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Toxins
Special Issues
Development of Separative Techniques for the Detection of Natural Toxins
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Development of Separative Techniques for the Detection of Natural Toxins

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

Deadline for manuscript submissions: closed (31 August 2021) | Viewed by 20620

Special Issue Editors

Dr. Vincenzo Lippolis

E-Mail Website
Guest Editor
Institute of Sciences of Food Production, National Research Council of Italy (CNR), 70126 Bari, Italy
Interests: fluorescence polarization spectroscopy; chromatographic methods; rapid/innovative methods; method development and validation; food quality/safety/authenticity
Special Issues, Collections and Topics in MDPI journals
Dr. Michelangelo Pascale

E-Mail Website
Guest Editor
National Research Council of Italy, Institute of Sciences of Food Production (CNR-ISPA), 70126 Bari, Italy
Interests: development and validation of analytical methods for food contaminants, sample preparation; chromatographic methods; rapid methods
Special Issues, Collections and Topics in MDPI journals

Special Issue Information

Dear Colleagues,

Natural toxins are biotoxins produced by some fungal species (mycotoxins), bacteria (exotoxins and endotoxins), algae (phycotoxins), plants (phytotoxins) and animals. They include molecules with a broad range of chemical structures and toxic activity that poses several challenges in their isolation, identification, and quantitative determination. In addition, several natural toxins can contaminate food and feed, as well as marine and freshwater environments, posing a serious risk to both human and animal health.

Separative techniques play a key role in the analysis of natural toxins and their metabolites, due to the complexity of the investigated matrices and the low amounts to detect. The separation of components is often performed prior to the instrumental detection. To date, the most used separative techniques are gas chromatography (GC), liquid chromatography (LC) and capillary electrophoresis (CE). Liquid chromatography combined to mass spectrometry (LC-MS) is the most used tool for the identification and quantification of these analytes, being the technique of choice when a multi-analyte determination is required. Recently, the use of high-resolution mass spectrometry (HRMS) has allowed the identification of novel toxins and advances in metabolomics studies.

This Special Issue is dedicated to recent applications based on separative techniques applied to the identification and quantification of natural toxins in different matrices, together with animal and plant toxin investigation. Chromatographic (GC, LC, lateral flow device), electrophoretic and multidimensional separative techniques, as well as novel separative techniques for sample preparation are welcome.

Dr. Vincenzo Lippolis
Dr. Michelangelo Pascale
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

  • Natural Toxins
  • Liquid Chromatography
  • Gas-Chromatography
  • Mass Spectrometry
  • Capillary Electrophoresis
  • Chromatographic-based rapid tests
  • sample preparation
  • method development
  • method validation, metabolomic

Published Papers (4 papers)

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Research

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14 pages, 3730 KiB  
Article
Monitoring Lipophilic Toxins in Seawater Using Dispersive Liquid—Liquid Microextraction and Liquid Chromatography with Triple Quadrupole Mass Spectrometry
by Ainhoa Oller-Ruiz, Natalia Campillo, Manuel Hernández-Córdoba, Javier Gilabert and Pilar Viñas
Toxins 2021, 13(1), 57; https://doi.org/10.3390/toxins13010057 - 13 Jan 2021
Cited by 7 | Viewed by 2258
Abstract
The use of dispersive liquid–liquid microextraction (DLLME) is proposed for the preconcentration of thirteen lipophilic marine toxins in seawater samples. For this purpose, 0.5 mL of methanol and 440 µL of chloroform were injected into 12 mL of sample. The enriched organic phase, [...] Read more.
The use of dispersive liquid–liquid microextraction (DLLME) is proposed for the preconcentration of thirteen lipophilic marine toxins in seawater samples. For this purpose, 0.5 mL of methanol and 440 µL of chloroform were injected into 12 mL of sample. The enriched organic phase, once evaporated and reconstituted in methanol, was analyzed by reversed-phase liquid chromatography with triple-quadrupole tandem mass spectrometry. A central composite design multivariate method was used to optimize the interrelated parameters affecting DLLME efficiency. The absence of any matrix effect in the samples allowed them to be quantified against aqueous standards. The optimized procedure was validated by recovery studies, which provided values in the 82–123% range. The detection limits varied between 0.2 and 5.7 ng L−1, depending on the analyte, and the intraday precision values were in the 0.1–7.5% range in terms of relative standard deviation. Ten water samples taken from different points of the Mar Menor lagoon were analyzed and were found to be free of the studied toxins. Full article
(This article belongs to the Special Issue Development of Separative Techniques for the Detection of Natural Toxins)
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14 pages, 1149 KiB  
Article
Analysis of α- and β-amanitin in Human Plasma at Subnanogram per Milliliter Levels by Reversed Phase Ultra-High Performance Liquid Chromatography Coupled to Orbitrap Mass Spectrometry
by Thomas P. Bambauer, Lea Wagmann, Armin A. Weber and Markus R. Meyer
Toxins 2020, 12(11), 671; https://doi.org/10.3390/toxins12110671 - 23 Oct 2020
Cited by 15 | Viewed by 2879
Abstract
Amatoxins are known to be one of the main causes of serious to fatal mushroom intoxication. Thorough treatment, analytical confirmation, or exclusion of amatoxin intake is crucial in the case of any suspected mushroom poisoning. Urine is often the preferred matrix due to [...] Read more.
Amatoxins are known to be one of the main causes of serious to fatal mushroom intoxication. Thorough treatment, analytical confirmation, or exclusion of amatoxin intake is crucial in the case of any suspected mushroom poisoning. Urine is often the preferred matrix due to its higher concentrations compared to other body fluids. If urine is not available, analysis of human blood plasma is a valuable alternative for assessing the severity of intoxications. The aim of this study was to develop and validate a liquid chromatography (LC)-high resolution tandem mass spectrometry (HRMS/MS) method for confirmation and quantitation of α- and β-amanitin in human plasma at subnanogram per milliliter levels. Plasma samples of humans after suspected intake of amatoxin-containing mushrooms should be analyzed and amounts of toxins compared with already published data as well as with matched urine samples. Sample preparation consisted of protein precipitation, aqueous liquid-liquid extraction, and solid-phase extraction. Full chromatographical separation of analytes was achieved using reversed-phase chromatography. Orbitrap-based MS allowed for sufficiently sensitive identification and quantification. Validation was successfully carried out, including analytical selectivity, carry-over, matrix effects, accuracy, precision, and dilution integrity. Limits of identification were 20 pg/mL and calibration ranged from 20 pg/mL to 2000 pg/mL. The method was applied to analyze nine human plasma samples that were submitted along with urine samples tested positive for amatoxins. α-Amanitin could be identified in each plasma sample at a range from 37–2890 pg/mL, and β-amanitin was found in seven plasma samples ranging from <20–7520 pg/mL. A LC-HRMS/MS method for the quantitation of amatoxins in human blood plasma at subnanogram per milliliter levels was developed, validated, and used for the analysis of plasma samples. The method provides a valuable alternative to urine analysis, allowing thorough patient treatment but also further study the toxicokinetics of amatoxins. Full article
(This article belongs to the Special Issue Development of Separative Techniques for the Detection of Natural Toxins)
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Review

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33 pages, 990 KiB  
Review
Overview of Recent Liquid Chromatography Mass Spectrometry-Based Methods for Natural Toxins Detection in Food Products
by Annalisa De Girolamo, Vincenzo Lippolis and Michelangelo Pascale
Toxins 2022, 14(5), 328; https://doi.org/10.3390/toxins14050328 - 4 May 2022
Cited by 21 | Viewed by 6684
Abstract
Natural toxins include a wide range of toxic metabolites also occurring in food and products, thus representing a risk for consumer health. In the last few decades, several robust and sensitive analytical methods able to determine their occurrence in food have been developed. [...] Read more.
Natural toxins include a wide range of toxic metabolites also occurring in food and products, thus representing a risk for consumer health. In the last few decades, several robust and sensitive analytical methods able to determine their occurrence in food have been developed. Liquid chromatography mass spectrometry is the most powerful tool for the simultaneous detection of these toxins due to its advantages in terms of sensitivity and selectivity. A comprehensive review on the most relevant papers on methods based on liquid chromatography mass spectrometry for the analysis of mycotoxins, alkaloids, marine toxins, glycoalkaloids, cyanogenic glycosides and furocoumarins in food is reported herein. Specifically, a literature search from 2011 to 2021 was carried out, selecting a total of 96 papers. Different approaches to sample preparation, chromatographic separation and detection mode are discussed. Particular attention is given to the analytical performance characteristics obtained in the validation process and the relevant application to real samples. Full article
(This article belongs to the Special Issue Development of Separative Techniques for the Detection of Natural Toxins)
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39 pages, 732 KiB  
Review
A Review: Sample Preparation and Chromatographic Technologies for Detection of Aflatoxins in Foods
by Kai Zhang and Kaushik Banerjee
Toxins 2020, 12(9), 539; https://doi.org/10.3390/toxins12090539 - 21 Aug 2020
Cited by 75 | Viewed by 7878
Abstract
As a class of mycotoxins with regulatory and public health significance, aflatoxins (e.g., aflatoxin B1, B2, G1 and G2) have attracted unparalleled attention from government, academia and industry due to their chronic and acute toxicity. Aflatoxins [...] Read more.
As a class of mycotoxins with regulatory and public health significance, aflatoxins (e.g., aflatoxin B1, B2, G1 and G2) have attracted unparalleled attention from government, academia and industry due to their chronic and acute toxicity. Aflatoxins are secondary metabolites of various Aspergillus species, which are ubiquitous in the environment and can grow on a variety of crops whereby accumulation is impacted by climate influences. Consumption of foods and feeds contaminated by aflatoxins are hazardous to human and animal health, hence the detection and quantification of aflatoxins in foods and feeds is a priority from the viewpoint of food safety. Since the first purification and identification of aflatoxins from feeds in the 1960s, there have been continuous efforts to develop sensitive and rapid methods for the determination of aflatoxins. This review aims to provide a comprehensive overview on advances in aflatoxins analysis and highlights the importance of sample pretreatments, homogenization and various cleanup strategies used in the determination of aflatoxins. The use of liquid-liquid extraction (LLE), supercritical fluid extraction (SFE), solid phase extraction (SPE) and immunoaffinity column clean-up (IAC) and dilute and shoot for enhancing extraction efficiency and clean-up are discussed. Furthermore, the analytical techniques such as gas chromatography (GC), liquid chromatography (LC), mass spectrometry (MS), capillary electrophoresis (CE) and thin-layer chromatography (TLC) are compared in terms of identification, quantitation and throughput. Lastly, with the emergence of new techniques, the review culminates with prospects of promising technologies for aflatoxin analysis in the foreseeable future. Full article
(This article belongs to the Special Issue Development of Separative Techniques for the Detection of Natural Toxins)
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