oslo, Norway
*
Author to whom correspondence should be addressed.
Received: 11 March 2019 / Revised: 28 March 2019 / Accepted: 11 April 2019 / Published: 13 April 2019
(This article belongs to the Special Issue Mycotoxins in Feed and Food Chain: Present Status and Future Concerns)
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Abstract

New protein sources in fish feed require the assessment of the carry-over potential of contaminants and anti-nutrients from feed ingredients into the fish, and the assessment of possible health risks for consumers. Presently, plant materials including wheat and legumes make up the largest part of aquafeeds, so evaluation of the transfer capabilities of typical toxic metabolites from plant-infesting fungi and of vegetable phytoestrogens into fish products is of great importance. With the aim of facilitating surveillance of relevant mycotoxins and isoflavones, we have developed and validated a multi-analyte LC-HRMS/MS method that can be used to ensure compliance to set maximum levels in feed and fish. The method performance characteristics were determined, showing high specificity for all 25 targeted analytes, which included 19 mycotoxins and three isoflavones and their corresponding aglycons with sufficient to excellent sensitivities and uniform analytical linearity in different matrices. Depending on the availability of matching stable isotope-labelled derivates or similar-structure homologues, calibration curves were generated either by using internal standards or by matrix-matched external standards. Precision and recovery data were in the accepted range, although they varied between the different analytes. This new method was considered as fit-for-purpose and applied for the analysis of customised fish feed containing wheat gluten, soy, or pea protein concentrate as well as salmon and zebrafish fed on diets with these ingredients for a period of up to eight weeks. Only mycotoxin enniatin B, at a level near the limit of detection, and low levels of isoflavones were detected in the feed, demonstrating the effectiveness of maximum level recommendations and modern feed processing technologies in the Norwegian aquaculture industry. Consequently, carry-over into fish muscle was not observed, confirming that fillets from plant-fed salmon were safe for human consumption. View Full-Text
Keywords: Atlantic salmon; zebrafish; liquid chromatography high-resolution mass spectrometry; mycotoxins; phytoestrogens; plant-based feed Atlantic salmon; zebrafish; liquid chromatography high-resolution mass spectrometry; mycotoxins; phytoestrogens; plant-based feed
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Johny, A.; Fæste, C.K.; Bogevik, A.S.; Berge, G.M.; Fernandes, J.M.; Ivanova, L. Development and Validation of a Liquid Chromatography High-Resolution Mass Spectrometry Method for the Simultaneous Determination of Mycotoxins and Phytoestrogens in Plant-Based Fish Feed and Exposed Fish. Toxins 2019, 11, 222.

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