Method performance verification for the combined detection and quantitation of the marine neurotoxins cyclic imines and brevetoxin shellfish metabolites in mussels (Mytilus edulis) and oysters (Crassostrea gigas) by UHPLC-MS/MS

O’Neill, Alison; Morrell, Nadine; Turner, Andrew D.; Maskrey, Benjamin H.

doi:10.1016/j.jchromb.2021.122864

Cited by 11 publications

(4 citation statements)

References 71 publications

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“…In this sense, there is a wide variety of LOQ and LOD data published for lipophilic toxin analyses using Agilent [22,23,26], Thermo [24,27] or Waters [20,21] mass spectrometers among others. Almost all of these papers reported LOQs and LODs values higher than those in the present work, except O'Neill et al [28] and Yang et al [27] with similar and slightly lower values, respectively. However, none of them combines the 14 toxins in the same run and in such a short time…”

Section: Loq/lodcontrasting

confidence: 51%

Development of a Fast Liquid Chromatography Coupled to Mass Spectrometry Method (LC-MS/MS) to Determine Fourteen Lipophilic Shellfish Toxins Based on Fused–Core Technology: In-House Validation

Rossignoli¹,

Mariño²,

Martín³

et al. 2021

Marine Drugs

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Prevalence and incidence of the marine toxins (paralytic, amnesic, and lipophilic toxins) including the so-called emerging toxins (these are, gymnodimines, pinnatoxins, or spirolides among others) have increased in recent years all over the world. Climate change, which is affecting the distribution of their producing phytoplankton species, is probably one of the main causes. Early detection of the toxins present in a particular area, and linking the toxins to their causative phytoplankton species are key tools to minimize the risk they pose for human consumers. The development of both types of studies requires fast and highly sensitive analytical methods. In the present work, we have developed a highly sensitive liquid chromatography-mass spectrometry methodology (LC-MS/MS), using a column with fused-core particle technology, for the determination of fourteen lipophilic toxins in a single run of 3.6 min. The performance of the method was evaluated for specificity, linearity, precision (repeatability and reproducibility) and accuracy by analysing spiked and naturally contaminated samples. The in-house validation was successful, and the limit of detection (LOD) and quantification (LOQ) for all the toxins were far below their regulatory action limits. The method is suitable to be considered in monitoring systems of bivalves for food control.

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Section: Loq/lodcontrasting

confidence: 51%

Development of a Fast Liquid Chromatography Coupled to Mass Spectrometry Method (LC-MS/MS) to Determine Fourteen Lipophilic Shellfish Toxins Based on Fused–Core Technology: In-House Validation

Rossignoli¹,

Mariño²,

Martín³

et al. 2021

Marine Drugs

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“…For emerging lipophilic toxins (method B), a methanolic 1 mM ammonium fluoride mobile phase was used, along with MS source conditions as described in [61]. Analytes targeted in these analyses included brevetoxins (BTXB2, BTXB4, BTXB5, s-desoxyBTXB2; and PbTX2, PbTX3), pinnatoxins (PnTX A, D, E, F, G, H), additional spirolides (13,19 didesmethyl spirolide C and 20-methyl spirolide C), and an additional gymnodimine (12methyl GYM), which have been associated with sodium channel activity in past studies [61,62]. Individual MRM transitions and parameters are described in Table 4 and were optimized prior to analysis under flow conditions.…”

Section: Uhplc-ms/ms Targeted Phycotoxin Analysismentioning

confidence: 99%

Gambierone and Sodium Channel Specific Bioactivity Are Associated with the Extracellular Metabolite Pool of the Marine Dinoflagellate Coolia palmyrensis

et al. 2023

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Tropical epibenthic dinoflagellate communities produce a plethora of bioactive secondary metabolites, including the toxins ciguatoxins (CTXs) and potentially gambierones, that can contaminate fishes, leading to ciguatera poisoning (CP) when consumed by humans. Many studies have assessed the cellular toxicity of causative dinoflagellate species to better understand the dynamics of CP outbreaks. However, few studies have explored extracellular toxin pools which may also enter the food web, including through alternative and unanticipated routes of exposure. Additionally, the extracellular exhibition of toxins would suggest an ecological function and may prove important to the ecology of the CP-associated dinoflagellate species. In this study, semi-purified extracts obtained from the media of a Coolia palmyrensis strain (DISL57) isolated from the U.S. Virgin Islands were assessed for bioactivity via a sodium channel specific mouse neuroblastoma cell viability assay and associated metabolites evaluated by targeted and non-targeted liquid chromatography tandem and high-resolution mass spectrometry. We found that extracts of C. palmyrensis media exhibit both veratrine enhancing bioactivity and non-specific bioactivity. LC-HR-MS analysis of the same extract fractions identified gambierone and multiple undescribed peaks with mass spectral characteristics suggestive of structural similarities to polyether compounds. These findings implicate C. palmyrensis as a potential contributor to CP and highlight extracellular toxin pools as a potentially significant source of toxins that may enter the food web through multiple exposure pathways.

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“…They are produced by several microalgal species such as Vulcanodinium rugosum and Alexandrium ostenfeldii and are distributed globally. CIs have been reported in algal samples from Scottish waters and in shellfish from Norway and the French Atlantic coast [ 243 , 245 , 246 ]. Their mechanism of action is understood and relies on the inhibition of nicotinic acetylcholine receptors (nAChRs) [ 247 ].…”

Section: Mechanism Of Action and Toxicity: The Need For Predefined To...mentioning

confidence: 99%

Current Trends and New Challenges in Marine Phycotoxins

et al. 2022

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Marine phycotoxins are a multiplicity of bioactive compounds which are produced by microalgae and bioaccumulate in the marine food web. Phycotoxins affect the ecosystem, pose a threat to human health, and have important economic effects on aquaculture and tourism worldwide. However, human health and food safety have been the primary concerns when considering the impacts of phycotoxins. Phycotoxins toxicity information, often used to set regulatory limits for these toxins in shellfish, lacks traceability of toxicity values highlighting the need for predefined toxicological criteria. Toxicity data together with adequate detection methods for monitoring procedures are crucial to protect human health. However, despite technological advances, there are still methodological uncertainties and high demand for universal phycotoxin detectors. This review focuses on these topics, including uncertainties of climate change, providing an overview of the current information as well as future perspectives.

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Method performance verification for the combined detection and quantitation of the marine neurotoxins cyclic imines and brevetoxin shellfish metabolites in mussels (Mytilus edulis) and oysters (Crassostrea gigas) by UHPLC-MS/MS

Cited by 11 publications

References 71 publications

Development of a Fast Liquid Chromatography Coupled to Mass Spectrometry Method (LC-MS/MS) to Determine Fourteen Lipophilic Shellfish Toxins Based on Fused–Core Technology: In-House Validation

Development of a Fast Liquid Chromatography Coupled to Mass Spectrometry Method (LC-MS/MS) to Determine Fourteen Lipophilic Shellfish Toxins Based on Fused–Core Technology: In-House Validation

Gambierone and Sodium Channel Specific Bioactivity Are Associated with the Extracellular Metabolite Pool of the Marine Dinoflagellate Coolia palmyrensis

Current Trends and New Challenges in Marine Phycotoxins

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