Publication: Targeted and untargeted approaches using liquid chromatography with high-resolution mass spectrometry for the determination of lipophilic marine biotoxins in seawater and mussel samples
Authors
Pastor Belda, Marta ; Arroyo Manzanares, Natalia ; Viñas López-Pelegrin, Pilar ; Sánchez Fernández, Olga ; Pérez Ruzafa, Ángel ; Campillo Seva, Natalia ; León Morán, Lixy Olinda
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Publisher
Elsevier
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DOI
https://doi.org/10.1016/j.marpolbul.2025.118688
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info:eu-repo/semantics/article
Description
Abstract
Marine 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.
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Citation
Marine Pollution Bulletin 222 (2026) 118688
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