Liquid chromatography with fluorimetric, mass spectrometric and tandem mass spectrometric detection for the investigation of the seafood-toxin-producing phytoplankton, Dinophysis acuta
作者： Kevin J James , Alan G Bishop , Marion Gillman , Séan S Kelly , Cilian Roden
DOI: 10.1016/S0021-9673(97)00158-1
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摘要: Abstract The diarrhoeic shellfish poisoning (DSP) toxins, okadaic acid (OA) and its isomer, dinophysistoxin-2 (DTX-2), were determined in the marine phytoplankton, Dinophysis acuta , harvested Ireland. Unialgal samples (22–100 cells) extracted derivatised using 9-anthryldiazomethane (ADAM) or 1-bromoacetylpyrene (BAP) analysed by liquid chromatography (LC). Isocratic elution on a C 18 reversed-phase column, with fluorimetric detection, was used to determine OA (58±7 pg/cell) DTX-2 (78±14 pg/cell). detection limit 0.1 ng OA/20 μl injection ADAM. Gradient LC, polymeric bonded phase, successfully separated mixtures containing both ADAM BAP toxins. Identification of DSP toxins confirmed isocratic micro LC tandem mass spectrometric (μLC–MS–MS) analysis free μLC–MS BAP-derivatised an ionspray (IS) interface, coupled atmospheric pressure ionisation (API) source. Collision induced dissociation (CID) ion spectra protonated molecule, [M+H] + at m / z 805 for DTX-2, identified three diagnostic fragment ions each analyte which selected reaction monitoring (SRM) LC–MS–MS analysis. 0.025 ng/0.2 injected. These studies showed that D. progenitor shellfish.
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