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Targeted and untargeted approaches using liquid chromatography with high-resolution mass spectrometry for the determination of lipophilic marine biotoxins in seawater and mussel samples

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dc.contributor.authorPastor Belda, Marta
dc.contributor.authorArroyo Manzanares, Natalia
dc.contributor.authorViñas López-Pelegrin, Pilar
dc.contributor.authorSánchez Fernández, Olga
dc.contributor.authorPérez Ruzafa, Ángel
dc.contributor.authorCampillo Seva, Natalia
dc.contributor.authorLeón Morán, Lixy Olinda
dc.contributor.departmentQuímica Analítica
dc.date.accessioned2026-02-24T08:14:27Z
dc.date.available2026-02-24T08:14:27Z
dc.date.copyright© 2025 The Authors
dc.date.issued2025-09-12
dc.description.abstractMarine biotoxins are naturally occurring compounds produced around the world by various species of microalgae, whose presence increases significantly due to harmful algal blooms. This phenomenon is a major public health concern, as a large amount of marine fauna is exposed to these biotoxins. The aim of this study was the improvement and application of dispersive liquid-liquid microextraction and liquid chromatography coupled to high-resolution mass spectrometry for the determination of eight lipophilic marine biotoxins, okadaic acid (OA), dinophysistoxin 1 (DTX-1), dinophysistoxin 2 (DTX-2), 16:0 7-O-acyl okadaic acid (DTX-3a), gambierone (GAM), 44-methylgambierone (44-GAM), yessotoxin (YTX), and homoyessotoxin (hYTX), and their derivatives in seawaters and mussels by targeted and untargeted approaches. The proposed method provided detection limits ranging from 0.0004 to 1.7 ng mL-1 in seawater and 0.06 to 119 ng g-1 in mussel samples, depending on the biotoxin. A total of 23 seawater samples collected in the Mar Menor lagoon between 2021 and 2023 were analyzed and several of them were found to contain OA and DTX-3a at concentration levels in the 0.006–1.5 ng mL-1 range. OA and DTX-2 were also found at maximum levels of 8.0 and 1.2 ng g-1, respectively, in several mussel samples from commercial origin. In addition, a suspect screening was developed in the untargeted approach to investigate the presence of other derivatives of the target marine biotoxins in the samples using a home-made database covering 93 compounds. An unsaturated ester derivative of OA/DTX-2 was detected in the seawater samples collected during a red tide.
dc.formatapplication/pdf
dc.identifier.citationMarine Pollution Bulletin 222 (2026) 118688
dc.identifier.doihttps://doi.org/10.1016/j.marpolbul.2025.118688
dc.identifier.urihttp://hdl.handle.net/10201/211421
dc.languageeng
dc.publisherElsevier
dc.relationEste estudio forma parte del programa ThinkInAzul (Proyecto PLASTOXIN) y ha contado con el apoyo del MCIU con financiación de la Unión Europea NextGenerationEU (PRTR-C17.I1) y de la Comunidad Autónoma de la Región de Murcia - Fundación Séneca. Proyecto español MCIN TED2021-129766B-C21/AEI/ 10.13039/501100011033/Unión Europea NextGenerationEU/PRTR. Algunos de los datos sobre el estado medioambiental y trófico del Mar Menor utilizados en este estudio se obtuvieron a través del proyecto «Seguimiento y modelización de la calidad del agua y el estado ecológico del Mar Menor y prevención de impactos», financiado por la Comunidad Autónoma de la Región de Murcia.
dc.relation.publisherversionhttps://www.sciencedirect.com/science/article/pii/S0025326X25011646
dc.rightsAttribution-NonCommercial-NoDerivatives 4.0 International*
dc.rights.accessRightsinfo:eu-repo/semantics/openAccess
dc.rights.urihttp://creativecommons.org/licenses/by-nc-nd/4.0/*
dc.subjectSeawater
dc.subjectMussels
dc.subjectDispersive liquid-liquid microextraction
dc.subjectLiquid chromatography
dc.subjectHigh-resolution mass spectrometry
dc.subjectLipophilic marine biotoxins
dc.subject.odsNo relacionado con ningún objetivo de desarrollo sostenible
dc.titleTargeted and untargeted approaches using liquid chromatography with high-resolution mass spectrometry for the determination of lipophilic marine biotoxins in seawater and mussel samples
dc.typeinfo:eu-repo/semantics/article
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