Abstract

The occurrence of marine harmful algae is increasing worldwide and, therefore, the accumulation of lipophilic marine toxins from harmful phytoplankton represents a food safety threat in the shellfish industry. Galicia, which is a commercially important EU producer of edible bivalve mollusk have been subjected to recurring cases of mussel farm closures, in the last decades. This work aimed to study the toxic profile of commercial mussels (Mytilus galloprovincialis) in order to establish a potential risk when ingested. For this, a total of 41 samples of mussels farmed in 3 Rías (Ares-Sada, Arousa, and Pontevedra) and purchased in 5 local markets were analyzed by liquid chromatography tandem mass spectrometry (LC–MS/MS). Chromatograms showed the presence of okadaic acid (OA), dinophysistoxin-2 (DTX-2), pectenotoxin-2 (PTX-2), azaspiracid-2 (AZA-2), and the emerging toxins 13-desmethyl spirolide C (SPX-13), and pinnatoxin-G (PnTX-G). Quantification of each toxin was determined using their own standard calibration in the range 0.1%–50 ng/mL (R2 > 0.99) and by considering the toxin recovery (62–110%) and the matrix correction (33–211%). Data showed that OA and DTX-2 (especially in the form of esters) are the main risk in Galician mollusks, which was detected in 38 samples (93%) and 3 of them exceeded the legal limit (160 µg/kg), followed by SPX-13 that was detected in 19 samples (46%) in quantities of up to 28.9 µg/kg. Analysis from PTX-2, AZA-2, and PnTX-G showed smaller amounts. Fifteen samples (37%) were positive for PTX-2 (0.7–2.9 µg/kg), 12 samples (29%) for AZA-2 (0.1–1.8 µg/kg), and PnTX-G was detected in 5 mussel samples (12%) (0.4 µg/kg–0.9 µg/kg). This is the first time Galician mollusk was contaminated with PnTX-G. Despite results indicating that this toxin was not a potential risk through the mussel ingestion, it should be considered in the shellfish safety monitoring programs through the LC–MS/MS methods.

Highlights

  • Marine phycotoxins are produced by harmful microalgae that bioaccumulate in the marine food chain [1]

  • Data showed that okadaic acid (OA) and DTX-2 are the main risk in Galician mollusks, which was detected in 38 samples (93%) and 3 of them exceeded the legal limit (160 μg/kg), followed by SPX-13 that was detected in 19 samples (46%)

  • The occurrence of lipophilic marine toxins from harmful phytoplankton are of growing concern for the Galicia region, both in terms of food safety and economic approaches

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Summary

Introduction

Marine phycotoxins are produced by harmful microalgae that bioaccumulate in the marine food chain [1]. They are of growing concern for the exploitation of marine living resources in many coastal areas. Every year there are almost 2000 cases of human intoxication due to the consumption of shellfish or fish with 15% mortality [1]. These toxic compounds constitute a threat to environment and human health and restrict the progress of aquaculture, which is one of the fastest growing food sectors in the world. The Galician farm areas (Rías) are coastal inlets formed by the sinking of riverbeds that extend from east to west like small fiords

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