The preparation of certified calibration solutions for azaspiracid-1, -2, and -3, potent marine biotoxins found in shellfish
| Autor: | Philipp Hess, Kelley Reeves, Shawna L. MacKinnon, Sheila Crain, John A. Walter, Ian W. Burton, Michael A. Quilliam, Cheryl M. Craft, Jeremy E. Melanson, Nils Rehmann, Ruth A. Perez, Patricia LeBlanc |
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| Rok vydání: | 2010 |
| Předmět: |
Magnetic Resonance Spectroscopy
mytilus-edulis ved/biology.organism_classification_rank.species Mass spectrometry Azadinium spinosum 01 natural sciences Biochemistry Ampoule Mass Spectrometry Analytical Chemistry 03 medical and health sciences chemistry.chemical_compound analogs Azaspiracid tandem mass-spectrometry Animals Spiro Compounds 14. Life underwater uncertainty Furans crms 030304 developmental biology Pyrans Shellfish 0303 health sciences Chromatography Molecular Structure ved/biology 010401 analytical chemistry toxins Nuclear magnetic resonance spectroscopy stability 6. Clean water reference materials 0104 chemical sciences Bivalvia Solutions mussels chemistry mass spectrometry/lc-ms Anhydrous Marine Toxins Methanol Stock solution performance |
| Zdroj: | Analytical and bioanalytical chemistry. 398(5) |
| ISSN: | 1618-2650 |
| Popis: | The original publication is available at http://www.springerlink.com/content/56n2nt56737jx505/ peer-reviewed 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. |
| Databáze: | OpenAIRE |
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