Journal Description
Separations
Separations
- formerly Chromatography - is an international, peer-reviewed, open access journal on separation and purification science and technology in all areas of chemical, biological, physical science, and separation performance published monthly online by MDPI. The Central European Group of Separation Sciences (CEGSS) is affiliated with Separations and their members receive discounts on the article processing charges.
- Open Access— free for readers, with article processing charges (APC) paid by authors or their institutions.
- High Visibility: indexed within Scopus, SCIE (Web of Science), CAPlus / SciFinder, and other databases.
- Rapid Publication: manuscripts are peer-reviewed and a first decision is provided to authors approximately 13.6 days after submission; acceptance to publication is undertaken in 2.9 days (median values for papers published in this journal in the second half of 2023).
- Recognition of Reviewers: reviewers who provide timely, thorough peer-review reports receive vouchers entitling them to a discount on the APC of their next publication in any MDPI journal, in appreciation of the work done.
- Companion journal: Purification.
Impact Factor:
2.6 (2022);
5-Year Impact Factor:
2.7 (2022)
Latest Articles
Accumulation of Particles in an Annular Centrifugal Contactor Cascade and the Effect upon the Extraction of Nitric Acid
Separations 2024, 11(6), 163; https://doi.org/10.3390/separations11060163 (registering DOI) - 23 May 2024
Abstract
Centrifugal contactors (CCs) are a technology candidate for the development of advanced reprocessing flowsheets. While they offer many advantages, such as process intensification, there are still uncertainties regarding their industrial deployment. The presence of particles in the process streams in particular may present
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Centrifugal contactors (CCs) are a technology candidate for the development of advanced reprocessing flowsheets. While they offer many advantages, such as process intensification, there are still uncertainties regarding their industrial deployment. The presence of particles in the process streams in particular may present a challenge to both performance and operability. Preliminary studies have been undertaken to evaluate the accumulation of particles in the contactors and the effect upon the extraction behaviour of nitric acid. Aluminium oxide (Al2O3) particles were suspended in the aqueous feed solution during the operation of a three-stage, 40 mm diameter CC cascade. The presence of insoluble solid particles in the aqueous feed, up to 7 g/L, were not observed to affect phase separation and entrainment under the experimental conditions investigated. The particles were centrifuged out of solution and accumulated as a thin cake/bed in the rotors of each stage. This work also illustrates that particles do entrain through the cascade. The predominant effect on the rate of accumulation was particle concentration in the aqueous feed solution, and increasing solids loading was observed to have an impact upon the extraction of nitric acid across the cascade.
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(This article belongs to the Section Separation Engineering)
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Hyphenation of Thermodesorption into GC × GC-TOFMS for Odorous Molecule Detection in Car Materials: Column Sets and Adaptation of Second Column Dimensions to TD Pressure Constraints
by
Romain Klein, José Dugay, Jérôme Vial, Didier Thiébaut, Guy Colombet, Donatien Barreteau and Guillaume Gruntz
Separations 2024, 11(6), 162; https://doi.org/10.3390/separations11060162 - 23 May 2024
Abstract
Vehicle interior air quality is an issue of growing interest among car manufacturers and customers. GC-MS is the benchmark method for the analysis of indoor air or material emissions. It is suitable for the quantification of target pollutants and the most abundant compounds.
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Vehicle interior air quality is an issue of growing interest among car manufacturers and customers. GC-MS is the benchmark method for the analysis of indoor air or material emissions. It is suitable for the quantification of target pollutants and the most abundant compounds. It fails, however, to uncover the true molecular complexity of these samples. In the present study, we describe the development of a TD-GC × GC-TOFMS method designed to detect polar and potentially odorous molecules in car material emissions. Attention is paid to the hyphenation of the thermodesorber and the gas chromatograph, both at software and hardware levels, and the constraints due to pressure limitations on the thermodesorber (evaluated at 414 kPa/60 psi at the end of the temperature ramp and at 138 kPa/20 psi at rest). A compromise was made for the 2D column length and diameter to balance separation and pressure (50 × 0.18 × 0.18 cm × mm × µm + 60 cm transfer line selected). On various materials, we were able to observe several hundreds of polar molecules, among them were between 75 and 150 odorants per material. This work lays the foundation for the widespread screening of potential odorants in car material emissions.
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(This article belongs to the Collection Feature Paper Collection in Section Chromatographic Separations)
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Open AccessArticle
Two-Dimensional Thin-Layer Chromatography as an Accessible, Low-Cost Tool for Lipid-Class Profile Screening
by
Zipora Tietel
Separations 2024, 11(6), 161; https://doi.org/10.3390/separations11060161 - 23 May 2024
Abstract
The interest in lipid composition profiling is significantly increasing as research reveals the immense importance of lipids in medicine, plant science, food and agriculture. However, lipidomic analysis requires high-end specialty equipment. We used two-dimensional thin-layer chromatography (2D-TLC) as a readily available, low-cost tool
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The interest in lipid composition profiling is significantly increasing as research reveals the immense importance of lipids in medicine, plant science, food and agriculture. However, lipidomic analysis requires high-end specialty equipment. We used two-dimensional thin-layer chromatography (2D-TLC) as a readily available, low-cost tool for basic lipidomic profiling of lipid classes in algal samples in the models Chlamydomonas reinhardtii, Auxenochlorella protothecoides, and Euglena gracilis, validating lipid class identification using an LC-MS/MS analysis. Algal lipid extracts were separated on a 2D-TLC plate, and TLC analysis was followed by scraping individual TLC spots off the plate, and a subsequent liquid chromatography separation and tandem mass spectrometry (LC-MS/MS) analysis. For comparison, crude lipid extracts were also injected directly to the LC-MS/MS system. Lipid class annotation was achieved by a combination of accurate mass, retention time information, neutral loss and fragment ion analysis by MS2Analyzer, and by matching spectra to LipidBlast MS/MS library. Overall, we were able to identify 15 lipid classes, and to adequately profile the lipid classes in all three organisms. This TLC method is thus suggested as an accessible tool for lipid class profiling of algal, plant, and food lipids, alike, when a rapid and simple analysis is required, e.g., for screening purposes.
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(This article belongs to the Special Issue Chromatography for the Separation and Detection of Metabolites)
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Open AccessArticle
Evaluation of CO2/H2O Co-Adsorption Models for the Anion Exchange Resin Lewatit VPOC 1065 under Direct Air Capture Conditions Using a Novel Lab Setup
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Florian M. Chimani, Aditya Anil Bhandari, Andreas Wallmüller, Gerhard Schöny, Stefan Müller and Josef Fuchs
Separations 2024, 11(6), 160; https://doi.org/10.3390/separations11060160 - 22 May 2024
Abstract
This study aimed to develop a laboratory-scale direct air capture unit for evaluating and comparing amine-based adsorbents under temperature vacuum swing adsorption conditions. The experimental campaign conducted with the direct air capture unit allowed for the determination of equilibrium loading, CO2 uptake
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This study aimed to develop a laboratory-scale direct air capture unit for evaluating and comparing amine-based adsorbents under temperature vacuum swing adsorption conditions. The experimental campaign conducted with the direct air capture unit allowed for the determination of equilibrium loading, CO2 uptake capacity, and other main performance parameters of the investigated adsorbent Lewatit VP OC 1065®. The investigations also helped to understand the co-adsorption of CO2 and H2O on the tested material, which is crucial for improving temperature vacuum swing adsorption processes. This was achieved by obtaining pure component isotherms for CO2 and H2O and using three different co-adsorption isotherm models from the literature. It was found that the weighted average dual-site Toth model emerged as the most accurate and reliable model for simulating this co-adsorption behaviour. Its predictions closely align with the experimental data, particularly in capturing the adsorption equilibrium at various temperatures. It was also observed that this lab-scale unit offers advantages over thermogravimetric analysis when conducting adsorption experiments on the chosen amine. The final aim of this study is to provide a pathway to develop devices for testing and developing efficient and cost-effective adsorbents for direct air capture.
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(This article belongs to the Topic Carbon Capture Science & Technology (CCST))
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Open AccessArticle
Effect of a Chitosan-Based Packaging Material on the Domestic Storage of “Ready-to-Cook” Meat Products: Evaluation of Biogenic Amines Production, Phthalates Migration, and In Vitro Antimicrobic Activity’s Impact on Aspergillus Niger
by
Antonella Maria Aresta, Nicoletta De Vietro, Giovanna Mancini and Carlo Zambonin
Separations 2024, 11(6), 159; https://doi.org/10.3390/separations11060159 - 21 May 2024
Abstract
The consumption of “ready-to-cook” foods has been experiencing rapid expansion due to modern lifestyles, and they are often sold in economical multipacks. These foods necessitate packaging that maintains their quality for extended periods of time during home storage once the original packaging is
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The consumption of “ready-to-cook” foods has been experiencing rapid expansion due to modern lifestyles, and they are often sold in economical multipacks. These foods necessitate packaging that maintains their quality for extended periods of time during home storage once the original packaging is opened. This study evaluates a chitosan-based film derived from low- and high-molecular-weight (MW) chitosan in acetic acid without synthetic additives as an alternative packaging material for “ready-to-cook” beef burgers. The burgers were stored at 8 °C after being removed from their sales packaging. A commercial polyethylene (PE) film designed for food use, devoid of polyvinylchloride (PVC) and additives, served as the reference material. The production of six biogenic amines (BAs), indicative of putrefactive processes, was monitored. Additionally, the release of four phthalates (PAEs), unintentionally present in the packaging films, was assessed using solid-phase microextraction coupled with gas chromatography/mass spectrometry (SPME-GC/MS). Microbiological tests were conducted to investigate the antimicrobial efficacy of the packaging against Aspergillus Niger NRR3112. The results showed that the chitosan-based films, particularly those with low MW (LMW), exhibited superior meat preservation compared to the PE films. Furthermore, they released PAEs below legal limits and demonstrated the complete inhibition of fungal growth. These findings highlight the potential of chitosan-based packaging as a viable and effective option for extending the shelf-life and maintaining the quality of “ready-to-cook” meat products during domestic storage.
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(This article belongs to the Section Analysis of Food and Beverages)
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Open AccessArticle
Polyphenols from Sage Leaves (Salvia officinalis L.): Environmentally Friendly Extraction under High Hydrostatic Pressure and Application as a Corrosion Inhibitor for Tinplate
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Maja Dent, Regina Fuchs-Godec, Sandra Pedisić, Dorotea Grbin, Verica Dragović-Uzelac, Damir Ježek and Tomislav Bosiljkov
Separations 2024, 11(5), 158; https://doi.org/10.3390/separations11050158 - 17 May 2024
Abstract
Due to the diversity of organic molecular structures present in sage extract, sage extract is a promising potential source of a cheap and effective biodegradable green corrosion inhibitor for tinplate in 3% NaCl solution, which was evaluated in this study. HHP proved to
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Due to the diversity of organic molecular structures present in sage extract, sage extract is a promising potential source of a cheap and effective biodegradable green corrosion inhibitor for tinplate in 3% NaCl solution, which was evaluated in this study. HHP proved to be a new and emerging technology for the useful extraction of polyphenols from sage as a functional ingredient from natural sources. Analysis of variance among all tested independent factors (ethanol concentration, HHP parameters and temperature) revealed significant differences (p < 0.05) in total polyphenol content as well as for rosmarinic acid as the major phenolic compound in sage extract, while extraction time had no effect (p ˃ 0.05). The optimum HHP conditions (600 MPa, 30% ethanol, 60 °C and 5 min) gave a maximum extraction yield of total polyphenols of 3811.84 mg/100 g. Sage-leaf extracts were found to be a mixture of phenolic acids, namely rosmarinic and salvianolic acid K, epicatechin and luteolin-7-O-glucuronide glycoside. The corrosion results show that the sage extract at a concentration of 0.6 g/L in 3% NaCl is an effective corrosion inhibitor (93%), forming a passivation layer of sage extract consisting of organic compounds such as polyphenols on the surface of tinplate.
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(This article belongs to the Special Issue Bioactive Compounds from Natural Sources: Extraction, Characterization, Evaluation and Application)
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Open AccessArticle
Characterization and Quantitation of Anthocyanins of the Pigmented Tea Cultivar TRI 2043 (Camellia sinensis L.) from Sri Lanka
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Philipp Hopfstock, Pitumpe Appuhamilage Nimal Punyasiri, Mats Kiene, Jeevan Dananjava Kottawa-Arachchi, Recep Gök and Peter Winterhalter
Separations 2024, 11(5), 157; https://doi.org/10.3390/separations11050157 - 16 May 2024
Abstract
Tea leaves are rich in diverse bioactive compounds. The tea accession TRI 2043 is unique due to its pigmented leaves caused by anthocyanins, clonal origin, resistance to blister blight disease, and high pubescence density. Because of its peculiarity, TRI 2043 is used to
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Tea leaves are rich in diverse bioactive compounds. The tea accession TRI 2043 is unique due to its pigmented leaves caused by anthocyanins, clonal origin, resistance to blister blight disease, and high pubescence density. Because of its peculiarity, TRI 2043 is used to produce high-quality silver tip tea, a premium type of tea that commands high prices. This study was carried out to clarify and elucidate the types of anthocyanins in this particular accession. Four different anthocyanin species were identified and quantitated as cyanidin-3-O-β-d-galactoside and delphinidin-3-O-β-d-galactoside equivalents for leaf blades and stems of the cultivar TRI 2043. The characterization was performed by comparison with commercially available reference substances and further confirmed using ion mobility high-resolution time-of-flight-mass spectrometry (IMS-HRTOF-MS). Quantitation was carried out using ultra-high-performance liquid chromatography ultraviolet–visible detection (UHPLC-UV-vis) with cyanidin-3-O-β-d-glucoside as an internal standard. E- and Z-geometric isomers of 6-p-coumaroyl derivates of delphinidin and cyanidin-3-O-β-d-galactopyranosides were observed, and collision cross section (CCS) values were determined for all four different anthocyanidin species. The content of anthocyanins in leaf blades of cultivar TRI 2043 was 856.32 ± 41.56 µg/g dry weight, with cyanidin being the more abundant anthocyanin (69.8%). Conversely, the stem material contained an anthocyanin amount of 459.5 ± 44.7 µg/g dry weight, with a higher content of delphinidin (69.6%). In summary, an enrichment strategy using analytical membrane chromatography was established to fully elucidate and quantify the anthocyanin profile of plant samples such as the special tea variety TRI 2043.
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(This article belongs to the Special Issue Bioactive Compounds in Foods: Separation, Extraction and Application)
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Open AccessArticle
Efficient Quality Control of Peptide Pools by UHPLC and Simultaneous UV and HRMS Detection
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Gaby Bosc-Bierne, Shireen Ewald, Oliver J. Kreuzer and Michael G. Weller
Separations 2024, 11(5), 156; https://doi.org/10.3390/separations11050156 - 16 May 2024
Abstract
Peptide pools consist of short amino acid sequences and have proven to be versatile tools in various research areas in immunology and clinical applications. They are commercially available in many different compositions and variants. However, unlike other reagents that consist of only one
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Peptide pools consist of short amino acid sequences and have proven to be versatile tools in various research areas in immunology and clinical applications. They are commercially available in many different compositions and variants. However, unlike other reagents that consist of only one or a few compounds, peptide pools are highly complex products which makes their quality control a major challenge. Quantitative peptide analysis usually requires sophisticated methods, in most cases isotope-labeled standards and reference materials. Usually, this would be prohibitively laborious and expensive. Therefore, an approach is needed to provide a practical and feasible method for quality control of peptide pools. With insufficient quality control, the use of such products could lead to incorrect experimental results, worsening the well-known reproducibility crisis in the biomedical sciences. Here we propose the use of ultra-high performance liquid chromatography (UHPLC) with two detectors, a standard UV detector at 214 nm for quantitative analysis and a high-resolution mass spectrometer (HRMS) for identity confirmation. To be cost-efficient and fast, quantification and identification are performed in one chromatographic run. An optimized protocol is shown, and different peak integration methods are compared and discussed. This work was performed using a peptide pool known as CEF advanced, which consists of 32 peptides derived from cytomegalovirus (CMV), Epstein–Barr virus (EBV) and influenza virus, ranging from 8 to 12 amino acids in length.
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(This article belongs to the Special Issue Peptide Synthesis, Separation and Purification)
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Open AccessCommunication
Coordination Ion Spray for Analysis of the Growth Hormones Releasing Peptides in Urine—An Application Study
by
Azamat Temerdashev, Elina Gashimova, Alice Azaryan, Yu-Qi Feng and Sanka N. Atapattu
Separations 2024, 11(5), 155; https://doi.org/10.3390/separations11050155 - 16 May 2024
Abstract
In this article, a comparison of ionization techniques is provided and discussed. Conventional liquid chromatography with an electrospray ionization source shows higher robustness and repeatability in comparison with liquid chromatography coupled with a coordination ion spray (CIS-MS) source using silver nitrate as the
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In this article, a comparison of ionization techniques is provided and discussed. Conventional liquid chromatography with an electrospray ionization source shows higher robustness and repeatability in comparison with liquid chromatography coupled with a coordination ion spray (CIS-MS) source using silver nitrate as the dopant. However, the higher sensitivity and possibility to collect more data in untargeted applications mean CIS-MS is emerging as an instrument used in specific applications. During this research, the limit of detection (LOD) for GHRP-2 and GHRP-6 was established at 0.2 ng/mL, and the lower limit of quantification (LLOQ) was 0.5 ng/mL for CIS-MS. For conventional ESI-MS combined with solid-phase extraction on weak cation exchange columns, the limit of detection was found to be 1 ng/mL, and the lower limit of quantification was 2 ng/mL.
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(This article belongs to the Topic Application of Liquid Chromatography-Mass Spectrometry and Related Techniques)
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Open AccessArticle
Improving the Current European Pharmacopoeia Enantio-Selective HPLC Method for the Determination of Enantiomeric Purity in Atorvastatin Calcium Salt Drug Substance
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Francesca Romana Mammone, Daniele Sadutto, Giulia D’Ettorre, Antonina Mosca and Roberto Cirilli
Separations 2024, 11(5), 154; https://doi.org/10.3390/separations11050154 - 16 May 2024
Abstract
Atorvastatin (ATV) is a well-established lipid-lowering agent. ATV has two stereogenic centers, and of the four possible stereoisomers, only the (3R,5R) form is used therapeutically. The European Pharmacopoeia (EP) monograph 2022 for ATV calcium salt describes a normal-phase high-performance
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Atorvastatin (ATV) is a well-established lipid-lowering agent. ATV has two stereogenic centers, and of the four possible stereoisomers, only the (3R,5R) form is used therapeutically. The European Pharmacopoeia (EP) monograph 2022 for ATV calcium salt describes a normal-phase high-performance liquid chromatography (HPLC) method for the determination of enantiomeric purity in both drug substance and working standard samples, based on a 150 mm × 4.6 mm Chiralpak AD-H column. The main problems with this method are the very long analysis time and the high solvent consumption. Here, an alternative chromatographic protocol was developed using the Chiralpak AD-3 column (250 mm × 4.6 mm) packed with 3 μm silica particles instead of the 5 μm silica particles of the Chiralpak AD-H chiral stationary phase and characterized by the same polysaccharide selector, amylose-tris(3,5-dimethylphenylcarbamate). Using a mobile phase consisting of a mixture of n-hexane-ethanol-formic acid 90:10:0.1 (v/v/v) as the mobile phase and setting the flow rate and column temperature to 1.0 mL min−1 and 35 °C, respectively, a simultaneous stereo-selective separation was achieved within 35 min without observing any overlap between the enantiomeric impurity peak and peaks related to other ATV impurities. Compared to HPLC EP conditions, the analysis time to elute all the potentially related substances was faster and significantly less mobile phase volume was required. The linearity of the method has been demonstrated in the range of 4.4 μg mL−1 to 1000 μg mL−1 (R2 > 0.999). At a concentration of 4.4 μg mL−1, which is 0.075% of the test solution (5.8 mg mL−1, as ATV free acid), the signal-to-noise ratio was found to be 20.
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(This article belongs to the Special Issue Application of Liquid Chromatography in Pharmaceutical and Toxicological Analysis)
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Open AccessArticle
Packed-Nanofiber Solid-Phase Extraction Coupled with High-Performance Liquid Chromatography Fluorescence for Determining Gut Microbiota–Host Cometabolites and Indoleamines in Human Urine
by
Lanlan Wei and Xuejun Kang
Separations 2024, 11(5), 153; https://doi.org/10.3390/separations11050153 - 16 May 2024
Abstract
Exercise reduces the risk of inflammatory diseases by modulating different tissue and cell types, including those within the gastrointestinal tract. Obtaining a more comprehensive understanding of pathophysiology requires monitoring of dynamic changes in cometabolites. This study aimed to develop a method for determining
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Exercise reduces the risk of inflammatory diseases by modulating different tissue and cell types, including those within the gastrointestinal tract. Obtaining a more comprehensive understanding of pathophysiology requires monitoring of dynamic changes in cometabolites. This study aimed to develop a method for determining gut microbiota–host cometabolites and indoleamines in human urine. Four key gut microbiota–host cometabolites were chromatographically separated by isocratic elution, with a running time of 10 min. The linearity of this method was confirmed over different concentration ranges: 1.0–400 ng/mL for melatonin (MEL), indole-3-propionic acid (3-IPA), indole (IND), and skatole (SKT). This method was extremely sensitive and stable and hence could be successfully applied to characterize the changes in gut microbiota–host cometabolites in human before- and after-running urine. The concentrations of MEL, 3-IPA, IND, and SKT in after-running urine were 84.0 ± 9.69, 25.9 ± 3.39, 343.7 ± 36.8, and 14.6 ± 1.36 ng/mL, respectively. Moreover, the concentrations in before-running urine were 54.2 ± 5.10, 14.4 ± 1.30, 250.8 ± 14.1, and 9.43 ± 1.07 ng/mL, respectively, which showed significantly less difference in concentrations (p < 0.05) in before- than after-running urine. Overall, the established method could simultaneously monitor gut microbiota–host cometabolites and hence can be further applied to clinical and comprehensive pathophysiological studies.
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(This article belongs to the Special Issue Preparation of Membranes and Their Application in Separation)
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Open AccessReview
Research Progress in the Separation of Chemical Components from Essential Oils by High-Speed Countercurrent Chromatography
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Linhong He, Zihao Zhong, Lijuan Zhang and Xi Bai
Separations 2024, 11(5), 152; https://doi.org/10.3390/separations11050152 - 15 May 2024
Abstract
Essential oils (EOs) are vital secondary metabolites in plants. They have garnered substantial attention owing to their distinct flavors and desirable attributes, including potent antioxidant, antibacterial, and antitumor properties. Nevertheless, the active constituents of EOs exhibit intricate chemical structures, and conventional separation techniques
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Essential oils (EOs) are vital secondary metabolites in plants. They have garnered substantial attention owing to their distinct flavors and desirable attributes, including potent antioxidant, antibacterial, and antitumor properties. Nevertheless, the active constituents of EOs exhibit intricate chemical structures, and conventional separation techniques are inadequate for purifying the individual chemical components from EOs. High-speed countercurrent chromatography, based on the principles of a hydrodynamic equilibrium system, has emerged as a liquid–liquid chromatographic separation method renowned for its ability to handle substantial single injection volumes and the absence of irreversible adsorption. Consequently, in recent years, this technique has been widely employed in the isolation and refinement of natural products. In this review, a comprehensive analysis is conducted, contrasting the merits and demerits of high-speed countercurrent chromatography with conventional separation methods. The solvent systems, elution modes, commonly employed detectors, and practical applications are reviewed in the context of high-speed countercurrent chromatography for essential oil separation and purification. Furthermore, this review offers a glimpse into the potential prospects of applying this technique, with the intention of serving as a valuable reference for the use of high-speed countercurrent chromatography in the purification of EOs.
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(This article belongs to the Special Issue HPLC or Other Chromatographic-Based Methods for Analysis of Bioactive Compounds in Plant, Food, and Pharmaceutical Products)
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Open AccessArticle
Feasibility of Different Methods for Separating n-Hexane and Ethanol
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Aleksandra Sander, Ana Petračić, Marko Rogošić, Mirela Župan, Leonarda Frljak and Matija Cvetnić
Separations 2024, 11(5), 151; https://doi.org/10.3390/separations11050151 - 15 May 2024
Abstract
Conventional distillation methods cannot effectively separate the components of an azeotropic mixture since both phases have the same composition, thereby preventing further separation. Additional techniques such as pressure swing distillation or distillation with entrainers are often employed to overcome this limitation and achieve
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Conventional distillation methods cannot effectively separate the components of an azeotropic mixture since both phases have the same composition, thereby preventing further separation. Additional techniques such as pressure swing distillation or distillation with entrainers are often employed to overcome this limitation and achieve separation. The aim of this investigation was to select the most effective method for separating n-hexane and ethanol. The feasibility of three methods was analyzed: reduced pressure distillation, extractive distillation, and liquid–liquid extraction. The mutual solubility of n-hexane and prepared deep eutectic solvents (DESs) (nine hydrophilic: choline chloride with glycerol, ethylene glycol, or carboxylic acid (malic, citric, glycolic); tetramethylammonium chloride with glycolic acid; lactic acid with glycerol; K2CO3 with glycerol or ethylene glycol; two hydrophobic: menthol with decanoic or dodecanoic acid) was experimentally determined. Extraction experiments were conducted to test the solubility of DESs in the feed mixture. The effect of changing DES-to-feed mass ratio was further investigated with choline chloride–glycerol (1:2). The same DES and both hydrophobic DESs were able to increase the relative volatility and enhance the separation of ethanol and n-hexane. Based on the obtained results, extraction was selected as the most effective method for the separation of n-hexane and ethanol.
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(This article belongs to the Section Purification Technology)
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Open AccessArticle
Characterization of the SPIRITAS: A Disposable Sampling Setup for Volatile Organic Compound Collection and Analysis
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David J. Mager, Yoni E. van Dijk, Özgü Varan, Susanne J. H. Vijverberg, Suzanne W. J. Terheggen-Lagro, Anke-Hilse Maitland-van der Zee, Hettie M. Janssens and Paul Brinkman
Separations 2024, 11(5), 150; https://doi.org/10.3390/separations11050150 - 14 May 2024
Abstract
Analyzing exhaled breath for volatile organic compounds (VOCs) using thermal desorption–gas chromatography–mass spectrometry (TD-GC-MS) offers a non-invasive diagnostic approach for various diseases. Despite its promise, the method faces challenges like sampling heterogeneity and high costs. Following the European Respiratory Society’s advocacy for methodological
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Analyzing exhaled breath for volatile organic compounds (VOCs) using thermal desorption–gas chromatography–mass spectrometry (TD-GC-MS) offers a non-invasive diagnostic approach for various diseases. Despite its promise, the method faces challenges like sampling heterogeneity and high costs. Following the European Respiratory Society’s advocacy for methodological standardization, we developed the SPIRITAS (Standardized Product for Inexpensive Respiratory InvesTigation: A breath Sampler), a low-cost, disposable breath sampler. This study evaluates the SPIRITAS’s effectiveness in detecting targeted VOCs. We tested the SPIRITAS using the Peppermint Experiment, a standardized protocol that allows for comparison between different breath sampling and analytical practices by assessing the ability to detect five peppermint-specific VOCs after ingestion of a 200-milligram peppermint oil capsule. We included ten subjects and performed six breath samples per participant, including a baseline measurement taken before ingestion. We used the Wilcoxon signed-rank test to evaluate whether baseline values were significantly lower than the peak values of the targeted VOCs. Additionally, we conducted an experiment utilizing humidified medical-grade air to identify any VOCs attributable to the SPIRITAS setup itself. Results showed successful detection of four out of five targeted “peppermint-associated” VOCs: alpha-pinene (p ≤ 0.01), beta-pinene (p ≤ 0.01), menthone (p = 0.01), and menthol (p = 0.02), indicating significant differences between the baseline and peak values in the volunteers’ breath. However, detection of eucalyptol was inconsistent. In addition, we identified 16 VOCs that were released by the SPIRITAS, one of which remains unidentified. Our findings underscore the SPIRITAS’s potential for clinical applications, paving the way for broader biomarker research. The combination of ease of use, low cost, reduced risk of contamination, and standardization makes SPIRITAS very suitable for large-scale international studies. Furthermore, we have demonstrated the SPIRITAS’s effectiveness in detecting specific VOCs and identified 16 compounds originating from the SPIRITAS, ensuring that these compounds would not be mis-qualified as potential biomarkers in future clinical studies.
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(This article belongs to the Section Chromatographic Separations)
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Open AccessEditor’s ChoiceArticle
Aluminum Removal from Rare Earth Chloride Solution through Regulated Hydrolysis via Electrochemical Method
by
Yaoyao Zhu, Jian Li, Dongyue Xie, Hui Zhang, Man Li, Binfeng Xu, Xuxia Zhang, Yangyang Xie and Tao Qi
Separations 2024, 11(5), 149; https://doi.org/10.3390/separations11050149 - 12 May 2024
Abstract
Due to the coexistence of Al3+ and RE3+ and their similar properties, the separation of aluminum from rare earths is difficult. In this study, selective precipitation was used to separate aluminum from rare earth chloride solution via electrochemical regulated hydrolysis. By
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Due to the coexistence of Al3+ and RE3+ and their similar properties, the separation of aluminum from rare earths is difficult. In this study, selective precipitation was used to separate aluminum from rare earth chloride solution via electrochemical regulated hydrolysis. By controlling the current density and electrolytic time, the rate of hydroxyl ion production was regulated, and the selective separation of rare earth and aluminum was realized according to the different precipitation sequences. By altering the temperature, current density, pH value, and other parameters, the separation performance of aluminum from rare earth in mixed rare earth chloride systems was systematically investigated. The removal rate of aluminum reached 88.35%, and the loss rate of rare earth was only 5.99% under optimized conditions. Compared with traditional neutralization hydrolysis, the new process showed higher efficiency and lower rare earth loss rate. Furthermore, a kinetic analysis of aluminum precipitation revealed that the reaction adhered to pseudo-first order kinetics. Additionally, the precipitate obtained via separation and filtration was amorphous alumina hydroxide with a small amount of rare earth attached. No reagent was consumed for the new process, which was more efficient and cleaner, providing a new idea for removing aluminum impurities from rare earth solutions.
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(This article belongs to the Section Purification Technology)
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Open AccessArticle
A Study of the Elemental Profiles of Wines from the North-Eastern Coast of the Black Sea
by
Lev A. Oganesyants, Alexandr L. Panasyuk, Dmitriy A. Sviridov, Olesya S. Egorova, Dilyara R. Akbulatova, Mikhail Y. Ganin, Aleksey A. Shilkin and Alexandr A. Il’in
Separations 2024, 11(5), 148; https://doi.org/10.3390/separations11050148 - 11 May 2024
Abstract
Due to the increasing consumer interest in wines with a controlled place of origin, PGI (Protected Geographical Indication) and PDO (Protected Designation of Origin), the most acute question is how to identify them. One of the most effective ways to confirm the place
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Due to the increasing consumer interest in wines with a controlled place of origin, PGI (Protected Geographical Indication) and PDO (Protected Designation of Origin), the most acute question is how to identify them. One of the most effective ways to confirm the place of origin of wine in global practice is a comprehensive study of the elemental profile using statistical analysis methods. In the period from 2020 to 2023, 152 grape samples of grapes were collected from various wineries in Crimea and Kuban. The grape must that was obtained from them was fermented in laboratory conditions. The elemental profile was determined in the prepared wines, which included 71 indicators. In the conducted work, it was revealed that wines from Crimea and Kuban differ statistically significantly in the concentration of the elements B, Ca, Cu, Mn, Na, Ni, Re, Si, Sn and U. At the same time, the contents of the elements U, Sn and Re prevail in wines from Crimea, and those of B, Ca, Cu, Mn, Na, Ni and Si prevail in wines from Kuban. At the same time, methods of univariate and multivariate statistics do not allow us to reliably classify wine samples from Crimea and Kuban by their place of origin. In order to reveal the non-linear dependence of the studied indicators in wines on the geographical place of grape growing, the method of a supervised learning Random Forest was used. After training the model on the dataset, the proportion of its correct predictions was 96%. The model used 61 parameters, among which the most important were Ni, Re, Ba, Rb, Na, U, Sb, Zn, Bi, Ag and Ti.
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(This article belongs to the Special Issue Analytical Methods for Food Quality and Safety Analysis)
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Open AccessArticle
Ultrasonic Pretreatment Combined with Microwave-Assisted Hydrodistillation for Extraction of Essential Oil from Melaleuca bracteata ‘Revolution Gold’ Leaves Scales Induced by Cellulase-Inorganic Salt and Its Anti-Fungal Activity
by
Yan Huang, Xiaonan Zhang, Fajian Zeng, Jinmei Chang and Zhiwei Liu
Separations 2024, 11(5), 147; https://doi.org/10.3390/separations11050147 - 9 May 2024
Abstract
In order to further develop the commercial use of Melaleuca bracteata (F. Muell), this report studied the extraction of essential oil from Melaleuca bracteata (F. Muell) leaves using ultrasonic pretreatment, cellulase-inorganic salt soaked and combined with microwave-assisted hydrodistillation. To optimize the primary contributing
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In order to further develop the commercial use of Melaleuca bracteata (F. Muell), this report studied the extraction of essential oil from Melaleuca bracteata (F. Muell) leaves using ultrasonic pretreatment, cellulase-inorganic salt soaked and combined with microwave-assisted hydrodistillation. To optimize the primary contributing parameters, the Box–Behnken design (BBD) was applied. The optimum yield of essential oil was 9.61 mL/kg DW at a microwave power of 510.77 W, lithium chloride dose of 63.56 μmol, and microwave irradiation period of 46.97 min. The essential oil included a total of 41 compounds, and methyl eugenol (76.53%) and methyl cinnamate (12.62%) were the main compounds. The inhibitory impact was notable when the essential oil concentration was 1.6 mg/mL. Therefore, it has the potential to replace chemical pesticides. When the concentration of the essential oil solution was 1.6 mg/mL, the three pathogenic species of fungus (Pseudocercospora psidii, Colletotrichum eriobotryae, and Colletotrichum siamense) were greatly affected; at this dose, the fungus was unable to develop and its growth diameter was 0 mm. Additionally, the fungus’s inhibition rate reached 100%.
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(This article belongs to the Topic Discovery of Bioactive Compounds from Natural Organisms and Their Molecular Mechanisms against Diseases)
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Open AccessArticle
Optimizing Operational Parameters for Lithium Hydroxide Production via Bipolar Membrane Electrodialysis
by
Guoxiang Wei, Mengmeng Wang, Chenxiao Lin, Chuan Xu and Jie Gao
Separations 2024, 11(5), 146; https://doi.org/10.3390/separations11050146 - 9 May 2024
Abstract
Traditional lithium hydroxide production techniques, like lithium sulfate and lithium carbonate causticizing methods, suffer from drawbacks including high specific energy consumption, time-consuming processes, and low recovery rates. The conversion of lithium chloride to lithium hydroxide using bipolar membrane electrodialysis is straightforward; however, the
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Traditional lithium hydroxide production techniques, like lithium sulfate and lithium carbonate causticizing methods, suffer from drawbacks including high specific energy consumption, time-consuming processes, and low recovery rates. The conversion of lithium chloride to lithium hydroxide using bipolar membrane electrodialysis is straightforward; however, the influence of operational parameters on bipolar membrane electrodialysis performance have not been investigated. Herein, the impact of the current density (20 mA/cm2~80 mA/cm2), feed concentration (0.5 M~2.5 M), initial feed pH (2.5, 3.5 and 4.5), and the volume ratio of the feed and base solution (1:1, 2:1 and 3:1) on the current efficiency and specific energy consumption in the bipolar membrane electrodialysis was systematically investigated. The bipolar membrane electrodialysis process showed promising results under optimal conditions with a current density of 50 mA/cm2 and an initial lithium chloride concentration of 1.5 M. This process achieved a current efficiency of 75.86% with a specific energy consumption of 3.65 kwh/kg lithium hydroxide while also demonstrating a lithium hydroxide recovery rate exceeding 90% with a purity of about 95%. This work will provide valuable guidance for hands on implementation of bipolar membrane electrodialysis technology in the production of LiOH.
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(This article belongs to the Section Purification Technology)
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Open AccessArticle
Natural Deep Eutectic Solvent-Based Ultrasound-Assisted Extraction of Flavonoids from Fagopyrum tataricum Bran
by
Zhou Xu, Xiaomei Da, Jipeng Qu and Shiming Xiao
Separations 2024, 11(5), 145; https://doi.org/10.3390/separations11050145 - 8 May 2024
Abstract
In this study, eleven kinds of flavonoids were identified from F. tataricum bran (FTB) by UPLC-Q-TOF-MS, and HPLC-DAD analysis revealed that four compounds, including rutin, quercetin, kaempferol, and nicotiflorin, were the most significant components. Subsequently, natural deep eutectic solvent-based ultrasound-assisted extraction (NADES-UAE) was
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In this study, eleven kinds of flavonoids were identified from F. tataricum bran (FTB) by UPLC-Q-TOF-MS, and HPLC-DAD analysis revealed that four compounds, including rutin, quercetin, kaempferol, and nicotiflorin, were the most significant components. Subsequently, natural deep eutectic solvent-based ultrasound-assisted extraction (NADES-UAE) was employed to extract flavonoids from FTB. Among the six kinds of NADES prepared, choline chloride–ethylene glycol (ChCl-EG) was identified as a promising candidate for extracting flavonoids due to its superior extraction performance. The extraction conditions were statistically investigated using response surface methodology conducted by Box-Behnken design (BBD). The optimal operational conditions were as follows: ultrasonic time 268 s, ultrasonic temperature 76 °C, and liquid–solid ratio 43 mL/g, which resulted in a high total flavonoid yield of 40.29 mg/g. Afterwards, the efficient extraction mechanism of NADES-UAE was comprehensively explored through FT-IR spectra, COSMO model, and microstructural analysis. In conclusion, NADES-UAE extraction is considered a green, efficient, and sustainable method for FTB flavonoids.
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(This article belongs to the Special Issue Extraction and Analysis of Chemical Compositions of Natural Products and Plants)
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Open AccessArticle
Degradation of Levofloxacin by Electroactivated Sodium Persulfate on Carbon Cloth Cathode Modified with Cerium-Based Metal Organic Frameworks (Ce-MOF) Derivatives
by
Xinbiao Mao, Mingyu Ou, Wenjun Zhao, Shuangting Yu and Hao Xu
Separations 2024, 11(5), 144; https://doi.org/10.3390/separations11050144 - 7 May 2024
Abstract
Levofloxacin (LFX), which is difficult to degrade effectively due to its molecular stability, has become an problem that needs to be solved urgently. The advanced oxidation technology of persulfate has received increasing attention from researchers. In this study, a Ce-MOF derivative (Ce-MOF-T) was
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Levofloxacin (LFX), which is difficult to degrade effectively due to its molecular stability, has become an problem that needs to be solved urgently. The advanced oxidation technology of persulfate has received increasing attention from researchers. In this study, a Ce-MOF derivative (Ce-MOF-T) was prepared by hydrothermal synthesis and calcination, which synergistically responded to electroactivation to generate sulfate radicals for the efficient degradation of LFX. It has been proven that electrical activation and the Ce-MOF derivatives work together to generate sulfate radicals and effectively degrade LFX. Ce-MOF-550-modified carbon cloth was used as the cathode and a platinum electrode as the anode, the concentration of LFX was 20 mg·L−1, the loading of Ce-MOF-550 was 15 mg, pH = 5, the concentration of sodium persulfate (PMS) was 0.3 g·L−1, the current density was 100 A·m−2, and the degradation rate was 82.05% after 1 h of reaction and 95% after 3 h of reaction. After five cycle tests, the degradation rate was still higher than 75.00%, indicating that the material had good stability. In addition, the degradation of LFX was consistent with a quasi-primary kinetic reaction with apparent rate constants of 2.26 × 10−2 min−1.
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(This article belongs to the Special Issue Applications of Electrochemistry in Water and Wastewater Treatment)
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