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Applications of Chromatographic Techniques in Biological, Food and Environmental Samples

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Special Issue Information
Keywords
Published Papers

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

Deadline for manuscript submissions: closed (30 April 2022) | Viewed by 22063

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Special Issue Editors

Prof. Dr. Valentina Fernandes Domingues

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Guest Editor

REQUIMTE/LAQV, Instituto Superior de Engenharia do Porto, Politécnico do Porto, 4249-015 Porto, Portugal
Interests: endocrine disruptors; pesticides, flame retardants; synthetic musks; plasticizers; sample preparation
Special Issues, Collections and Topics in MDPI journals

Prof. Dr. Manuela Correia

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Guest Editor

REQUIMTE/LAQV, Instituto Superior de Engenharia do Porto, Politécnico do Porto, 4249-015 Porto, Portugal
Interests: Analytical chemistry; chromatography; sample preparation; environmental chemistry; food safety; micropollutants; pesticides; pharmaceuticals

Special Issue Information

Dear Colleagues,

In the last century, chromatography has evolved in many ways and has contributed to enlarging scientific knowledge about our world. Since the first applications made by Tswett, significant changes have occurred in the equipment, detector, and column technology. Moreover, sample preparation has also evolved towards simple, greener, miniaturized and less expensive methods, being an essential aspect of chromatography in the development of new analytical methodologies.

Nowadays, chromatography is a powerful analytical tool that enables researchers to determine pollutants and drugs at trace levels, and also to identify new compounds and to characterize the composition of different matrices, such as biological, food and environmental samples. The number of analytes reported in the literature is increasing annually, with many of them present at low concentrations, making the analysis of samples evermore challenging.

This Special Issue is intended to provide a forum for reporting state-of-the-art developments of chromatographic techniques and sample preparation in biological, food, and environmental samples considering a broad perspective from experts in the fields of biomonitoring, food quality, food safety, health, and environmental research.

We invite researchers to contribute to this Special Issue with original research articles and reviews on a few pertinent topics, including but not limited to:

- Biomonitoring

- Food quality

- Food safety

- Health

- Micropollutants

- Endocrine disruptors

- Pesticides

- Pharmaceuticals

- Environmental samples

- Biological samples characterization

Prof. Dr. Valentina Fernandes Domingues
Prof. Dr. Manuela Correia
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

Chromatography
Food
Environment
Biological samples
Pollutants
Endocrine disruptors

Published Papers (9 papers)

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Research

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18 pages, 2884 KiB

Open AccessArticle

Unveiling Chemical Cues of Insect-Tree and Insect-Insect Interactions for the Eucalyptus Weevil and Its Egg Parasitoid by Multidimensional Gas Chromatographic Methods

by Davide Mendes, Sofia Branco, Maria Rosa Paiva, Stefan Schütz, Eduardo P. Mateus and Marco Gomes da Silva

Molecules 2022, 27(13), 4042; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules27134042 - 23 Jun 2022

Cited by 1 | Viewed by 1583

Abstract

Multidimensional gas chromatography is, presently, an established and powerful analytical tool, due to higher resolving power than the classical 1D chromatographic approaches. Applied to multiple areas, it allows to isolate, detect and identify a larger number of compounds present in complex matrices, even in trace amounts. Research was conducted to determine which compounds, emitted by host plants of the eucalyptus weevil, Gonipterus platensis, might mediate host selection behavior. The identification of a pheromone blend of G. platensis is presented, revealing to be more attractive to weevils of both sexes, than the individual compounds. The volatile organic compounds (VOCs) were collected by headspace solid phase microextraction (HS-SPME), MonoTrap^TM disks, and simultaneous distillation-extraction (SDE). Combining one dimensional (1D) and two-dimensional (2D) chromatographic systems—comprehensive and heart-cut two-dimensional gas chromatography (GC×GC and H/C-MD-GC, respectively) with mass spectrometry (MS) and electroantennographic (EAD) detection, enabled the selection and identification of pertinent semiochemicals which were detected by the insect antennal olfactory system. The behavioral effect of a selected blend of compounds was assessed in a two-arm olfactometer with ten parallel walking chambers, coupled to video tracking and data analysis software. An active blend, composed by cis and trans-verbenol, verbenene, myrtenol and trans-pinocarveol was achieved. Full article

(This article belongs to the Special Issue Applications of Chromatographic Techniques in Biological, Food and Environmental Samples)

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14 pages, 1294 KiB

Open AccessArticle

Determination of Glycerophospholipids in Biological Material Using High-Performance Liquid Chromatography with Charged Aerosol Detector HPLC-CAD—A New Approach for Isolation and Quantification

by Magdalena Rosłon, Małgorzata Jaworska and Elżbieta L. Anuszewska

Molecules 2022, 27(10), 3356; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules27103356 - 23 May 2022

Cited by 2 | Viewed by 2731

Abstract

The method of using high-performance liquid chromatography with a charged aerosol detector method (HPLC-CAD) was developed for the separation and determination of phospholipids isolated from cell membranes. The established cell lines—normal and neoplastic prostate cells and normal skin fibroblasts and melanoma cells—were selected for the study. Chromatographic separation was performed in the diol stationary phase using a gradient elution based on a mixture of n-hexane, isopropanol and water with the addition of triethylamine and acetic acid as buffer additives. Taking the elements of the Folch and Bligh–Dyer methods, an improved procedure for lipid isolation from biological material was devised. Ultrasound-assisted extraction included three extraction steps and changed the composition of the extraction solvent, which led to higher recovery of the tested phospholipids. This method was validated by assessing the analytical range, precision, intermediate precision and accuracy. The analytical range was adjusted to the expected concentrations in cell extracts of various origins (from 40 µg/mL for PS up to 10 mg/mL for PC). Both precision and intermediate precision were at a similar level and ranged from 3.5% to 9.0%. The recovery for all determined phospholipids was found to be between 95% and 110%. The robustness of the method in terms of the use of equivalent columns was also confirmed. Due to the curvilinear response of CAD, the quantification was based on an internal standard method combined with a power function transformation of the normalized peak areas, allowing the linearization of the signal with an R² greater than 0.996. The developed method was applied for the isolation and determination of glycerophospholipids from cell membranes, showing that the profile of the tested substances was characteristic of various types of cells. This method can be used to assess changes in metabolism between normal cells and neoplastic cells or cells with certain pathologies or genetic changes. Full article

(This article belongs to the Special Issue Applications of Chromatographic Techniques in Biological, Food and Environmental Samples)

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13 pages, 1918 KiB

Open AccessArticle

Chromatographic Determination of Total Selenium in Biofortified Allium sp. following Piazselenol Formation and Micro-Solid-Phase Extraction

by Bogdan M. Bosca and Augustin C. Mot

Molecules 2021, 26(21), 6730; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules26216730 - 06 Nov 2021

Cited by 1 | Viewed by 2065

Abstract

Herein, a method based on selective piazselenol formation is applied for total selenium determination in biofortified Allium species. Piazselenol is formed by reacting Se(IV) with an aromatic diamine, namely 4-nitro-1,2-phenylenediamine, in acidic medium. Samples were digested in a nitric acid/hydrogen peroxide open system, followed by selenate reduction in hydrochloric acid. Reaction conditions were optimized in terms of pH, temperature, reaction time, and other auxiliary reagents for interference removal, namely, EDTA and hydroxylamine. For the extraction of the selectively formed 4-nitro-piazselenol, micro-solid-phase extraction (μSPE) was applied, and the analysis and detection of the corresponding complex was performed by HPLC coupled with DAD. An external standard calibration curve was developed (R² = 0.9994) with good sensitivity, and was used to calculate the total selenium content from several Allium plants material, with good intermediate precision (RSD% < 16%). The accuracy of the method was evaluated using both, a comparison with an accepted reference method from our previously published data, as well as three certified reference material with recoveries between 84–126%. The limit of detection was determined to be 0.35 μg/g (in solids) and 1.1 μg/L (in solution), while the limit of quantification was 1.07 μg/g and 3.4 μg/L (in solution). Using the proposed method, selenium content can be quickly and accurately determined in several types of samples. In addition, this study present experimental conditions for overcoming the interferences that might be encountered in selenium determination using piazselenol. Full article

(This article belongs to the Special Issue Applications of Chromatographic Techniques in Biological, Food and Environmental Samples)

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15 pages, 319 KiB

Open AccessArticle

Validation and Evaluation of Selected Organic Pollutants in Shrimp and Seawater Samples from the NW Portuguese Coast

by Maria Luz Maia, Cristina Delerue-Matos, Conceição Calhau and Valentina Fernandes Domingues

Molecules 2021, 26(19), 5774; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules26195774 - 23 Sep 2021

Cited by 4 | Viewed by 1815

Abstract

The development of coastal regions has contributed to the intensification of environmental contamination, which can accumulate in aquatic biota, such as shrimps. These crustaceans, besides being delicious and being a good source of nutrients, can also accumulate environmental pollutants. Amongst others, these include organochlorine pesticides (OCPs), organophosphorus pesticides (OPPs), brominated flame retardants (BFRs), polychlorinated biphenyls (PCBs) and synthetic musks (SMs). These pollutants, classified as endocrine disruptors, are related to adverse effects in humans and since one of the major routes of exposition is ingestion, this is a cause for concern regarding their presence in food. The aim of the present study was to quantify the presence of environmental pollutants in shrimp samples and in the water from their habitat along the northwest Portuguese coast. In seawater samples, only two OCPs (lindane and DDD) and one BFR (BTBPE) were detected, and in shrimp samples, one OCP (DDD) and three SMs (HHCB, AHTN and ketone) were found. Bioaccumulation and the risk assessment of dietary exposure of SMs in shrimp samples were investigated. It was observed that all shrimp samples analyzed significantly presented bioaccumulation of the three SMs found. Concentrations of SMs detected in shrimp samples do not present a health risk for the adult Portuguese population. Full article

(This article belongs to the Special Issue Applications of Chromatographic Techniques in Biological, Food and Environmental Samples)

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14 pages, 1892 KiB

Open AccessArticle

Multi-Matrix Approach for the Analysis of Bicalutamide Residues in Oncology Centers by HPLC–FLD

by M. Francisca Portilha-Cunha, Teresa I. A. Gouveia, Alicia L. Garcia-Costa, Arminda Alves and Mónica S. F. Santos

Molecules 2021, 26(18), 5561; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules26185561 - 13 Sep 2021

Cited by 2 | Viewed by 1624

Abstract

Cytostatics are toxic pharmaceuticals, whose presence in surfaces puts healthcare workers at risk. These drugs might also end up in hospital effluents (HWW), potentially damaging aquatic ecosystems. Bicalutamide is a cytostatic extensively consumed worldwide, but few analytical methods exist for its quantification and most of them require advanced techniques, such as liquid chromatography mass spectrometry (LC-MS), which are very complex and expensive for large monitoring studies. Therefore, a simple but reliable multi-matrix high performance liquid chromatographic method, with fluorescence detection, was developed and validated to rapidly screen abnormal concentrations of bicalutamide in HWW and relevant contamination levels of bicalutamide in indoor surfaces (>100 pg/cm²), prior to confirmation by LC-MS. The method presents good linearity and relatively low method detection limits (HWW: 0.14 ng/mL; surfaces: 0.28 pg/cm²). Global uncertainty was below 20% for concentrations higher than 25 ng/mL (HWW) and 50 pg/cm² (surfaces); global uncertainty was little affected by the matrix. Therefore, a multi-matrix assessment could be achieved with this method, thus contributing to a holistic quantification of bicalutamide along the cytostatic circuit. Bicalutamide was not detected in any of the grab samples from a Portuguese hospital, but an enlarged sampling is required to conclude about its occurrence and exposure risks. Full article

(This article belongs to the Special Issue Applications of Chromatographic Techniques in Biological, Food and Environmental Samples)

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12 pages, 2262 KiB

Open AccessArticle

Lipemia in the Plasma Sample Affects Fentanyl Measurements by Means of HPLC-MS² after Liquid-Liquid Extraction

by Marta Tikhomirov, Tomasz Śniegocki and Błażej Poźniak

Molecules 2021, 26(15), 4514; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules26154514 - 27 Jul 2021

Cited by 7 | Viewed by 2402

Abstract

Examination of fentanyl levels is frequently performed in certain scientific evaluations and forensic toxicology. It often involves the collection of very variable blood samples, including lipemic plasma or serum. To date, many works have reported the methods for fentanyl detection, but none of them have provided information about the impact on the assay performance caused by an excessive amount of lipids. This aspect may be, however, very important for highly lipophilic drugs like fentanyl. To address this issue, we developed the liquid chromatography method with mass spectrometry detection and utilized it to investigate the impact of lipids presence in rabbit plasma on the analytical method performance and validation. The validation procedure, conducted for normal plasma and lipemic plasma separately, resulted in good selectivity, sensitivity and linearity. The limits of detection and quantification were comparable between the two matrices, being slightly lower in normal plasma (0.005 and 0.015 µg/L) than in lipemic plasma (0.008 and 0.020 µg/L). Liquid–liquid extraction provided a low matrix effect regardless of the lipid levels in the samples (<10%), but pronounced differences were found in the recovery and accuracy. In the normal plasma, this parameter was stable and high (around 100%), but in the lipemic matrix, much more variable and less efficient results were obtained. Nevertheless, this difference had no impact on repeatability and reproducibility. In the present work, we provided reliable, convenient and sensitive method for fentanyl detection in the normal and lipemic rabbit plasma. However, construction of two separate validation curves was necessary to provide adequate results since the liquid-liquid extraction was utilized. Therefore, special attention should be paid during fentanyl quantification that involves lipemic plasma samples purified by this technique. Full article

(This article belongs to the Special Issue Applications of Chromatographic Techniques in Biological, Food and Environmental Samples)

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9 pages, 691 KiB

Open AccessArticle

Validation of a Simple HPLC-Based Method for Lysine Quantification for Ruminant Nutrition

by João Albuquerque, Susana Casal, Rebeca Cruz, Ingrid Van Dorpe, Margarida Rosa Garcez Maia, António José Mira Fonseca, Ana Rita Jordão Cabrita, Ana Rute Neves and Salette Reis

Molecules 2021, 26(14), 4173; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules26144173 - 09 Jul 2021

Cited by 4 | Viewed by 2714

Abstract

Robust and selective quantification methods are required to better analyze feed supplementation effectiveness with specific amino acids. In this work, a reversed-phase high-performance liquid chromatography method with fluorescence detection is proposed and validated for lysine quantification, one of the most limiting amino acids in ruminant nutrition and essential towards milk production. To assess and widen method applicability, different matrices were considered: namely Li₂CO₃ buffer (the chosen standard reaction buffer), phosphate buffer solution (to mimic media in cellular studies), and rumen inoculum. The method was validated for all three matrices and found to be selective, accurate (92% ± 2%), and precise at both the inter- and intra-day levels in concentrations up to 225 µM, with detection and quantification limits lower than 1.24 and 4.14 µM, respectively. Sample stability was evaluated when stored at room temperature, 4 °C, and −20 °C, showing consistency for up to 48 h regardless of the matrix. Finally, the developed method was applied in the quantification of lysine on real samples. The results presented indicate that the proposed method can be applied towards free lysine quantification in ruminant feeding studies and potentially be of great benefit to dairy cow nutrition supplementation and optimization. Full article

(This article belongs to the Special Issue Applications of Chromatographic Techniques in Biological, Food and Environmental Samples)

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13 pages, 1742 KiB

Open AccessArticle

Using Design of Experiments to Optimize a Screening Analytical Methodology Based on Solid-Phase Microextraction/Gas Chromatography for the Determination of Volatile Methylsiloxanes in Water

by Fábio Bernardo, Providencia González-Hernández, Nuno Ratola, Verónica Pino, Arminda Alves and Vera Homem

Molecules 2021, 26(11), 3429; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules26113429 - 05 Jun 2021

Cited by 5 | Viewed by 2326

Abstract

Volatile methylsiloxanes (VMSs) constitute a group of compounds used in a great variety of products, particularly personal care products. Due to their massive use, they are continually discharged into wastewater treatment plants and are increasingly being detected in wastewater and in the environment at low concentrations. The aim of this work was to develop and validate a fast and reliable methodology to screen seven VMSs in water samples, by headspace solid-phase microextraction (HS-SPME) followed by gas chromatography with flame ionization detection (GC-FID). The influence of several factors affecting the extraction efficiency was investigated using a design of experiments approach. The main factors were selected (fiber type, sample volume, ionic strength, extraction and desorption time, extraction and desorption temperature) and optimized, employing a central composite design. The optimal conditions were: 65 µm PDMS/Divinylbenzene fiber, 10 mL sample, 19.5% NaCl, 39 min extraction time, 10 min desorption time, and 33 °C and 240 °C as extraction and desorption temperature, respectively. The methodology was successfully validated, showing low detection limits (up to 24 ng/L), good precision (relative standard deviations below 15%), and accuracy ranging from 62% to 104% in wastewater, tap, and river water samples. Full article

(This article belongs to the Special Issue Applications of Chromatographic Techniques in Biological, Food and Environmental Samples)

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Review

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27 pages, 3227 KiB

Open AccessReview

Chromatographic-Based Platforms as New Avenues for Scientific Progress and Sustainability

by José S. Câmara, Cátia Martins, Jorge A. M. Pereira, Rosa Perestrelo and Sílvia M. Rocha

Molecules 2022, 27(16), 5267; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules27165267 - 18 Aug 2022

Cited by 3 | Viewed by 2686

Abstract

Chromatography was born approximately one century ago and has undergone outstanding technological improvements in innovation, research, and development since then that has made it fundamental to advances in knowledge at different levels, with a relevant impact on the well-being and health of individuals. Chromatography boosted a comprehensive and deeper understanding of the complexity and diversity of human–environment interactions and systems, how these interactions affect our life, and the several societal challenges we are currently facing, namely those related to the sustainability of our planet and the future generations. From the life sciences, which allowed us to identify endogenous metabolites relevant to disease mechanisms, to the OMICS field, nanotechnology, clinical and forensic analysis, drug discovery, environment, and “foodprint”, among others, the wide range of applications of today’s chromatographic techniques is impressive. This is fueled by a great variability of powerful chromatographic instruments currently available, with very high sensitivity, resolution, and identification capacity, that provide a strong basis for an analytical platform able to support the challenging demands of the postgenomic and post COVID-19 eras. Within this context, this review aims to address the great utility of chromatography in helping to cope with several societal-based challenges, such as the characterization of disease and/or physiological status, and the response to current agri-food industry challenges of food safety and sustainability, or the monitoring of environmental contamination. These are increasingly important challenges considering the climate changes, the tons of food waste produced every day, and the exponential growth of the human population. In this context, the principles governing the separation mechanisms in chromatography as well the different types and chromatographic techniques will be described. In addition, the major achievements and the most important technological advances will be also highlighted. Finally, a set of studies was selected in order to evince the importance of different chromatographic analyses to understand processes or create fundamental information in the response to current societal challenges. Full article

(This article belongs to the Special Issue Applications of Chromatographic Techniques in Biological, Food and Environmental Samples)

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