Improved method for preparation and use of 9-anthryldiazomethane for derivatization of hydroxycarboxylic acids

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DOIResolve DOI: http://doi.org/10.1016/S0021-9673(98)00069-7
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TypeArticle
Journal titleJournal of Chromatography A
ISSN0021-9673
Volume807
Issue2
Pages229239
AbstractApplication 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.
Publication date
LanguageEnglish
AffiliationNational Research Council Canada; NRC Institute for Marine Biosciences
Peer reviewedYes
NPARC number23001017
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Record identifiera47a780e-faed-460a-9f99-f7781ec1b620
Record created2016-11-29
Record modified2016-11-29
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