Comparison of LC-MS methods for the quantitation of ciguatoxins in fish – A collaborative study
Ciguatoxins (CTXs) are marine biotoxins that can contaminate seafood and if consumed can result in ciguatera poisoning (CP). The analysis of CTXs is challenging, as they occur in complex tissue matrices, cause CP symptoms at trace amounts (<1 μg kg<sup>-1</sup>), and certified reference materials are not available. Currently, no standard operating protocols exist for sample preparation or instrumental analysis. Five laboratories worldwide participated in this first-time method comparison study, which used sample extracts containing different CTX groups (CTX4A group, CTX3C group, C-CTX-1) to identify factors impacting CTX quantitation using LC-MS/MS and LC-HRMS. Matrix effects were found to significantly influence CTX quantitation, along with factors such as instrument, eluents, or selected precursor ion. CTXs were quantified using commercially available, non-certified CTX1B and CTX3C standards. Analogues of the CTX groups behaved differently with regard to matrix effects and suitable calibrants with differences between laboratories exceeding a factor of 10 in some cases.
Authors
- Christopher R. Loeffler (ORCID: https://orcid.org/0000-0002-5744-5743)
- Cintia Flores (ORCID: https://orcid.org/0000-0002-7766-5639)
- Astrid Spielmeyer
- Vincent Hort (ORCID: https://orcid.org/0000-0003-0765-2063)
- F. Real (ORCID: https://orcid.org/0000-0001-6526-0354)
- Caroline Desbourdes
- Jorge Diogène (ORCID: https://orcid.org/0000-0002-6567-6891)
- Andres Sanchez‐Henao (ORCID: https://orcid.org/0000-0003-3413-4755)
- Jean Turquet
- Maria Rambla-Alegre (ORCID: https://orcid.org/0000-0003-4276-276X)
- J. Sam Murray (ORCID: https://orcid.org/0000-0002-5844-6246)
- Mònica Campàs (ORCID: https://orcid.org/0000-0002-1220-7100)
- Emillie Passfield (ORCID: https://orcid.org/0009-0000-5793-8161)
- Lourdes Barreiro-Crespo
Institutions
- Universidad de Las Palmas de Gran Canaria (ES)
- Federal Institute for Risk Assessment (DE)
- Laboratoire de Biotechnologie et Chimie Marines (FR)
- Institute of Agrifood Research and Technology (ES)
- Arvalis - Institut du Végétal (FR)
- Continental (Canada) (CA)
- Agence Nationale de Sécurité Sanitaire de l’Alimentation, de l’Environnement et du Travail (FR)
- Institute of Environmental Assessment and Water Research (ES)
- Processus Infectieux en Milieu Insulaire Tropical (RE)
- Universitat Rovira i Virgili (ES)
- Cawthron Institute (NZ)
Publication Details
- Journal
- Food Chemistry X
- Published
- 2025-11-09
- DOI
- https://doi.org/10.1016/j.fochx.2025.103277
- Primary Topic
- Marine Toxins and Detection Methods
- Type
- article
- Field-Weighted Citation Impact
- 0.00
Funders
- Università degli Studi di Napoli Federico II
- Banco Santander
- European Food Safety Authority
- Centres de Recerca de Catalunya
- Generalitat de Catalunya
- Ministry of Business, Innovation and Employment
- Ministerio de Ciencia e Innovación
- Universidad de Las Palmas de Gran Canaria
- Agence Nationale de Sécurité Sanitaire de l’Alimentation, de l’Environnement et du Travail
- Agencia Canaria de Investigación, Innovación y Sociedad de la Información
- Serono Symposia International Foundation
- Agencia Estatal de Investigación
- H2020 European Research Council