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Separations
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Women in Separations
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Women in Separations

A special issue of Separations (ISSN 2297-8739).

Deadline for manuscript submissions: closed (30 November 2023) | Viewed by 29250

Special Issue Editors

Prof. Dr. Victoria Samanidou

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Guest Editor
Laboratory of Analytical Chemistry, School of Chemistry, Aristotle University of Thessaloniki, 54124 Thessaloniki, Greece
Interests: analytical chemistry; sample preparation; chromatography; HPLC; method validation; method development; separation science; food analysis; bioanalysis; environmental analysis; green analytical chemistry; sorptive extraction; microextraction techniques
Special Issues, Collections and Topics in MDPI journals
Dr. Natasa Kalogiouri

E-Mail Website
Guest Editor
Laboratory of Analytical Chemistry, School of Chemistry, Aristotle University of Thessaloniki, Thessaloniki, Greece
Interests: analytical chemistry; microextraction sample preparation techniques; high-pressure liquid chromatography; gas chromatography; high-resolution mass spectrometry; 2D chromatographic systems; metabolomics; chemometrics
Special Issues, Collections and Topics in MDPI journals
Dr. Maria Touraki

E-Mail Website
Guest Editor
Development and Molecular Biology, Department of Biology, School of Sciences, Aristotle University of Thessaloniki (A.U.TH.), 54124 Thessaloniki, Greece
Interests: probiotics; pharmaceuticals; ROS; host–pathogen interactions; natural antimicrobials; method development; bioanalysis; environmental analysis

Special Issue Information

Beyond any doubt, separation techniques play a dominant role in all scientific and routine analysis laboratories. Among them, the use of instrumental chromatographic techniques enables fast and reproductive analytical results to be obtained. Chromatographic techniques are widely used for the elucidation of components in various fields, such as in food analysis, biological studies, pharmaceutical analysis, forensics, toxicology, environmental analysis, archaeology, etc. Separation mechanisms are militarized to cover all analytical requirements. In parallel with the outstanding role of separation techniques in a variety of scientific fields, we would particularly like to highlight the impact of female researchers in the field of chromatographic separations in this Special Issue, to serve as motivation for females pursuing a STEM career.

Hence, we would like to invite well-established scientists to share the results of their research with the scientific community, through this Special Issue, with the aim to compile manuscripts written or lead by women.

Prof. Dr. Victoria Samanidou
Dr. Natasa Kalogiouri
Dr. Maria Touraki
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

  • analytical chemistry
  • method development
  • chromatographic separation
  • female scientists

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Published Papers (7 papers)

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Research

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19 pages, 3803 KiB  
Article
A Comparative Study of Chamomile Essential Oils and Lipophilic Extracts Obtained by Conventional and Greener Extraction Techniques: Chemometric Approach to Chemical Composition and Biological Activity
by Gökhan Zengin, Adriano Mollica, Jelena Arsenijević, Branimir Pavlić, Zoran Zeković, Kouadio Ibrahime Sinan, Linlin Yan, Aleksandra Cvetanović Kljakić and Slavica Ražić
Separations 2023, 10(1), 18; https://doi.org/10.3390/separations10010018 - 29 Dec 2022
Cited by 11 | Viewed by 4721
Abstract
Bearing in mind the centuries-old traditional use of chamomile, but also the increasing demand for its products in modern industry, oriented toward sustainable development, there are increasing efforts for the efficient extraction of high-value compounds of this plant, as well as obtaining its [...] Read more.
Bearing in mind the centuries-old traditional use of chamomile, but also the increasing demand for its products in modern industry, oriented toward sustainable development, there are increasing efforts for the efficient extraction of high-value compounds of this plant, as well as obtaining its products with added value. With that goal, conventional and contemporary separation techniques were applied in this work. Both hydrodistillation processes (HD), conducted in a traditional manner and coupled with microwave irradiation (MWHD), were used for essential oil isolation. In parallel with those procedures, chamomile lipophilic extracts were obtained by Soxhlet extraction applying organic solvents and using supercritical fluid extraction as a greener approach. The obtained extracts and essential oils were characterized in terms of chemical composition (GC analysis, contents of total phenolics and flavonoids) and biological potential. GC analysis revealed that oxygenated sesquiterpenes and non-terpene compounds were the dominant compounds. α-Bisabolol oxide A (29.71–34.41%) and α-bisabolol oxide B (21.06–25.83%) were the most abundant individual components in samples obtained by distillation while in supercritical and Soxhlet extracts, major compounds were α-bisabolol oxide A and pentacosane. The biological potential of essential oils and extracts was tested by applying a set of analyzes to estimate the inhibition of biologically important enzymes (amylase, glucosidase, acetylcholinesterase, butyrylcholinesterase, tyrosinase) and antioxidant capacity (DPPH, ABTS, CUPRAC, FRAP, chelating and total antioxidant capacity). The results suggested essential oils as better antioxidants, while the extracts were proven to be better inhibitors of the tested enzymes. Principal Component Analysis was conducted using the experimental results of the composition of extracts and EOs of chamomile obtained by different separation techniques, showing clear discrimination between methods applied in correlation with the chemical profile. Molecular docking was applied for the identification of the main active principles present in the essential oil, among which α-bisabolol-oxide B (cp3) showed a higher affinity for tyrosinase. Full article
(This article belongs to the Special Issue Women in Separations)
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14 pages, 2138 KiB  
Article
Study of Different Chiral Columns for the Enantiomeric Separation of Azoles Using Supercritical Fluid Chromatography
by Laura Toribio, Irene Magdaleno, Beatriz Martín-Gómez, María T. Martín, Silvia Valverde and Ana M. Ares
Separations 2023, 10(1), 9; https://doi.org/10.3390/separations10010009 - 23 Dec 2022
Cited by 4 | Viewed by 2703
Abstract
The enantiomeric separation of antifungal compounds is an arduous task in pharmaceutical and biomedical fields due to the different properties that each diastereoisomer presents. The enantioseparation of a group of fungicides (sulconazole, bifonazole, triadimefon and triadimenol) using supercritical fluid chromatography was achieved in [...] Read more.
The enantiomeric separation of antifungal compounds is an arduous task in pharmaceutical and biomedical fields due to the different properties that each diastereoisomer presents. The enantioseparation of a group of fungicides (sulconazole, bifonazole, triadimefon and triadimenol) using supercritical fluid chromatography was achieved in this work. For this goal, four different chiral columns based on polysaccharide derivatives, as well as the effect of different chromatographic parameters such as temperature, type and percentage of organic modifier (methanol, ethanol and isopropanol), were thoroughly investigated. The inversion of the elution order of enantiomers as a result of a change in the stationary phase or organic modifier was also evaluated by employing a circular dichroism detector. The best separation conditions, in terms of the enantioresolution and analysis time, were obtained with the Lux® Cellulose-2 column using isopropanol as the organic modifier. Full article
(This article belongs to the Special Issue Women in Separations)
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14 pages, 2407 KiB  
Article
Development of an HPLC-DAD Method for the Extraction and Quantification of 5-Fluorouracil, Uracil, and 5-Fluorodeoxyuridin Monophosphate in Cells and Culture Media of Lactococcus lactis
by Petros Mavromatis, Kyriaki Stampouli, Angeliki Vliora, Anna Mayilyan, Victoria Samanidou and Maria Touraki
Separations 2022, 9(11), 376; https://doi.org/10.3390/separations9110376 - 17 Nov 2022
Cited by 4 | Viewed by 3937
Abstract
The drug 5-fluorouracil (5-FU) is a common cancer chemotherapeutic, presenting toxicity. Mild toxicity is treated with administration of probiotics. The interaction of these probiotics with the drug may have a crucial effect on its therapeutic efficacy. In the present work, a method for [...] Read more.
The drug 5-fluorouracil (5-FU) is a common cancer chemotherapeutic, presenting toxicity. Mild toxicity is treated with administration of probiotics. The interaction of these probiotics with the drug may have a crucial effect on its therapeutic efficacy. In the present work, a method for the quantification of uracil, 5-FU, and its active metabolite 5-fluorodeoxyuridin monophosphate in cells and culture medium of the probiotic L. lactis is presented. Extraction using H2O containing 0.05% v/v formic acid (1:5 v/v) was followed by ammonium sulphate protein precipitation and SPE. Analysis was conducted in a Nucleosil column using a gradient of water, formic acid, and acetonitrile. Calibration curves were constructed for 5-FU (5–100 μg/mL), uracil (5–20 μg/mL), and 5-fluorodeoxyuridin monophosphate (5–20 μg/mL) using 5-bromouracil as the internal standard (R2 ≥ 0.999). The photodegradation of 5-FU amounted to 36.2% at 96 h. An administration experiment in the dark revealed a decline in 5-FU concentration in the culture media (88.3%) and uptake by the cells, while the uracil and FdUMP levels increased in the cells. The inactive metabolite 5,6 dihydrofluorouracil was detected in the medium. Our results demonstrate that uptake and metabolism of 5-FU in L. lactis cells leads to a decline in the drug levels and in the formation of both the active and the inactive metabolites of the drug. Full article
(This article belongs to the Special Issue Women in Separations)
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10 pages, 1130 KiB  
Article
Development and Validation of an HPLC-FLD Method for the Determination of NDMA and NDEA Nitrosamines in Lisinopril Using Pre-Column Denitrosation and Derivatization Procedure
by Eleni Tsanaktsidou, Lamprini Kanata, Sofia Almpani, Constantinos K. Zacharis and Catherine K. Markopoulou
Separations 2022, 9(11), 347; https://doi.org/10.3390/separations9110347 - 4 Nov 2022
Cited by 2 | Viewed by 2831
Abstract
In order to meet the analytical requirements of the European Medicines Agency (EMA), a new HPLC-FLD method was successfully developed using dansyl chloride for the derivatization and determination of the genotoxic impurities N-Nitrosodimethylamine (NDMA) and N-Nitrosodiethylamine (NDEA) in Lisinopril API and [...] Read more.
In order to meet the analytical requirements of the European Medicines Agency (EMA), a new HPLC-FLD method was successfully developed using dansyl chloride for the derivatization and determination of the genotoxic impurities N-Nitrosodimethylamine (NDMA) and N-Nitrosodiethylamine (NDEA) in Lisinopril API and its final product. Samples’ pretreatment includes liquid–liquid microextraction, denitrosation, and derivatization steps. To optimize the process, the parameters contributing to high sensitivity and yielding reliable results were thoroughly studied and optimized using one-factor-at-a-time and experimental design approaches. The analytes were pre-column derivatized with Dansyl-Cl and analyzed by HPLC-fluorescence (λem/λem = 340/530) using a C18 column and a mixture of phosphate buffer (pH = 2.8; 20 mM)/acetonitrile 55:45 v/v as the mobile phase. The six-level concentration calibration was shown to be linear, with R equal to 0.9995 for both analytes. The limit of detection (LOD) was satisfactory and equal to 4.7 and 0.04 ng/mL for NDMA and NDEA, respectively. Precision was less than 13.4% in all cases, and the average recoveries were equal to 109.2 and 98.1% for NDMA and NDEA, respectively. The proposed procedure is relatively easy, rapid, and suitable for the determination of the two nitrosamines in routine analysis tests. Full article
(This article belongs to the Special Issue Women in Separations)
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Review

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16 pages, 821 KiB  
Review
Solid Phase Microextraction—A Promising Tool for Graft Quality Monitoring in Solid Organ Transplantation
by Kamil Łuczykowski, Natalia Warmuzińska and Barbara Bojko
Separations 2023, 10(3), 153; https://doi.org/10.3390/separations10030153 - 23 Feb 2023
Cited by 2 | Viewed by 1673
Abstract
Solid organ transplantation is a life-saving intervention for patients suffering from end-stage organ failure. Although improvements in surgical techniques, standards of care, and immunosuppression have been observed over the last few decades, transplant centers have to face the problem of an insufficient number [...] Read more.
Solid organ transplantation is a life-saving intervention for patients suffering from end-stage organ failure. Although improvements in surgical techniques, standards of care, and immunosuppression have been observed over the last few decades, transplant centers have to face the problem of an insufficient number of organs for transplantation concerning the growing demand. An opportunity to increase the pool of organs intended for transplantation is the more frequent use of organs from extended criteria and the development of analytical methods allowing for a better assessment of the quality of organs to minimize the risk of post-transplant organ injury and rejection. Therefore, solid-phase microextraction (SPME) has been proposed in various studies as an effective tool for determining compounds of significance during graft function assessment or for the chemical profiling of grafts undergoing various preservation protocols. This review summarizes how SPME addresses the analytical challenges associated with different matrices utilized in the peri-transplant period and discusses its potential as a diagnostic tool in future work. Full article
(This article belongs to the Special Issue Women in Separations)
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25 pages, 1744 KiB  
Review
Green Extraction Techniques for the Determination of Active Ingredients in Tea: Current State, Challenges, and Future Perspectives
by Ioulia Maria Koina, Yiannis Sarigiannis and Evroula Hapeshi
Separations 2023, 10(2), 121; https://doi.org/10.3390/separations10020121 - 9 Feb 2023
Cited by 26 | Viewed by 9358
Abstract
In recent years, the scientific community has turned its attention to the further study and application of green chemistry as well as to sustainable development in reducing the consumption of raw materials, solvents, and energy. The application of green chemistry aims to ensure [...] Read more.
In recent years, the scientific community has turned its attention to the further study and application of green chemistry as well as to sustainable development in reducing the consumption of raw materials, solvents, and energy. The application of green chemistry aims to ensure the protection of the environment and to also, consequently, improve the quality of human life. It offers several benefits, both socially and economically. In the last few decades, new alternative non-conventional green extraction methodologies have been developed for the purposes of the extraction of active ingredient compounds from various raw products. The main objective of this literature review is to present the current knowledge and future perspectives regarding the green extraction of tea species in respect of the isolation of safe active biomolecules, which can be used as commercially available products—both as dietary supplements and pharmaceutical formulations. More specifically, in this literature review, the intention is to investigate several different extraction techniques, such as ultrasonic-assisted extraction, ultrasonic-assisted extraction with DESs, the microwave assisted-extraction method, and the reflux method. These are presented in respect of their role in the isolation of bioactive molecules regarding different tea species. Furthermore, following the literature review conducted in this study, the commonly used green extraction methods were found to be the ultrasound-assisted method and the microwave-assisted method. In addition to these, the use of a green solvent, in regard to its role in the maximum extraction yield of active ingredients in various species of tea, was emphasized. Catechins, alkaloids (such as caffeine), gallic acid, and flavonoids were the main extracted bioactive molecules that were isolated from the several tea species. From this literature review, it can be demonstrated that green tea has been widely studied at a rate of 52% in respect of the included research studies, followed by black tea at 26%, as well as white tea and oolong tea at 11% each. Regarding the determination of the bioactive molecules, the most utilized analytical method was found in the combination of high-performance liquid chromatography (HPLC) with a photodiode array detector (PDA) and mass spectrophotometry (MS) at a usage rate of about 80%. This method was followed by the utilization of UPLC and GC at 12% and 8%, respectively. In the future, it will be necessary to study the combination of green extraction techniques with other industry strategies, such as an encapsulation at the micro and nano scale, for the purposes of preparing stable final products with antioxidant properties where, finally, they can be safely consumed by humans. Full article
(This article belongs to the Special Issue Women in Separations)
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Other

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8 pages, 1371 KiB  
Viewpoint
A Critical Appraisal of the Separation Protocols Proposed for the Implementation of the Health Claim on “Olive Oil Polyphenols” (EC Regulation 432/2012)
by Maria Z. Tsimidou
Separations 2022, 9(11), 351; https://doi.org/10.3390/separations9110351 - 7 Nov 2022
Cited by 2 | Viewed by 1779
Abstract
The analysis of the secoiridoid type of phenolic compounds present in virgin olive oil has become a challenging area of research since the first evidence of their presence in the polar fraction of the oil. Separation techniques, mainly liquid chromatographic ones, prevailed over [...] Read more.
The analysis of the secoiridoid type of phenolic compounds present in virgin olive oil has become a challenging area of research since the first evidence of their presence in the polar fraction of the oil. Separation techniques, mainly liquid chromatographic ones, prevailed over the years of application toward elucidation of their structure, content determination and collection of evidence on cultivar, origin, processing and storage conditions dependence. One of the latest challenges in their analysis was related to the need to address the requirement set by EC Regulation 432/2012 for the implementation of the health claim on ‘olive oil polyphenols’. The present work considers in a chronological order the original articles, viewpoints, review articles and other published efforts that appeared in the literature after the issuing of the relevant EFSA scientific opinion in 2011. The EFSA health claim created a lot of expectations among producers of virgin olive oil and boosted research for the development of a ‘fit for the purpose’ analytical protocol. Emphasis is given to the dedicated separation protocols that have been developed in the last 10 years and to the progress in their validation in comparison to the features of the method that were recently adopted by the International Olive Council. Full article
(This article belongs to the Special Issue Women in Separations)
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