Editor’s Choice Articles

Editor’s Choice articles are based on recommendations by the scientific editors of MDPI journals from around the world. Editors select a small number of articles recently published in the journal that they believe will be particularly interesting to readers, or important in the respective research area. The aim is to provide a snapshot of some of the most exciting work published in the various research areas of the journal.

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26 pages, 1814 KiB  
Review
Potential of Advanced Oxidation as Pretreatment for Microplastics Biodegradation
by Kristina Bule Možar, Martina Miloloža, Viktorija Martinjak, Matija Cvetnić, Hrvoje Kušić, Tomislav Bolanča, Dajana Kučić Grgić and Šime Ukić
Separations 2023, 10(2), 132; https://doi.org/10.3390/separations10020132 - 15 Feb 2023
Cited by 10 | Viewed by 3541
Abstract
In the last two decades, microplastics (MP) have been identified as an emerging environmental pollutant. Due to their small size, MP particles may easily enter the food chain, where they can have adverse effects on organisms and the environment in general. The common [...] Read more.
In the last two decades, microplastics (MP) have been identified as an emerging environmental pollutant. Due to their small size, MP particles may easily enter the food chain, where they can have adverse effects on organisms and the environment in general. The common methods for the removal of pollutants from the environment are not fully effective in the elimination of MP; thus, it is necessary to find a more suitable treatment method(s). Among the various approaches tested, biodegradation is by far the most environmentally friendly and economically acceptable remediation approach. However, it has serious drawbacks, generally related to the rather low removal rate and often insufficient efficiency. Therefore, it would be beneficial to use some of the less economical but more efficient methods as pretreatment prior to biodegradation. Such pretreatment would primarily serve to increase the roughness and hydrophilicity of the surface of MP, making it more susceptible to bioassimilation. This review focuses on advanced oxidation processes (AOPs) as treatment methods that can enhance the biodegradation of MP particles. It considers MP particles of the six most commonly used plastic polymers, namely: polyethylene, polypropylene, polystyrene, polyvinyl chloride, polyethylene terephthalate and polyurethane. The review highlights organisms with a high potential for biodegradation of selected MP particles and presents the potential benefits that AOP pretreatment can provide for MP biodegradation. Full article
(This article belongs to the Special Issue Separation and Analysis of Micro- and Nanoplastics in the Environment)
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15 pages, 1700 KiB  
Article
Effect of Extraction Methods on Essential Oil Composition: A Case Study of Irish Bog Myrtle-Myrica gale L.
by Shipra Nagar, Maria Pigott, Sophie Whyms, Apolline Berlemont and Helen Sheridan
Separations 2023, 10(2), 128; https://doi.org/10.3390/separations10020128 - 14 Feb 2023
Cited by 2 | Viewed by 2881
Abstract
Myrica gale is an aromatic peatland shrub that has reported traditional use as an insect repellent. Different extraction methodologies were used in this study to isolate the essential oil of Myrica gale L., including Clevenger hydrodistillation (CH) and microwave-assisted hydrodistillation (MAH). The oils, [...] Read more.
Myrica gale is an aromatic peatland shrub that has reported traditional use as an insect repellent. Different extraction methodologies were used in this study to isolate the essential oil of Myrica gale L., including Clevenger hydrodistillation (CH) and microwave-assisted hydrodistillation (MAH). The oils, isolated from different plant parts (leaves, fruit and branches) collected in summer and autumn, were analysed by GC-MS and the volatiles from plant tissue were directly analysed by headspace-GC-MS. A total of 58 components were identified, including 15 monoterpene hydrocarbons (22.78–98.98%), 14 oxygenated monoterpenes (0.91–43.02%), 13 sesquiterpene hydrocarbons (0.05–24.98%), 3 oxygenated sesquiterpenes (0.07–13.16%) and 13 other compounds (0.05–5.21%). Headspace sampling furnished monoterpenes, while CH and MAH extracted monoterpenes and sesquiterpenes, with α-pinene (6.04–70.45%), eucalyptol (0.61–33.80%), limonene (2.27–20.73%) and α-phellandrene (2.33–15.61%) as major components in all plant parts. Quantitative differences occurred between extraction methodologies, with MAH yielding higher quantities of monoterpene and sesquiterpene hydrocarbons and CH targeting oxygenated counterparts. Leaves gave more complex chemical fingerprints than branches and fruit, and the summer collection yielded more components than the autumn collections. An OPLS-DA model was applied to the GC-MS data to compare the chemical profiles based on the extraction techniques and plant parts, and molecular networks were obtained for monoterpenes and sesquiterpenes connected via biosynthetic pathways. The essential oil profile of Myrica gale was influenced by the season of collection, plant part and extraction method. Full article
(This article belongs to the Section Analysis of Natural Products and Pharmaceuticals)
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15 pages, 5263 KiB  
Article
Preparation of Fe3O4-Reduced Graphene-Activated Carbon from Wastepaper in the Dispersive Solid-Phase Extraction and UHPLC-PDA Determination of Antibiotics in Human Plasma
by Pantaleone Bruni, Pasquale Avino, Vincenzo Ferrone, Serena Pilato, Nadia Barbacane, Valentino Canale, Giuseppe Carlucci and Stefania Ferrari
Separations 2023, 10(2), 115; https://doi.org/10.3390/separations10020115 - 07 Feb 2023
Cited by 2 | Viewed by 1409
Abstract
In this work, a sorbent was prepared from wastepaper samples enriched with iron oxide particles and graphene oxide and used in the solid phase extraction of antibiotics. The precursor underwent a carbothermal reduction to promote the formation of paramagnetic phases useful for the [...] Read more.
In this work, a sorbent was prepared from wastepaper samples enriched with iron oxide particles and graphene oxide and used in the solid phase extraction of antibiotics. The precursor underwent a carbothermal reduction to promote the formation of paramagnetic phases useful for the recovery of the sorbent during the analysis, and to disperse and fix graphene and the iron oxide in a durable way throughout the cellulose structure. Characterizations were carried out to evaluate the composition (Raman, XRD and EDX) and the morphological structure (SEM) of the material. A UHPLC-PDA method was developed for the simultaneous determination of antibiotics from different drug families (carbapenems, fluoroquinolones, β-lactams) using a 120 SB-C 18 poroshell column (50 × 2.1 mm I.D., 2.7 um particle size) and a mobile phase consisting of 10 mM acetate buffer at pH 5 (Line A) and acetonitrile (Line B) both containing 0.1% of triethylamine. A gradient elution was used for the separation of the analytes, while for the quantitative analysis each analyte was determined at its maximum wavelength. Several experiments were carried out to evaluate the influence of different parameters involving the dispersive magnetic solid phase extraction of these analytes. Samples were extracted using 25 mg of sorbent at pH 5 and desorbed in 5 min using methanol. We report herein on some of the outstanding advantages of using carbon-based sorbent, such as lower toxicity, scalability, improved absorption capacity, target selectivity and stability in acidic medium. Moreover, from the results obtained it is evident that, despite the use of some recycled materials, the performances obtained were comparable or even superior to the methods reported in the literature. Full article
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15 pages, 1210 KiB  
Article
Investigation of Imidazolium-Based Ionic Liquids as Additives for the Separation of Urinary Biogenic Amines via Capillary Electrophoresis
by Natalia Kaczmarczyk, Natalia Treder, Piotr Kowalski, Alina Plenis, Anna Roszkowska, Tomasz Bączek and Ilona Olędzka
Separations 2023, 10(2), 116; https://doi.org/10.3390/separations10020116 - 07 Feb 2023
Cited by 2 | Viewed by 1152
Abstract
Ionic liquids (ILs), such as imidazoles, can be used to prevent the sorption of analytes onto the walls of the capillary. Prior works have confirmed that coating the capillary wall with a cationic layer can increase its surface stability, thereby improving the repeatability [...] Read more.
Ionic liquids (ILs), such as imidazoles, can be used to prevent the sorption of analytes onto the walls of the capillary. Prior works have confirmed that coating the capillary wall with a cationic layer can increase its surface stability, thereby improving the repeatability of the separation process. In this study, micellar electrokinetic chromatography (MEKC) is employed to evaluate how two ILs with different anions—namely, 1-hexyl-3-methylimidazolium chloride [HMIM+Cl] and 1-hexyl-3-methylimidazolium tetrafluoroborate [HMIM+BF4]—affect the separation efficiency for biogenic amines (BAs) such as metanephrine (M), normetanephrine (NM), vanilmandelic acid (VMA), and homovanillic acid (HVA) in urine samples. To this end, solid-phase extraction (SPE) is employed using different sample pH values, with the results demonstrating that HVA and VMA is easily extracted at a sample pH of 5.5, while a sample pH of 9.0 facilitated the extraction of M and NM. In the applied SPE protocol, selected analytes were isolated from urine samples using hydrophilic–lipophilic-balanced (HLB) columns and eluted with methanol (MeOH). The validation data confirmed the method’s linearity (R2 > 0.996) for all analytes within the range of 0.25–10 µg/mL. The applicability of the optimized SPE-MEKC-UV method was confirmed by employing it to quantify clinically relevant BAs in real urine samples from pediatric neuroblastoma (NBL) patients. Full article
(This article belongs to the Special Issue Ionic Liquids in Separation Technology)
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45 pages, 3584 KiB  
Review
The State of Critical and Strategic Metals Recovery and the Role of Nuclear Techniques in the Separation Technologies Development: Review
by Nelson R. Kiprono, Tomasz Smolinski, Marcin Rogowski and Andrzej G. Chmielewski
Separations 2023, 10(2), 112; https://doi.org/10.3390/separations10020112 - 05 Feb 2023
Cited by 3 | Viewed by 2590
Abstract
The extraction of useful minerals or geological materials from the Earth’s crust, most typically from various sources, is crucial to a country’s development and progress. Mineral-rich countries use these resources to transform their economies and propel them toward long-term prosperity. There is an [...] Read more.
The extraction of useful minerals or geological materials from the Earth’s crust, most typically from various sources, is crucial to a country’s development and progress. Mineral-rich countries use these resources to transform their economies and propel them toward long-term prosperity. There is an urgent need for the world to increase mineral exploration efforts, improve the recycling of important metal-containing resources, and extract them using upgraded hydrometallurgical procedures with high recovery efficiency. This review paper highlights the importance of strategic and critical metals in the economy and the role of nuclear techniques in the analysis, process optimization, and remediation of metals using solvent extraction, adsorption, and chromatographic resins. Radiotracer analysis, X-Ray Fluorescence spectrometry (XRF), Neutron Activation Analysis (NAA), and X-Ray Diffraction (XRD) are appropriate for improving laboratory-based hydrometallurgical processes, with future technical and economic benefits. The development and installation of novel instruments to provide the real-time control of mining and mineral processing plants for improved control have the potential to aid in the recovery of a broad range of metals. Full article
(This article belongs to the Special Issue Recent Advances in Metal Separations and Recovery)
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28 pages, 2055 KiB  
Review
Identification and Isolation Techniques for Plant Growth Inhibitors in Rice
by Nguyen Thi Hai Anh, La Hoang Anh, Nguyen Phuong Mai, Nguyen Van Quan and Tran Dang Xuan
Separations 2023, 10(2), 105; https://doi.org/10.3390/separations10020105 - 03 Feb 2023
Cited by 2 | Viewed by 3224
Abstract
Plant growth inhibitors (PGIs) in rice (Oryza sativa), or rice allelochemicals, are secondary metabolites that are either exudated by rice plants to cope with natural competitors or produced during the decomposition of rice by-products in the paddy fields. Of these, the [...] Read more.
Plant growth inhibitors (PGIs) in rice (Oryza sativa), or rice allelochemicals, are secondary metabolites that are either exudated by rice plants to cope with natural competitors or produced during the decomposition of rice by-products in the paddy fields. Of these, the major groups of rice PGIs include phenolics, flavonoids, terpenoids, alkaloids, steroids, and fatty acids, which also exhibit potential medicinal and pharmaceutical properties. Recently, the exploitation of rice PGIs has attracted considerable attention from scientists worldwide. The biosynthesis, exudation, and release of PGIs are dependent on environmental conditions, relevant gene expression, and biodiversity among rice varieties. Along with the mechanism clarification, numerous analytical methods have been improved to effectively support the identification and isolation of rice PGIs during the last few decades. This paper provides an overview of rice PGIs and techniques used for determining and extracting those compounds from rice. In particular, the features, advantages, and limitations of conventional and upgraded extraction methods are comprehensively reported and discussed. The conventional extraction methods have been gradually replaced by advanced techniques consisting of pressurized liquid extraction (PLE), microwave-assisted extraction (MAE), and solid-phase extraction (SPE). Meanwhile, thin-layer chromatography (TLC), liquid chromatography (LC), gas chromatography (GC), mass spectrometry (MS), nuclear magnetic resonance (NMR), high-resolution mass spectrometry (HR-MS), infrared spectroscopy (IR), near-infrared spectroscopy (NIRS), and X-ray crystallography are major tools for rice PGI identification and confirmation. With smart agriculture becoming more prevalent, the statistics of rice PGIs and extraction methods will help to provide useful datasets for building an autonomous model for safer weed control. Conceivably, the efficient exploitation of rice PGIs will not only help to increase the yield and economic value of rice but may also pave the way for research directions on the development of smart and sustainable rice farming methods. Full article
(This article belongs to the Special Issue Separation, Extraction and Purification of Natural Products)
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19 pages, 3792 KiB  
Article
Screening the Efficacy of a Microbial Consortium of Bacteria and Fungi Isolated from Different Environmental Samples for the Degradation of LDPE/TPS Films
by Dajana Kučić Grgić, Martina Miloloža, Vesna Ocelić Bulatović, Šime Ukić, Miroslav Slouf and Veronika Gajdosova
Separations 2023, 10(2), 79; https://doi.org/10.3390/separations10020079 - 24 Jan 2023
Cited by 5 | Viewed by 2738
Abstract
In this study, a screening of the efficacy of a microbial consortium of bacteria and fungi isolated from activated sludge, river sediment, and compost for the degradation of LDPE/TPS was performed. According to the morphological and biochemical characterization, eight bacteria, Bacillus sonorensis, [...] Read more.
In this study, a screening of the efficacy of a microbial consortium of bacteria and fungi isolated from activated sludge, river sediment, and compost for the degradation of LDPE/TPS was performed. According to the morphological and biochemical characterization, eight bacteria, Bacillus sonorensis, Bacillus subtilis, Lysinibacillus massiliensis, Bacillus licheniformis, Bacillus indicus, Bacillus megaterium, Bacillus cereus, and Pseudomonas alcaligenes, five molds, Aspergillus sp. 1, Aspergillus sp. 2, Trichoderma sp., Rhizopus sp., Penicillium sp., and Alternaria sp., and a yeast, Candida parapsilosis, were identified. The first experiment E1 was inoculated with microorganisms isolated from activated sludge and river sediment, and E2 with microorganisms isolated from compost. In both experiments, different types of polymeric materials, low density polyethylene (E1-1 and E2-1), thermoplastic starch (E1-2 and E2-2), low density polyethylene + thermoplastic starch (E1-3 and E2-3), low density polyethylene + thermoplastic starch + styrene-ethylene-styrene (E1-4 and E2-4) were added. The obtained results, weight loss, SEM, and FTIR analysis showed that the microorganisms in both experiments were able to degrade polymeric materials. The mixed culture of microorganisms in experiments E1-2 and E2-2 completely degraded TPS (thermoplastic starch). The percent weight losses of LDPE, LDPE+20% TPS, and LDPE+20% TPS+SEBS in experiment E1 were 3.3184%, 14.1152%, and 16.0062% and in experiment E2 were 3.9625%, 20.4520% and 21.9277%, respectively. SEM microscopy shows that the samples with a LDPE matrix exhibited moderate surface degradation and negligible oxidative degradation under the given conditions. FTIR/ATR data demonstrate that degradation was more intense in E2 than in E1. Full article
(This article belongs to the Section Environmental Separations)
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37 pages, 1502 KiB  
Review
Factors Influencing the Prediction Accuracy of Model Peptides in Reversed-Phase Liquid Chromatography
by Othman Al Musaimi, Oscar M. Mercado-Valenzo and Daryl R. Williams
Separations 2023, 10(2), 81; https://doi.org/10.3390/separations10020081 - 24 Jan 2023
Cited by 2 | Viewed by 1935
Abstract
Hydrophobicity is an important physicochemical property of peptides in solution. As well as being strongly associated with peptide stability and aggregation, hydrophobicity governs the solution based chromatographic separation processes, specifically reversed-phase liquid chromatography (RPLC). In addition, hydrophobicity is a major physicochemical property of [...] Read more.
Hydrophobicity is an important physicochemical property of peptides in solution. As well as being strongly associated with peptide stability and aggregation, hydrophobicity governs the solution based chromatographic separation processes, specifically reversed-phase liquid chromatography (RPLC). In addition, hydrophobicity is a major physicochemical property of peptides in comparison to H-bonding, electrostatic, and aromatic properties in intermolecular interactions. However, a wide range of molecular factors can influence peptide hydrophobicity, with accurate predictions depending on specific peptide amino acid compositions, structure, and conformation. It is noticeable that peptide composition, the position of the amino acid, and its neighbouring groups play a crucial role in the elution process. In light of this, the same amino acid behaved differently depending on its position and neighbouring amino acid in the peptide chain. Extra attention should be paid to the denaturation process during the course of elution, as it has been shown to complicate and alter the elution pattern. This paper reports on the key peptide properties that can alter hydrophobicity and, consequently, the RPLC elution behaviour of the peptides, and it will conclude by proposing improved prediction algorithms for peptide elution in RPLC. Full article
(This article belongs to the Special Issue Advances in Chromatographic Analysis of Bioactive Compounds)
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16 pages, 4682 KiB  
Article
Dimethyl Carbonate as a Mobile-Phase Modifier for Normal-Phase and Hydrophilic Interaction Liquid Chromatography
by Philip D. Boes, Sophie R. Elleman and Neil D. Danielson
Separations 2023, 10(2), 70; https://doi.org/10.3390/separations10020070 - 18 Jan 2023
Cited by 5 | Viewed by 2108
Abstract
We studied the use of dimethyl carbonate (DMC) as a non-toxic, aprotic modifier for hydrophilic liquid interaction chromatography (HILIC) and as a modifier for normal-phase liquid chromatography (LC). A comparison of ethyl acetate (EA) and DMC as organic mobile-phase modifiers in hexane for [...] Read more.
We studied the use of dimethyl carbonate (DMC) as a non-toxic, aprotic modifier for hydrophilic liquid interaction chromatography (HILIC) and as a modifier for normal-phase liquid chromatography (LC). A comparison of ethyl acetate (EA) and DMC as organic mobile-phase modifiers in hexane for normal-phase LC of phthalates was conducted with a silica column and showed that retention factors (k) at the same modifier percentage were about a factor of two greater for DMC. Detection at 215 nm, possible with DMC, allowed for the better detection of the phthalates by a factor of 10, compared with EA detection, best at a 254 nm wavelength. Using a core-shell silica column, HILIC separations of trans-ferulic acid, syringic acid, and vanillic acid were compared between acetonitrile (MeCN) and DMC as the organic portion of the mobile phase, from 80–95%. The analyte retention for DMC, when compared to MeCN, was about 1.5 times greater, with only a moderate increase in back pressure. Plate count and peak asymmetry were somewhat better for the DMC chromatograms, compared to those with MeCN. Seven mono- and di-hydroxybenzoic acid positional isomers could be resolved effectively with DMC. Sorbate and benzoate preservatives in commercial drinks were also determined. Full article
(This article belongs to the Special Issue Novel Applications of Separation Technology)
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15 pages, 1348 KiB  
Article
Improved Method for the Detection of Highly Polar Pesticides and Their Main Metabolites in Foods of Animal Origin: Method Validation and Application to Monitoring Programme
by Emanuela Verdini, Veronica Maria Teresa Lattanzio, Biancamaria Ciasca, Laura Fioroni and Ivan Pecorelli
Separations 2023, 10(1), 44; https://doi.org/10.3390/separations10010044 - 10 Jan 2023
Cited by 2 | Viewed by 2173
Abstract
The application of polar pesticides in agricultural production has been of great interest due to their low costs and their high effectiveness. For this reason, the possibility of their transfer to foods of animal origin is of great concern for human health. The [...] Read more.
The application of polar pesticides in agricultural production has been of great interest due to their low costs and their high effectiveness. For this reason, the possibility of their transfer to foods of animal origin is of great concern for human health. The manuscript describes the implementation and validation of an analytical method to detect polar pesticides, at regulatory levels, in three foods of animal origin, including bovine fat, chicken eggs, and cow milk. The method was fully validated to detect glyphosate, glufosinate, and their respective metabolites in the above-mentioned foods obtaining fit-for-purpose sensitivity, recoveries (76–119%), repeatability (≤20%), within-laboratory reproducibility (≤20%), and experimental measurement uncertainty less than 50% as required by the SANTE/11312/2021 criteria. Given the satisfactory results, the applicability of the method to additional molecules belonging to the same category (AMPA, cyanuric acid, ethephon, fosetyl aluminum, HEPA, maleic hydrazide, and N-acetyl-glyphosate) was also evaluated in order to meet possible future requests. Finally, the implemented method was applied to analyse samples over the period of March 2021 to August 2022 from two Italian regions (Umbria and Marche) within the national monitoring programme. In agreement with previously available data, none of the samples analysed showed the presence of glyphosate and glufosinate at levels above the legal limit. Full article
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19 pages, 6437 KiB  
Article
The Effect of the Elemental Composition of Municipal Sewage Sludge on the Phosphorus Recycling during Pyrolysis, with a Focus on the Char Chemistry—Modeling and Experiments
by Naeimeh Vali, Aurélie Combres, Aida Hosseinian and Anita Pettersson
Separations 2023, 10(1), 31; https://doi.org/10.3390/separations10010031 - 04 Jan 2023
Cited by 2 | Viewed by 1253
Abstract
The present study investigates how the original sewage sludge characteristics influence the composition of sewage sludge-based chars for land applications. Sewage sludge from two different wastewater treatment plants in Sweden was pyrolyzed at 500, 700, and 900 °C, and the resulting chars were [...] Read more.
The present study investigates how the original sewage sludge characteristics influence the composition of sewage sludge-based chars for land applications. Sewage sludge from two different wastewater treatment plants in Sweden was pyrolyzed at 500, 700, and 900 °C, and the resulting chars were analyzed. Thermodynamic equilibrium calculations (TEC), together with chemical fractionation, were implemented to simulate the char after the pyrolysis process at different temperatures. The results showed that, in general, for both the municipal sewage sludge (MSS), phosphorus (P) was significantly retained in the char at various temperatures. However, no specific correlation could be found between the pyrolysis temperature and the amount of P remaining. With regard to the heavy metals removed from the char after the pyrolysis reaction, the concentrations of copper, chromium, lead, nickel, zinc, and cadmium were below the limits of the Swedish regulations for farmland application. Full article
(This article belongs to the Special Issue Application of Green Separation Technology in Wastewater Treatment)
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28 pages, 2983 KiB  
Review
Mass Spectrometric Methods for Non-Targeted Screening of Metabolites: A Future Perspective for the Identification of Unknown Compounds in Plant Extracts
by Michael Sasse and Matthias Rainer
Separations 2022, 9(12), 415; https://doi.org/10.3390/separations9120415 - 07 Dec 2022
Cited by 1 | Viewed by 3533
Abstract
Phyto products are widely used in natural products, such as medicines, cosmetics or as so-called “superfoods”. However, the exact metabolite composition of these products is still unknown, due to the time-consuming process of metabolite identification. Non-target screening by LC-HRMS/MS could be a technique [...] Read more.
Phyto products are widely used in natural products, such as medicines, cosmetics or as so-called “superfoods”. However, the exact metabolite composition of these products is still unknown, due to the time-consuming process of metabolite identification. Non-target screening by LC-HRMS/MS could be a technique to overcome these problems with its capacity to identify compounds based on their retention time, accurate mass and fragmentation pattern. In particular, the use of computational tools, such as deconvolution algorithms, retention time prediction, in silico fragmentation and sophisticated search algorithms, for comparison of spectra similarity with mass spectral databases facilitate researchers to conduct a more exhaustive profiling of metabolic contents. This review aims to provide an overview of various techniques and tools for non-target screening of phyto samples using LC-HRMS/MS. Full article
(This article belongs to the Special Issue Novel Applications of Separation Technology)
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37 pages, 1644 KiB  
Review
Heterogeneous Catalytic Ozonation: Solution pH and Initial Concentration of Pollutants as Two Important Factors for the Removal of Micropollutants from Water
by Savvina Psaltou, Manassis Mitrakas and Anastasios Zouboulis
Separations 2022, 9(12), 413; https://doi.org/10.3390/separations9120413 - 06 Dec 2022
Cited by 7 | Viewed by 1308
Abstract
There are several publications on heterogeneous catalytic ozonation; however, their conclusions and the comparisons between them are not always consistent due to the variety of applied experimental conditions and the different solid materials used as catalysts. This review attempts to limit the major [...] Read more.
There are several publications on heterogeneous catalytic ozonation; however, their conclusions and the comparisons between them are not always consistent due to the variety of applied experimental conditions and the different solid materials used as catalysts. This review attempts to limit the major influencing factors in order to reach more vigorous conclusions. Particularly, it highlights two specific factors/parameters as the most important for the evaluation and comparison of heterogeneous catalytic ozonation processes, i.e., (1) the pH value of the solution and (2) the initial concentration of the (micro-)pollutants. Based on these, the role of Point of Zero Charge (PZC), which concerns the respective solid materials/catalysts in the decomposition of ozone towards the production of oxidative radicals, is highlighted. The discussed observations indicate that for the pH range 6–8 and when the initial organic pollutants’ concentrations are around 1 mg/L (or even lower, i.e., micropollutant), then heterogeneous catalytic ozonation follows a radical mechanism, whereas the applied solid materials show their highest catalytic activity under their neutral charge. Furthermore, carbons are considered as a rather controversial group of catalysts for this process due to their possible instability under intense ozone oxidizing conditions. Full article
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16 pages, 2001 KiB  
Article
Bioactive Phytochemical Composition of Grape Pomace Resulted from Different White and Red Grape Cultivars
by Petronela Anca Onache, Elisabeta-Irina Geana, Corina Teodora Ciucure, Alina Florea, Dorin Ioan Sumedrea, Roxana Elena Ionete and Ovidiu Tița
Separations 2022, 9(12), 395; https://doi.org/10.3390/separations9120395 - 28 Nov 2022
Cited by 10 | Viewed by 2441
Abstract
Grapes are rich in phenolic compounds, being important for human health with anti-inflammatory, antiatherosclerotic, antimutagenic, anticarcinogenic, antibacterial, antiviral, and antimicrobial activity. The winemaking of the grapes generates significant amounts of waste. These wastes contain bioactive compounds in their biomass that can be used [...] Read more.
Grapes are rich in phenolic compounds, being important for human health with anti-inflammatory, antiatherosclerotic, antimutagenic, anticarcinogenic, antibacterial, antiviral, and antimicrobial activity. The winemaking of the grapes generates significant amounts of waste. These wastes contain bioactive compounds in their biomass that can be used as a source of food improvement or as a source of nutrition supplementation. This study looks at the content of bioactive compounds, the polyphenolic profile, and the antioxidant activity in different white and red grape pomaces. The investigation of bioactive characteristics (total polyphenols, total flavonoids, catechins, tannins, and antioxidant activity) was carried out by UV-Vis spectrophotometric methods, while the individual polyphenolic composition was investigated by target and screening UHPLC-HRMS/MS analysis. Principal components (PCA) and the heat maps analysis allows the discrimination between the grape pomace resulted from white grape cultivars (Muscat Ottonel and Tamaioasa Romaneasca) and red grape pomaces (Cabernet Sauvignon, Merlot, Feteasca Neagra, Burgund Mare, Pinot Nore), with the identification of the specific phenolic compounds for each grape pomace type. Full article
(This article belongs to the Section Analysis of Food and Beverages)
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28 pages, 1968 KiB  
Review
Metal-Chelating Peptides Separation Using Immobilized Metal Ion Affinity Chromatography: Experimental Methodology and Simulation
by Rachel Irankunda, Jairo Andrés Camaño Echavarría, Cédric Paris, Loïc Stefan, Stéphane Desobry, Katalin Selmeczi, Laurence Muhr and Laetitia Canabady-Rochelle
Separations 2022, 9(11), 370; https://doi.org/10.3390/separations9110370 - 14 Nov 2022
Cited by 14 | Viewed by 3792
Abstract
Metal-Chelating Peptides (MCPs), obtained from protein hydrolysates, present various applications in the field of nutrition, pharmacy, cosmetic etc. The separation of MCPs from hydrolysates mixture is challenging, yet, techniques based on peptide-metal ion interactions such as Immobilized Metal Ion Affinity Chromatography (IMAC) seem [...] Read more.
Metal-Chelating Peptides (MCPs), obtained from protein hydrolysates, present various applications in the field of nutrition, pharmacy, cosmetic etc. The separation of MCPs from hydrolysates mixture is challenging, yet, techniques based on peptide-metal ion interactions such as Immobilized Metal Ion Affinity Chromatography (IMAC) seem to be efficient. However, separation processes are time consuming and expensive, therefore separation prediction using chromatography modelling and simulation should be necessary. Meanwhile, the obtention of sorption isotherm for chromatography modelling is a crucial step. Thus, Surface Plasmon Resonance (SPR), a biosensor method efficient to screen MCPs in hydrolysates and with similarities to IMAC might be a good option to acquire sorption isotherm. This review highlights IMAC experimental methodology to separate MCPs and how, IMAC chromatography can be modelled using transport dispersive model and input data obtained from SPR for peptides separation simulation. Full article
(This article belongs to the Section Bioanalysis/Clinical Analysis)
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40 pages, 3706 KiB  
Review
Magnetic Technologies and Green Solvents in Extraction and Separation of Bioactive Molecules Together with Biochemical Objects: Current Opportunities and Challenges
by Xueting Feng, Hang Song, Tenghe Zhang, Shun Yao and Yan Wang
Separations 2022, 9(11), 346; https://doi.org/10.3390/separations9110346 - 03 Nov 2022
Cited by 7 | Viewed by 2675
Abstract
Currently, magnetic technology and green solvents are widely used in chemical engineering, environmental engineering and other fields as they are environmentally friendly, easy to operate and highly efficient. Moreover, a magnetic field has positive effect on many physicochemical processes. However, related new methods, [...] Read more.
Currently, magnetic technology and green solvents are widely used in chemical engineering, environmental engineering and other fields as they are environmentally friendly, easy to operate and highly efficient. Moreover, a magnetic field has positive effect on many physicochemical processes. However, related new methods, materials, strategies and applications in separation science still need to be developed. In this review, a series of meaningful explorations of magnetic technologies for the separation of natural products and biologic objects, including magnetic ionic liquids and other magnetic solvents and fluids, magnetic nanoparticles and magnetic fields, and the development of magnetic separators were reviewed. Furthermore, the difficulties in the application and development of magnetic separation technology were discussed on the basis of comparison and data analysis, especially for the selection of magnetic materials and magnetic field sources. Finally, the progress in the development of magnetic separators was also elaborated for researchers, mainly including that of the new high-efficiency magnetic separator through multi-technology integration and the optimization of traditional magnetic separators, which help current techniques break through their bottleneck as a powerful driving force. Full article
(This article belongs to the Section Purification Technology)
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21 pages, 3869 KiB  
Article
Solubility of CO2 in 2-Amino-2-methyl-1-propanol (AMP) and 3-(Methylamino)propylamine (MAPA): Experimental Investigation and Modeling with the Cubic-Plus-Association and the Modified Kent-Eisenberg Models
by Giannis Kontos, Maria Anna Soldatou, Evangelos Tzimpilis and Ioannis Tsivintzelis
Separations 2022, 9(11), 338; https://doi.org/10.3390/separations9110338 - 02 Nov 2022
Cited by 2 | Viewed by 1992
Abstract
CO2 capture attracts significant research efforts in order to reduce the volume of greenhouse gases emitted from fossil fuels combustion. Among the studied processes, chemical absorption represents a mature approach and, in this direction, new solvents, alternatives to monoethanolamine (MEA), have been [...] Read more.
CO2 capture attracts significant research efforts in order to reduce the volume of greenhouse gases emitted from fossil fuels combustion. Among the studied processes, chemical absorption represents a mature approach and, in this direction, new solvents, alternatives to monoethanolamine (MEA), have been suggested. In this work, the solubility of CO2 in aqueous solutions of 2-amino-2-methyl-1-propanol (AMP) and 3-(methylamino)propylamine (MAPA), which were recently suggested as constituents of novel phase change solvent mixtures, is experimentally measured at 298, 313, 323, and 333 K and in a wide range of pressures, up to approximately 7 bar. As the available literature experimental data for MAPA aqueous solutions are very limited, the experimental results of this study were compared to respective literature data for AMP, and a very satisfactory agreement was observed. The new experimental data were correlated with the cubic-plus-association (CPA) and the modified Kent-Eisenberg models. It was observed that both models rather satisfactorily correlate the experimental data, with the Kent-Eisenberg model presenting more accurate correlations. Full article
(This article belongs to the Section Analysis of Energies)
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27 pages, 3372 KiB  
Review
Purification Technologies for NOx Removal from Flue Gas: A Review
by Zihan Zhu and Bin Xu
Separations 2022, 9(10), 307; https://doi.org/10.3390/separations9100307 - 13 Oct 2022
Cited by 18 | Viewed by 7495
Abstract
Nitrogen oxide (NOx) is a major gaseous pollutant in flue gases from power plants, industrial processes, and waste incineration that can have adverse impacts on the environment and human health. Many denitrification (de-NOx) technologies have been developed to reduce NOx emissions in the [...] Read more.
Nitrogen oxide (NOx) is a major gaseous pollutant in flue gases from power plants, industrial processes, and waste incineration that can have adverse impacts on the environment and human health. Many denitrification (de-NOx) technologies have been developed to reduce NOx emissions in the past several decades. This paper provides a review of the recent literature on NOx post-combustion purification methods with different reagents. From the perspective of changes in the valence of nitrogen (N), purification technologies against NOx in flue gas are classified into three approaches: oxidation, reduction, and adsorption/absorption. The removal processes, mechanisms, and influencing factors of each method are systematically reviewed. In addition, the main challenges and potential breakthroughs of each method are discussed in detail and possible directions for future research activities are proposed. This review provides a fundamental and systematic understanding of the mechanisms of denitrification from flue gas and can help researchers select high-performance and cost-effective methods. Full article
(This article belongs to the Section Environmental Separations)
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16 pages, 1002 KiB  
Article
Plant Poisons in the Garden: A Human Risk Assessment
by Samantha L. Bowerbank, Matteo D. Gallidabino and John R. Dean
Separations 2022, 9(10), 308; https://doi.org/10.3390/separations9100308 - 13 Oct 2022
Cited by 2 | Viewed by 2669
Abstract
A study of the plants, and their associated poisons, in the Poison Garden at The Alnwick Garden was undertaken across a calendar year. By selecting 25 plants in the Poison Garden, we have been able to develop a single chromatographic method for the [...] Read more.
A study of the plants, and their associated poisons, in the Poison Garden at The Alnwick Garden was undertaken across a calendar year. By selecting 25 plants in the Poison Garden, we have been able to develop a single chromatographic method for the determination and quantification of 15 plant toxins by liquid chromatography mass spectrometry (LC-MS). Chromatographic separation was achieved on a C18 column (3.5 µm, 100 × 4.6 mm) with a gradient method using water +0.1% formic acid and methanol +0.1% formic acid. The developed method was validated for precision, linearity, limits of detection and quantification and extraction recoveries. The method showed good linearity with a R2 value of >0.995 for all 15 compounds with good precision of 10.7%, 6.7% and 0.3% for the low, medium and high calibration points, respectively. The LC-MS method was used to analyse 25 plant species, as well as their respective parts (i.e., bulb, flower, fruit, leaf, pollen, seed, stem and root), to assess the human risk assessment to children (aged 1 to <2 years) in relation to the plant toxin and its respective LD50. The analysis found that the greatest potential health risks were due to the ingestion of Colchicum autumnale and Atropa belladonna. As a caution, all identified plants should be handled with care with additional precautionary steps to ensure nil contact by children because of the potential likelihood of hand-to-mouth ingestion. Full article
(This article belongs to the Section Environmental Separations)
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17 pages, 3861 KiB  
Article
Evaluation of Pulsed Electric Field-Assisted Extraction on the Microstructure and Recovery of Nutrients and Bioactive Compounds from Mushroom (Agaricus bisporus)
by Mara Calleja-Gómez, Juan Manuel Castagnini, Ester Carbó, Emilia Ferrer, Houda Berrada and Francisco J. Barba
Separations 2022, 9(10), 302; https://doi.org/10.3390/separations9100302 - 10 Oct 2022
Cited by 14 | Viewed by 2219
Abstract
Pulsed electric field (PEF) is a sustainable innovative technology that allows for the recovery of nutrients and bioactive compounds from vegetable matrices. A. bisporus was chosen for its nutritional value and the effect of PEF pretreatment was evaluated using different conditions of electric [...] Read more.
Pulsed electric field (PEF) is a sustainable innovative technology that allows for the recovery of nutrients and bioactive compounds from vegetable matrices. A. bisporus was chosen for its nutritional value and the effect of PEF pretreatment was evaluated using different conditions of electric field (2–3 kV/cm), specific energy (50–200 kJ/kg) and extraction time (0–6 h) to obtain the best conditions for nutrient and bioactive compound extraction. Spectrophotometric methods were used to evaluate the different compounds, along with an analysis of mineral content by inductively coupled plasma mass spectrometry (ICP-MS) and the surface was evaluated using scanning electron microscopy (SEM). In addition, the results were compared with those obtained by conventional extraction (under constant shaking without PEF pretreatment). After evaluating the extractions, the best extraction conditions were 2.5 kV/cm, 50 kJ/kg and 6 h which showed that PEF extraction increased the recovery of total phenolic compounds in 96.86%, carbohydrates in 105.28%, proteins in 11.29%, and minerals such as P, Mg, Fe and Se. These results indicate that PEF pretreatment is a promising sustainable technology to improve the extraction of compounds and minerals from mushrooms showing microporation on the surface, positioning them as a source of compounds of great nutritional interest. Full article
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15 pages, 4564 KiB  
Article
Filter Modified with Hydrophilic and Oleophobic Coating for Efficient and Affordable Oil/Water Separation
by Hunter Ross, Huyen Nguyen, Brian Nguyen, Ashton Foster, James Salud, Mike Patino, Yong X. Gan and Mingheng Li
Separations 2022, 9(10), 269; https://doi.org/10.3390/separations9100269 - 28 Sep 2022
Cited by 6 | Viewed by 2692
Abstract
To mitigate the damage of oil spills, a filter modified with a hydrophilic and oleophobic coating is proposed for affordable and efficient oil separation and recovery from water. The sol–gel method was chosen to produce a colloidal suspension of titanium dioxide particles for [...] Read more.
To mitigate the damage of oil spills, a filter modified with a hydrophilic and oleophobic coating is proposed for affordable and efficient oil separation and recovery from water. The sol–gel method was chosen to produce a colloidal suspension of titanium dioxide particles for its ease of production and its versatility in application for many different substrates, including paper and cloth fabric. After immersing the substrates into a titanium-containing solution, three techniques were applied to increase the production of titanium dioxide—microwave-assisted, refrigeration, and ultra-sonication. Contact angle tests were done to investigate the change in the filter’s oleophobicity. The titanium dioxide present on the surface of the filter was amorphous, but all treatment methods showed an improvement in oleophobicity. All treated filters improved oil filtration performance by up to eighty percent. The filters isolated motor oil from a mixture while allowing water to pass through. The coated filters also displayed photocatalytic activity by degrading methylene blue on its surface when exposed to sunlight, demonstrating the filter’s self-cleaning ability. For real-world applications, the filter can be supported by a stainless mesh for enhanced strength and durability. While being dragged through the water, the filter collects the surface oil, allowing water to pass through via gravity. Full article
(This article belongs to the Special Issue Novel Applications of Separation Technology)
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17 pages, 4397 KiB  
Review
Review of Hydrogen Sulfide Removal from Various Industrial Gases by Zeolites
by Tao Yu, Zhuo Chen, Zhendong Liu, Jianhong Xu and Yundong Wang
Separations 2022, 9(9), 229; https://doi.org/10.3390/separations9090229 - 25 Aug 2022
Cited by 10 | Viewed by 4467
Abstract
Hydrogen sulfide (H2S) removal from various industrial gases is crucial because it can cause huge damage to humans, the environment, and industrial production. Zeolite possesses huge specific surface area and well-developed pore structure, making it a promising adsorbent for H2 [...] Read more.
Hydrogen sulfide (H2S) removal from various industrial gases is crucial because it can cause huge damage to humans, the environment, and industrial production. Zeolite possesses huge specific surface area and well-developed pore structure, making it a promising adsorbent for H2S removal. This review attempts to comprehensively compile the current studies in the literature on H2S removal in gas purification processes using zeolites, including experimental and simulation studies, mechanism theory, and practical applications. Si/Al ratio, cations of zeolite, industrial gas composition and operating conditions, and H2S diffusion in zeolites affect desulfurization performance. However, further efforts are still needed to figure out the influence rules of the factors above and H2S removal mechanisms. Based on an extensive compilation of literature, we attempt to shed light on new perspectives for further research in the future. Full article
(This article belongs to the Special Issue Advances in Separation Engineering)
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26 pages, 955 KiB  
Review
An Overview of Methods for L-Dopa Extraction and Analytical Determination in Plant Matrices
by Carmen Tesoro, Filomena Lelario, Rosanna Ciriello, Giuliana Bianco, Angela Di Capua and Maria Assunta Acquavia
Separations 2022, 9(8), 224; https://doi.org/10.3390/separations9080224 - 17 Aug 2022
Cited by 12 | Viewed by 4252
Abstract
L-dopa is a precursor of dopamine used as the most effective symptomatic drug treatment for Parkinson’s disease. Most of the L-dopa isolated is either synthesized chemically or from natural sources, but only some plants belonging to the Fabaceae family contain significant amounts of [...] Read more.
L-dopa is a precursor of dopamine used as the most effective symptomatic drug treatment for Parkinson’s disease. Most of the L-dopa isolated is either synthesized chemically or from natural sources, but only some plants belonging to the Fabaceae family contain significant amounts of L-dopa. Due to its low stability, the unambiguous determination of L-dopa in plant matrices requires appropriate technologies. Several analytical methods have been developed for the determination of L-dopa in different plants. The most used for quantification of L-dopa are mainly based on capillary electrophoresis or chromatographic methods, i.e., high-performance liquid chromatography (HPLC), coupled to ultraviolet-visible or mass spectrometric detection. HPLC is most often used. This paper aims to give information on the latest developments in the chemical study of L-dopa, emphasizing the extraction, separation and characterization of this compound by chromatographic, electrochemical and spectral techniques. This study can help select the best possible strategy for determining L-dopa in plant matrices using advanced analytical methods. Full article
(This article belongs to the Section Analysis of Natural Products and Pharmaceuticals)
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18 pages, 4429 KiB  
Article
Metabolomic and Proteomic Profile of Dried Hop Inflorescences (Humulus lupulus L. cv. Chinook and cv. Cascade) by SPME-GC-MS and UPLC-MS-MS
by Paola Nezi, Vittoria Cicaloni, Laura Tinti, Laura Salvini, Matteo Iannone, Sara Vitalini and Stefania Garzoli
Separations 2022, 9(8), 204; https://doi.org/10.3390/separations9080204 - 06 Aug 2022
Cited by 15 | Viewed by 2595
Abstract
Hop (Humulus lupulus L.) is grown mainly for the production of beer. The flowers of the female plant give it the bitter taste and pungent aroma. There are a large number of hop varieties differing in their α-acid content, essential oil levels [...] Read more.
Hop (Humulus lupulus L.) is grown mainly for the production of beer. The flowers of the female plant give it the bitter taste and pungent aroma. There are a large number of hop varieties differing in their α-acid content, essential oil levels and odor profiles. Aside from their use in brewing, more recently, hops have been used for the pharmacological properties of its derivatives that are of great importance to the pharmaceutical industry. Hop is known to have a fairly complex chemistry characterized by the presence of a variety of sesquiterpenoids, diterpenoids and triterpenoids, phytoestrogens and flavonoids. Additionally, considering the countless applications in the pharmacological sector in recent years, a chemical characterization of the different cultivars is essential to better identify the source of specific secondary metabolites. For this purpose, the dried inflorescences of two hop cultivars, Chinook and Cascade, were investigated using Solid-Phase Microextraction-Gas Chromatography-Mass Spectrometry and Liquid Chromatography-Tandem Mass Spectrometry (SPME-GC-MS and LC-MS-MS) to describe their metabolomic and proteomic profile. Furthermore, thanks to an in-depth statistical survey, it was possible to carry out a comparative study highlighting interesting implications deriving from this investigative study. Full article
(This article belongs to the Special Issue Feature Papers in Separations from Editorial Board Members)
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20 pages, 2698 KiB  
Article
Simultaneous Extraction of Four Antibiotic Compounds from Soil and Water Matrices
by Alison M. Franklin, Danielle M. Andrews, Clinton F. Williams and John E. Watson
Separations 2022, 9(8), 200; https://doi.org/10.3390/separations9080200 - 02 Aug 2022
Cited by 7 | Viewed by 2461
Abstract
The incidence of antibiotic resistance is on the rise and becoming a major health concern. Analyzing the presence of antibiotic compounds in the environment is critical for determining the potential health effects for humans, animals, and ecosystems. For this study, methods were developed [...] Read more.
The incidence of antibiotic resistance is on the rise and becoming a major health concern. Analyzing the presence of antibiotic compounds in the environment is critical for determining the potential health effects for humans, animals, and ecosystems. For this study, methods were developed to simultaneously isolate and quantify four antibiotics important in human medicine (sulfamethoxazole—SMX, trimethoprim—TMP, lincomycin—LIN, and ofloxacin—OFL) in water and soil matrices. For water analysis, different solid phase extraction (SPE) cartridges (Oasis HLB plus and Phenomenex Strata-X) were compared. The Oasis HLB Plus SPE cartridge provided the highest and most consistent recoveries with 118 ± 5%, 86 ± 4%, 83 ± 5%, and 75 ± 1% for SMX, TMP, LIN, and OFL, respectively. For soil analysis, different pre-treatments (grinding and freeze-drying) and soil extraction methodologies (liquid-solid extraction and accelerated solvent extraction (ASE)) were compared. The ASE system resulted in the highest overall recoveries of SMX, TMP, LIN, and OFL with an optimal extracting solution of acetonitrile/water (v/v, 50:50, pH 2.8). When the soil was ground and freeze-dried, trimethoprim recovery increased and when soil was ground, but not freeze-dried, LIN and OFL recoveries increased, while sulfamethoxazole recoveries decreased when soil was ground and freeze-dried. Based on this research, matrix characteristics, especially pH, as well as the pKa’s and functional groups of the antibiotics need to be carefully considered when attempting to extract antibiotic compounds from a water or soil environment. Full article
(This article belongs to the Special Issue Analytical Separation Techniques for Environmental Analysis)
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13 pages, 3769 KiB  
Article
Fog Droplet Collection by Corona Discharge in a Needle–Cylinder Electrostatic Precipitator with a Water Cooling System
by Hui Fu, Wenyi Xu, Zhen Liu and Keping Yan
Separations 2022, 9(7), 169; https://doi.org/10.3390/separations9070169 - 06 Jul 2022
Cited by 9 | Viewed by 2290
Abstract
In this study, a needle–cylinder electrostatic precipitator with a water cooling system was designed to enhance the harvest of atmospheric water in wet flue gas. The effects of flow rate, temperature and particles on the collection of fog droplets were investigated. Meanwhile, the [...] Read more.
In this study, a needle–cylinder electrostatic precipitator with a water cooling system was designed to enhance the harvest of atmospheric water in wet flue gas. The effects of flow rate, temperature and particles on the collection of fog droplets were investigated. Meanwhile, the energy efficiency of water collection was analyzed at different voltages. The results show that the current decreases with the increase of air relative humidity under the same voltage, and the breakdown voltage increases obviously. Concurrently, by appropriately reducing the wet flue gas flow velocity, the residence time of fog droplets in the electric field can be increased, fully charging the droplets and improving the water collection efficiency. Moreover, experiments revealed that through decreasing the flue gas temperature, both the water collection rate and energy efficiency can be improved. In addition, the presence of particles in wet gas can improve the water collection rate by 5~8% at different discharge voltages. Finally, based on energy efficiency analysis, with the increase of voltage, although the water collection rate increased, the energy efficiency decreased. Full article
(This article belongs to the Section Environmental Separations)
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20 pages, 5122 KiB  
Article
Comparative Study of Natural Antioxidants from Glycine max, Anethum graveolensand Pimpinella anisum Seed and Sprout Extracts Obtained by Ultrasound-Assisted Extraction
by Fanica Balanescu, Anna Cazanevscaia Busuioc, Andreea Veronica Dediu Botezatu, Steluta Gosav, Sorin Marius Avramescu, Bianca Furdui and Rodica Mihaela Dinica
Separations 2022, 9(6), 152; https://doi.org/10.3390/separations9060152 - 13 Jun 2022
Cited by 6 | Viewed by 2342
Abstract
The study aimed to evaluate the antioxidant potential of sprout and seed extracts from three species of plants, namely Glycine max (GMsp-sprouts, GMsd-seeds), Anethum graveolens (AGsp-sprouts, AGsd-seeds) and Pimpinella anisum (PAsp-sprouts, PAsd-seeds), which are widely accepted by consumers and have various applications in [...] Read more.
The study aimed to evaluate the antioxidant potential of sprout and seed extracts from three species of plants, namely Glycine max (GMsp-sprouts, GMsd-seeds), Anethum graveolens (AGsp-sprouts, AGsd-seeds) and Pimpinella anisum (PAsp-sprouts, PAsd-seeds), which are widely accepted by consumers and have various applications in food flavoring, and also in natural medical treatments in the pharmaceutical industries. These plants are rich in valuable compounds that show a remarkable antioxidant power and are associated with many health benefits. Ethanol extracts were obtained by ultrasound-assisted extraction and they were comparatively evaluated for their in vitro antioxidant properties. The extracts were characterized by HPTLC, HPLC-DAD, total phenol content (TPC), total flavonoid content (TFC) analysis and antioxidant activities with different assays, such as total antioxidant capacity (TAC), 2,2′-azino-bis (3-ethylbenzothiazoline-6-sulfonic acid) radical cation decolorization assay (ABTS), 1,1-diphenyl 1-2-picryl-hydrazyl (DPPH) and iron binding ability of chelators. Our results showed that the sprout and seed extracts of the studied plants exhibited a high content of phytochemicals and promising antioxidant properties. The highest polyphenols content was detected for AGsd (53.02 ± 0.57 mg/g DW), PAsd (48.75 ± 0.34 mg/g DW) and the highest flavonoids content for PAsp (26.84 ± 0.57 mg/g DW). Moreover, the presence of valuable compounds was demonstrated by using HPTLC, FT-IR and HPLC-DAD techniques. In order to have a better understanding of the relationship between the biological properties and the electronic structure, a molecular modelling study of genistein was also conducted. Our approach to the comparative assessment of these three plant species was based on a priori knowledge from literature data; however, this study demonstrated that these plant extracts of seeds and also sprouts are excellent sources of natural antioxidants. Significant additional differences that were found in the phytochemical composition could be exploited in future research for pharmaceutical purposes. Full article
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12 pages, 678 KiB  
Article
HPLC-MS, GC and NMR Profiling of Bioactive Lipids of Human Milk and Milk of Dairy Animals (Cow, Sheep, Goat, Buffalo, Camel, Red Deer)
by Kirill Lagutin, Andrew MacKenzie, Stephen Bloor, Dawn Scott and Mikhail Vyssotski
Separations 2022, 9(6), 145; https://doi.org/10.3390/separations9060145 - 07 Jun 2022
Cited by 11 | Viewed by 2884
Abstract
For non-bovine milks, information regarding bioactive lipids is fragmented, unreliable or unavailable. The purpose of the current study was to analyse bioactive lipids in the milk of dairy animals using modern analytical methods to achieve the most reliable results. Bioactive lipids in human [...] Read more.
For non-bovine milks, information regarding bioactive lipids is fragmented, unreliable or unavailable. The purpose of the current study was to analyse bioactive lipids in the milk of dairy animals using modern analytical methods to achieve the most reliable results. Bioactive lipids in human milk were also analysed and used as a reference. A suite of modern analytical methods was employed, namely High Performance Liquid Chromatography-Mass Spectrometry (HPLC-MS), Gas Chromatography (GC) and Nuclear Magnetic Resonance (NMR). The total lipid content was determined, and phospholipid, fatty acid, neutral glycosphingolipids and ganglioside (GM3 and GD3) levels were measured. Lipid classes in selected milks were reliably characterised for the first time, including gangliosides in deer, camel and sheep; cerebrosides in deer, camel and buffalo; plasmalogens in deer, buffalo and goat and phospholipids in deer. Our study demonstrated the advantage of utilising a range of analytical techniques in order to characterise a diverse set of bioactive lipids. Full article
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15 pages, 2685 KiB  
Article
Measuring Vitamin D3 Metabolic Status, Comparison between Vitamin D Deficient and Sufficient Individuals
by Laura de los Santos Castillo-Peinado, Mónica Calderón-Santiago, Aura Dulcinea Herrera-Martínez, Soraya León-Idougourram, María Ángeles Gálvez-Moreno, Rafael Luis Sánchez-Cano, Roger Bouillon, Jose Manuel Quesada-Gómez and Feliciano Priego-Capote
Separations 2022, 9(6), 141; https://doi.org/10.3390/separations9060141 - 03 Jun 2022
Cited by 5 | Viewed by 1746
Abstract
The main branch of vitamin D3 metabolism involves several hydroxylation reactions to obtain mono-, di- and trihydroxylated metabolites, including the circulating and active forms—25(OH)D3 and 1,25(OH)2D3, respectively. However, most clinical trials strictly target the determination of 25(OH)D [...] Read more.
The main branch of vitamin D3 metabolism involves several hydroxylation reactions to obtain mono-, di- and trihydroxylated metabolites, including the circulating and active forms—25(OH)D3 and 1,25(OH)2D3, respectively. However, most clinical trials strictly target the determination of 25(OH)D3 to offer a view of the metabolic status of vitamin D3. Due to the growing interest in expanding this restricted view, we have developed a method for measuring vitamin D3 metabolism by determination of vitamin D3, 25(OH)D3, 24,25(OH)2D3, 1,25(OH)2D3 and 1,24,25(OH)3D3 in human plasma. The method was based on SPE–LC–MS/MS with a large volume injection of human plasma (240 µL). Detection of di- and trihydroxymetabolites, found at the picogram per milliliter level, was attained by the combined action of high preconcentration and clean-up effects. The method allows obtaining information about ratios such as the known vitamin D metabolite ratio (24,25(OH)2D3/25(OH)D3), which can provide complementary views of vitamin D3 metabolic status. The method was applied to a cohort of obese patients and a reference cohort of healthy volunteers to find metabolic correlations between target analytes as well as differences as a function of vitamin D levels within and between cohorts. Full article
(This article belongs to the Special Issue Chromatographic Analysis of Biological Samples)
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12 pages, 1274 KiB  
Article
Validation of an Analytical Method for the Determination of Thiabendazole in Various Food Matrices
by Sun-Il Choi, Xionggao Han, Se-Jeong Lee, Xiao Men, Geon Oh, Doo-Sik Lee and Ok-Hwan Lee
Separations 2022, 9(6), 135; https://doi.org/10.3390/separations9060135 - 27 May 2022
Cited by 7 | Viewed by 3029
Abstract
In many countries, thiabendazole is used as a fungicide to prevent the decay of food and to lengthen storage periods. However, in Korea, thiabendazole is unauthorised and does not have standards or specifications for use as a food additive. In this study, a [...] Read more.
In many countries, thiabendazole is used as a fungicide to prevent the decay of food and to lengthen storage periods. However, in Korea, thiabendazole is unauthorised and does not have standards or specifications for use as a food additive. In this study, a simple analytical method was developed and validated using the HPLC–PDA method to detect thiabendazole in foods frequently consumed in South Korea. The calibration curve was obtained using samples of solid and liquid foods containing banana and citrus fruits containing concentrations in the range of 0.31–20.00 μg/mL with a satisfactory coefficient of determination (R2) of 0.999. The limit of detection (LOD) values for the solid and liquid food samples were 0.009 and 0.017 μg/mL, respectively, and the limit of quantification (LOQ) values were 0.028 and 0.052 μg/mL. The intra-day and inter-day precision values were less than 1.33% (relative standard deviation), and the recoveries of thiabendazole from spiked solid and liquid food samples ranged from 93.61 to 98.08% at concentration levels of 2.5, 5, and 10 μg/mL. In addition, the expanded uncertainties of the measu-rements ranged from 0.57 to 3.12%. These results showed that the developed method was appropriate for the quantitative analysis of thiabendazole in solid and liquid foods containing banana and citrus fruits. Full article
(This article belongs to the Section Analysis of Food and Beverages)
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18 pages, 7895 KiB  
Article
Modified Polyethersulfone Ultrafiltration Membrane for Enhanced Antifouling Capacity and Dye Catalytic Degradation Efficiency
by Mingming Wang, Feiyun Sun, Haojie Zeng, Xiaoli Su, Guofei Zhou, Hao Liu and Dingyu Xing
Separations 2022, 9(4), 92; https://doi.org/10.3390/separations9040092 - 04 Apr 2022
Cited by 11 | Viewed by 2808
Abstract
Catalytic membranes, as a combination of heterogeneous advanced oxidation and membrane technology reaction systems, have important application prospects in the treatment of dyes and other organics. In practical applications, it is still challenging to construct catalytic membranes with excellent removal efficiency and fouling [...] Read more.
Catalytic membranes, as a combination of heterogeneous advanced oxidation and membrane technology reaction systems, have important application prospects in the treatment of dyes and other organics. In practical applications, it is still challenging to construct catalytic membranes with excellent removal efficiency and fouling mitigation. Herein, molybdenum disulfide-iron oxyhydroxide (MoS2-FeOOH) was fabricated using iron oxide and MoS2 nanoflakes, which were synthesized by the hydrothermal method. Furthermore, by changing the concentration of MoS2-FeOOH, the MoS2-FeOOH/polyethersulfone (PES) composite ultrafiltration membrane was obtained with improved hydrophilicity, permeability, and antifouling capacity. The pure water flux of the composite membrane reached 385.3 L/(m2·h), which was 1.7 times that of the blank PES membrane. Compared with the blank membrane, with the increase of MoS2-FeOOH content, the MoS2-FeOOH/PES composite membranes had better adsorption capacity and catalytic performance, and the membrane with 3.0% MoS2-FeOOH content (M4) could be achieved at a 60.2% methylene blue (MB) degradation rate. In addition, the membrane flux recovery ratio (FRR) of the composite membrane also increased from 25.6% of blank PES membrane (M0) to more than 70% after two cycles of bovine serum albumin (BSA) filtration and hydraulic cleaning. The membrane with 2.25% MoS2-FeOOH content (M3) had the best antifouling performance, with the largest FRR and the smallest irreversible ratio (Rir). Catalytic self-cleaning of the composite membrane M3 recovered 95% of the initial flux with 0.1 mol/L H2O2 cleaning. The MoS2-FeOOH/PES composite membranes with the functions of excellent rejection and antifouling capacity have a good prospect in the treatment of printing and dyeing wastewater composed of soluble dyes. Full article
(This article belongs to the Section Materials in Separation Science)
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21 pages, 1176 KiB  
Review
Separation of Serum and Plasma Proteins for In-Depth Proteomic Analysis
by Joseph Paul and Timothy D. Veenstra
Separations 2022, 9(4), 89; https://doi.org/10.3390/separations9040089 - 01 Apr 2022
Cited by 14 | Viewed by 8460
Abstract
There are probably no biological samples that did more to spur interest in proteomics than serum and plasma. The belief was that comparing the proteomes of these samples obtained from healthy and disease-affected individuals would lead to biomarkers that could be used to [...] Read more.
There are probably no biological samples that did more to spur interest in proteomics than serum and plasma. The belief was that comparing the proteomes of these samples obtained from healthy and disease-affected individuals would lead to biomarkers that could be used to diagnose conditions such as cancer. While the continuing development of mass spectrometers with greater sensitivity and resolution has been invaluable, the invention of strategic strategies to separate circulatory proteins has been just as critical. Novel and creative separation techniques were required because serum and plasma probably have the greatest dynamic range of protein concentration of any biological sample. The concentrations of circulating proteins can range over twelve orders of magnitude, making it a challenge to identify low-abundance proteins where the bulk of the useful biomarkers are believed to exist. The major goals of this article are to (i) provide an historical perspective on the rapid development of serum and plasma proteomics; (ii) describe various separation techniques that have made obtaining an in-depth view of the proteome of these biological samples possible; and (iii) describe applications where serum and plasma proteomics have been employed to discover potential biomarkers for pathological conditions. Full article
(This article belongs to the Special Issue Separations and Analysis of Proteins in Biological Samples)
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21 pages, 1708 KiB  
Article
Adverse Effects of Arsenic Uptake in Rice Metabolome and Lipidome Revealed by Untargeted Liquid Chromatography Coupled to Mass Spectrometry (LC-MS) and Regions of Interest Multivariate Curve Resolution
by Miriam Pérez-Cova, Romà Tauler and Joaquim Jaumot
Separations 2022, 9(3), 79; https://doi.org/10.3390/separations9030079 - 18 Mar 2022
Cited by 11 | Viewed by 3295
Abstract
Rice crops are especially vulnerable to arsenic exposure compared to other cereal crops because flooding growing conditions facilitates its uptake. Besides, there are still many unknown questions about arsenic’s mode of action in rice. Here, we apply two untargeted approaches using liquid chromatography [...] Read more.
Rice crops are especially vulnerable to arsenic exposure compared to other cereal crops because flooding growing conditions facilitates its uptake. Besides, there are still many unknown questions about arsenic’s mode of action in rice. Here, we apply two untargeted approaches using liquid chromatography coupled to mass spectrometry (LC-MS) to unravel the effects on rice lipidome and metabolome in the early stages of growth. The exposure is evaluated through two different treatments, watering with arsenic-contaminated water and soil containing arsenic. The combination of regions of interest (ROI) and multivariate curve resolution (MCR) strategies in the ROIMCR data analyses workflow is proposed and complemented with other multivariate analyses such as partial least square discriminant analysis (PLS-DA) for the identification of potential markers of arsenic exposure and toxicity effects. The results of this study showed that rice metabolome (and lipidome) in root tissues seemed to be more affected by the watering and soil treatment. In contrast, aerial tissues alterations were accentuated by the arsenic dose, rather than with the watering and soil treatment itself. Up to a hundred lipids and 40 metabolites were significantly altered due to arsenic exposure. Major metabolic alterations were found in glycerophospholipids, glycerolipids, and amino acid-related pathways. Full article
(This article belongs to the Section Chromatographic Separations)
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23 pages, 4583 KiB  
Review
The Bright and Dark Sides of Reactive Oxygen Species Generated by Copper–Peptide Complexes
by Urszula K. Komarnicka, Monika K. Lesiów, Maciej Witwicki and Alina Bieńko
Separations 2022, 9(3), 73; https://doi.org/10.3390/separations9030073 - 11 Mar 2022
Cited by 6 | Viewed by 3308
Abstract
Copper ions bind to biomolecules (e.g., peptides and proteins) playing an essential role in many biological and physiological pathways in the human body. The resulting complexes may contribute to the initiation of neurodegenerative diseases, cancer, and bacterial and viral diseases, or act as [...] Read more.
Copper ions bind to biomolecules (e.g., peptides and proteins) playing an essential role in many biological and physiological pathways in the human body. The resulting complexes may contribute to the initiation of neurodegenerative diseases, cancer, and bacterial and viral diseases, or act as therapeutics. Some compounds can chemically damage biological macromolecules and initiate the development of pathogenic states. Conversely, a number of these compounds may have antibacterial, antiviral, and even anticancer properties. One of the most significant current discussions in Cu biochemistry relates to the mechanisms of the positive and negative actions of Cu ions based on the generation of reactive oxygen species, including radicals that can interact with DNA molecules. This review aims to analyze various peptide–copper complexes and the mechanism of their action. Full article
(This article belongs to the Section Bioanalysis/Clinical Analysis)
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15 pages, 1438 KiB  
Article
Fractionation of Metal(loid)s in Three European Mine Wastes by Sequential Extraction
by Chiamaka Belsonia Opara, Sabine Kutschke and Katrin Pollmann
Separations 2022, 9(3), 67; https://doi.org/10.3390/separations9030067 - 02 Mar 2022
Cited by 6 | Viewed by 3036
Abstract
Mine waste can constitute an environmental hazard, especially when poorly managed. Environmental assessment is essential for estimating potential threats and optimizing mine waste management. This study evaluated the potential environmental risk of sulfidic mine waste samples originating from the Neves Corvo Mine, Portugal, [...] Read more.
Mine waste can constitute an environmental hazard, especially when poorly managed. Environmental assessment is essential for estimating potential threats and optimizing mine waste management. This study evaluated the potential environmental risk of sulfidic mine waste samples originating from the Neves Corvo Mine, Portugal, and the closed Freiberg mining district, Germany. Metal(loid)s in the waste samples were partitioned into seven operationally defined fractions using the Zeien and Brummer sequential extraction scheme. The results showed similar partitioning patterns for the elements in the waste rock and tailing samples from Neves Corvo Mine; most metal(loid)s showed lower mobility, as they were mainly residual-bound. On the contrary, the Freiberg tailing sample had considerably elevated (24–37%) mobile fractions of Zn, Co, Cd, and Mn. The majority of Fe (83–96%) in all samples was retained in the residual fractions, while Ca was highly mobile. Overall, Pb was the most mobile toxic element in the three samples. A large portion of Pb (32–57%) was predominantly found in the most mobilizable fractions of the studied waste samples. This study revealed that the three mine wastes have contamination potential for Pb and Zn, which can be easily released into the environment from these waste sources. Full article
(This article belongs to the Section Environmental Separations)
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15 pages, 1951 KiB  
Review
Separation and Recycling Potential of Rare Earth Elements from Energy Systems: Feed and Economic Viability Review
by Ajay B. Patil, Viktoria Paetzel, Rudolf P. W. J. Struis and Christian Ludwig
Separations 2022, 9(3), 56; https://doi.org/10.3390/separations9030056 - 24 Feb 2022
Cited by 24 | Viewed by 5381
Abstract
This review explores the potential of separating and recycling rare earth elements (REEs) from different energy conversion systems, such as wind turbines, electric vehicles batteries, or lighting devices. The REEs include 17 elements (with global production of 242 kilometric tons in 2020) that [...] Read more.
This review explores the potential of separating and recycling rare earth elements (REEs) from different energy conversion systems, such as wind turbines, electric vehicles batteries, or lighting devices. The REEs include 17 elements (with global production of 242 kilometric tons in 2020) that can be found abundantly in nature. However, they are expensive and complicated to extract and separate with many environmental challenges. The overall demand for REEs is continuously growing (with a 10% yearly increase) and it is quite clear that recycling has to be developed as a supply strategy in addition to conventional mining. However, the success of both mining and recycling depends on appropriate separation and processing technologies. The overall REE recycling situation today is very weak (only 2% of REEs are recovered by recycling processes compared with 90% for iron and steel). The biggest recycling potentials rely on the sectors of lamp phosphors (17%), permanent magnets (7%), and NiMH batteries (10%) mainly at the end-of-life stage of the products. The profitability of rare earth recycling mostly depends on the prices of the elements to accommodate the processing costs. Therefore, end-of-life REE recycling should focus on the most valuable and critical REEs. Thus, the relevant processes, feed, and economic viability warrant the detailed review as reported here. Full article
(This article belongs to the Collection State of the Art in Separation and Analysis of Energies)
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12 pages, 713 KiB  
Article
Monitoring of Aflatoxin M1 in Various Origins Greek Milk Samples Using Liquid Chromatography Tandem Mass Spectrometry
by Anthi Panara, Maria Katsa, Marios Kostakis, Erasmia Bizani and Nikolaos S. Thomaidis
Separations 2022, 9(3), 58; https://doi.org/10.3390/separations9030058 - 24 Feb 2022
Cited by 9 | Viewed by 2936
Abstract
Aflatoxin M1(AFM1), a major metabolite of Aflatoxin B1(AFB1), has been identified as a potential contaminant in dairy products. Because of its possible carcinogenicity, the legislation limits as set by Commission Regulation (EC) No. 1881/2006 are very strict, namely 0.050 μg kg−1 in [...] Read more.
Aflatoxin M1(AFM1), a major metabolite of Aflatoxin B1(AFB1), has been identified as a potential contaminant in dairy products. Because of its possible carcinogenicity, the legislation limits as set by Commission Regulation (EC) No. 1881/2006 are very strict, namely 0.050 μg kg−1 in milk and 0.025 μg kg−1 in infant formulas. To meet these requirements, a sensitive and accurate method was developed, employing liquid chromatography tandem mass spectrometry (UPLC-MS/MS). Ιmmunoaffinity columns (R-Biopharm) were used for sample purification and preconcentration of the analyte of interest. The quantification of AFM1 was conducted using fortified milk samples, while Aflatoxin B2 (AFB2) was used as an internal standard (IS). The method was validated in terms of linearity, precision, trueness, limits of detection and quantification and uncertainty. The performance criteria for the method were evaluated based on European Commission Regulation (EC) No. 401/2006 and its most recent amendment, as well as the suggested criteria for revision by the EU Reference Laboratory for Mycotoxins and Plant Toxins. The recovery was in the range of 77.9–81.0% for all fortification levels (0.025–0.050–0.075 μg kg−1), with RSDR values (Relative Standard Deviation of intermediate precision) ranging from 6.1% to 12%. The method’s detection and quantification limits were 0.0027 μg kg−1 and 0.0089 μg kg−1, respectively. The occurrence of AFM1 was investigated in 40 samples of different animal origin (cow, goat and sheep milk) provided by Greek producers. Full article
(This article belongs to the Section Analysis of Food and Beverages)
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27 pages, 28582 KiB  
Review
Small-Pore Zeolite Membranes: A Review of Gas Separation Applications and Membrane Preparation
by Zishu Cao, Ninad D. Anjikar and Shaowei Yang
Separations 2022, 9(2), 47; https://doi.org/10.3390/separations9020047 - 09 Feb 2022
Cited by 17 | Viewed by 5055
Abstract
There have been significant advancements in small-pore zeolite membranes in recent years. With pore size closely related to many energy- or environment-related gas molecules, small-pore zeolite membranes have demonstrated great potential for the separation of some interested gas pairs, such as CO2 [...] Read more.
There have been significant advancements in small-pore zeolite membranes in recent years. With pore size closely related to many energy- or environment-related gas molecules, small-pore zeolite membranes have demonstrated great potential for the separation of some interested gas pairs, such as CO2/CH4, CO2/N2 and N2/CH4. Small-pore zeolite membranes share some characteristics but also have distinctive differences depending on their framework, structure and zeolite chemistry. Through this mini review, the separation performance of different types of zeolite membranes with respect to interested gas pairs will be compared. We aim to give readers an idea of membrane separation status. A few representative synthesis conditions are arbitrarily chosen and summarized, along with the corresponding separation performance. This review can be used as a quick reference with respect to the influence of synthesis conditions on membrane quality. At the end, some general findings and perspectives will be discussed. Full article
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19 pages, 1146 KiB  
Review
Chiral Pesticides with Asymmetric Sulfur: Extraction, Separation, and Determination in Different Environmental Matrices
by Rocío López-Cabeza and Antonio Francioso
Separations 2022, 9(2), 29; https://doi.org/10.3390/separations9020029 - 26 Jan 2022
Cited by 11 | Viewed by 2987
Abstract
Chiral pesticides with S atoms as asymmetric centers are gaining great importance in the search for new pesticides with new modes of action. As for the rest of the chiral pesticides, the determination of the stereoisomers separately has become crucial in the environmental [...] Read more.
Chiral pesticides with S atoms as asymmetric centers are gaining great importance in the search for new pesticides with new modes of action. As for the rest of the chiral pesticides, the determination of the stereoisomers separately has become crucial in the environmental risks assessment of these pesticides. Therefore, the development of suitable extraction and clean-up methods as well as efficient stereoselective analytical techniques for stereoisomers determination in environmental samples is essential. Currently, liquid/solid phase extraction, microextraction, and QuEChERS-based methods are most commonly used to obtain chiral pesticides from environmental samples. Gas, liquid, and supercritical fluid chromatography together with capillary electrophoresis techniques are the most important for the determination of the stereoisomers of chiral pesticides containing S atoms in its structure. In this study, all these techniques are briefly reviewed, and the advantages and disadvantages of each are discussed. Full article
(This article belongs to the Section Analysis of Natural Products and Pharmaceuticals)
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17 pages, 3034 KiB  
Article
Flavonoids Extraction Kinetics, Antimicrobial Activity and Radical Scavenging Potential of Bulgarian Woundwort (Solidago virgaurea L.)
by Zvezdelina Yaneva, Evgeni Simeonov, Nikolina Rusenova, Donika Ivanova, Galina Nikolova, Yanka Karamalakova, Chavdar Chilev and Georgi Beev
Separations 2022, 9(2), 27; https://doi.org/10.3390/separations9020027 - 21 Jan 2022
Cited by 6 | Viewed by 3218
Abstract
The medicinal plant woundwort (Solidago virgaurea L.) characterizes by diuretic, antimutagenic, anti-inflammatory activity and it has been applied for urinary tract, nephrolithiasis and prostate disorders treatment. The aim of the present study was to analyze the extraction kinetics of catechin, epigallocatechin and [...] Read more.
The medicinal plant woundwort (Solidago virgaurea L.) characterizes by diuretic, antimutagenic, anti-inflammatory activity and it has been applied for urinary tract, nephrolithiasis and prostate disorders treatment. The aim of the present study was to analyze the extraction kinetics of catechin, epigallocatechin and quercetin from Bulgarian woundwort extracts, to assess the antibacterial potential of the medicinal plant extracts against four bacterial strains (Staphylococcus aureus ATCC25923, Escherichia coli ATCC 25922, Pseudomonas aeruginosa ATCC 27853 and Bacillus cereus), their antioxidant capacity and radical scavenging potential. The concentrations of the flavonoids in the extracts obtained at different extraction conditions (solvent, temperature, extraction time) were determined by newly-developed by the scientific team RP-HPLC-PDA methodologies. The agar well diffusion method was applied to evaluate the antibacterial activity of the plant extracts. The 70% EtOH extracts at 20 °C displayed significantly higher antibacterial activity against the foodborne pathogenic bacteria S. aureus and P. aeruginosa as compared to the 70% and 98% EtOH extracts at 30 °C and 20 °C, respectively. The medicinal plant exhibited satisfactory antioxidant potential and radical-scavenging activity. Full article
(This article belongs to the Section Analysis of Natural Products and Pharmaceuticals)
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14 pages, 2096 KiB  
Article
Determination of Selenomethionine, Selenocystine, and Methylselenocysteine in Egg Sample by High Performance Liquid Chromatography—Inductively Coupled Plasma Mass Spectrometry
by Yue Zhao, Min Wang, Mengrui Yang, Jian Zhou and Tongtong Wang
Separations 2022, 9(2), 21; https://doi.org/10.3390/separations9020021 - 18 Jan 2022
Cited by 9 | Viewed by 2725
Abstract
The deficiency of selenium in dietary is recognized as a global problem. Eggs, as one of the most widely consumed food products, were readily enriched with selenium and became an important intake source of selenium for humans. In order to better understand the [...] Read more.
The deficiency of selenium in dietary is recognized as a global problem. Eggs, as one of the most widely consumed food products, were readily enriched with selenium and became an important intake source of selenium for humans. In order to better understand the speciation and bioaccessibility of selenium in eggs, a simple and reliable approach that could be easily used in a routine laboratory was attempted to develop for analyzing selenium species. Three of organic selenium species (selenocystine, methylselenocysteine, and selenomethionine) in liquid whole egg were completely released by enzymatic hydrolysis and detected by high performance liquid chromatography in combination with inductively coupled plasma mass spectrometry (HPLC-ICP-MS). All the parameters in enzymatic hydrolysis and separation procedures were optimized. The effect of matrix in analysis was critically evaluated by standard addition calibrations and external calibrations. Under the optimal conditions, the spike recoveries of selenium species at 0.1–0.4 μg g−1 spike levels all exceeded 80%. This method was successfully applied to the determination of selenium species in fresh egg and cooked eggs. Full article
(This article belongs to the Special Issue Advances of Accurate Quantification Methods in Food Analysis)
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44 pages, 14112 KiB  
Review
Review of New Approaches for Fouling Mitigation in Membrane Separation Processes in Water Treatment Applications
by Mervette El Batouti, Nouf F. Alharby and Mahmoud M. Elewa
Separations 2022, 9(1), 1; https://doi.org/10.3390/separations9010001 - 21 Dec 2021
Cited by 43 | Viewed by 7835
Abstract
This review investigates antifouling agents used in the process of membrane separation (MS), in reverse osmosis (RO), ultrafiltration (UF), nanofiltration (NF), microfiltration (MF), membrane distillation (MD), and membrane bioreactors (MBR), and clarifies the fouling mechanism. Membrane fouling is an incomplete substance formed on [...] Read more.
This review investigates antifouling agents used in the process of membrane separation (MS), in reverse osmosis (RO), ultrafiltration (UF), nanofiltration (NF), microfiltration (MF), membrane distillation (MD), and membrane bioreactors (MBR), and clarifies the fouling mechanism. Membrane fouling is an incomplete substance formed on the membrane surface, which will quickly reduce the permeation flux and damage the membrane. Foulant is colloidal matter: organic matter (humic acid, protein, carbohydrate, nano/microplastics), inorganic matter (clay such as potassium montmorillonite, silica salt, metal oxide, etc.), and biological matter (viruses, bacteria and microorganisms adhering to the surface of the membrane in the case of nutrients) The stability and performance of the tested nanometric membranes, as well as the mitigation of pollution assisted by electricity and the cleaning and repair of membranes, are reported. Physical, chemical, physico-chemical, and biological methods for cleaning membranes. Biologically induced biofilm dispersion effectively controls fouling. Dynamic changes in membrane foulants during long-term operation are critical to the development and implementation of fouling control methods. Membrane fouling control strategies show that improving membrane performance is not only the end goal, but new ideas and new technologies for membrane cleaning and repair need to be explored and developed in order to develop future applications. Full article
(This article belongs to the Special Issue Advances in Novel Polymeric Membranes and Membrane Process)
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9 pages, 4796 KiB  
Article
Green Stability Indicating Organic Solvent-Free HPLC Determination of Remdesivir in Substances and Pharmaceutical Dosage Forms
by Adel Ehab Ibrahim, Sami El Deeb, Emad Mahmoud Abdelhalim, Ahmed Al-Harrasi and Rania Adel Sayed
Separations 2021, 8(12), 243; https://doi.org/10.3390/separations8120243 - 12 Dec 2021
Cited by 22 | Viewed by 4401
Abstract
A green liquid chromatographic method is considered in this work to minimize the environmental impact of waste solvents. One important principle is to replace or eliminate the use of hazardous organic solvents. Organic impurities in any active pharmaceutical ingredient could arise either during [...] Read more.
A green liquid chromatographic method is considered in this work to minimize the environmental impact of waste solvents. One important principle is to replace or eliminate the use of hazardous organic solvents. Organic impurities in any active pharmaceutical ingredient could arise either during the process of its synthesis, or as degradation products developed throughout the shelf-life. Remdesivir (RDS) is an antiviral drug, approved by the US Food and Drug Adminstration (-FDA), to treat SARS-Cov-2 virus during its pandemic crisis. We studied the stability of remdesivir against several degradation pathways using the organic solvent-free liquid chromatographic technique. Separation was performed on RP-C18 stationary phase using mixed-micellar mobile phase composed of a mixture of 0.025 M Brij-35, 0.1 M sodium lauryl sulfate (SLS), and 0.02 M disodium hydrogen phosphate, adjusted to pH 6.0. The mobile phase flow rate was 1 mL min−1, and detection was carried out at a wavelength of 244 nm. We profiled the impurities that originated in mild to drastic degradation conditions. The method was then validated according to International Conference of Harmonization (ICH) guidelines within a linearity range of 5–100 μg mL−1 and applied successfully for the determination of the drug in its marketed dosage form. A brief comparison was established with reported chromatographic methods, including a greenness assessment on two new metrics (GAPI and AGREE). This study is the first to be reported as eco-friendly, solvent-free, and stability indicating LC methodology for RDS determination and impurity profiling. Full article
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18 pages, 1144 KiB  
Article
Development of a New LC-MS/MS Screening Method for Detection of 120 NPS and 43 Drugs in Blood
by Fabio Vaiano, Elisabetta Bertol, Maria Mineo, Laura Pietrosemoli, Jolanda Rubicondo, Claudiu T. Supuran and Fabrizio Carta
Separations 2021, 8(11), 221; https://doi.org/10.3390/separations8110221 - 17 Nov 2021
Cited by 10 | Viewed by 5877
Abstract
In the last few years, liquid chromatography coupled with mass spectrometry (LC/MS) has been increasingly used for screening purposes in forensic toxicology. These techniques have the advantages of low time/resource-consuming and high versatility and have been applied in numerous new multi-analytes methods. The [...] Read more.
In the last few years, liquid chromatography coupled with mass spectrometry (LC/MS) has been increasingly used for screening purposes in forensic toxicology. These techniques have the advantages of low time/resource-consuming and high versatility and have been applied in numerous new multi-analytes methods. The new psychoactive substance (NPS) phenomenon provided a great impulse to this wide-range approach, but it is also important to keep the attention on “classical” psychoactive substances, such as benzodiazepines (BDZ). In this paper, a fully validated screening method in blood for the simultaneous detection of 163 substances (120 NPS and 43 other drugs) by a dynamic multiple reaction monitoring analysis through LC-MS/MS is described. The method consists of a deproteinization of 200 µL of blood with acetonitrile. The LC separation is achieved with a 100 mm long C18 column in 35 min. The method was very sensitive, with limits of quantification from 0.02 to 1.5 ng/mL. Matrix effects did not negatively affect the analytical sensitivity. This method proved to be reliable and was successfully applied to our routinary analytical activity in several forensic caseworks, allowing the identification and quantification of many BDZs and 3,4-methylenedioxypyrovalerone (MDPV). Full article
(This article belongs to the Section Forensics/Toxins)
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17 pages, 544 KiB  
Review
A Review on the Nanofiltration Process for Treating Wastewaters from the Petroleum Industry
by Shahryar Jafarinejad and Milad Rabbani Esfahani
Separations 2021, 8(11), 206; https://doi.org/10.3390/separations8110206 - 04 Nov 2021
Cited by 25 | Viewed by 3670
Abstract
Activities and/or processes in different segments of the petroleum industry, including upstream and downstream, generate aqueous waste streams containing oil and various contaminants that require treatment/purification before release/reuse. Nanofiltration (NF) technology has been approved as an efficient technology for treating wastewater streams from [...] Read more.
Activities and/or processes in different segments of the petroleum industry, including upstream and downstream, generate aqueous waste streams containing oil and various contaminants that require treatment/purification before release/reuse. Nanofiltration (NF) technology has been approved as an efficient technology for treating wastewater streams from the petroleum industry. The primary critical issues in an NF treatment process can be listed as mitigation of membrane fouling; selection of appropriate pre-treatment process; and selection of a suitable, cost-effective, non-hazardous cleaning strategy. In this study, NF separation mechanisms, membrane fabrication/modification, effective factors on NF performance, and fouling are briefly reviewed. Then, a summary of recent NF treatment studies on various petroleum wastewaters and performance evaluation is presented. Finally, based on the gaps identified in the field, the conclusions and future perspectives are discussed. Full article
(This article belongs to the Section Environmental Separations)
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16 pages, 38028 KiB  
Review
Recent Advances on the Development of Chemosensors for the Detection of Mercury Toxicity: A Review
by Shiva Prasad Kollur, Chandan Shivamallu, Shashanka K. Prasad, Ravindra Veerapur, Sharanagouda S. Patil, Charley A. Cull, Johann F. Coetzee and Raghavendra G. Amachawadi
Separations 2021, 8(10), 192; https://doi.org/10.3390/separations8100192 - 18 Oct 2021
Cited by 13 | Viewed by 3507
Abstract
The harmful impact of mercury on biological systems is of great concern. Regardless of the efforts made by the regulating agencies, a decrease in Hg2+ concentration has not been realized, and hence mercury accumulation in the environment remains of utmost concern. Designing [...] Read more.
The harmful impact of mercury on biological systems is of great concern. Regardless of the efforts made by the regulating agencies, a decrease in Hg2+ concentration has not been realized, and hence mercury accumulation in the environment remains of utmost concern. Designing novel and efficient probes for recognition and detection of toxic metals in environmental samples has been of primary importance. Among the available techniques, probe designs involving the study of spectral properties has been preferred because of its obvious ease of instrumentation. Furthermore, occurrence of significant changes in the visible portion of electronic spectra enables detection by the naked eye, thereby endorsing the preference for development of probes with off-on binary responses to aid in the in-field sample analysis. The prominence is further streamlined to the use of fluorescence to help characterize on-response the cellular detection of Hg2+ with ease. In order to overcome the problem of developing efficient probes or sensors bearing fluorescence on-response mechanism that can work effectively in physiological conditions, various methodologies, such as chemo-dosimetric reaction mechanisms for the designing of new luminescent ligands, are being adopted. Additionally, modified charge transfer processes are also being considered for optical detection of the mercury (II) ion. In this review, all such possible techniques have been discussed in detail. Full article
(This article belongs to the Section Materials in Separation Science)
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10 pages, 217 KiB  
Article
Study on the Stability of Antibiotics, Pesticides and Drugs in Water by Using a Straightforward Procedure Applying HPLC-Mass Spectrometric Determination for Analytical Purposes
by Salvatore Barreca, Carola Forni, Luisa Colzani, Laura Clerici, Daniela Daverio and Pierluisa Dellavedova
Separations 2021, 8(10), 179; https://doi.org/10.3390/separations8100179 - 09 Oct 2021
Cited by 10 | Viewed by 2052
Abstract
The stability of analytes is a critical point in chemical analysis, especially in the field of trace levels residue analysis. Nowadays, due to advances in analytical technology and in separation sciences, the analyses of water have been improved. Unfortunately, in this context, one [...] Read more.
The stability of analytes is a critical point in chemical analysis, especially in the field of trace levels residue analysis. Nowadays, due to advances in analytical technology and in separation sciences, the analyses of water have been improved. Unfortunately, in this context, one of the most critical issues in water analysis include compound stability from sampling station to laboratory procedures. This study was carried out to explore the stability of several compounds in water from sampling to analysis concerning analytes reported in implementing decision 2018/840—Watch List. During method development and validation, the stability of compounds was investigated to detect the best operating conditions concerning sampling, extraction and analysis. In this paper, we report a study on the stability of antibiotics, pesticides and drugs in water determined using a straight-forward procedure applying mass spectrometric detection for analytical purposes. The laboratory tests were performed in Milli-Q water and surface water by analyzing samples through direct injection, solvent mixture (Water/ACN) and solid phase extraction system from time 0 to 168 h. All the analytes of the WL are stable in aqueous solutions with the addition of at least 25% ACN even after 168 h, and the analytes have shown a matrix effect on recovery of some analytes such as Famoxadone from sampling results (recovery in surface water 72%). For all the analytes investigated, recoveries were between 70 and 130% by using SPE procedures before UHPLC-MS/MS analysis, which is in good agreement with method validation procedures. Full article
(This article belongs to the Special Issue HPLC: A Key Tool for Analytical Chemistry)
15 pages, 978 KiB  
Article
Chemical and Antioxidant Characterization of the Portuguese Heather Honey from Calluna vulgaris
by Luís Rodrigues da Silva, Renan Campos Chisté and Eduarda Fernandes
Separations 2021, 8(10), 177; https://doi.org/10.3390/separations8100177 - 08 Oct 2021
Cited by 9 | Viewed by 2066
Abstract
The Calluna vulgaris honey produced in Portugal, concerning its phenolic compounds and abscisic acids profiles, as well as its antioxidant activity and the protective effect against oxidative damage in human erythrocytes were herein performed for the first time. The phenolic and abscisic acid [...] Read more.
The Calluna vulgaris honey produced in Portugal, concerning its phenolic compounds and abscisic acids profiles, as well as its antioxidant activity and the protective effect against oxidative damage in human erythrocytes were herein performed for the first time. The phenolic and abscisic acid profiles were tentatively identified by LC-MS/MS (17 compounds). The total content of phenolics and abscisic acids was 15,446.4 µg/g of honey extract, with catechin derivatives and abscisic acids being major constituents. The highest scavenging capacity was found against reactive nitrogen species. Additionally, the honey extract prevented ROO-induced oxidative damage in erythrocytes collected from human blood, by inhibiting hemolysis, lipid peroxidation and hemoglobin oxidation. In conclusion, C. vulgaris honey contains high content of catechin derivatives and abscisic acids that may be responsible for its biological activity, characterized by a strong antioxidant capacity, which adds up to the nutritional value of this delicacy. Full article
(This article belongs to the Section Analysis of Food and Beverages)
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24 pages, 1428 KiB  
Review
Deep Eutectic Solvents (DESs) as Green Extraction Media of Beneficial Bioactive Phytochemicals
by Ali Sami Dheyab, Mohd Fadzelly Abu Bakar, Mohamed AlOmar, Siti Fatimah Sabran, Ahmad Fathi Muhamad Hanafi and Azman Mohamad
Separations 2021, 8(10), 176; https://doi.org/10.3390/separations8100176 - 07 Oct 2021
Cited by 35 | Viewed by 5349
Abstract
Deep eutectic solvents (DES) are a mixture of two or more components and are classified as ionic solvents with special properties such as low volatility, high solubility, low melting points, low-cost materials and are less toxic to humans. Using DES has been suggested [...] Read more.
Deep eutectic solvents (DES) are a mixture of two or more components and are classified as ionic solvents with special properties such as low volatility, high solubility, low melting points, low-cost materials and are less toxic to humans. Using DES has been suggested as an eco-friendly, green method for extraction of bioactive compounds from medicinal plants and are a safe alternative for nutritional, pharmaceutical and various sector applications. Conventional solvent extraction methods present drawbacks such as long extraction period, safety issues, harmful to the environment, costly and large volume of solvents required. The extraction method with DES leads to higher extraction yield and better bioactivity results as compared to the conventional solvents. This review provides a summary of research progress regarding the advantages of using DES to extract bioactive compounds such as phenolic acid, flavonoids, isoflavones, catechins, polysaccharides, curcuminoids, proanthocyanidin, phycocyanin, gingerols, ginsenosides, anthocyanin, xanthone, volatile monoterpenes, tannins, lignin, pectin, rutin, tert-butyl hydroquinone, chlorogenic acids, resveratrol and others, as opposed to using conventional solvents. The bioactivity of the extracts is determined using antioxidant, antibacterial and antitumor activities. Hence, DESs are considered potential green media with selective and efficient properties for extracting bioactive ingredients from medicinal plants. Full article
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14 pages, 1880 KiB  
Article
Designing Safer Solvents to Replace Methylene Chloride for Liquid Chromatography Applications Using Thin-Layer Chromatography as a Screening Tool
by Apekshya Sharma, Evan Yu, Gregory Morose, David Trung Nguyen and Wan-Ting Chen
Separations 2021, 8(10), 172; https://doi.org/10.3390/separations8100172 - 06 Oct 2021
Cited by 8 | Viewed by 6191
Abstract
Methylene chloride, commonly known as dichloromethane (DCM), is a widely used chemical for chromatography separation within the polymer, chemical, and pharmaceutical industries. With the ability to effectively solvate heterocyclic compounds, and properties including a low boiling point, high density, and low cost, DCM [...] Read more.
Methylene chloride, commonly known as dichloromethane (DCM), is a widely used chemical for chromatography separation within the polymer, chemical, and pharmaceutical industries. With the ability to effectively solvate heterocyclic compounds, and properties including a low boiling point, high density, and low cost, DCM has become the solvent of choice for many different applications. However, DCM has high neurotoxicity and is carcinogenic, with exposure linked to damage to the brain and the central nervous system, even at low exposure levels. This research focuses on sustainability and works towards finding safer alternative solvents to replace DCM in pharmaceutical manufacturing. The research was conducted with three active pharmaceutical ingredients (API) widely used in the pharmaceutical industry: acetaminophen, aspirin, and ibuprofen. Thin-layer chromatography (TLC) was used to investigate if an alternative solvent or solvent blend could show comparable separation performance to DCM. The use of the Hansen Solubility Parameter (HSP) theory and solubility testing allowed for the identification of potential alternative solvents or solvent blends to replace DCM. HSP values for the three APIs were experimentally determined and used to identify safer solvents and blends that could potentially replace DCM. Safer solvents or binary solvent blends were down-selected based on their dissolution power, safety, and price. The down-selected solvents (e.g., ethyl acetate) and solvent blends were further evaluated using three chemical hazard classification approaches to find the best fitting nonhazardous replacement to DCM. Several safer solvent blends (e.g., mixtures composed of methyl acetate and ethyl acetate) with adequate TLC performance were identified. Results from this study are expected to provide guidance for identifying and evaluating safer solvents to separate APIs using chromatography. Full article
(This article belongs to the Special Issue Separations in Biomedical Analysis)
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