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Main Authors: León-Morán, Lixy Olinda, Pastor-Belda, Marta, Arroyo-Manzanares, Natalia, Pérez-Ruzafa, Ángel, Campillo, Natalia, Viñas, Pilar
Format: Artículo científico
Language:en
Published: Environmental research 2026
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Online Access:https://pubmed.ncbi.nlm.nih.gov/41895573/
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author León-Morán, Lixy Olinda
Pastor-Belda, Marta
Arroyo-Manzanares, Natalia
Pérez-Ruzafa, Ángel
Campillo, Natalia
Viñas, Pilar
author_facet León-Morán, Lixy Olinda
Pastor-Belda, Marta
Arroyo-Manzanares, Natalia
Pérez-Ruzafa, Ángel
Campillo, Natalia
Viñas, Pilar
León-Morán, Lixy Olinda
Pastor-Belda, Marta
Arroyo-Manzanares, Natalia
Pérez-Ruzafa, Ángel
Campillo, Natalia
Viñas, Pilar
collection PubMed - marine biology
contents Monitoring of regulated and non-regulated biotoxins in marine organisms using liquid-phase microextraction and liquid chromatography coupled with high-resolution mass spectrometry. León-Morán, Lixy Olinda Pastor-Belda, Marta Arroyo-Manzanares, Natalia Pérez-Ruzafa, Ángel Campillo, Natalia Viñas, Pilar Marine Toxins Liquid Phase Microextraction Chromatography, Liquid Animals Mass Spectrometry Aquatic Organisms Environmental Monitoring The increase in marine biotoxins produced by microalgae has resulted in a significant rise in their presence in marine organisms. Although regulations have been established to control these compounds, identifying new emerging non-regulated biotoxins is complicated by the lack of available analytical standards. This study aimed to determine different biotoxins in marine organisms by liquid chromatography coupled with high-resolution mass spectrometry using a hybrid quadrupole-time-of-flight analyzer for both targeted and untargeted approaches. Solid-liquid extraction was used to isolate the analytes from the marine organisms, followed by dispersive liquid-liquid microextraction for cleaning and preconcentration purposes. Limits of detection in the 0.002-12.2 ng g range were obtained for the target analytes, eight regulated biotoxins (azaspiracids 1-5, AZAs 1-5; okadaic acid, OA; dinophysistoxins 1-2, DTXs 1-2) and other six non-regulated biotoxins (gymnodimine, GYM; 13-desmethylspirolide C, 13-SPX C; 13,19-didesmethylspirolide C, 13,19-SPX C; 20-methylspirolide G, 20-SPX G; pinnatoxin G, PnTX G; pectenotoxin 2, PTX-2). Five target analytes, GYM, 13-SPX C, PnTX G, OA and DTX-2, were found in several samples. Additionally, a suspect screening was developed in the untargeted approach considering a database of 456 compounds belonging to same target biotoxins groups. Several biotoxins (16-GYM, GYMs E and a 13-SPX C isomer) were identified in the studied samples. The presence of GYMs E in marine animal tissues has been reported for the first time in this study to the best of our knowledge. Furthermore, in vitro cytotoxicity assays were performed with OA and 13-SPX C on SAF-1 cells as marine organism model.
format Artículo científico
id pubmed_41895573
institution PubMed
language en
publishDate 2026
publisher Environmental research
record_format pubmed
spellingShingle Monitoring of regulated and non-regulated biotoxins in marine organisms using liquid-phase microextraction and liquid chromatography coupled with high-resolution mass spectrometry.
León-Morán, Lixy Olinda
Pastor-Belda, Marta
Arroyo-Manzanares, Natalia
Pérez-Ruzafa, Ángel
Campillo, Natalia
Viñas, Pilar
Marine Toxins
Liquid Phase Microextraction
Chromatography, Liquid
Animals
Mass Spectrometry
Aquatic Organisms
Environmental Monitoring
Monitoring of regulated and non-regulated biotoxins in marine organisms using liquid-phase microextraction and liquid chromatography coupled with high-resolution mass spectrometry. León-Morán, Lixy Olinda Pastor-Belda, Marta Arroyo-Manzanares, Natalia Pérez-Ruzafa, Ángel Campillo, Natalia Viñas, Pilar Marine Toxins Liquid Phase Microextraction Chromatography, Liquid Animals Mass Spectrometry Aquatic Organisms Environmental Monitoring The increase in marine biotoxins produced by microalgae has resulted in a significant rise in their presence in marine organisms. Although regulations have been established to control these compounds, identifying new emerging non-regulated biotoxins is complicated by the lack of available analytical standards. This study aimed to determine different biotoxins in marine organisms by liquid chromatography coupled with high-resolution mass spectrometry using a hybrid quadrupole-time-of-flight analyzer for both targeted and untargeted approaches. Solid-liquid extraction was used to isolate the analytes from the marine organisms, followed by dispersive liquid-liquid microextraction for cleaning and preconcentration purposes. Limits of detection in the 0.002-12.2 ng g range were obtained for the target analytes, eight regulated biotoxins (azaspiracids 1-5, AZAs 1-5; okadaic acid, OA; dinophysistoxins 1-2, DTXs 1-2) and other six non-regulated biotoxins (gymnodimine, GYM; 13-desmethylspirolide C, 13-SPX C; 13,19-didesmethylspirolide C, 13,19-SPX C; 20-methylspirolide G, 20-SPX G; pinnatoxin G, PnTX G; pectenotoxin 2, PTX-2). Five target analytes, GYM, 13-SPX C, PnTX G, OA and DTX-2, were found in several samples. Additionally, a suspect screening was developed in the untargeted approach considering a database of 456 compounds belonging to same target biotoxins groups. Several biotoxins (16-GYM, GYMs E and a 13-SPX C isomer) were identified in the studied samples. The presence of GYMs E in marine animal tissues has been reported for the first time in this study to the best of our knowledge. Furthermore, in vitro cytotoxicity assays were performed with OA and 13-SPX C on SAF-1 cells as marine organism model.
title Monitoring of regulated and non-regulated biotoxins in marine organisms using liquid-phase microextraction and liquid chromatography coupled with high-resolution mass spectrometry.
topic Marine Toxins
Liquid Phase Microextraction
Chromatography, Liquid
Animals
Mass Spectrometry
Aquatic Organisms
Environmental Monitoring
url https://pubmed.ncbi.nlm.nih.gov/41895573/