Abstract
Cyclic imines (CIs) are being considered as emerging toxins in the European Union, and a scientific opinion has been published by the European Food Safety Authority (EFSA) in which an assessment of the risks to human health related to their consumption has been carried out. Recommendations on the EFSA opinion include the search for data occurrence of CIs in shellfish and using confirmatory methods by liquid chromatography-tandem mass spectrometry (LC-MS/MS), which need to be developed and optimized. The aim of this work is the application of LC-MS/MS to the analysis of gymnodimines (GYMs), spirolides (SPXs), pinnatoxins (PnTXs), and pteriatoxins (PtTXs) in mussels from Galician Rias, northwest Spain, the main production area in Europe, and therefore a representative emplacement for their evaluation. Conditions were adjusted using commercially available certified reference standards of GYM-A, SPX-1, and PnTX-G and evaluated through quality control studies. The EU-Harmonised Standard Operating Procedure for determination of lipophilic marine biotoxins in molluscs by LC-MS/MS was followed, and the results obtained from the analysis of eighteen samples from three different locations that showed the presence of PnTXs and SPXs are presented and discussed. Concentrations of PnTX-G and SPX-1 ranged from 1.8 to 3.1 µg/kg and 1.2 to 6.9 µg/kg, respectively, and PnTX-A was detected in the group of samples with higher levels of PnTX-G after a solid phase extraction (SPE) step used for the concentration of extracts.
Highlights
Gymnodimines (GYMs), spirolides (SPXs), pinnatoxins (PnTXs), pteriatoxins (PtTXs), prorocentrolides, spiro-prorocentrimine, portimines, and symbioimines belong to cyclic imines (CIs), a family of marine biotoxins produced by dinoflagellates and accumulated in shellfish [1,2,3]
CIs have a mode of action based on the inhibition of nicotinic acetylcholine receptors, and neurotoxic effects were observed in toxicological assays, as of yet there has been no reported information about human intoxication linked to their assimilation [6,7,8]
The m/z 164 fragment ion (C11H18N+) is common to all reported pinnatoxins and pteriatoxins in addition to the majority of spirolides, and a m/z 572 fragment ion can be utilized as a PnTX- and PtTX-specific product ion for selected reaction monitoring (SRM) detection and confirmation of these toxins in samples [26,29]
Summary
Gymnodimines (GYMs), spirolides (SPXs), pinnatoxins (PnTXs), pteriatoxins (PtTXs), prorocentrolides, spiro-prorocentrimine, portimines, and symbioimines belong to cyclic imines (CIs), a family of marine biotoxins produced by dinoflagellates and accumulated in shellfish [1,2,3]. These compounds share as a common structural motif an imine group in a cyclic moiety, which has been identified as a pharmacophore with biological activity [4,5]. Public Health 2020, 17, 281; doi:10.3390/ijerph17010281 www.mdpi.com/journal/ijerph
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