Quantitation of Tetrodotoxin and Its Analogues with a Combination of Liquid Chromatography-Tandem Mass Spectrometry and Quantitative 1H-NMR Spectroscopy

Ryuichi Watanabe, Masato Tanioka, Hajime Uchida, Ryoji Matsushima, Hiroshi Oikawa, Masahiro Matsumiya, Mari Yotsu-Yamashita, Toshiyuki Suzuki

研究成果: Article査読

3 被引用数 (Scopus)

抄録

Tetrodotoxin and its analogues are the causative toxins of pufferfish poisoning. Tetrodotoxin has been recently detected in bivalve mollusks collected in New Zealand and Europe, highlighting the need to include tetrodotoxin in monitoring programs for bivalves by instrumental methods. In the present study, tetrodotoxin and its analogues in commercially available tetrodotoxin reagents were quantitated accurately by quantitative 1H-nuclear magnetic resonance (qNMR) spectroscopy. The results were applied to estimate relative molar responses of tetrodotoxin and its analogues in hydrophilic interaction liquid chromatography-tandem mass spectrometry (HILIC/MS/MS). All four components (tetrodotoxin hemilactal form (1), tetrodotoxin 10,7-lactone form (2), 4-epitetrodotoxin (3), and 4,9-anhydrotetrodotoxin (4)) generated by equilibrating tetrodotoxin in aqueous solution were prepared as a mixture. From the HSQC spectrum of the mixture, the separated signals derived from three components, excluding 1, were selected and used for the quantitation. In addition, the relative molar responses of 3 and 4 on HILIC/MS/MS were calculated to be 0.73 and 0.46, respectively. These values could be useful for quantitation of 3 and 4 using the tetrodotoxin standard by HILIC/MS/MS. Our results also indicate that qNMR is useful for preparation of tetrodotoxin certified reference material.

本文言語English
ページ(範囲)12911-12917
ページ数7
ジャーナルJournal of Agricultural and Food Chemistry
67
46
DOI
出版ステータスPublished - 2019 11 20

ASJC Scopus subject areas

  • 化学 (全般)
  • 農業および生物科学(全般)

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