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Analysis of domoic acid and related compounds by mass spectrometry and gas chromatography/mass spectrometry as N ‐trifluoroacetyl‐ O ‐silyl derivatives
Author(s) -
Pleasance Stephen,
Xie Mei,
LeBlanc Yves,
Quilliam Michael A.
Publication year - 1990
Publication title -
biomedical and environmental mass spectrometry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.475
H-Index - 121
eISSN - 1096-9888
pISSN - 0887-6134
DOI - 10.1002/bms.1200190707
Subject(s) - domoic acid , chemistry , chromatography , mass spectrometry , silylation , derivatization , gas chromatography–mass spectrometry , bstfa , gas chromatography , marine toxin , organic chemistry , toxin , biochemistry , catalysis
A method is presented for the analysis of shellfish tissue for domoic acid, a neurotoxic amino acid responsible for cases of amnesic shellfish poisoning. Tissue extracts are first taken through a two‐stage solid‐phase extraction clean‐up, using reversed‐phase and strong cation exchange cartridges. A two‐stage derivatization, using N ‐methyl‐bis‐trifluoroacetamide followed by either N ‐methyl‐ tert ‐butyldimethylsilyltrifluoroacetamide or N , O ‐bis‐trimethylsilyltrifluoroacetamide, is then used to produce an N ‐trifluoroacetyl‐ O ‐silyl derivative which can be analyzed by mass spectrometry with introduction via direct inlet probe, moving‐belt liquid chromatograph/mass spectrometer interface, or capillary column gas chromatography. The N ‐trifluoroacetyl‐ O ‐tert‐butyldimethylsilyl derivative, which has good stability towards hydrolysis, provides a spectrum well suited to gas chromatography/mass spectrometry (GC/MS) using selected ion recording. GC/MS data for two related compounds, kainic acid and dihydrokainic acid, are also reported. The latter is used as an internal standard for quantification of domoic acid, although the method reported is intended primarily for confirmation of the toxin and related compounds in shellfish tissue.