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LC-MS/MS Analysis of Cyanotoxins in Bivalve Mollusks: Method Development, Validation and First Evidence of Occurrence of Nodularin in Mussels (Mytilus edulis) and Oysters (Magallana gigas) from the West Coast of Sweden
Swedish Food Agcy, Sci Dept, Box 622, SE-75126 Uppsala, Sweden.;Univ Nacl Colombia, Sci Fac, Chem Dept, Cr 45 N 26-85,POB 111321, Bogota, Colombia..
Swedish Food Agcy, Sci Dept, Box 622, SE-75126 Uppsala, Sweden.;Stockholm Water & Waste Co, Bryggerivagen 10, SE-10636 Stockholm, Sweden..
Uppsala University, Disciplinary Domain of Science and Technology, Chemistry, Department of Chemistry - BMC, Analytical Chemistry.ORCID iD: 0000-0001-9682-6840
Swedish Food Agcy, Sci Dept, Box 622, SE-75126 Uppsala, Sweden..
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2023 (English)In: Toxins, E-ISSN 2072-6651, Vol. 15, no 5, article id 329Article in journal (Refereed) Published
Abstract [en]

In this paper, an LC-MS/MS method for the simultaneous identification and quantification of cyanotoxins with hydrophilic and lipophilic properties in edible bivalves is presented. The method includes 17 cyanotoxins comprising 13 microcystins (MCs), nodularin (NOD), anatoxin-a (ATX-a), homoanatoxin (h-ATX) and cylindrospermopsin (CYN). A benefit to the presented method is the possibility for the MS detection of MC-LR-[Dha7] and MC-LR-[Asp3] as separately identified and MS-resolved MRM signals, two congeners which were earlier detected together. The performance of the method was evaluated by in-house validation using spiked mussel samples in the quantification range of 3.12-200 mu g/kg. The method was found to be linear over the full calibration range for all included cyanotoxins except CYN for which a quadratic regression was used. The method showed limitations for MC-LF (R-2 = 0.94), MC-LA (R-2 <= 0.98) and MC-LW (R-2 <= 0.98). The recoveries for ATX-a, h-ATX, CYN, NOD, MC-LF and MC-LW were lower than desired (<70%), but stable. Despite the given limitations, the validation results showed that the method was specific and robust for the investigated parameters. The results demonstrate the suitability of the method to be applied as a reliable monitoring tool for the presented group of cyanotoxins, as well as highlight the compromises that need to be included if multi-toxin methods are to be used for the analysis of cyanotoxins with a broader range of chemical properties. Furthermore, the method was used to analyze 13 samples of mussels (Mytilus edulis) and oysters (Magallana gigas) collected in the 2020-2022 summers along the coast of Bohuslan (Sweden). A complementary qualitative analysis for the presence of cyanotoxins in phytoplankton samples collected from marine waters around southern Sweden was performed with the method. Nodularin was identified in all samples and quantified in bivalve samples in the range of 7-397 <= g/kg. Toxins produced by cyanobacteria are not included in the European Union regulatory monitoring of bivalves; thus, the results presented in this study can be useful in providing the basis for future work including cyanotoxins within the frame of regulatory monitoring to increase seafood safety.

Place, publisher, year, edition, pages
MDPI MDPI, 2023. Vol. 15, no 5, article id 329
Keywords [en]
LC-MS/MS, cyanotoxins, nodularin, bivalves, mussels, seafood safety
National Category
Ecology
Identifiers
URN: urn:nbn:se:uu:diva-506971DOI: 10.3390/toxins15050329ISI: 000997911500001PubMedID: 37235362OAI: oai:DiVA.org:uu-506971DiVA, id: diva2:1779270
Funder
Swedish Foundation for Strategic Research, SM19-0005Available from: 2023-07-04 Created: 2023-07-04 Last updated: 2024-12-03Bibliographically approved

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Retrato, Mark Dennis ChicoBergquist, JonasZuberovic, Aida

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