Derivatization of azaspiracid biotoxins for analysis by liquid chromatography with fluorescence detection

Download
  1. Get@NRC: Derivatization of azaspiracid biotoxins for analysis by liquid chromatography with fluorescence detection (Opens in a new window)
DOIResolve DOI: http://doi.org/10.1016/j.chroma.2011.09.017
AuthorSearch for: ; Search for: ; Search for: ; Search for:
TypeArticle
Journal titleJournal of Chromatography A
Volume1218
Issue44
Pages80898096; # of pages: 8
SubjectShellfish poisoning toxins; Phycotoxins; 9-Anthryldiazomethane; Derivatization; Fluorescence detection; Certified reference materials
AbstractAzaspiracids (AZAs) are an important group of regulated lipophilic biotoxins that cause shellfish poisoning. Currently, the only widely available analytical method for quantitation of AZAs is liquid chromatography-mass spectrometry (LC-MS). Alternative methods for AZA analysis are needed for detailed characterization work required in the preparation of certified reference materials (CRMs) and by laboratories not equipped with LC-MS. Chemical derivatization of the amine and carboxyl groups on AZAs was investigated for the purpose of facilitating analysis by LC with fluorescence detection (FLD). Experiments towards chemical modification of AZA1 at the amine achieved only limited success. Derivatization of the carboxyl group, on the other hand, proved successful using the 9-anthryldiazomethane (ADAM) method previously applied to the okadaic acid (OA) group toxins. Extraction and clean-up methods were investigated for shellfish tissue samples and a post-reaction solid phase extraction procedure was developed for the AZA ADAM derivatives. Chromatographic separations were developed for the LC-FLD analysis of derivatized AZAs alone or in the presence of other derivatized toxins. This new analytical method for analysis of AZAs enabled verification of AZA1-3 concentrations in recently certified reference materials. The method demonstrated good linearity, repeatability and accuracy showing its potential as an alternative to LC-MS for measurement of AZAs.
Publication date
LanguageEnglish
AffiliationNRC Institute for Marine Biosciences; National Research Council Canada
Peer reviewedYes
NRC number54047
NPARC number19649685
Export citationExport as RIS
Report a correctionReport a correction
Record identifierf274e295-ac10-4321-a4b9-8fd5c0b5fbd3
Record created2012-04-02
Record modified2016-05-09
Bookmark and share
  • Share this page with Facebook (Opens in a new window)
  • Share this page with Twitter (Opens in a new window)
  • Share this page with Google+ (Opens in a new window)
  • Share this page with Delicious (Opens in a new window)