Liquid chromatographic post-column oxidation method for analysis of paralytic shellfish toxins in mussels, clams, scallops, and oysters : single-laboratory validation

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TypeArticle
Journal titleJournal of AOAC International
ISSN1060-3271
Volume92
Issue6
Pages16901704; # of pages: 15
AbstractA single-laboratory validation study was conducted for the LC post-column oxidation analysis of paralytic shellfish toxins (PST): saxitoxin (STX); neosaxitoxin (NEO); gonyautoxins (GTX)1-5; decarbamoyl gonyautoxins (dcGTX) 2 and 3; decarbamoyl saxitoxin (dcSTX); and N-sulfocarbamoyl-gonyautoxin-2 and 3 (C1 and C2) in mussels (Mytilus edulis), soft shell clams (Mya arenaria), scallops (Placopectin magellanicus), and oysters (Crassostrea virginicus). The instrumental technique was developed for the analysis of PST in shellfish as an alternative to the precolumn oxidation method, AOAC Official Method 2005.06, and a replacement for the current AOAC biological method 959.08. The method used reversed-phase LC with post-column oxidation and fluorescence detection. Test materials for method recovery were prepared by fortification of blank material with a cocktail of PST. Materials used to determine method repeatability and intermediate precision were prepared by blending blank material with naturally incurred material. The target total toxicity levels evaluated in the study were 0.40, 0.80, and 1.60 mg STX·diHCl equivalents per kilogram [(eq/kg) ½, 1, and 2 times the regulatory limit]. Linearity, recovery, and within-laboratory precision parameters of the method were evaluated. Correlation coefficients of the calibration curves for all toxins studied were >0.99. Total toxin recovery ranged from 94 to 106% at the three levels of interest. Repeatability and intermediate precision RSD ranged from 2 to 7% and 2 to 8%, respectively. The method LOD and LOQ (assuming the presence of all toxins) were determined to be equivalent to 0.18 and 0.39 mg STX·diHCl eq/kg. The method is intended for a regulatory framework and will be submitted for an AOAC collaborative study.
Publication date
Linkhttp://aoac.publisher.ingentaconnect.com/content/aoac/jaoac/2009/00000092/00000006/art00012
LanguageEnglish
AffiliationNational Research Council Canada; NRC Institute for Marine Biosciences
Peer reviewedYes
NRC number51730
NPARC number21268218
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Record identifier7b73da8f-beb4-4670-a061-e74094c7bba7
Record created2013-06-05
Record modified2016-05-09
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