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Liquid chromatographic mass spectrometric methods for the determination of marine polyether toxins
R W Dickey1, F A Bencsath, H R Granade
1US Food and Drug Administration, Division of Seafood Research, Dauphin Island, AL 36528.
Abstract:
Experiments with novel nitrogenous coumarin-based reagents yielded moderately fluorescent derivatives of brevetoxin-3 and ciguatoxin-1. The diethylaminocoumarin-carbamic acid esters of brevetoxin-3 were resolved by high performance liquid chromatography into two derivative peaks that correspond to substitutions at the C-37 and C-41 hydroxyls. The derivatives produced intense molecular ions under fast atom bombardment ionization conditions, confirming derivative identity. Ciguatoxin-1 was also successfully derivatized, resolved, and identified by HPLC-fluorometry with an estimated lower limit of detection of 0.5 to 1.0 ng.