title: A mussel tissue certified reference material for multiple phycotoxins. Part 1: design and preparation.
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.
authors.affiliation: National Research Council Canada, Institute for Marine Biosciences, Halifax, NS, Canada. pearse.mccarron@nrc-cnrc.gc.ca
authors.forename: Pearse
authors.initials: P
authors.lastname: McCarron
authors.forename: Håkan
authors.initials: H
authors.lastname: Emteborg
authors.forename: Cíara
authors.initials: C
authors.lastname: Nulty
authors.forename: Thomas
authors.initials: T
authors.lastname: Rundberget
authors.forename: Jared I
authors.initials: JI
authors.lastname: Loader
authors.forename: Katharina
authors.initials: K
authors.lastname: Teipel
authors.forename: Christopher O
authors.initials: CO
authors.lastname: Miles
authors.forename: Michael A
authors.initials: MA
authors.lastname: Quilliam
authors.forename: Philipp
authors.initials: P
authors.lastname: Hess
mesh_terms: D000818:Animals; D049872:Bivalvia / Q000737:chemistry*; D002853:Chromatography, Liquid / Q000592:standards; D005612:Freeze Drying; D008387:Marine Toxins / Q000032:analysis*; D013058:Mass Spectrometry / Q000592:standards*; D012015:Reference Standards
chemical_list: D008387:Marine Toxins