A mussel tissue certified reference material for multiple phycotoxins. Part 1: design and preparation |
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Authors: | McCarron Pearse Emteborg Håkan Nulty Cíara Rundberget Thomas Loader Jared I Teipel Katharina Miles Christopher O Quilliam Michael A Hess Philipp |
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Institution: | (1) National Research Council Canada, Institute for Marine Biosciences, 1411 Oxford St, Halifax, NS, B3H 3Z1, Canada;(2) Marine Institute, Rinville, Oranmore, Galway, Ireland;(3) European Commission, Joint Research Centre, Institute for Reference Materials and Measurements, Retieseweg 111, 2440 Geel, Belgium;(4) National Veterinary Institute, P.O. Box 750 Sentrum, 0106 Oslo, Norway;(5) AgResearch Ltd., Private Bag 3123, Hamilton, 3240, New Zealand;(6) Present address: FDA Gulf Coast Seafood Laboratory, 1 Iberville Street, Dauphin Island, AL 36528, USA;(7) Present address: Ifremer, Rue de l’?le d’Yeu, Nantes, 44311 Nantes Cedex 03, France |
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Abstract: | The development of multi-analyte methods for lipophilic shellfish toxins based on liquid chromatography–mass spectrometry
permits rapid screening and analysis of samples for a wide variety of toxins in a single run. Validated methods and appropriate
certified reference materials (CRMs) are required to ensure accuracy of results. CRMs are essential for accurate instrument
calibration, for assessing the complete analytical method from sample extraction to data analysis and for verifying trueness.
However, CRMs have hitherto only been available for single toxin groups. Production of a CRM containing six major toxin groups
was achieved through an international collaboration. Preparation of this material, CRM-FDMT1, drew on information from earlier
studies as well as improved methods for isolation of toxins, handling bulk tissues and production of reference materials.
Previous investigations of stabilisation techniques indicated freeze-drying to be a suitable procedure for preparation of
shellfish toxin reference materials and applicable to a wide range of toxins. CRM-FDMT1 was initially prepared as a bulk wet
tissue homogenate containing domoic acid, okadaic acid, dinophysistoxins, azaspiracids, pectenotoxin-2, yessotoxin and 13-desmethylspirolide
C. The homogenate was then freeze-dried, milled and bottled in aliquots suitable for distribution and analysis. The moisture
content and particle size distribution were measured, and determined to be appropriate. A preliminary toxin analysis of the
final material showed a comprehensive toxin profile. |
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