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Analytical Methods for Food and Environmental Pollutants: Current and Future Perspectives

A special issue of Molecules (ISSN 1420-3049). This special issue belongs to the section "Analytical Chemistry".

Deadline for manuscript submissions: 31 July 2025 | Viewed by 6522

Special Issue Editors

Dr. Julia Martín

E-Mail Website
Guest Editor
Departamento de Química Analítica, Universidad de Sevilla, E-41011 Sevilla, Spain
Interests: analytical chemistry; food and environmental chemistry; method development; sample preparation; chromatographic techniques; chemometrics
Special Issues, Collections and Topics in MDPI journals
Prof. Dr. Esteban Alonso

E-Mail Website
Guest Editor
Departamento de Química Analítica, Escuela Politécnica Superior, Universidad de Sevilla, C/Virgen de África 7, E-41011 Sevilla, Spain
Interests: environmental analytical chemistry; separation methods (GC-MS/MS, LC–MS/MS); sample treatment; priority and emerging pollutants (organic compounds, metals and radioisotopes)
Special Issues, Collections and Topics in MDPI journals

Special Issue Information

Dear Colleagues,

Modern analytical chemistry has been described as an effort to detect an increasing number of exotic and emerging contaminants at trace levels. The acquisition of accurate chemical data in food and environmental systems and effective management of pollutants are essential for food quality and safety and for environmental preservation, respectively. This special issue aims to cover the most significant developments and innovative use of analytical methods to investigate relevant pollutants. Contributions focusing on the following areas of pollutant analysis are warmly invited:

  • Sampling (passive sampling, improving sample representativeness).
  • Sample preparation (new developments for enhanced solvent extractions, alternative phases for sorptive extractions, new configurations and strategies in microextractions).
  • Analytical instrumentation (hyphenated techniques using mass spectrometry for organic pollutants, atomic spectrometry for trace metals and metalloids, sensors and biosensors in field pollution control).
  • Chemometric tools (quantitative methods and statistical evaluation).
Dr. Julia Martín

Prof. Dr. Esteban Alonso
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 single-blind 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

  • emerging pollutants
  • food samples
  • environmental samples
  • sampling
  • sample preparation
  • analytical instrumentation
  • chemometric tools

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Published Papers (6 papers)

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Research

16 pages, 969 KiB  
Article
Green Analytical Method Using Single-Drop Microextraction Followed by Gas Chromatography for Nitro Compound Detection in Environmental Water and Forensic Rinse Water
by Tamara Pócsová, Senad Okanovič and Svetlana Hrouzková
Molecules 2025, 30(9), 1894; https://doi.org/10.3390/molecules30091894 - 24 Apr 2025
Viewed by 181
Abstract
The extensive use of nitro compounds in agriculture, industry, armaments, and pharmaceuticals, along with their toxic effects on living organisms, necessitates efficient and environmentally sustainable analytical methods. Traditional extraction techniques often involve practices that are not eco-friendly, such as the use of large [...] Read more.
The extensive use of nitro compounds in agriculture, industry, armaments, and pharmaceuticals, along with their toxic effects on living organisms, necessitates efficient and environmentally sustainable analytical methods. Traditional extraction techniques often involve practices that are not eco-friendly, such as the use of large volumes of solvents, toxic chemicals, and the generation of significant waste; therefore, the single-drop microextraction technique was involved in overcoming these limitations. This study shows an environmentally friendly method for nitro compound analysis focusing on NB (Nitrobenzene), 2-NT (2-Nitrotoluene), 3-NT (3-Nitrotoluene), 4-NT (4-Nitrotoluene), 1,3-DNB (1,3-Dinitrobenzene), 1,2-DNB (1,2-Dinitrobenzene), 2,4-DNT (2,4-Dinitrotoluene), and TNT (Trinitrotoluene). To separate and to detect selected nitro compounds, gas chromatography with an electron capture detector was utilized, which is highly selective for analytes containing nitro groups. To determine optimal experimental conditions, extraction parameters were studied, including the impact of salt addition, temperature, and pH on extraction efficiency. Key performance parameters, such as limit of detection (LOD), limit of quantification (LOQ), repeatability, extraction recoveries, calibration range, and matrix effects, were assessed. The LOD values ranged from 0.01 to 0.09 μg/L in deionized water, 0.01 to 0.06 μg/L in tap water, 0.01 to 0.03 μg/L in seawater, and 0.03 to 0.11 μg/L in model forensic rinse water. The optimized method was successfully applied to the determination of nitro compounds in real environmental water samples and forensic rinse water samples. The environmental sustainability and greenness of the proposed method was evaluated with the AGREE, AGREEprep, and AESA techniques. Full article
(This article belongs to the Special Issue Analytical Methods for Food and Environmental Pollutants: Current and Future Perspectives)
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11 pages, 1685 KiB  
Article
Unambiguous Determination of Benzo[a]pyrene and Dibenzo[a,l]pyrene in HPLC Fractions via Room-Temperature Fluorescence Excitation–Emission Matrices
by George T. Knecht, Stephanie D. Nauth, Juan C. Gomez Alvarado, Anthony M. Santana, Hector C. Goicoechea and Andres D. Campiglia
Molecules 2025, 30(7), 1550; https://doi.org/10.3390/molecules30071550 - 31 Mar 2025
Cited by 1 | Viewed by 247
Abstract
When high-performance liquid chromatography (HPLC) is used for the analysis of polycyclic aromatic hydrocarbons (PAHs) in complex samples, further examination of HPLC fractions is recommended to confirm PAH assignments solely based on retention times. Gas chromatography–mass spectrometry (GC-MS) has been particularly relevant in [...] Read more.
When high-performance liquid chromatography (HPLC) is used for the analysis of polycyclic aromatic hydrocarbons (PAHs) in complex samples, further examination of HPLC fractions is recommended to confirm PAH assignments solely based on retention times. Gas chromatography–mass spectrometry (GC-MS) has been particularly relevant in the unambiguous determination of PAHs with remarkably similar retention times. The combination of HPLC and GC requires lengthy analysis times to ensure proper assignments. This article presents an approach for the analysis of co-eluted PAHs with no need for further chromatographic separation. Benzo[a]pyrene (BaP) and dibenzo[a,l]pyrene (DBalP) were directly determined in a co-eluted HPLC fraction via room-temperature fluorescence excitation–emission matrices (RTF-EEMs). RTF-EEMs can be recorded in a matter of seconds with a spectrofluorometer equipped with a multichannel detection system. The spectral overlapping of BaP and DBalP was resolved using parallel factor analysis (PARAFAC). The analytical advantages of this approach were demonstrated with the trace analysis (ng/mL) of these two PAHs in pre-concentrated tobacco extracts. Full article
(This article belongs to the Special Issue Analytical Methods for Food and Environmental Pollutants: Current and Future Perspectives)
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11 pages, 3351 KiB  
Article
Emulsive Liquid–Liquid Microextraction for the Determination of Phthalic Acid Esters in Environmental Water Samples
by Xinyuan Bi, Chi Zhang, Xiaorong Xue, Shangjun Su, Zhiping Yang, Xu Jing and Qiang Zhang
Molecules 2024, 29(24), 5908; https://doi.org/10.3390/molecules29245908 - 14 Dec 2024
Cited by 1 | Viewed by 743
Abstract
A convenient, rapid, and environmentally friendly method, emulsive liquid–liquid microextraction combined with high-performance liquid chromatography, was established to determine phthalic acid esters in tap, river, lake, and sea water. After the method’s optimization, we obtained the appropriate volume of the extractant and pure [...] Read more.
A convenient, rapid, and environmentally friendly method, emulsive liquid–liquid microextraction combined with high-performance liquid chromatography, was established to determine phthalic acid esters in tap, river, lake, and sea water. After the method’s optimization, we obtained the appropriate volume of the extractant and pure water, the number of strokes, the separation methods, the mass volume fraction of the demulsifier, the demulsifier volume, the sample volume, the salt amount, and the pH conditions. This method requires only 200 μL of heptanoic acid (fatty acid) as the extractant and 75 mg of sodium acetate as demulsifiers for fast microextraction and separation, respectively, avoiding the use of further equipment. Emulsive liquid–liquid microextraction offers substantial advantages over dispersive liquid–liquid microextraction by eliminating the need for toxic dispersants, thereby preventing any influences of dispersants on the partition coefficients. The linear range of detection ranged from 0.5 to 50 μg L−1, with a limit of detection of 0.2 μg L−1 and a limit of quantitation of 0.5 μg L−1. The recoveries ranged from 80.2% to 106.3%, and the relative standard deviations ranged between 0.5% and 6.7%. Five greenness metrics confirmed that this method is environmentally friendly and aligns with the principles of green analytical chemistry. The proposed method achieved a greenness score of 8.42, surpassing that of other methods as evaluated using the SPMS. The novel method may well be a valuable technique for determining phthalic acid esters in water samples. Full article
(This article belongs to the Special Issue Analytical Methods for Food and Environmental Pollutants: Current and Future Perspectives)
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18 pages, 1625 KiB  
Article
Systematic Comparison of Extract Clean-Up with Currently Used Sorbents for Dispersive Solid-Phase Extraction
by Michelle Peter and Christoph Müller
Molecules 2024, 29(19), 4656; https://doi.org/10.3390/molecules29194656 - 30 Sep 2024
Cited by 3 | Viewed by 1155
Abstract
Dispersive solid-phase extraction (dSPE) is a crucial step for multiresidue analysis used to remove matrix components from extracts. This purification prevents contamination of instrumental equipment and improves method selectivity, sensitivity, and reproducibility. Therefore, a clean-up step is recommended, but an over-purified extract can [...] Read more.
Dispersive solid-phase extraction (dSPE) is a crucial step for multiresidue analysis used to remove matrix components from extracts. This purification prevents contamination of instrumental equipment and improves method selectivity, sensitivity, and reproducibility. Therefore, a clean-up step is recommended, but an over-purified extract can lead to analyte loss due to adsorption to the sorbent. This study provides a systematic comparison of the advantages and disadvantages of the well-established dSPE sorbents PSA, GCB, and C18 and the novel dSPE sorbents chitin, chitosan, multi-walled carbon nanotube (MWCNT), and Z-Sep® (zirconium-based sorbent). They were tested regarding their clean-up capacity by visual inspection, UV, and GC-MS measurements. The recovery rates of 98 analytes, including pesticides, active pharmaceutical ingredients, and emerging environmental pollutants with a broad range of physicochemical properties, were determined by GC-MS/MS. Experiments were performed with five different matrices, commonly used in food analysis (spinach, orange, avocado, salmon, and bovine liver). Overall, Z-Sep® was the best sorbent regarding clean-up capacity, reducing matrix components to the greatest extent with a median of 50% in UV and GC-MS measurements, while MWCNTs had the largest impact on analyte recovery, with 14 analytes showing recoveries below 70%. PSA showed the best performance overall. Full article
(This article belongs to the Special Issue Analytical Methods for Food and Environmental Pollutants: Current and Future Perspectives)
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12 pages, 990 KiB  
Article
Multiclass Analysis for the Determination of Pharmaceuticals and Their Main Metabolites in Leafy and Root Vegetables
by Carmen Mejías, Marina Arenas, Julia Martín, Juan Luis Santos, Irene Aparicio and Esteban Alonso
Molecules 2024, 29(15), 3471; https://doi.org/10.3390/molecules29153471 - 24 Jul 2024
Viewed by 1166
Abstract
The irrigation of soils with reclaimed contaminated wastewater or its amendment with sewage sludge contributes to the uptake of pharmaceuticals by vegetables growing in the soil. A multiresidue method has been devised to determine five pharmaceuticals and nine of their main metabolites in [...] Read more.
The irrigation of soils with reclaimed contaminated wastewater or its amendment with sewage sludge contributes to the uptake of pharmaceuticals by vegetables growing in the soil. A multiresidue method has been devised to determine five pharmaceuticals and nine of their main metabolites in leafy and root vegetables. The method employs ultrasound-assisted extraction, clean-up via dispersive solid-phase extraction, and analysis through liquid chromatography–tandem mass spectrometry. Box–Behnken design was used to refine variables such as extraction solvent volume, time of extraction, number of extraction cycles, and the type and amount of d-SPE sorbent. The method achieved linearity (R2) greater than 0.994, precision (relative standard deviation) under 16% for most compounds, and detection limits ranging from 0.007 to 2.25 ng g−1 dry weight. This method was applied to a leafy vegetable (lettuce) and to a root vegetable (carrot) sourced from a local market. Parent compounds were detected at higher concentrations than their metabolites, with the exception of carbamazepine-10,11-epoxide. Full article
(This article belongs to the Special Issue Analytical Methods for Food and Environmental Pollutants: Current and Future Perspectives)
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9 pages, 1653 KiB  
Article
Sorption of Polycyclic Aromatic Sulfur Heterocycles (PASH) on Nylon Microplastics at Environmentally Relevant Concentrations
by Stephanie D. Nauth and Andres D. Campiglia
Molecules 2024, 29(7), 1653; https://doi.org/10.3390/molecules29071653 - 7 Apr 2024
Viewed by 1460
Abstract
Microplastics have garnered an infamous reputation as a sorbate for many concerning environmental pollutants and as a delivery vehicle for the aquatic food chain through the ingestion of these contaminated small particulates. While sorption mechanisms have been extensively studied for polycyclic aromatic hydrocarbons, [...] Read more.
Microplastics have garnered an infamous reputation as a sorbate for many concerning environmental pollutants and as a delivery vehicle for the aquatic food chain through the ingestion of these contaminated small particulates. While sorption mechanisms have been extensively studied for polycyclic aromatic hydrocarbons, polycyclic aromatic sulfur heterocycles (PASHs) have not been investigated, partly due to their low concentrations in aquatic ecosystems. Herein, an analytical methodology is presented for the analysis of dibenzothiophene, benzo[b]naphtho[1,2-b]thiophene, benzo[b]naphtho[2,1-b]thiophene, benzo[b]naphtho[2,3-b]thiophene, chryseno[4,5-bcd]thiophene and dinaphtho[1,2-b:1′,2′-d]thiophene at relevant environmental concentrations based on solid phase extraction and high-performance liquid chromatography. The sorption uptake behavior and the sorption kinetics of the three benzo[b]napthothiophene isomers were then investigated on nylon microplastics to provide original information on their environmental fate and avoid human contamination through the food chain. The obtained information might also prove relevant to the development of successful remediation approaches for aquatic ecosystems. Full article
(This article belongs to the Special Issue Analytical Methods for Food and Environmental Pollutants: Current and Future Perspectives)
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