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

Abstract

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

High resolution mass spectrometry for quantitative analysis and untargeted screening of algal toxins in mussels and passive samplers

“…Indeed, lower LoDs were expected for PTX2 in mussel compared to passive sampler, as the mussel matrix caused ion enhancement for PTX2. This was not the case, perhaps reflecting the high level of variability previously associated with this toxin [6,13]. With regard to regulatory levels for toxins, satisfactory detection limits were obtained on both low and high resolution mass spectrometers for methanol, mussel and SPATT matrices.…”

“…To achieve this goal, different studies have developed and validated quantitative methods for the analysis of phycotoxins, typically using low resolution mass spectrometry (LRMS) [4][5][6][7][8][9]. This technique is now being increasingly used for monitoring [10,11] and for characterization of reference materials [12,13].…”

Cyanobacterial Toxins of the Laurentian Great Lakes, Their Toxicological Effects, and Numerical Limits in Drinking Water

“…In particular, okadaic acid is associated with chronic diseases such as tumor production and cancer. Okadaic acid is a marine biotoxin produced by dinoflagellates and it accumulates in various host tissues including shellfish and sponges [175,176,177]. It is a tumor promoter and potent inhibitor of PP1/2A.…”

Generation of a panel of high affinity antibodies and development of a biosensor-based immunoassay for the detection of okadaic acid in shellfish

“…2074/2005. A number of alternative methods have already been proposed for the detection of OA and derivatives including liquid chromatography-mass spectrometry (LC-MS)-based analysis, which inter-laboratory validation study demonstrated its suitability as alternative detection method ( Van den Top et al, 2011), and a colorimetric protein phosphatase 2A (PP2A) assay was also demonstrated suitable as alternative method (Smienk et al, 2012(Smienk et al, , 2013. Immunoassays have also been developed for the detection of OA, such as ELISA-based assay developed by Kreuzer et al (1999), which relied on commercial antibodies.…”