Abstract

When considering the geographical expansion of marine toxins, the emergence of new toxins and the associated risk for human health, there is urgent need for versatile and efficient analytical methods that are able to detect a range, as wide as possible, of known or emerging toxins. Current detection methods for marine toxins rely on a priori defined target lists of toxins and are generally inappropriate for the detection and identification of emerging compounds. The authors describe the implementation of a recent approach for the non-targeted analysis of marine toxins in shellfish with a focus on a comprehensive workflow for the acquisition and treatment of the data generated after liquid chromatography coupled with high resolution mass spectrometry (LC-HRMS) analysis. First, the study was carried out in targeted mode to assess the performance of the method for known toxins with an extended range of polarities, including lipophilic toxins (okadaic acid, dinophysistoxins, azaspiracids, pectenotoxins, yessotoxins, cyclic imines, brevetoxins) and domoic acid. The targeted method, assessed for 14 toxins, shows good performance both in mussel and oyster extracts. The non-target potential of the method was then challenged via suspects and without a priori screening by blind analyzing mussel and oyster samples spiked with marine toxins. The data processing was optimized and successfully identified the toxins that were spiked in the blind samples.

Highlights

  • Marine toxins are natural compounds produced by certain microalgae that can contaminate a wide variety of marine species, including fish, crabs, or filter feeding bivalves, such as mussels, oysters, scallops, and clams [1]

  • To assess the potential of the LC-high resolution mass spectrometry (HRMS) method to detect marine toxins as part of a non-targeted analysis, the authors performed a proof of concept study as a first essential step toward a reliable characterization of samples naturally contaminated with unknown marine toxins and the identification of the toxins

  • Since there are no guidelines for the validation of a non-targeted method, the LC-HRMS

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Summary

Introduction

Marine toxins are natural compounds produced by certain microalgae that can contaminate a wide variety of marine species, including fish, crabs, or filter feeding bivalves (shellfish), such as mussels, oysters, scallops, and clams [1]. To protect human health from these toxigenic compounds and to avoid food poisoning, the presence of certain toxins in food destined for human consumption is regulated within the European Union (EU) [5,6] and is submitted to monitoring programs. These regulations clearly mention the toxins to monitor, the thresholds that should not be surpassed and the methods of analysis. To perform official monitoring of some toxins, such as saxitoxins and lipophilic toxins, chemical methods replace animal bioassays [8,9] This is the case of liquid chromatography coupled with mass spectrometry (LC-MS). Methods using high resolution mass spectrometry (HRMS) have been recently developed and used for the analysis of a larger panel of marine toxins in a single run [16,17,18]

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