National Research Council of Canada. NRC Institute for Marine Biosciences
Application of a method for the "in situ" generation of 9-anthryldiazomethane (ADAM) to the derivatization of the carboxyl function in diarrhetic shellfish poisoning (DSP) toxins revealed the formation of artifact products. Using liq. chromatog.-mass spectrometry, it was detd. that these artifacts were due to base-catalyzed reactions between the solvent, Et acetate, and the hydroxyl groups of the analyte to produce O-acetylated ADAM derivs. Using a new formulation, with THF as solvent, it was possible to eliminate these artifact reactions. Various reaction parameters have also been re-optimized to ensure quant. derivatizations. An assessment method was developed that was useful not only for optimizing reaction parameters, but also for evaluating the reagent potency before use on important samples. Finally, application of the method to the detn. of DSP toxins in plankton and mussel tissue was demonstrated.