Jump to main content
US EPA
United States Environmental Protection Agency
Search
Search
Main menu
Environmental Topics
Laws & Regulations
About EPA
Health & Environmental Research Online (HERO)
Contact Us
Print
Feedback
Export to File
Search:
This record has one attached file:
Add More Files
Attach File(s):
Display Name for File*:
Save
Citation
Tags
HERO ID
1038054
Reference Type
Journal Article
Title
Quantitative analysis of azaspiracids in Azadinium spinosum cultures
Author(s)
Jauffrais, T; Herrenknecht, C; Séchet, V; Sibat, M; Tillmann, U; Krock, B; Kilcoyne, J; Miles, CO; Mccarron, P; Amzil, Z; Hess, P
Year
2012
Is Peer Reviewed?
Yes
Journal
Analytical and Bioanalytical Chemistry
ISSN:
1618-2642
EISSN:
1618-2650
Volume
403
Issue
3
Page Numbers
833-846
Language
English
PMID
22367288
DOI
10.1007/s00216-012-5849-2
Abstract
Azaspiracids (AZAs) are secondary metabolites of Azadinium spinosum that can accumulate in shellfish and cause food poisoning when consumed. We describe here an analytical procedure for the determination of AZAs in cultures of A. spinosum with a focus on the formation of AZA methyl esters as artefacts during extraction and sample pre-treatment. A. spinosum cells were collected from bioreactor cultures using centrifugation or filtration. Different extraction procedures were evaluated for formation of methyl ester artefacts, yield, and matrix effects. Filtration of cultures using glass-fibre filters led to increased formation of methyl esters, and centrifugation is recommended for recovery of cells. The extraction solvent (methanol (MeOH), acetone, and acetonitrile (MeCN)) did not significantly affect the yield of AZAs as long as the organic content was 80% or higher. However, the use of MeOH as extraction solvent led to increased formation of methyl esters. AZA1 recovery over two successive extractions was 100% at the 95% confidence level for acetone and MeOH. In standard-addition experiments, no significant matrix effects were observed in extracts of A. spinosum or Azadinium obesum up to a sample size of 4.5 × 10(9) μm(3). Moreover, experiments carried out to clarify the formation and structure of methylated AZA analogues led to the description of two AZA methyl esters and to the correction of the chemical structures of AZAs29-32.
Keywords
Extraction procedure; Extraction artefact; Matrix effects; LC-MS/MS; Azaspiracid methyl ester; Dinoflagellate; Liquid chromatography-mass spectrometry
Tags
IRIS
•
Methanol (Non-Cancer)
Search 2012
WOS
ProQuest
Search Jan 30 2013
WOS
ToxNet
Home
Learn about HERO
Using HERO
Search HERO
Projects in HERO
Risk Assessment
Transparency & Integrity