Liquid chromatography with mass spectrometry: Detection of lipophilic shellfish toxins

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TypeArticle
Journal titleJournal of Association of Official Analytical Chemists
Volume88
Issue5
Pages13711382; # of pages: 12
Subjectliquid chromatography; mass spectrometry; shellfish toxins
AbstractA rapid multiple toxin method based on liquid chromatography with mass spectrometry (LC/MS) was developed for the detection of okadaic acid (OA), dinophysistoxin-1 (DTX-1), DTX-2, yessotoxin (YTX), homoYTX, 45-hydroxy-YTX, 45-hydroxyhomo-YTX, pectenotoxin-1 (PTX-1), PTX-2, azaspiracid-1 (AZA-1), AZA-2, and AZA-3. Toxins were extracted from shellfish using methanol–water (80%, v/v) and were analyzed using a C8 reversed-phase column with a 5 mM ammonium acetate–acetonitrile mobile phase under gradient conditions. The method was validated for the quantitative detection of OA, YTX, PTX-2, and AZA-1 in 4 species (mussels, Mytilus edulis; cockles, Cerastoderma edule; oysters, Crassostrea gigas; king scallop, Pecten maximus) of shellfish obtained from United Kingdom (UK) waters. Matrix interferences in the determination of the toxins in these species were investigated. The validated linear range of the method was 13–250 µg/kg for OA, PTX-2, and AZA-1 and 100–400 µg/kg for YTX. Recovery and precision ranged between 72–120 and 1–22%, respectively, over a fortification range of 40–160 µg/kg for OA, PTX-2, and AZA-1 and 100–400 µg/kg for YTX. The limit of detection, reproducibility, and repeatability of analysis showed acceptable performance characteristics. A further LC/MS method using an alkaline hydrolysis step was assessed for the detection of OA, DTX-1, and DTX-2 in their esterified forms. In combination with the LC/MS multiple toxin method, this allows detection of all toxin groups described in Commission Decision 2002/225/EC.
Publication date
PublisherAOAC International
Copyright noticeCopyright © AOAC INTERNATIONAL 2007 All Rights Reserved
Linkhttp://www.atypon-link.com/AOAC/doi/pdf/10.5555/jaoi.2005.88.5.1371
http://www.atypon-link.com/AOAC/loi/jaoi
LanguageEnglish
AffiliationNRC Institute for Marine Biosciences; National Research Council Canada; Measurement Science and Standards
Peer reviewedYes
NRC number1674
NPARC number3538088
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Record identifierf46ee715-e923-438e-99ad-73c1a658ec9a
Record created2009-03-01
Record modified2016-05-09
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