Ultrahigh-Performance Hydrophilic Interaction Liquid Chromatography with Tandem Mass Spectrometry Method for the Determination of Paralytic Shellfish Toxins and Tetrodotoxin in Mussels, Oysters, Clams, Cockles, and Scallops: Collaborative Study

Turner, Andrew D.; Dhanji‐Rapkova, Monika; Fong, Sum Y T; Hungerford, James M.; McNabb, Paul; Boundy, Michael J.; Harwood, D. Tim; Aanrud, S; Alfonso, Carmen; Alvarez, M. J. Moreno; Amzil, Zouher; Antelo, Álvaro; Arévalo, Fabiola; Barrera, M; Braekevelt, E; Bunæs, J; Cagide, Eva; Cangini, Monica; Carrasco, Daniel E.; Casey, Melanie; Chan, P; Faulkner, Dorothea; Gago-Martı́nez, Ana; Gibbs, Ryan; Hatfield, Robert G.; Hayman, Colin M.; Hiroshi, Onuma; Hort, Vincent; Hutchinson, Joseph P.; Jordan, Timothy B.; Mariappan, Meena; Leão, José Manuel; Maskrey, Benjamin H.; McCarron, Pearse; McGrath, Sara C.; Milandri, Anna; Milandri, S.; Moroño, Á.; Murray, Shauna A.; Nicolas, Marina; Queijo, A; Pompei, Marinella; Réveillon, D; Rourke, Wade A; Salgado, C.; Savar, Véronique; Stokes, Brian J.; Suárez‐Isla, Benjamin A.; Suzuki, Tadanao; Thomas, Krista; Watanabe, Ryuichi

doi:10.5740/jaoacint.19-0240

Cited by 63 publications

(54 citation statements)

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“…Since for both these methods, the concentration factor associated with sample preparation was similar to our method, the difference in sensitivity is due to the performance of the instruments used. An inter-laboratory validation of the HILIC-MS/MS method for the analysis of toxins belonging to the saxitoxin group (PSP), and of TTX in bivalve molluscs, conducted by Turner et al, demonstrated the wide range of sensitivity of MS instrument models [23]. The system used in the present work was classified in the "medium sensitivity" group, whereas the instruments used the above-mentioned studies belonged to the "high sensitivity" group.…”

Section: Discussionmentioning

confidence: 65%

“…For bivalve molluscs, recoveries ranged from 99 to 108%. To the best of our knowledge, the trueness of this method is the best among all in-house-validated procedures [8,16,20,21,23,24]. For gastropods, recoveries ranged from 74 to 80%.…”

Section: Discussionmentioning

confidence: 95%

“…Additional chromatographic methods were necessary for column cleaning, equilibration and storage. These methods are fully described in references [19,20,23,47]. In the present study, 2 µL were injected into the system.…”

Section: Liquid Chromatography Conditionsmentioning

confidence: 99%

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First Detection of Tetrodotoxin in Bivalves and Gastropods from the French Mainland Coasts

Hort

Arnich

Guérin

et al. 2020

Toxins

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In 2015, tetrodotoxins (TTXs) were considered a potential threat in Europe since several studies had shown the presence of these toxins in European bivalve molluscs. In this study, we investigated the occurrence of TTXs in 127 bivalve samples (mussels and oysters) and in 66 gastropod samples (whelks) collected all along the French mainland coasts in 2017 and 2018. Analyses were carried out after optimization and in-house validation of a performing hydrophilic interaction liquid chromatography associated with tandem mass spectrometry (HILIC-MS/MS) method. The concentration set by European Food Safety Authority (EFSA) not expected to result in adverse effects (44 µg TTX equivalent/kg) was never exceeded, but TTX was detected in three mussel samples and one whelk sample (1.7–11.2 µg/kg). The tissue distribution of TTX in this whelk sample showed higher concentrations in the digestive gland, stomach and gonads (7.4 µg TTX/kg) than in the rest of the whelk tissues (below the limit of detection of 1.7 µg TTX/kg). This is the first study to report the detection of TTX in French molluscs.

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Section: Discussionmentioning

confidence: 65%

Section: Discussionmentioning

confidence: 95%

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First Detection of Tetrodotoxin in Bivalves and Gastropods from the French Mainland Coasts

Hort

Arnich

Guérin

et al. 2020

Toxins

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“…The presence of toxins in benthic invertebrates that may be washed ashore has societal implications, with beach scavenged crabs and starfish implicated in recent canine deaths [ 42 ]. Anecdotally A. diaphanum was found among the stomach contents of a dog that had died following a beach walk in 2005 (pers.comm [ 114 ]) and implicated in multiple dog deaths in 2006 [ 115 ], however, in neither case were PSTs tested for and no archived samples were stored for retrospective analysis. Consequently, further studies on the spatial, temporal and taxonomic patterns in toxins in benthic invertebrates, especially those that are known to be washed ashore after periods of disturbance, could usefully be undertaken.…”

Section: Discussionmentioning

confidence: 99%

Multiple New Paralytic Shellfish Toxin Vectors in Offshore North Sea Benthos, a Deep Secret Exposed

et al. 2020

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In early 2018, a large easterly storm hit the East Anglian coast of the UK, colloquially known as the ‘Beast from the East’, which also resulted in mass strandings of benthic organisms. There were subsequent instances of dogs consuming such organisms, leading to illness and, in some cases, fatalities. Epidemiological investigations identified paralytic shellfish toxins (PSTs) as the cause, with toxins present in a range of species and concentrations exceeding 14,000 µg STX eq./kg in the sunstar Crossaster papposus. This study sought to better elucidate the geographic spread of any toxicity and identify any key organisms of concern. During the summers of 2018 and 2019, various species of benthic invertebrates were collected from demersal trawl surveys conducted across a variety of locations in the North Sea. An analysis of the benthic epifauna using two independent PST testing methods identified a ‘hot spot’ of toxic organisms in the Southern Bight, with a mean toxicity of 449 µg STX eq./kg. PSTs were quantified in sea chervil (Alcyonidium diaphanum), the first known detection in the phylum bryozoan, as well as eleven other new vectors (>50 µg STX eq./kg), namely the opisthobranch Scaphander lignarius, the starfish Anseropoda placenta, Asterias rubens, Luidia ciliaris, Astropecten irregularis and Stichastrella rosea, the brittlestar Ophiura ophiura, the crustaceans Atelecyclus rotundatus and Munida rugosa, the sea mouse Aphrodita aculeata, and the sea urchin Psammechinus miliaris. The two species that showed consistently high PST concentrations were C. papposus and A. diaphanum. Two toxic profiles were identified, with one dominated by dcSTX (decarbamoylsaxitoxin) associated with the majority of samples across the whole sampling region. The second profile occurred only in North-Eastern England and consisted of mostly STX (Saxitoxin) and GTX2 (gonyautoxin 2). Consequently, this study highlights widespread and variable levels of PSTs in the marine benthos, together with the first evidence for toxicity in a large number of new species. These findings highlight impacts to ‘One Health’, with the unexpected sources of toxins potentially creating risks to animal, human and environmental health, with further work required to assess the severity and geographical/temporal extent of these impacts.

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“…Multiple methods for PSTs have been utilized in recent decades, namely, the mouse bioassay (Association of Official Analytical Chemists (AOAC) method 959.08), the receptor binding assay (AOAC method 2011.27) [55], the pre-column (AOAC method 2005.06) [56] and post-column (AOAC method 2011.02) [57] AOAC certified methods for PSTs, and the internationally validated LC-MS/MS method [58], as well as other mass spectrometric methods reported in the literature [59]; multiple ELISAs for both neosaxitoxin and STX PST analogs have also been developed [60].…”

Section: Introductionmentioning

confidence: 99%

Limnological Differences in a Two-Basin Lake Help to Explain the Occurrence of Anatoxin-a, Paralytic Shellfish Poisoning Toxins, and Microcystins

Smith

Conroe²,

Schulz

et al. 2020

Toxins

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Chautauqua Lake, New York, is a two-basin lake with a deeper, cooler, and less nutrient-rich Northern Basin, and a warmer, shallower, nutrient-replete Southern Basin. The lake is populated by a complex mixture of cyanobacteria, with toxigenic strains that produce microcystins, anatoxins, and paralytic shellfish poisoning toxins (PSTs). Samples collected from 24 sites were analyzed for these three toxin classes over four years spanning 2014–2017. Concentrations of the three toxin groups varied widely both within and between years. During the study, the mean and median concentrations of microcystins, anatoxin-a, and PSTs were 91 and 4.0 μg/L, 0.62 and 0.33 μg/L, and 32 and 16 μg/L, respectively. Dihydro-anatoxin was only detected once in Chautauqua Lake, while homo-anatoxin was never detected. The Northern Basin had larger basin-wide higher biomass blooms with higher concentrations of toxins relative to the more eutrophied Southern Basin, however blooms in the North Basin were infrequent. Chlorophyll concentrations and toxins in the two basins were correlated with different sets of environmental and physical parameters, suggesting that implementing controls to reduce toxin loads may require applications focused on more than reductions in cyanobacterial bloom density (e.g., reduction of phosphorus inputs), and that lake limnological factors and morphology are important determinants in the selection of an appropriate management strategy. Chautauqua Lake is a drinking water source and is also heavily used for recreation. Drinking water from Chautauqua Lake is unlikely to be a significant source of exposure to cyanotoxins due to the location of the intakes in the deeper North Basin, where there were generally low concentrations of toxins in open water; however, toxin levels in many blooms exceeded the US Environmental Protection Agency’s recreational guidelines for exposure to cyanotoxins. Current cyanotoxin monitoring in Chautauqua Lake is focused on microcystins. However, the occurrence of blooms containing neurotoxic cyanotoxins in the absence of the microcystins indicates this restricted monitoring may not be sufficient when aiming to protect against exposure to cyanotoxins. The lake has a large number of tourist visitors; thus, special care should be taken to prevent recreational exposure within this group.

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Ultrahigh-Performance Hydrophilic Interaction Liquid Chromatography with Tandem Mass Spectrometry Method for the Determination of Paralytic Shellfish Toxins and Tetrodotoxin in Mussels, Oysters, Clams, Cockles, and Scallops: Collaborative Study

Cited by 63 publications

References 1 publication

First Detection of Tetrodotoxin in Bivalves and Gastropods from the French Mainland Coasts

First Detection of Tetrodotoxin in Bivalves and Gastropods from the French Mainland Coasts

Multiple New Paralytic Shellfish Toxin Vectors in Offshore North Sea Benthos, a Deep Secret Exposed

Limnological Differences in a Two-Basin Lake Help to Explain the Occurrence of Anatoxin-a, Paralytic Shellfish Poisoning Toxins, and Microcystins

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