Detection of Cyclic Imine Toxins in Dietary Supplements of Green Lipped Mussels (Perna canaliculus) and in Shellfish Mytilus chilensis.

Paz Otero,M Carmen Louzao,Carmen Vale,Luis M Botana,Andrea Boente-Juncal,Celia Costas

doi:10.3390/toxins12100613

Abstract

Seafood represents a significant part of the human staple diet. In the recent years, the identification of emerging lipophilic marine toxins has increased, leading to the potential for consumers to be intoxicated by these toxins. In the present work, we investigate the presence of lipophilic marine toxins (both regulated and emerging) in commercial seafood products from non-European locations, including mussels Mytilus chilensis from Chile, clams Tawerea gayi and Metetrix lyrate from the Southeast Pacific and Vietnam, and food supplements based on mussels formulations of Perna canaliculus from New Zealand. All these products were purchased from European Union markets and they were analyzed by UPLC-MS/MS. Results showed the presence of the emerging pinnatoxin-G in mussels Mytilus chilensis at levels up to 5.2 µg/kg and azaspiracid-2 and pectenotoxin-2 in clams Tawera gayi up to 4.33 µg/kg and 10.88 µg/kg, respectively. This study confirms the presence of pinnatoxins in Chile, one of the major mussel producers worldwide. Chromatograms showed the presence of 13-desmethyl spirolide C in dietary supplements in the range of 33.2–97.9 µg/kg after an extraction with water and methanol from 0.39 g of the green lipped mussels powder. As far as we know, this constitutes the first time that an emerging cyclic imine toxin in dietary supplements is reported. Identifying new matrix, locations, and understanding emerging toxin distribution area are important for preventing the risks of spreading and contamination linked to these compounds.

Highlights

Lipophilic marine toxins in mollusc constitute an important threat to human health and high number of intoxications occur every year [1]
We investigate the presence of lipophilic marine toxins in both, molluscs from non-European Union (EU) locations (New Zealand, Chile, SouthEast Pacific, and Vietnam) but commercialized in Europe and marine food supplements
The availability of certified reference standard pinnatoxin G (PnTX-G) has allowed it to be included in the EU-Harmonized Standard Operating Procedure (SOP) together with SPXs and the other toxins currently legislated

Summary

Introduction

Lipophilic marine toxins in mollusc constitute an important threat to human health and high number of intoxications occur every year [1]. The legislated group of lipophilic marine toxins includes four different chemical groups: yessotoxins (YTXs) azaspiracids (AZAs), pectenotoxins (PTXs), and okadaic acid (OA) and its derivatives, the dinophysistoxins (DTXs). When LC-MS methodology is used, the concentration in a sample has to be referred to a predominant toxin of the group, named the reference compound (RC) and using the toxicity equivalency factors (TEFs) values for the other analogues from the same group [2,3]. Several countries have proposed limits in molluscs for some lipophilic toxins, for example, in the European Union (EU), levels in shellfish for human consumption have to be below 3.75 mg eq YTX/kg, 0.16 mg eq AZA, and 0.16 mg eq OA/Kg (for the OA and PTX toxin group) [4,5]. Until 2013, all official determinations were performed through in vivo assays, but after that year, the analysis by LC-MS/MS were progressively increasing, according to the legislation

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Results

Conclusion