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Refinement and in-house validation of the AOAC HPLC method (2005.06): the determination of paralytic shelfish poisoning toxins by liquid chromatography and fluorescence detection

Project Code: ZB1803

14/12/2010

The Association of Official Analytical Chemists (AOAC) HPLC method 2005.06 has recently been approved as an Official Method by the European Commission for the detection and quantitation of a number of paralytic shellfish poisoning (PSP) toxins in certain harvested shellfish products. The method describes the analysis of the acetic acid extracts of shellfish homogenates after clean up, fractionation and pre-column oxidation of PSP toxins with periodate and peroxide oxidants. The method consists of two parts, a screening step to qualitatively analyse for the presence of PSP toxins, and a fully quantitative step whereby the concentrations of individual toxin and total PSP toxicity are determined. The AOAC 2005.06 method was subjected to a single laboratory validation scheme conducted at the Cefas laboratory between March and November 2007 for common mussels (Mytilus edulis). As part of the validation scheme, parallel testing was performed whereby a number of shellfish acquired under the OC monitoring programmes were analysed by both MBA and AOAC HPLC methodologies. Validation was conducted for the PSP toxins specified in the AOAC 2005.06 method and which are currently available as certified reference standards (National Research Council, Canada (NRCC)). The following toxins were included; the N-hydroxylated toxins (neosaxitoxin (NEO) and gonyautoxins (GTX) 1 and 4 together (GTX1,4), and the non N-hydroxylated toxins saxitoxin (STX), gonyautoxins (GTX) 2 and 3 together (GTX2,3), and 5 (GTX5), decarbamoyl saxitoxin (dcSTX) and N-sulfocarbamoyl toxins C1 and C2 (C1,2)). Additionally, the validation was extended to the non N-hydroxylated arbamoylgonyautoxin-2 and 3 (dcGTX2,3) and the N-hydroxylated decarbamoylneosaxitoxin (dcNEO), not covered by the AOAC method but both recently made available as certified reference standards. The work followed on from an earlier validation exercise of an HPLC screening method.

Overall, the results presented show the validated HPLC method is safe to be implemented for mussels, but may result in greater analytical costs for routine analysis.

The Final Report below can also be found at: http://www.food.gov.uk/multimedia/pdfs/aoachplc.pdf

See also the related report ZB1807: Validation of HPLC method for scallops, clams and razors, and Pacific and Native oysters, at:

http://www.foodbase.org.uk/results.php?f_category_id=&f_report_id=612

Final report

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