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Toxins
Special Issues
Analytical Chemistry Techniques in Toxin Detection
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Analytical Chemistry Techniques in Toxin Detection

A special issue of Toxins (ISSN 2072-6651).

Deadline for manuscript submissions: closed (20 June 2023) | Viewed by 11525

Special Issue Editors

Dr. Pablo Estévez Bastos

E-Mail Website
Guest Editor
1. Biomedical Research Centre (CINBIO), Department of Analytical and Food Chemistry, University of Vigo, 36310 Vigo, Spain
2. Department of Pharmaceutical Chemistry, University of California, San Francisco, San Francisco, CA 94107, USA
Interests: chromatography; mass spectrometric analysis and biological assays for toxins and related metabolites; reference materials; sample preparation; method validation
Dr. Naomasa Oshiro

E-Mail Website
Guest Editor
Division of Biomedical Food Research, National Institute of Health Sciences, 3-25-26 Tonomachi, Kawasaki 210-9501, Kanagawa, Japan
Interests: analysis of marine biotoxins; chemistry and etiology of marine biotoxins; epidemiology of seafood poisoning; ciguatera poisoning
Special Issues, Collections and Topics in MDPI journals

Special Issue Information

Dear Colleagues,

Over recent decades, a significant increase in the development of detection methods for the monitoring of toxins has been reported. Analytical chemistry techniques, such as liquid chromatography (LC) coupled to different detection modes (UV, FLD, MS/MS, HRMS), are being selected to substitute biological methods, such as the Mouse bioassay. These analytical chemistry techniques allow the sensitive identification and quantification of specific toxins. The new developments in detection technology, as well as the increase in the production of toxins reference materials, are allowing the implementation of analytical chemistry techniques in routine analysis laboratories and the subsequent protection of public health.

This Special Issue aims to present a collection of analytical chemistry techniques used in the detection and quantitation of marine and freshwater toxins, and related metabolites. Topics of interest include the development and/or validation of methods of analysis, the monitoring of toxins in the environment or food, and the identification or characterization of novel toxins or related metabolites.

Dr. Pablo Estévez Bastos
Dr. Naomasa Oshiro
Guest Editors

Manuscript Submission Information

Manuscripts should be submitted online at www.mdpi.com by registering and logging in to this website. Once you are registered, click here to go to the submission form. Manuscripts can be submitted until the deadline. All submissions that pass pre-check are peer-reviewed. Accepted papers will be published continuously in the journal (as soon as accepted) and will be listed together on the special issue website. Research articles, review articles as well as short communications are invited. For planned papers, a title and short abstract (about 100 words) can be sent to the Editorial Office for announcement on this website.

Submitted manuscripts should not have been published previously, nor be under consideration for publication elsewhere (except conference proceedings papers). All manuscripts are thoroughly refereed through a double-blind peer-review process. A guide for authors and other relevant information for submission of manuscripts is available on the Instructions for Authors page. Toxins is an international peer-reviewed open access monthly journal published by MDPI.

Please visit the Instructions for Authors page before submitting a manuscript. The Article Processing Charge (APC) for publication in this open access journal is 2700 CHF (Swiss Francs). Submitted papers should be well formatted and use good English. Authors may use MDPI's English editing service prior to publication or during author revisions.

Keywords

  • analytical methods
  • detection and quantification
  • marine biotoxins
  • food safety
  • phycotoxin
  • cyanotoxin

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Published Papers (5 papers)

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Research

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10 pages, 6594 KiB  
Communication
Tetrodotoxin Derivatization with a Newly Designed Boron Reagent Leads to Conventional Reversed-Phase Liquid Chromatography
by Shimba Kawasue, Kyoko Kuniyoshi, Masashi Uema and Naomasa Oshiro
Toxins 2024, 16(6), 260; https://doi.org/10.3390/toxins16060260 - 4 Jun 2024
Viewed by 993
Abstract
Tetrodotoxin (TTX) is a representative natural toxin causing pufferfish food poisoning, which is especially prominent in East and Southeast Asia, including Japan. TTX has been analyzed through post-column derivatization high-performance liquid chromatography (HPLC), ion-pair LC-MS(/MS), and hydrophilic interaction liquid chromatography (HILIC)-MS(/MS) as alternatives [...] Read more.
Tetrodotoxin (TTX) is a representative natural toxin causing pufferfish food poisoning, which is especially prominent in East and Southeast Asia, including Japan. TTX has been analyzed through post-column derivatization high-performance liquid chromatography (HPLC), ion-pair LC-MS(/MS), and hydrophilic interaction liquid chromatography (HILIC)-MS(/MS) as alternatives to the mouse bioassay method. However, post-column derivatization requires a system for online derivatization reactions, and with the ion-pair LC-MS approach, it is difficult to remove residual ion-pair reagents remaining in the equipment. Moreover, HILIC-MS provides poor separation compared to reversed-phase (RP) HPLC and requires a long time to reach equilibration. Therefore, we decided to develop a TTX analytical method using pre-column derivatization and RP HPLC for the rapid assessment of outbreak samples, including food remnants. In this study, we focused on the vic-diol moiety of TTX and designed a new derivatization reagent coded as NBD-H-DAB. This NBD-H-DAB was synthesized from 4-hydrazino-7-nitro-2,1,3-benzoxadiazole (NBD-H) and 3-fluoro-2-formylphenylboronic acid (FFPBA) with a simple reaction system and rapidly converted to its boronate form, coded NBD-H-PBA, in an aqueous reaction solution. The NBD-H-PBA demonstrated appropriate hydrophobicity to be retained on the RP analytical column and successfully detected with a UV spectrometer. It was easily reacted with the vic-diol moiety of TTX (C6 and C11) to synthesized a boronic ester. The derivatized TTX could be detected using the RP HPLC-UV, and the limit of detection in the fish flesh samples was 0.06 mg/kg. This novel pre-column derivatization of TTX with NBD-H-PBA proves capable for the analysis of TTX. Full article
(This article belongs to the Special Issue Analytical Chemistry Techniques in Toxin Detection)
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17 pages, 4127 KiB  
Article
Detection of Extremely Low Level Ciguatoxins through Monitoring of Lithium Adduct Ions by Liquid Chromatography-Triple Quadrupole Tandem Mass Spectrometry
by Manami Kobayashi, Junichi Masuda and Naomasa Oshiro
Toxins 2024, 16(4), 170; https://doi.org/10.3390/toxins16040170 - 27 Mar 2024
Cited by 1 | Viewed by 1531
Abstract
Ciguatera poisoning (CP) is the most common type of marine biotoxin food poisoning worldwide, and it is caused by ciguatoxins (CTXs), thermostable polyether toxins produced by dinoflagellate Gambierdiscus and Fukuyoa spp. It is typically caused by the consumption of large fish high on [...] Read more.
Ciguatera poisoning (CP) is the most common type of marine biotoxin food poisoning worldwide, and it is caused by ciguatoxins (CTXs), thermostable polyether toxins produced by dinoflagellate Gambierdiscus and Fukuyoa spp. It is typically caused by the consumption of large fish high on the food chain that have accumulated CTXs in their flesh. CTXs in trace amounts are found in natural samples, and they mainly induce neurotoxic effects in consumers at concentrations as low as 0.2 µg/kg. The U.S. Food and Drug Administration has established CTX maximum permitted levels of 0.01 µg/kg for CTX1B and 0.1 µg/kg for C-CTX1 based on toxicological data. More than 20 variants of the CTX1B and CTX3C series have been identified, and the simultaneous detection of trace amounts of CTX analogs has recently been required. Previously published works using LC-MS/MS achieved the safety levels by monitoring the sodium adduct ions of CTXs ([M+Na]+ > [M+Na]+). In this study, we optimized a highly sensitive method for the detection of CTXs using the sodium or lithium adducts, [M+Na]+ or [M+Li]+, by adding alkali metals such as Na+ or Li+ to the mobile phase. This work demonstrates that CTXs can be successfully detected at the low concentrations recommended by the FDA with good chromatographic separation using LC-MS/MS. It also reports on the method’s new analytical conditions and accuracy using [M+Li]+. Full article
(This article belongs to the Special Issue Analytical Chemistry Techniques in Toxin Detection)
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15 pages, 4785 KiB  
Article
Measuring Marine Biotoxins in a Hypersaline Coastal Lagoon
by Ainhoa Oller-Ruiz, Nuria Alcaraz-Oliver, Gema Férez and Javier Gilabert
Toxins 2023, 15(9), 526; https://doi.org/10.3390/toxins15090526 - 26 Aug 2023
Cited by 1 | Viewed by 1213
Abstract
Marine biotoxins have posed a persistent problem along various coasts for many years. Coastal lagoons are ecosystems prone to phytoplankton blooms when altered by eutrophication. The Mar Menor is the largest hypersaline coastal lagoon in Europe. Sixteen marine toxins, including lipophilic toxins, yessotoxins, [...] Read more.
Marine biotoxins have posed a persistent problem along various coasts for many years. Coastal lagoons are ecosystems prone to phytoplankton blooms when altered by eutrophication. The Mar Menor is the largest hypersaline coastal lagoon in Europe. Sixteen marine toxins, including lipophilic toxins, yessotoxins, and domoic acid (DA), in seawater samples from the Mar Menor coastal lagoon were measured in one year. Only DA was detected in the range of 44.9–173.8 ng L−1. Environmental stressors and mechanisms controlling the presence of DA in the lagoon are discussed. As an enrichment and clean-up method, we employed solid phase extraction to filter and acidify 75 mL of the sample, followed by pre-concentration through a C18 SPE cartridge. The analytes were recovered in aqueous solutions and directly injected into the liquid chromatography system (LC-MS), which was equipped with a C18 column. The system operated in gradient mode, and we used tandem mass spectrometry (MS/MS) with a triple quadrupole (QqQ) in the multiple reaction monitoring mode (MRM) for analysis. The absence of matrix effects was checked and the limits of detection for most toxins were low, ranging from 0.05 to 91.2 ng L−1, depending on the compound. To validate the measurements, we performed recovery studies, falling in the range of 74–122%, with an intraday precision below 14.9% RSD. Full article
(This article belongs to the Special Issue Analytical Chemistry Techniques in Toxin Detection)
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Review

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40 pages, 4411 KiB  
Review
Ciguatera Fish Poisoning in the Caribbean Sea and Atlantic Ocean: Reconciling the Multiplicity of Ciguatoxins and Analytical Chemistry Approach for Public Health Safety
by Ivannah Pottier, Richard J. Lewis and Jean-Paul Vernoux
Toxins 2023, 15(7), 453; https://doi.org/10.3390/toxins15070453 - 10 Jul 2023
Cited by 7 | Viewed by 3664
Abstract
Ciguatera is a major circumtropical poisoning caused by the consumption of marine fish and invertebrates contaminated with ciguatoxins (CTXs): neurotoxins produced by endemic and benthic dinoflagellates which are biotransformed in the fish food-web. We provide a history of ciguatera research conducted over the [...] Read more.
Ciguatera is a major circumtropical poisoning caused by the consumption of marine fish and invertebrates contaminated with ciguatoxins (CTXs): neurotoxins produced by endemic and benthic dinoflagellates which are biotransformed in the fish food-web. We provide a history of ciguatera research conducted over the past 70 years on ciguatoxins from the Pacific Ocean (P-CTXs) and Caribbean Sea (C-CTXs) and describe their main chemical, biochemical, and toxicological properties. Currently, there is no official method for the extraction and quantification of ciguatoxins, regardless their origin, mainly due to limited CTX-certified reference materials. In this review, the extraction and purification procedures of C-CTXs are investigated, considering specific objectives such as isolating reference materials, analysing fish toxin profiles, or ensuring food safety control. Certain in vitro assays may provide sufficient sensitivity to detect C-CTXs at sub-ppb levels in fish, but they do not allow for individual identification of CTXs. Recent advances in analysis using liquid chromatography coupled with low- or high-resolution mass spectrometry provide new opportunities to identify known C-CTXs, to gain structural insights into new analogues, and to quantify C-CTXs. Together, these methods reveal that ciguatera arises from a multiplicity of CTXs, although one major form (C-CTX-1) seems to dominate. However, questions arise regarding the abundance and instability of certain C-CTXs, which are further complicated by the wide array of CTX-producing dinoflagellates and fish vectors. Further research is needed to assess the toxic potential of the new C-CTX and their role in ciguatera fish poisoning. With the identification of C-CTXs in the coastal USA and Eastern Atlantic Ocean, the investigation of ciguatera fish poisoning is now a truly global effort. Full article
(This article belongs to the Special Issue Analytical Chemistry Techniques in Toxin Detection)
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20 pages, 2701 KiB  
Review
Contribution of Mass Spectrometry to the Advances in Risk Characterization of Marine Biotoxins: Towards the Characterization of Metabolites Implied in Human Intoxications
by Pablo Estevez and Ana Gago-Martinez
Toxins 2023, 15(2), 103; https://doi.org/10.3390/toxins15020103 - 22 Jan 2023
Cited by 3 | Viewed by 2435
Abstract
A significant spread and prevalence of algal toxins and, in particular, marine biotoxins have been observed worldwide over the last decades. Marine biotoxins are natural contaminants produced during harmful algal blooms being accumulated in seafood, thus representing a threat to human health. Significant [...] Read more.
A significant spread and prevalence of algal toxins and, in particular, marine biotoxins have been observed worldwide over the last decades. Marine biotoxins are natural contaminants produced during harmful algal blooms being accumulated in seafood, thus representing a threat to human health. Significant progress has been made in the last few years in the development of analytical methods able to evaluate and characterize the different toxic analogs involved in the contamination, Liquid Chromatography coupled to different detection modes, including Mass Spectrometry, the method of choice due to its potential for separation, identification, quantitation and even confirmation of the different above-mentioned analogs. Despite this, the risk characterization in humans is still limited, due to several reasons, including the lack of reference materials or even the limited access to biological samples from humans intoxicated during these toxic events and episodes, which hampered the advances in the evaluation of the metabolites responsible for the toxicity in humans. Mass Spectrometry has been proven to be a very powerful tool for confirmation, and in fact, it is playing an important role in the characterization of the new biotoxins analogs. The toxin metabolization in humans is still uncertain in most cases and needs further research in which the implementation of Mass Spectrometric methods is critical. This review is focused on compiling the most relevant information available regarding the metabolization of several marine biotoxins groups, which were identified using Mass Spectrometry after the in vitro exposition of these toxins to liver microsomes and hepatocytes. Information about the presence of metabolites in human samples, such as human urine after intoxication, which could also be used as potential biomarkers for diagnostic purposes, is also presented. Full article
(This article belongs to the Special Issue Analytical Chemistry Techniques in Toxin Detection)
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