| Téléchargement | - Voir la version finale : Reductive amination for LC–MS signal enhancement and confirmation of the presence of Caribbean ciguatoxin-1 in fish (PDF, 1.9 Mio)
- Voir les données supplémentaires : Reductive amination for LC–MS signal enhancement and confirmation of the presence of Caribbean ciguatoxin-1 in fish (PDF, 1.0 Mio)
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| DOI | Trouver le DOI : https://doi.org/10.3390/toxins14060399 |
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| Auteur | Rechercher : Kryuchkov, FedorIdentifiant ORCID : https://orcid.org/0000-0002-8611-9330; Rechercher : Robertson, AlisonIdentifiant ORCID : https://orcid.org/0000-0002-2537-0943; Rechercher : Mudge, Elizabeth M.1; Rechercher : Miles, Christopher O.1Identifiant ORCID : https://orcid.org/0000-0001-8537-4439; Rechercher : Van Gothem, Soetkien; Rechercher : Uhlig, SilvioIdentifiant ORCID : https://orcid.org/0000-0001-6419-9563 |
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| Affiliation | - Conseil national de recherches du Canada. Centre de recherche en métrologie
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| Bailleur de fonds | Rechercher : The Research Council of Norway; Rechercher : National Science Foundation |
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| Format | Texte, Article |
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| Sujet | ciguatoxin; Caribbean ciguatoxin; Girard's reagent; quaternary ammonium; LC-MS; derivatization |
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| Résumé | Ciguatera poisoning is a global health concern caused by the consumption of seafood containing ciguatoxins (CTXs). Detection of CTXs poses significant analytical challenges due to their low abundance even in highly toxic fish, the diverse and in-part unclarified structures of many CTX congeners, and the lack of reference standards. Selective detection of CTXs requires methods such as liquid chromatography coupled to tandem mass spectrometry (LC–MS/MS) or high-resolution MS (LC–HRMS). While HRMS data can provide greatly improved resolution, it is typically less sensitive than targeted LC–MS/MS and does not reliably comply with the FDA guidance level of 0.1 µg/kg CTXs in fish tissue that was established for Caribbean CTX-1 (C-CTX-1). In this study, we provide a new chemical derivatization approach employing a fast and simple one-pot derivatization with Girard’s reagent T (GRT) that tags the C-56-ketone intermediate of the two equilibrating C-56 epimers of C-CTX-1 with a quaternary ammonium moiety. This derivatization improved the LC–MS/MS and LC–HRMS responses to C-CTX-1 by approximately 40- and 17-fold on average, respectively. These improvements in sensitivity to the GRT-derivative of C-CTX-1 are attributable to: the improved ionization efficiency caused by insertion of a quaternary ammonium ion; the absence of adduct-ions and water-loss peaks for the GRT derivative in the mass spectrometer, and; the prevention of on-column epimerization (at C-56 of C-CTX-1) by GRT derivatization, leading to much better chromatographic peak shapes. This C-CTX-1–GRT derivatization strategy mitigates many of the shortcomings of current LC–MS analyses for C-CTX-1 by improving instrument sensitivity, while at the same time adding selectivity due to the reactivity of GRT with ketones and aldehydes. |
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| Date de publication | 2022-06-09 |
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| Maison d’édition | MDPI |
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| Licence | |
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| Dans | |
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| Langue | anglais |
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| Publications évaluées par des pairs | Oui |
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| Exporter la notice | Exporter en format RIS |
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| Signaler une correction | Signaler une correction (s'ouvre dans un nouvel onglet) |
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| Identificateur de l’enregistrement | ec6fef9a-9c51-4b7c-883f-fa3edf17850f |
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| Enregistrement créé | 2022-07-15 |
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| Enregistrement modifié | 2022-07-15 |
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