4.7 Article

Determination of Gonyautoxin-4 in Echinoderms and Gastropod Matrices by Conversion to Neosaxitoxin Using 2-Mercaptoethanol and Post-Column Oxidation Liquid Chromatography with Fluorescence Detection

Journal

TOXINS
Volume 8, Issue 1, Pages -

Publisher

MDPI
DOI: 10.3390/toxins8010011

Keywords

paralytic shellfish poisoning; toxins; post-column oxidation fluorescence; interfering matrix peaks; thiol compounds

Funding

  1. Portuguese Fundation of Science and Technology (FCT) [UID/Multi/04423/2013]
  2. MARBIOTECH within the Scientific Resaerch and Technological Development (SR&TD) Integrated Program [NORTE-07-0124-FEDER-000047]
  3. Programa Operacional Regional do Norte (ON.2-O Novo Norte)
  4. NOVOMAR [0687-NOVOMAR-1-P]
  5. European Regional Development Fund
  6. FCT [SFRH/BD/73269/2010]
  7. European Fund for Economic and Regional Development (FEDER)
  8. Ministerio de Economia y Competitividad [AGL2012-40185-CO2-01, AGL2014-58210-R]
  9. Conselleria de Cultura, Educacion e Ordenacion Universitaria [GRC2013-016]
  10. CDTI under India&Spain Innovating Program (ISIP) Programme, Spain [IDI-20130304 APTAFOOD]
  11. European Union [312184 PHARMASEA]
  12. Fundação para a Ciência e a Tecnologia [SFRH/BD/73269/2010] Funding Source: FCT

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Paralytic Shellfish Toxin blooms are common worldwide, which makes their monitoring crucial in the prevention of poisoning incidents. These toxins can be monitored by a variety of techniques, including mouse bioassay, receptor binding assay, and liquid chromatography with either mass spectrometric or pre- or post-column fluorescence detection. The post-column oxidation liquid chromatography with fluorescence detection method, used routinely in our laboratory, has been shown to be a reliable method for monitoring paralytic shellfish toxins in mussel, scallop, oyster and clam species. However, due to its high sensitivity to naturally fluorescent matrix interferences, when working with unconventional matrices, there may be problems in identifying toxins because of naturally fluorescent interferences that co-elute with the toxin peaks. This can lead to erroneous identification. In this study, in order to overcome this challenge in echinoderm and gastropod matrices, we optimized the conversion of Gonyautoxins 1 and 4 to Neosaxitoxin with 2-mercaptoethanol. We present a new and less time-consuming method with a good recovery (82.2%, RSD 1.1%, n = 3), requiring only a single reaction step.

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