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A mussel tissue certified reference material for multiple phycotoxins. Part 3: homogeneity and stability
McCarron, P.; Emteborg, H.; Giddings, S.; Wright, E.; Quilliam, M. (2011). A mussel tissue certified reference material for multiple phycotoxins. Part 3: homogeneity and stability. Anal. Bioanal. Chem. 400(3): 847-858.
In: Analytical and Bioanalytical Chemistry. Springer: Heidelberg. ISSN 1618-2642; e-ISSN 1618-2650, more
Peer reviewed article  

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Author keywords
    Shellfish toxins; Phycotoxins; CRM-FDMT1; Stability; Homogeneity; LC-MS;HPLC

Authors  Top 
  • McCarron, P.
  • Emteborg, H., more
  • Giddings, S.
  • Wright, E.
  • Quilliam, M.

    A candidate certified reference material (CRM) for multiple shellfish toxins (domoic acid, okadaic acid and dinophysistoxins, pectenotoxins, yessotoxin, azaspiracids and spirolides) has been prepared as a freeze-dried powder from mussel tissues (Mytilus edulis). Along with the certified values, the most important characteristics for a reference material to be fit-for-purpose are homogeneity and stability. Acceptable between-bottle homogeneity was found for this CRM. Within-bottle homogeneity was assessed using domoic acid, and it was shown that repeated subsampling of the CRM can be performed precisely down to 0.35 g. Both short- and long-term stability studies carried out under isochronous conditions demonstrated excellent stability of the various toxins present in the material. While degradation of some analytes was observed at +60°C in short-term studies, it was determined that shipping at ambient temperature is adequate. No instability was detected in long-term stability studies, and it was shown that the material can be held at +18°C safely for up to 1 year. To guarantee stability of the CRM over its lifetime the stock will be maintained at -20°C. The results of the homogeneity and stability testing show that CRM–FDMT1 is appropriate for its intended use in quality assurance and quality control of shellfish toxin analysis methods.

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