DOI | Resolve DOI: https://doi.org/10.1016/j.toxicon.2003.10.003 |
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Author | Search for: Miles, Christopher O.; Search for: Wilkins, Alistair L.; Search for: Munday, Rex; Search for: Dines, Mark H.; Search for: Hawkes, Allan D.; Search for: Briggs, Lyn R.; Search for: Sandvik, Morten; Search for: Jensen, Dwayne J.; Search for: Cooney, Janine M.; Search for: Holland, Patrick T.; Search for: Quilliam, Michael A.1; Search for: MacKenzie, A. Lincoln; Search for: Beuzenberg, Veronica; Search for: Towers, Neale R. |
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Affiliation | - National Research Council of Canada. Measurement Science and Standards
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Format | Text, Article |
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Subject | Pectenotoxin-2; Pectenotoxin-2 seco acid; okadaic acid diol ester; NMR; enzymatic hydrolysis; LC–MS; Dinophysis acuta; toxicity |
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Abstract | We have developed a simple and effective method for isolating pectenotoxin-2 (PTX-2) from Dinophysis cells collected from a natural bloom. A two-step extraction procedure followed by two column chromatography steps produced PTX-2 in high purity suitable for use as an analytical standard and for toxicological studies. Incubation of purified PTX-2 with the supernatant from ultracentrifuged blue (Mytilus edulis) or Greenshell® (Perna canaliculus) mussel hepatopancreas homogenate caused rapid conversion to pectenotoxin-2 seco acid (PTX-2 SA). Purification of PTX-2 SA was achieved by solvent extraction followed by column chromatography. PTX-2 and PTX-2 SA were fully characterized by LC–MS and NMR, and full 1H and 13C NMR assignments were obtained. Okadaic acid C8-diol ester was isolated during the purification of PTX-2, and its identity confirmed by NMR and LC–MS analyses. Pectenotoxin-2 seco acid methyl ester, identified by LC–MS, was also produced during the hydrolytic procedure due to the presence of methanol. PTX-2 was acutely toxic to mice by i.p. injection (LD50=219 µg/kg) but no effects were seen with PTX-2 SA at 5000 µg/kg. Neither PTX-2 nor PTX-2 SA was overtly toxic to mice by the oral route at doses up to 5000 µg/kg. No diarrhea was observed in mice dosed with either compound, suggesting that pectenotoxins do not belong in the diarrhetic shellfish poison group. |
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Publication date | 2004-01 |
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Terms of use | - Copyright 2003 Elsevier Ltd. All rights reserved.
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In | |
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Language | English |
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Peer reviewed | Yes |
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NRC number | 1371 |
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NPARC number | 3538361 |
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Export citation | Export as RIS |
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Report a correction | Report a correction (opens in a new tab) |
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Record identifier | 410cc8c2-7ca2-4cf4-955c-d0198d06e085 |
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Record created | 2009-03-01 |
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Record modified | 2020-04-17 |
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