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Determination of Lipophilic Marine

Biotoxins in Molluscs by LC-MS/MS

using Offline Extraction

Francesca G. Bellagambi, Department of Chemistry and Industrial Chemistry, University of Pisa, Italy

Cláudia P. B. Martins, Thermo Fisher Scientific, Barcelona, Spain

Michal Godula, Thermo Fisher Scientific, Prague, Czech Republic

Alessio Ceccarini, Department of Chemistry and Industrial Chemistry, University of Pisa, Italy

Application Note 63552

Key Words

TSQ Quantum Ultra, Food Safety, Marine Biotoxins

Introduction

In recent years many countries have had to deal with the

consequences of toxic microalgal blooms in both marine

and fresh water, such as the deaths of wild animals and

domestic livestock.

Several cases of poisoning in humans have been associated

with the direct consumption of shellfish, fish, or water

contaminated by algal toxins. People may also come into

contact with toxins during recreational activities along sea

coasts affected by episodes of algal blooms. Depending

on the type of toxin involved, there are forms of mild

and usually self-limiting symptoms, characterized by

gastrointestinal disorders or allergic-like episodes. Much

more severe symptoms of the neurological type can lead

to death.

The foods most frequently involved in episodes of

human poisoning are represented by bivalve molluscs.

These shellfish can accumulate and concentrate any

biotoxins present in the plankton they ingest through

filtering large quantities of water for trophical reasons.

It is not possible to evaluate shellfish edibility by an

organoleptic examination alone. While human ingestion

of contaminated food with biotoxins can lead to the

onset of different clinical symptoms, in shellfish it usually

has only marginal effects. An important risk factor lies

in the thermostability of such molecules which are not

completely inactivated by common physical treatments for

fish products (cooking, smoking, salting, freezing, housing),

but remain virtually unchanged in the finished product.

There are a series of regulations issued by the European

Union (EU) that relate to marine biotoxins. One is

Regulation (EC) No 853/2004 which concerns the

control of lipophilic toxins, establishing maximum levels

for lipophilic toxins in bivalve molluscs destined for

human consumption:

1

For okadaic acid, dinophysistoxins, and pectenotoxins

together – 160 micrograms of okadaic acid equivalents

per kilogram

For yessotoxin – 1 milligram of yessotoxin equivalent

per kilogram

For azaspiracids – 160 micrograms of azaspiracid

equivalents per kilogram