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

Hester J. van den Top (1) , Arjen Gerssen (1) , Pearse Mccarron (2) , Hans van Egmond (3)

1 RIKILT Institute of Food Safety, Wageningen UR
2 Institute for Marine Biosciences
3 RIKILT Institute of Food Safety, Wageningen UR,

Thirteen laboratories participated in an interlaboratory 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 done 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 for 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.

Mots clés: Life Sciences

Hester J. van den Top, Arjen Gerssen, Pearse Mccarron, Hans van Egmond. Quantitative determination of marine lipophilic toxins in mussels, oysters and cockles using liquid chromatography - mass spectrometry. Interlaboratory validation study. Food Additives and Contaminants, 2011, pp.1. ⟨10.1080/19440049.2011.608382⟩. ⟨hal-00741567⟩