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An interlaboratory study was conducted for the determination of paralytic shellfish poisoning (PSP) toxins in shellfish. The method used liquid chromatography with fluorescence detection after prechromatographic oxidation of the toxins with hydrogen peroxide and periodate. The PSP toxins studied were saxitoxin (STX), neosaxitoxin (NEO), gonyautoxins 2 and 3 (GTX2,3 together), gonyautoxins 1 and 4 (GTX1,4 together), decarbamoyl saxitoxin (dcSTX), B-1 (GTX5), C-1 and C-2 (C1,2 together), and C-3 and C-4 (C3,4 together). B-2 (GTX6) toxin was also included, but for qualitative identification only. Samples of mussels, both blank and naturally contaminated, were mixed and homogenized to provide a variety of PSP toxin mixtures and concentration levels. The same procedure was followed with samples of clams, oysters, and scallops. Twenty-one samples in total were sent to 21 collaborators who agreed to participate in the study. Results were obtained from 18 laboratories representing 14 different countries.

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SummaryIn this paperwe report results obtained from analysis of domoic acid and its analogues, toxins responsible for incidents of amnesic shellfish poisoning (ASP) in several places world-wide, by use of liquid chromatography coupled with electrospray ionization mass spectrometry. Different chromatographic and mass spectrometry conditions were evaluated with the aim of achieving the best chromatographic performance combined with the optimum mass spectrometric response. From the results obtained it can be concluded that LC-MS is powerful tool for the selective and sensitive determination of domoic acid and its isomers in naturally contaminated samples.In this paper we report work performed to optimize liquid chromatography coupled with electrospray ionization mass spectrometry for the analysis of ASP toxins, with the aim of achieving the highest chromatographic resolution combined with optimum mass spectrometric response. Different conditions, focusing especially on mobile-phase composition and different mass spectrometric settings such as nebulizer pressure, drying gas temperature, capillary voltage, drying gas flow, and fragmentor voltage, were evaluated to find the optimum conditions for LC-MS analysis. These optimized conditions were then used to calibrate the LC-MS system for application to the analysis of shellfish extracts naturally contaminated with ASP toxins.