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The preparation of certified calibration solutions for azaspiracid-1, -2, and -3, potent marine biotoxins found in shellfish |
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| Authors: | Ruth A Perez Nils Rehmann Sheila Crain Patricia LeBlanc Cheryl Craft Shawna MacKinnon Kelley Reeves Ian W Burton John A Walter Philipp Hess Michael A Quilliam Jeremy E Melanson |
| Institution: | 1. National Research Council of Canada, Institute for Marine Biosciences, 1411 Oxford Street, Halifax, Nova Scotia, B3H 3Z1, Canada 2. Marine Institute, Rinville, Oranmore, Co., Galway, Ireland 3. Research and Productivity Council of New Brunswick, 921 College Hill Rd., Fredericton, NB, E3B 6Z9, Canada 4. Ifremer, Centre de Nantes, Département Environnement Microbiologie et Phycotoxines, Rue de l’Ile d’Yeu, 44311, Nantes, Cedex 03, France |
| 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 CD3OH 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. |
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