Quantitative determination of marine lipophilic toxins in mussels, oysters and cockles using liquid chromatography-mass spectrometry : inter-laboratory validation study

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DOIResolve DOI: http://doi.org/10.1080/19440049.2011.608382
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TypeArticle
Journal titleFood Additives & Contaminants: Part A: Chemistry, Analysis, Control, Exposure & Risk Assessment
Volume28
Issue12
Pages17451757; # of pages: 13
SubjectLC/MS; inter-laboratory validation; phycotoxins; DSP; natural toxicants; seafood
AbstractThirteen laboratories participated in an inter-laboratory study to evaluate the method performance characteristics of a liquid chromatography-tandem mass spectrometric method (LC-MS/MS) for marine lipophilic shellfish toxins. Method performance characteristics were evaluated for mussel (Mytilus edulis), oyster (Crassostrea gigas) and cockle (Cerastoderma edule) matrices. The specific toxin analogues tested included okadaic acid (OA), dinophysistoxins-1 and -2 (DTX1, -2), azaspiracids-1, -2 and -3 (AZA1, -2, -3), pectenotoxin-2 (PTX2), yessotoxin (YTX), and 45-OH-yessotoxin (45-OH-YTX). The instrumental technique was developed as an alternative to the still widely applied biological methods (mouse or rat bioassay). Validation was conducted according to the AOAC-harmonised protocol for the design, conduct and interpretation of method-performance studies. Eight different test materials were sent as blind duplicates to the participating laboratories. Twelve laboratories returned results that were accepted to be included in the statistical evaluation. The method precision was expressed as HORRATs. For the individual toxins (except for 45-OH-YTX) HORRATs were found to be ≤1.8 (median HORRAT = 0.8) in all tested materials. The recoveries of OA-, AZA- and YTX-group toxins were within the range of 80-108% and PTX2 was within the range of 62-93%. Based on the acceptable values for precision and recovery, it was concluded that the method is suitable for official control purposes to quantitatively determine OA/DTXs, AZAs, YTXs and PTX2 in shellfish.
Publication date
LanguageEnglish
AffiliationNRC Institute for Marine Biosciences; National Research Council Canada
Peer reviewedYes
NPARC number19649679
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Record identifierec88984c-01a6-4baa-b44f-334c5a317253
Record created2012-04-02
Record modified2016-05-09
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