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Title: The preparation of certified calibration solutions for azaspiracid-1, -2, and -3, potent marine biotoxins found in shellfish
Authors: Perez, R
Rehmann, N
Crain, S
LeBlanc, P
Craft, C
MacKinnon, S
Reeves, K
Burton, I W
Walter, J A
Hess, P
Quilliam, M A
Melanson, J E
Keywords: Reference materials
Mass spectrometry/LC-MS
Marine Toxins
Issue Date: 2010
Publisher: Springer Verlag
Citation: Perez, R., Rehmann, N., Crain, S., LeBlanc, P., Craft, C., MacKinnon, S., Reeves, K., Burton, I. W., Walter, J. A., Hess, P., Quiliam, M. A., Melanson, J. E. The preparation of certified calibration solutions for azaspiracid-1, -2, and -3, potent marine biotoxins found in shellfish. Anal. Bioanal. Chem. (2010) 398: 2243-2252
Series/Report no.: Analytical and Bioanalytical Chemistry;398 (5)
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. Purity was assessed by liquid chromatography–mass spectrometry (LC-MS) and nuclear magnetic resonance (NMR) spectroscopy. Final concentration of each AZA in a CD3OH stock solution was determined accurately 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 AZA1, 1.52 ± 0.05 μmol/L for AZA2, and 1.37 ± 0.13 μmol/L for 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.
Description: The original publication is available at
ISSN: 1618-2642
Appears in Collections:Peer Reviewed Scientific Papers

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