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High-Throughput Analytical and Separation Approaches for the Determination of Organic...
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High-Throughput Analytical and Separation Approaches for the Determination of Organic Contaminants in Environmental Samples

A special issue of Separations (ISSN 2297-8739). This special issue belongs to the section "Environmental Separations".

Deadline for manuscript submissions: closed (30 April 2023) | Viewed by 9535

Special Issue Editors

Dr. Massimo Del Bubba

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Guest Editor
Department of Chemistry, Università degli Studi di Firenze, Florence, Italy
Interests: liquid chromatography; gas chromatography; mass spectrometry; environmental analytical chemistry; food analytical chemistry
Dr. Fabio Gosetti

E-Mail Website
Guest Editor
Department of Earth and Environmental Sciences, University of Milano-Bicocca, 20126 Milano, Italy
Interests: HPLC/MS; UHPLC/MS; mass spectrometry; unknown degradation products of pesticides; environmental pollutants; non-target analysis; method development and validation; food analysis
Special Issues, Collections and Topics in MDPI journals

Special Issue Information

Dear Colleagues,

Modern environmental analytical chemistry must increasingly face the demand of analytical methods which are not only accurate, precise, and robust, but also characterized by high analytical throughput. In this context, in recent years, various analytical approaches have been developed for the rapid determination of organic micropollutants in environmental samples, also by automated procedures (e.g., QuEChERS extractions, solid phase microextraction, and online solid phase extraction coupled with gas and/or liquid chromatography). 

This Special Issue aims at collecting contributions on the most recent advances in the field of separation science applied to the analysis of organic micropollutants in environmental samples. Topics of interest include but are not limited to the development and optimization of extraction, clean-up, and instrumental analysis methods for environmental samples, as well as application of advanced chemometrics tools for method set-up. Analytical methods devoted to the analysis of micropollutants in food samples are also welcome since they are informative on human exposure to environmental contamination.

This Special Issue aims to provide readers with a selection of papers that represent the current state of the art of analytical methods devoted to the determination of organic micropollutants in environmental matrices.

Dr. Massimo Del Bubba
Dr. Fabio Gosetti
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. Separations 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 2600 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

  • solid phase extraction
  • solid phase microextraction
  • QuEChERS
  • microwave extraction
  • ultrasound assisted extraction
  • gas chromatography
  • liquid chromatography
  • mass spectrometry
  • environmental monitoring
  • food safety

Published Papers (4 papers)

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Research

14 pages, 2462 KiB  
Article
Online Membrane Sampling for the Mass Spectrometric Analysis of Oil Sands Process Affected Water-Derived Naphthenic Acids in Real-World Samples
by Joseph Monaghan, Dylan Steenis, Ian J. Vander Meulen, Kerry M. Peru, John V. Headley, Chris G. Gill and Erik T. Krogh
Separations 2023, 10(4), 228; https://0-doi-org.brum.beds.ac.uk/10.3390/separations10040228 - 25 Mar 2023
Viewed by 1099
Abstract
Large volumes of oil sands process-affected waters (OSPW) result from heavy oil extraction in Alberta, Canada. Currently, a toxic legacy of ca. 500 Mm3 is stored in tailings ponds under a zero-discharge policy. OSPW is a complex mixture of suspended and dissolved [...] Read more.
Large volumes of oil sands process-affected waters (OSPW) result from heavy oil extraction in Alberta, Canada. Currently, a toxic legacy of ca. 500 Mm3 is stored in tailings ponds under a zero-discharge policy. OSPW is a complex mixture of suspended and dissolved materials including a wide range of inorganic and organic contaminants. Classically defined naphthenic acids (NAs; CnH2n+ZO2) are one of the primary toxic fractions in OSPW and have therefore been the subject of considerable research interest. Most studies employ considerable sample cleanup followed by liquid chromatography and/or high-resolution mass spectrometry (HRMS) for the characterization of these complex mixtures. However, these strategies can be time- and cost-intensive, limiting the scope of research and adoption for regulatory purposes. Condensed phase membrane introduction mass spectrometry (CP-MIMS) is emerging as a “fit-for-purpose” approach for the analysis of NAs. This technique directly interfaces the mass spectrometer with an aqueous sample using a hydrophobic semi-permeable membrane, requiring only pH adjustment to convert NAs to a membrane-permeable form. Here, we examine the perm-selectivity of classical NAs (O2) relative to their more oxidized counterparts (O3–O7) and heteroatomic (N, S) species collectively termed naphthenic acid fraction compounds (NAFCs). The investigation of 14 model compounds revealed that classically defined NAs are greater than 50-fold more membrane permeable than their oxidized/heteroatomic analogs. HRMS analysis of real OSPW extracts with and without membrane clean-up further supported selectivity towards the toxic O2 class of NAs, with >85% of the overall signal intensity attributable to O2 NAs in the membrane permeate despite as little as 34.7 ± 0.6% O2 NAs observed in the directly infused mixture. The information collected with HRMS is leveraged to refine our method for analysis of NAs at unit mass resolution. This new method is applied to 28 archived real-world samples containing NAs/NAFCs from constructed wetlands, OSPW, and environmental monitoring campaigns. Concentrations ranged from 0–25 mg/L O2 NAs and the results measured by CP-MIMS (unit mass) and SPE-HRMS (Orbitrap) showed good agreement (slope = 0.80; R2 = 0.76). Full article
(This article belongs to the Special Issue High-Throughput Analytical and Separation Approaches for the Determination of Organic Contaminants in Environmental Samples)
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11 pages, 518 KiB  
Article
Release of Selected Non-Intentionally Added Substances (NIAS) from PET Food Contact Materials: A New Online SPE-UHPLC-MS/MS Multiresidue Method
by Riccardo Aigotti, Nicola Giannone, Alberto Asteggiano, Enrica Mecarelli, Federica Dal Bello and Claudio Medana
Separations 2022, 9(8), 188; https://0-doi-org.brum.beds.ac.uk/10.3390/separations9080188 - 23 Jul 2022
Cited by 2 | Viewed by 2461
Abstract
Food contact materials (FCMs) are an underestimated source of food chemical contaminants and a potentially relevant route of human exposure to chemicals that are harmful to the endocrine system. Foods and water are the main sources of exposure due to contact with the [...] Read more.
Food contact materials (FCMs) are an underestimated source of food chemical contaminants and a potentially relevant route of human exposure to chemicals that are harmful to the endocrine system. Foods and water are the main sources of exposure due to contact with the packaging materials, often of polymeric nature. European Regulation 10/2011 requires migration tests on FCMs and foodstuffs to evaluate the presence of listed substances (authorized monomers and additives) and non-intentionally added substances (NIAS) not listed in the regulation and not subjected to restrictions. The tests are required to ensure the compliance of packaging materials for the contained foods. NIAS are a heterogeneous group of substances classified with a potential estrogenic or androgenic activity. Subsequently, the evaluation of the presence of these molecules in foods and water is significant. Here we present an online SPE/UHPLC-tandem MS method to quantify trace levels of NIAS in food simulants (A: aqueous 3% acetic acid; B: aqueous 20% ethanol) contained in PET preformed bottles. The use of online SPE reduces systemic errors thanks to the automation of the technique. For the developed analytical method, we evaluate the limit of detection (LOD), the limit of quantitation (LOQ), selectivity, RSD% and BIAS% for LLOQ for a total of twelve NIAS, including monomers, antioxidants, UV-filters and additives. LOD ranged between 0.002 µg/L for bisphenol S and 13.6 µg/L for 2,6-di-tert-butyl-4-methylphenol (BHT). LOQs are comprised between 0.01 µg/L for bisphenol S and 42.2 µg/L for BHT. The online-SPE/UHPLC-tandem MS method is applied to the food simulants contained in several types of PET packaging materials to evaluate the migration of the selected NIAS. The results show the presence (µg/L) of NIAS in the tested samples, underlining the need for a new regulation for these potentially toxic molecules. Full article
(This article belongs to the Special Issue High-Throughput Analytical and Separation Approaches for the Determination of Organic Contaminants in Environmental Samples)
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15 pages, 1207 KiB  
Article
Optimization and Validation of a Method Based on QuEChERS Extraction and Gas Chromatographic-Mass Spectrometric Analysis for the Determination of Polycyclic Aromatic Hydrocarbons and Polychlorinated Biphenyls in Olive Fruits Irrigated with Treated Wastewaters
by Maria Concetta Bruzzoniti, Luca Rivoira, Michele Castiglioni, Enrico Cagno, Ahmed Kettab, Donatella Fibbi and Massimo Del Bubba
Separations 2022, 9(3), 82; https://0-doi-org.brum.beds.ac.uk/10.3390/separations9030082 - 21 Mar 2022
Cited by 3 | Viewed by 2628
Abstract
The wastewater reuse is an important measure to face water shortage, thus improving the resilience of agricultural production chains. However, treated wastewater can contain residual organic micropollutants residues that may result in crop contamination. Among edible crops, olive is the most important agricultural [...] Read more.
The wastewater reuse is an important measure to face water shortage, thus improving the resilience of agricultural production chains. However, treated wastewater can contain residual organic micropollutants residues that may result in crop contamination. Among edible crops, olive is the most important agricultural product in the Mediterranean region. Methods to assess the contamination of organic micropollutants such as polycyclic aromatic hydrocarbons (PAHs) and polychlorinated biphenyls (PCBs) in olives are poorly investigated. Given the complexity of olives, this study focused on the development and validation of a method for the simultaneous extraction of PAHs and PCBs from olives, and subsequent analysis by gas chromatography coupled with mass spectrometry detection. Extraction was optimized through a QuEChERS protocol, studying the effect of the extraction solvent (CH2Cl2, cyclohexane, CH3CN) and of the dispersive-solid phase extraction (d-SPE) sorbent (octadecyl silica, Florisil, primary secondary amine, Z-Sep) on the recovery of micropollutants. The best recoveries (94–122%, relative standard deviations below 5%) were obtained using CH3CN/H2O and a double purification step with Z-Sep and Florisil. The method developed for PAHs and PCBs, which showed good intra-day (<2.7%) and inter-day (<2.9%) precision and low matrix effect (|ME| < 14%), was applied to the analysis of olives grown by irrigation with reclaimed wastewaters. Full article
(This article belongs to the Special Issue High-Throughput Analytical and Separation Approaches for the Determination of Organic Contaminants in Environmental Samples)
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15 pages, 8184 KiB  
Article
Fabric Phase Sorptive Extraction for the Determination of Anthracyclines in Sewage
by Sergio Santana-Viera, Alejandro Canino-Byreing, María Esther Torres-Padrón, Zoraida Sosa-Ferrera, José Juan Santana-Rodríguez, Abuzar Kabir and Kenneth G. Furton
Separations 2022, 9(3), 69; https://0-doi-org.brum.beds.ac.uk/10.3390/separations9030069 - 04 Mar 2022
Cited by 2 | Viewed by 2281
Abstract
Anthracyclines are a group of antineoplastic compounds used to treat acute leukemia and other cancers, and they are excreted after consumption by patients. These chemicals are often found in sewage at very low concentration levels. For this reason, the development of sensitive analytical [...] Read more.
Anthracyclines are a group of antineoplastic compounds used to treat acute leukemia and other cancers, and they are excreted after consumption by patients. These chemicals are often found in sewage at very low concentration levels. For this reason, the development of sensitive analytical methodologies capable of determining them at low concentrations is of prime importance. A simple, fast and sensitive analytical method using fabric phase sorptive extraction (FPSE) followed by ultra-high performance liquid chromatography with fluorescence detection (UHPLC-FD) has been developed and validated for the extraction of anthracyclines from sewage samples. FPSE is a green, cheap, simple, selective and rapid sample preparation technique. The different parameters that affect the performance of the FPSE process, including extraction time, eluting solvent, elution time and pH, were optimized. The developed method showed satisfactory reproducibility, with intraday and interday RSD values lower than 15% for all the compounds and limits of detection between 0.1–0.15 µg·L−1. The unique combination of sample preparation by this micro-extraction technique with fluorescence detector have resulted in the satisfactory extraction of highly polar anthracyclines, without any noticeable matrix effect, a very common shortcoming of exhaustive sample preparation technique such as solid phase extraction (SPE) and mass spectrometry. Full article
(This article belongs to the Special Issue High-Throughput Analytical and Separation Approaches for the Determination of Organic Contaminants in Environmental Samples)
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