The preparation of certified calibration solutions for azaspiracid-1, -2, and -3, potent marine biotoxins found in shellfish

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DOIResolve DOI: http://doi.org/10.1007/s00216-010-4161-2
AuthorSearch for: ; Search for: ; Search for: ; Search for: ; Search for: ; Search for: ; Search for: ; Search for: ; Search for: ; Search for: ; Search for: ; Search for:
TypeArticle
Journal titleAnalytical and Bioanalytical Chemistry
Volume398
Issue5
Pages22432252; # of pages: 10
SubjectReference materials; Mass spectrometry/LC-MS; Marine toxins
AbstractThe 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 3OH 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.
Publication date
LanguageEnglish
AffiliationNRC Institute for Marine Biosciences; National Research Council Canada
Peer reviewedYes
NRC number51766
NPARC number12745771
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Record identifier5675642f-2b1a-4196-ba4f-22f72c4f0e03
Record created2009-10-28
Record modified2016-05-09
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