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Chromatography and Spectroscopy in Food, Environmental, and Pharmaceutical Sciences

A Special Issue of Molecules (ISSN 1420-3049) belonging to the section "Analytical Chemistry".

Deadline for manuscript submissions: 30 April 2027 | Viewed by 3689

Editors


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Guest Editor
Department of Biosciences, Biotechnologies and Environment, University of Bari “Aldo Moro”, 70126 Bari, Italy
Interests: the development and validation of innovative, cost-effective, highly sensitive and specific analytical methods, mainly based on the use of chromatographic techniques coupled with mass spectrometry; determination of pesticides in environmental matrices, nutraceuticals, drugs and tumor markers in biological fluids, mycotoxins in food products, and proteomics studies
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Guest Editor
Department of Biosciences, Biotechnologies and Environment, University of Bari “Aldo Moro”, 70126 Bari, Italy
Interests: the identification and chemical characterization (in terms of VOCs, PM, PAHs, heavy metals, etc.) of indoor and outdoor air pollution sources; the development and in-field implementation of sensor-based networks for real-time monitoring of outdoor and indoor air pollutants; breath analysis in terms of VOCs and inorganic gaseous metabolites for early detection of chronic and oncologic diseases

Special Issue Information

Dear Colleagues,

In environmental, food, and pharmaceutical sciences, the development and rigorous validation of analytical methodologies are essential to the collection of reliable, accurate, and reproducible data, thereby safeguarding both product quality, environmental safety and human health. Air pollution, which is largely driven by anthropogenic activities, exerts profound yet often imperceptible effects on human health and ecosystems, while food may serve as a vector for contaminants that are difficult to detect and pose potential long-term health risks.

On the other hand, many foods are rich in bioactive compounds with proven preventive and therapeutic properties which contribute to overall human well-being. These compounds can be isolated for use in dietary supplements or incorporated directly into food products. Efficient extraction protocols are therefore crucial to fully exploit their nutritional and pharmacological potential. In this context, the valorization of plant- and animal-derived by-products from industrial processing waste is gaining increasing relevance, offering sustainable alternatives to conventional natural sources. Advancements in this area not only enhance extraction yields but also significantly reduce environmental impact.

This Special Issue, “Chromatography and Spectroscopy in Food, Environmental, and Pharmaceutical Sciences,” will address a broad spectrum of topics, including (but not limited to) the development of innovative chromatographic and spectroscopic techniques for the separation, identification, and quantification of bioactive compounds and environmental pollutants; advanced low-impact extraction approaches for the recovery of phytonutrients and/or removal of contaminants; and the practical application of these methodologies within the environmental, food, and pharmaceutical industries.

We welcome our colleagues to contribute original research articles and reviews to this Special Issue to provide the scientific community with the most recent advances in chromatography- and spectroscopy-based analytical strategies for the study of phytochemicals and pollutants across these interdisciplinary fields.

Dr. Antonella Maria Aresta
Dr. Alessia Di Gilio
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 250 words) can be sent to the Editorial Office for assessment.

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 single-anonymized peer-review process. A guide for authors and other relevant information for submission of manuscripts is available on the Instructions for Authors page. Molecules is an international peer-reviewed open access semimonthly 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

  • chromatographic techniques
  • phytochemicals
  • pollutants
  • mass spectrometry
  • functional foods
  • extraction techniques
  • biological assays
  • pollutant abatement
  • nutraceuticals or additives

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Published Papers (4 papers)

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Research

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18 pages, 705 KB  
Article
Aflatoxin M1 Enrichment in Buffalo Mozzarella and Ricotta: Case Study on Naturally Contaminated Milk and Exploratory Analysis of Sterigmatocystin and Aflatoxicol
by Maurizio Cossu, Stefano Sdogati, Andrea Sanna, Serenella Orsini, Ivan Pecorelli, Tommaso Pacini, Gilberto Giangolini, Roberto Condoleo, Carlo Boselli and Valentina D’Onofrio
Molecules 2026, 31(18), 3316; https://doi.org/10.3390/molecules31183316 (registering DOI) - 18 Sep 2026
Abstract
Mycotoxins, including sterigmatocystin (STC), aflatoxicol (AFL), aflatoxin B1 (AFB1), and its metabolite aflatoxin M1 (AFM1), represent a major food safety concern in the dairy industry due to their high toxicity and thermal stability. While AFM1 in [...] Read more.
Mycotoxins, including sterigmatocystin (STC), aflatoxicol (AFL), aflatoxin B1 (AFB1), and its metabolite aflatoxin M1 (AFM1), represent a major food safety concern in the dairy industry due to their high toxicity and thermal stability. While AFM1 in milk is strictly regulated, there is a substantial lack of specific guidelines and scientific data regarding its behavior and enrichment factors (EFs) in buffalo-derived products. Furthermore, knowledge gaps persist regarding the transfer and stability of co-occurring molecules like STC and AFL. This study evaluated the distribution and fate of AFM1, STC, and AFL during traditional, laboratory-scale cheesemaking of buffalo mozzarella and ricotta. Fourteen trials were conducted using bulk tank milk naturally contaminated with AFM1, alongside an exploratory trial utilizing toxin-free milk artificially spiked with all three targets. Mass balance and specific EFs were calculated across all processing streams. AFM1 was detected in all raw milk samples, showing a strong affinity for caseins. Approximately half of the initial milk AFM1 content was retained in mozzarella (50.3 ± 3.3%), whereas ricotta retained only a minor fraction (6.9 ± 0.7%), with the majority lost in the second whey (30.7 ± 1.3%). The mean EFs were 2.3 ± 0.3 for mozzarella and 1.1 ± 0.2 for ricotta. AFL was never detected in milk samples while STC was mainly present at concentrations < 1 ng/kg. In the spiked trial, AFL demonstrated stability with an EF of 1.5 in mozzarella, while STC displayed potential degradation within the milk matrix and during sample storage. The experimental EFs determined for buffalo mozzarella and ricotta are lower than the standard factors currently applied by Italian regulations for non-bovine dairy products. These accurate, matrix-specific estimations are essential to prevent the under-reporting of non-compliant samples and to refine international consumer risk assessment models. Full article
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17 pages, 1391 KB  
Article
A Validated LC-MS/MS Method for Simultaneous Determination of Cortisol and Cortisone in Grey Wolf Hair for Application in Ecological Studies
by Arkadiusz Jastrzębski, Kinga Ożga-Wybranowska, Rafał Łopucki, Sabina Nowak, Robert W. Mysłajek and Ilona Sadok
Molecules 2026, 31(14), 2420; https://doi.org/10.3390/molecules31142420 - 10 Jul 2026
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Abstract
Hair is an easily obtainable, non-invasive biomatrix that allows for the assessment of long-term physiological responses to environmental and anthropogenic stressors in wildlife populations. Herein, an ultra-high-performance liquid chromatography–electrospray ionization–tandem mass spectrometry (UHPLC-ESI-MS/MS) method was validated to verify its suitability for the simultaneous [...] Read more.
Hair is an easily obtainable, non-invasive biomatrix that allows for the assessment of long-term physiological responses to environmental and anthropogenic stressors in wildlife populations. Herein, an ultra-high-performance liquid chromatography–electrospray ionization–tandem mass spectrometry (UHPLC-ESI-MS/MS) method was validated to verify its suitability for the simultaneous determination of cortisol (CORT) and its metabolite, cortisone (CORN), in hair samples collected from wild-living grey wolves (Canis lupus). Hair samples were extracted with methanol and purified using solid-phase extraction on Strata-X cartridges, which enabled effective mitigation of matrix effects. Data for the glucocorticoids were normalized using internal standards. The method demonstrated good linearity for the target stress hormones, with satisfactory precision (RSD < 15%) and limits of quantification of 4.13 pg/mg for CORT and 2.49 pg/mg for CORN in the hair matrix. Analysis of authentic wolf hair samples revealed CORT and CORN concentrations in the ranges of <4.13–11.86 pg/mg and <2.49–3.67 pg/mg, respectively. The CORT results showed a strong positive correlation with those obtained using enzymatic immunoassays. The method may be applied to assess the impact of stressors on the welfare of wolves, e.g., providing a useful tool for monitoring recovering European populations as they face new challenges associated with expansion into potentially suboptimal habitats. Full article
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15 pages, 770 KB  
Article
Exploring the Volatile Fingerprinting of Young Portuguese Monovarietal Red Wines by HS-SPME-GC×GC-TOFMS: A Five-Year Study
by Sousa Gastão-Muchecha, Nuno Martins, Raquel Garcia and Maria João Cabrita
Molecules 2025, 30(24), 4814; https://doi.org/10.3390/molecules30244814 - 18 Dec 2025
Cited by 2 | Viewed by 1103
Abstract
The aroma of wine is a defining quality attribute, determined mainly by volatile organic compounds (VOCs) originating from grape metabolism, fermentation, and maturation. This study aimed to characterize the VOC composition of young monovarietal red wines from the Alentejo region (Portugal), produced from [...] Read more.
The aroma of wine is a defining quality attribute, determined mainly by volatile organic compounds (VOCs) originating from grape metabolism, fermentation, and maturation. This study aimed to characterize the VOC composition of young monovarietal red wines from the Alentejo region (Portugal), produced from Alicante Bouschet, Touriga Nacional, and Trincadeira across five consecutive vintages (2020–2024). Headspace solid-phase microextraction (HS-SPME) coupled with comprehensive two-dimensional gas chromatography–time-of-flight mass spectrometry (GC×GC-ToFMS) was applied for VOC profiling, followed by multivariate statistical analyses. A strict identification and reproducibility criterion was applied to ensure longitudinal consistency over the five vintages. MANOVA analysis revealed significant effects (p < 0.001) of both grape variety and vintage on VOC distribution. Esters were the most abundant and discriminant group, while aldehydes and terpenes contributed markedly to varietal differentiation. Alicante Bouschet wines were associated with fruity ethyl esters, Touriga Nacional with monoterpenes (citronellol, terpinolene, α-farnesene) and aromatic alcohols, and Trincadeira with aldehydes and sesquiterpenes. Canonical discriminant analysis (CDA) achieved clear separation among varieties and vintages, with the first two canonical functions accounting for over 70% of the total variance. Heatmap analysis highlighted distinctive terpene and C13-norisoprenoid profiles across samples. These findings demonstrate the pivotal role of VOCs in defining Alentejo wine typicity and support their use as chemical markers for authenticity and PDO valorization. Full article
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Review

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26 pages, 2973 KB  
Review
Chloramphenicol Residue Analysis in Food and Environmental Matrices: Regulatory Framework and Advances in Trace-Level Determination
by Antonella Maria Aresta, Nicoletta De Vietro, Giovanna Mancini and Carlo Zambonin
Molecules 2026, 31(9), 1440; https://doi.org/10.3390/molecules31091440 - 27 Apr 2026
Cited by 4 | Viewed by 1291
Abstract
Chloramphenicol is a broad-spectrum antimicrobial agent whose use in food-producing animals is prohibited in many countries due to its association with severe adverse effects, including idiosyncratic aplastic anemia and genotoxicity. Despite these restrictions, chloramphenicol residues continue to be detected in food products, environmental [...] Read more.
Chloramphenicol is a broad-spectrum antimicrobial agent whose use in food-producing animals is prohibited in many countries due to its association with severe adverse effects, including idiosyncratic aplastic anemia and genotoxicity. Despite these restrictions, chloramphenicol residues continue to be detected in food products, environmental compartments, and biological matrices, highlighting the need for reliable and sensitive analytical monitoring. This review provides a comprehensive overview of current analytical strategies for the detection of drugs in food and environmental samples, covering screening and confirmatory techniques, sample preparation approaches, and regulatory aspects. Rapid screening methods, such as enzyme-linked immunosorbent assays (ELISAs), lateral flow immunoassays (LFIAs), and biosensors based on antibodies, aptamers, and molecularly imprinted polymers, enable fast and cost-effective preliminary detection. Recent advances in nanomaterials and signal amplification strategies, including fluorescent reporters and surface-enhanced Raman scattering (SERS), have significantly improved sensitivity and assay performance. However, confirmatory methods based on liquid chromatography coupled with tandem mass spectrometry (LC–MS/MS) remain the reference standard due to their superior selectivity, sensitivity, and quantitative reliability. Attention is given to sample preparation workflows, including QuEChERS-based protocols and microextraction techniques, which enable efficient analysis of complex matrices. Finally, current regulatory frameworks and analytical challenges related to zero-tolerance policies are discussed, emphasizing the importance of robust and validated analytical methods for effective monitoring and food safety assurance. Full article
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