title: The preparation of certified calibration solutions for azaspiracid-1, -2, and -3, potent marine biotoxins found in shellfish.
abstract: The production and certification of a series of azaspiracid (AZA) calibration solution reference materials is described. Azaspiracids were isolated from contaminated mussels, purified by preparative liquid chromatography and dried under vacuum to the anhydrous form. The purity was assessed by liquid chromatography-mass spectrometry and nuclear magnetic resonance spectroscopy. The final concentration of each AZA in a CD(3)OH stock solution was determined by quantitative NMR spectroscopy. This solution was then diluted very accurately in degassed, high purity methanol to a concentration of 1.47 ± 0.08 μmol/L for CRM-AZA1, 1.52 ± 0.05 μmol/L for CRM-AZA2, and 1.37 ± 0.13 μmol/L for CRM-AZA3. Aliquots were dispensed into argon-filled glass ampoules, which were immediately flame-sealed. The calibration solutions are suitable for method development, method validation, calibration of liquid chromatography or mass spectrometry instrumentation and quality control of shellfish monitoring programs.
authors.affiliation: National Research Council of Canada, Institute for Marine Biosciences, 1411 Oxford Street, Halifax, Nova Scotia B3H 3Z1, Canada.
authors.forename: Ruth A
authors.initials: RA
authors.lastname: Perez
authors.forename: Nils
authors.initials: N
authors.lastname: Rehmann
authors.forename: Sheila
authors.initials: S
authors.lastname: Crain
authors.forename: Patricia
authors.initials: P
authors.lastname: LeBlanc
authors.forename: Cheryl
authors.initials: C
authors.lastname: Craft
authors.forename: Shawna
authors.initials: S
authors.lastname: MacKinnon
authors.forename: Kelley
authors.initials: K
authors.lastname: Reeves
authors.forename: Ian W
authors.initials: IW
authors.lastname: Burton
authors.forename: John A
authors.initials: JA
authors.lastname: Walter
authors.forename: Philipp
authors.initials: P
authors.lastname: Hess
authors.forename: Michael A
authors.initials: MA
authors.lastname: Quilliam
authors.forename: Jeremy E
authors.initials: JE
authors.lastname: Melanson
mesh_terms: D000818:Animals; D049872:Bivalvia / Q000737:chemistry; D005663:Furans / Q000032:analysis*; D009682:Magnetic Resonance Spectroscopy; D008387:Marine Toxins / Q000032:analysis*; D013058:Mass Spectrometry; D015394:Molecular Structure; D011714:Pyrans / Q000032:analysis*; D012758:Shellfish; D012996:Solutions / Q000737:chemistry; D013141:Spiro Compounds / Q000032:analysis*; D000095702:Polyether Toxins
chemical_list: D005663:Furans; D008387:Marine Toxins; D011714:Pyrans; D012996:Solutions; D013141:Spiro Compounds; C406592:azaspiracid; D000095702:Polyether Toxins; C520447:azaspiracid-2; C520446:azaspiracid-3