The preparation of certified calibration solutions for azaspiracid-1, -2, and -3, potent marine biotoxins found in shellfish.
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.
Perez
Ruth A
RA
National Research Council of Canada, Institute for Marine Biosciences, 1411 Oxford Street, Halifax, Nova Scotia B3H 3Z1, Canada.
Rehmann
Nils
N
Crain
Sheila
S
LeBlanc
Patricia
P
Craft
Cheryl
C
MacKinnon
Shawna
S
Reeves
Kelley
K
Burton
Ian W
IW
Walter
John A
JA
Hess
Philipp
P
Quilliam
Michael A
MA
Melanson
Jeremy E
JE
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
D005663:Furans; D008387:Marine Toxins; D011714:Pyrans; D012996:Solutions; D013141:Spiro Compounds; C406592:azaspiracid; D000095702:Polyether Toxins; C520447:azaspiracid-2; C520446:azaspiracid-3