Abstract
Domoic acid, the shellfish toxin discovered in 1987 off the eastern coast of Canada and northern US is determined by isocratic reversed-phase LC with UV detection at 242 nm. Extraction from shellfish tissue is achieved with 0.1 mol/l HCl or water, with minimal cleanup before LC analysis. Detection limits are around 0.5 μg/g. Results can be confirmed by pre-chromatographic derivatization at either the — NH or — COOH moiety. An LC screening method using pre-chromatographic oxidation has been developed for paralytic shellfish poison (PSP, comprised mainly of 12 related compounds). The individual toxins in the PSP family produced single products with periodate oxidation. However, they could not all be separated using a variety of chromatography systems including reversed-phase and ion-pair chromatography with heptane sulfonate or tetrabythyl-ammonium ion. Detection limits were about 0.05 μg/g total PSP toxin in shellfish. Saxitoxin could be detected at 5–10 pg per injection. Comparisons of this method with the mouse bioassay and the post-column technique showed reasonable agreement between results.
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