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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Article
Green Stability Indicating Organic Solvent-Free HPLC Determination of Remdesivir in Substances and Pharmaceutical Dosage Forms
Separations 2021, 8(12), 243; https://doi.org/10.3390/separations8120243 - 12 Dec 2021
Cited by 5 | Viewed by 2483
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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Article
Development of a New LC-MS/MS Screening Method for Detection of 120 NPS and 43 Drugs in Blood
Separations 2021, 8(11), 221; https://doi.org/10.3390/separations8110221 - 17 Nov 2021
Cited by 2 | Viewed by 2626
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 Special Issue Application of Chromatography in Forensic Toxicology and Pharmacology)
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Article
Designing Safer Solvents to Replace Methylene Chloride for Liquid Chromatography Applications Using Thin-Layer Chromatography as a Screening Tool
Separations 2021, 8(10), 172; https://doi.org/10.3390/separations8100172 - 06 Oct 2021
Cited by 2 | Viewed by 1850
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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Article
Non-Targeted Chemical Characterization of JUUL Virginia Tobacco Flavored Aerosols Using Liquid and Gas Chromatography
Separations 2021, 8(9), 130; https://doi.org/10.3390/separations8090130 - 24 Aug 2021
Cited by 7 | Viewed by 2640
Abstract
The chemical constituents of JUUL Virginia Tobacco pods with 3.0% and 5.0% nicotine by weight (VT3 and VT5) were characterized by non-targeted analyses, an approach to detect chemicals that are not otherwise measured with dedicated methods or that are not known beforehand. Aerosols [...] Read more.
The chemical constituents of JUUL Virginia Tobacco pods with 3.0% and 5.0% nicotine by weight (VT3 and VT5) were characterized by non-targeted analyses, an approach to detect chemicals that are not otherwise measured with dedicated methods or that are not known beforehand. Aerosols were generated using intense and non-intense puffing regimens and analyzed by gas chromatography electron ionization mass spectrometry and liquid chromatography electrospray ionization high resolving power mass spectrometry. All compounds above 0.7 µg/g for GC–MS analysis or above 0.5 µg/g for LC–HRMS analysis and differing from blank measurements were identified and semi-quantified. All identifications were evaluated and categorized into five groups: flavorants, harmful and potentially harmful constituents, extractables and/or leachables, reaction products, and compounds that could not be identified/rationalized. For VT3, 79 compounds were identified using an intense puffing regimen and 69 using a non-intense puffing regimen. There were 60 compounds common between both regimens. For VT5, 85 compounds were identified with an intense puffing regimen and 73 with a non-intense puffing regimen; 67 compounds were in common. For all nicotine concentrations, formulations and puffing regimens, reaction products accounted for the greatest number of compounds (ranging from 70% to 75%; 0.08% to 0.1% by mass), and flavorants comprised the second largest number of compounds (ranging from for 15% to 16%; 0.1 to 0.2% by mass). A global comparison of the compounds detected in JUUL aerosol to those catalogued in cigarette smoke indicated an approximate 50-fold decrease in chemical complexity. Both VT3 and VT5 aerosols contained 59 unique compounds not identified in cigarette smoke. Full article
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Article
Quantification of Histidine-Containing Dipeptides in Dolphin Serum Using a Reversed-Phase Ion-Pair High-Performance Liquid Chromatography Method
Separations 2021, 8(8), 128; https://doi.org/10.3390/separations8080128 - 23 Aug 2021
Cited by 2 | Viewed by 1614
Abstract
The quantification of histidine-containing dipeptides (anserine, carnosine, and balenine) in serum might be a diagnostic tool to assess the health condition of animals. In this study, an existing reversed-phase ion-pair high-performance liquid chromatography (HPLC)–ultraviolet detection method was improved and validated to quantify serum [...] Read more.
The quantification of histidine-containing dipeptides (anserine, carnosine, and balenine) in serum might be a diagnostic tool to assess the health condition of animals. In this study, an existing reversed-phase ion-pair high-performance liquid chromatography (HPLC)–ultraviolet detection method was improved and validated to quantify serum anserine, carnosine, and balenine levels in the dolphin. The serum was deproteinized with trichloroacetic acid and directly injected into the HPLC system. Chromatographic separation of the three histidine-containing dipeptides was achieved on a TSK–gel ODS-80Ts (4.6 mm × 150 mm, 5 µm) analytical column using a mobile phase of 50 mmol/L potassium dihydrogen phosphate (pH 3.4) containing 6 mmol/L 1-heptanesulfonic acid and acetonitrile (96:4). The standard curve ranged from 0.1 µmol/L to 250 µmol/L. The average accuracy of the intra- and inter-analysis of anserine, carnosine, and balenine was 97–106%. The relative standard deviations of total precision (RSDr) of anserine, carnosine, and balenine in dolphin serum were 5.9%, 4.1%, and 2.6%, respectively. The lower limit of quantification of these compounds was 0.11–0.21 µmol/L. These results indicate that the improved method is reliable and concise for the simultaneous determination of anserine, carnosine, and balenine in dolphin serum, and may be useful for evaluation of health conditions in dolphins. Furthermore, this method can also be applied to other biological samples. Full article
(This article belongs to the Special Issue Separations in Biomedical Analysis)
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Article
Detailed Group-Type Characterization of Plastic-Waste Pyrolysis Oils: By Comprehensive Two-Dimensional Gas Chromatography Including Linear, Branched, and Di-Olefins
Separations 2021, 8(7), 103; https://doi.org/10.3390/separations8070103 - 16 Jul 2021
Cited by 11 | Viewed by 2257
Abstract
Plastic-waste pyrolysis oils contain large amounts of linear, branched, and di-olefinic compounds. This makes it not obvious to determine the detailed group-type composition in particular to the presence of substantial amounts of N-, S-, and O-containing heteroatomic compounds. The thorough evaluation of different [...] Read more.
Plastic-waste pyrolysis oils contain large amounts of linear, branched, and di-olefinic compounds. This makes it not obvious to determine the detailed group-type composition in particular to the presence of substantial amounts of N-, S-, and O-containing heteroatomic compounds. The thorough evaluation of different column combinations for two-dimensional gas chromatography (GC × GC), i.e., non-polar × polar and polar × non-polar, revealed that the second combination had the best performance, as indicated by the bi-dimensional resolution of the selected key compounds. By coupling the GC × GC to multiple detectors, such as the flame ionization detector (FID), a sulfur chemiluminescence detector (SCD), a nitrogen chemiluminescence detector (NCD), and a mass spectrometer (MS), the identification and quantification were possible of hydrocarbon, oxygen-, sulfur-, and nitrogen-containing compounds in both naphtha (C5–C11) and diesel fractions (C7–C23) originating from plastic-waste pyrolysis oils. Group-type quantification showed that large amounts of α-olefins (36.39 wt%, 35.08 wt%), iso-olefins (8.77 wt%, 9.06 wt%), and diolefins (4.21 wt%, 4.20 wt%) were present. Furthermore, oxygen-containing compounds (alcohols, ketones, and ethers) could be distinguished from abundant hydrocarbon matrix, by employing Stabilwax as the first column and Rxi-5ms as the second column. Ppm levels of sulfides, thiophenes, and pyridines could also be quantified by the use of selective SCD and NCD detectors. Full article
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Article
LC-ESI-QTOF-MS/MS Profiling and Antioxidant Activity of Phenolics from Custard Apple Fruit and By-Products
Separations 2021, 8(5), 62; https://doi.org/10.3390/separations8050062 - 09 May 2021
Cited by 7 | Viewed by 2221
Abstract
Custard apple is an edible fruit grown in tropical and subtropical regions. Due to its abundant nutrient content and perceived health benefits, it is a popular food for consumption and is utilized as a medicinal aid. Although some published research had provided the [...] Read more.
Custard apple is an edible fruit grown in tropical and subtropical regions. Due to its abundant nutrient content and perceived health benefits, it is a popular food for consumption and is utilized as a medicinal aid. Although some published research had provided the phenolic compound of custard apple, the comprehensive phenolic profiling of Australian grown custard apple is limited. Hence, this research aimed to evaluate the phenolic content and antioxidant potential by various phenolic content and antioxidant assays, followed by characterization and quantification of the phenolic profile using LC-ESI-QTOF-MS/MS and HPLC-PDA. African Pride peel had the highest value in TPC (61.69 ± 1.48 mg GAE/g), TFC (0.42 ± 0.01 mg QE/g) and TTC (43.25 ± 6.70 mg CE/g), followed by Pink’s Mammoth peel (19.37 ± 1.48 mg GAE/g for TPC, 0.27 ± 0.03 mg QE/g for TFC and 10.25 ± 1.13 mg CE/g for TTC). African Pride peel also exhibited the highest antioxidant potential for TAC (43.41 ± 1.66 mg AAE/g), FRAP (3.60 ± 0.14 mg AAE/g) and ABTS (127.67 ± 4.60 mg AAE/g), whereas Pink’s Mammoth peel had the highest DPPH (16.09 ± 0.34 mg AAE/g), RPA (5.32 ± 0.14 mg AAE/g), OH-RSA (1.23 ± 0.25 mg AAE/g) and FICA (3.17 ± 0.18 mg EDTA/g). LC-ESI-QTOF-MS/MS experiment successfully characterized 85 phenolic compounds in total, encompassing phenolic acids (20), flavonoids (42), stilbenes (4), lignans (6) and other polyphenols (13) in all three parts (pulp, peel and seeds) of custard apple. The phenolic compounds in different portions of custard apples were quantified by HPLC-PDA, and it was shown that African Pride peel had higher concentrations of the most abundant phenolics. This is the first study to provide the comprehensive phenolic profile of Australian grown custard apples, and the results highlight that each part of custard apple can be a rich source of phenolics for the utilization of custard apple fruit and waste in the food, animal feeding and nutraceutical industries. Full article
(This article belongs to the Special Issue Advances in Food and Biological Samples Analysis)
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Article
Andean Blueberry of the Genus Disterigma: A High-Resolution Mass Spectrometric Approach for the Comprehensive Characterization of Phenolic Compounds
Separations 2021, 8(5), 58; https://doi.org/10.3390/separations8050058 - 02 May 2021
Cited by 10 | Viewed by 1758
Abstract
Wild neotropical blueberries, endemic of Central and South American areas, are promising yet still undisclosed sources of bioactive compounds. Most research studies have addressed wild and cultivated blueberries from Europe and North America, despite the extremely wide variety of wild neotropical species. In [...] Read more.
Wild neotropical blueberries, endemic of Central and South American areas, are promising yet still undisclosed sources of bioactive compounds. Most research studies have addressed wild and cultivated blueberries from Europe and North America, despite the extremely wide variety of wild neotropical species. In the present paper, for the first time, the phenolic composition of Disterigma alaternoides was investigated through ultra-high-performance liquid chromatography coupled to high-resolution mass-spectrometric analysis followed by accurate data analysis and compound validation with a dedicated structure-based workflow. D. alaternoides, which belongs to a closely related genus to that of the common blueberry, grows exclusively in the Andean regions over 2000 above sea level. Thanks to the dedicated analytical platform, 249 phenolic compounds were tentatively identified, including several anthocyanins, flavonoids, phenolic acids, and proanthocyanidins. Thenature and heterogeneity of identified phenolic compounds demonstrate once more the need for a more profound knowledge of such still uncharted matrices. Full article
(This article belongs to the Special Issue Chromatographic Analysis of Biological Samples)
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Article
Enhanced Adsorption Capacities of Fungicides Using Peanut Shell Biochar via Successive Chemical Modification with KMnO4 and KOH
Separations 2021, 8(4), 52; https://doi.org/10.3390/separations8040052 - 15 Apr 2021
Cited by 8 | Viewed by 1630
Abstract
This study explored the effects of peanut shell biochar (PSB) on the adsorption capacities of fungicides with and without successive chemical modifications, using KMnO4 and KOH (PSBOX-A), in order to provide a valuable understanding of their adsorption mechanisms and behaviors. [...] Read more.
This study explored the effects of peanut shell biochar (PSB) on the adsorption capacities of fungicides with and without successive chemical modifications, using KMnO4 and KOH (PSBOX-A), in order to provide a valuable understanding of their adsorption mechanisms and behaviors. To this end, the physicochemical properties of PSB and PSBOX-A were examined by using the Brunauer–Emmett–Teller method, Fourier transform infrared spectroscopy, and scanning electron microscopy with an energy dispersive X-ray spectrometer. The effects of temperature, ionic strength, and humic acids on the adsorption of fungicides, using PSB and PSBOX-A, were estimated through batch experiments. Furthermore, adsorption kinetics, isotherms, and thermodynamics were studied. The maximum adsorption capacities of fungicides by PSBOX-A were estimated to be more notable (Qmax of carbendazim = 531.2 μmol g−1, Qmax of pyrimethanil = 467.7 μmol g−1, and Qmax of tebuconazole = 495.1 μmol g−1) than PSB (Qmax of carbendazim = 92.6 μmol g−1, Qmax of pyrimethanil = 61.7 μmol g−1, and Qmax of tebuconazole = 66.7 μmol g−1). These findings suggest that successive chemical modification using KMnO4 and KOH could potentially be used to effectively fabricate PSB to remove fungicides in water-treatment processes. Full article
(This article belongs to the Special Issue Sustainable Water and Wastewater Purification Technologies)
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Article
Adsorption Characteristics of Phosphate Ions by Pristine, CaCl2 and FeCl3-Activated Biochars Originated from Tangerine Peels
Separations 2021, 8(3), 32; https://doi.org/10.3390/separations8030032 - 13 Mar 2021
Cited by 7 | Viewed by 1611
Abstract
This study has evaluated the removal efficiencies of phosphate ions (PO43−) using pristine (TB) and chemical-activated tangerine peel biochars. The adsorption kinetics and isotherm presented that the enhanced physicochemical properties of TB surface through the chemical activation with CaCl2 [...] Read more.
This study has evaluated the removal efficiencies of phosphate ions (PO43−) using pristine (TB) and chemical-activated tangerine peel biochars. The adsorption kinetics and isotherm presented that the enhanced physicochemical properties of TB surface through the chemical activation with CaCl2 (CTB) and FeCl3 (FTB) were helpful in the adsorption capacities of PO43− (equilibrium adsorption capacity: FTB (1.655 mg g−1) > CTB (0.354 mg g−1) > TB (0.104 mg g−1)). The adsorption kinetics results revealed that PO43− removal by TB, CTB, and FTB was well fitted with the pseudo-second-order model (R2 = 0.999) than the pseudo-first-order model (R2 ≥ 0.929). The adsorption isotherm models showed that the Freundlich equation was suitable for PO43− removal by TB (R2 = 0.975) and CTB (R2 = 0.955). In contrast, the Langmuir equation was proper for PO43− removal by FTB (R2 = 0.987). The PO43− removal efficiency of CTB and FTB decreased with the ionic strength increased due to the compression of the electrical double layer on the CTB and FTB surfaces. Besides, the PO43− adsorptions by TB, CTB, and FTB were spontaneous endothermic reactions. These findings demonstrated FTB was the most promising method for removing PO43− in waters. Full article
(This article belongs to the Special Issue Sustainable Water and Wastewater Purification Technologies)
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Article
Enhanced Photocatalytic Activity of CuWO4 Doped TiO2 Photocatalyst Towards Carbamazepine Removal under UV Irradiation
Separations 2021, 8(3), 25; https://doi.org/10.3390/separations8030025 - 26 Feb 2021
Cited by 17 | Viewed by 2575
Abstract
Abatement of contaminants of emerging concerns (CECs) in water sources has been widely studied employing TiO2 based heterogeneous photocatalysis. However, low quantum energy yield among other limitations of titania has led to its modification with other semiconductor materials for improved photocatalytic activity. [...] Read more.
Abatement of contaminants of emerging concerns (CECs) in water sources has been widely studied employing TiO2 based heterogeneous photocatalysis. However, low quantum energy yield among other limitations of titania has led to its modification with other semiconductor materials for improved photocatalytic activity. In this work, a 0.05 wt.% CuWO4 over TiO2 was prepared as a powder composite. Each component part synthesized via the sol-gel method for TiO2, and CuWO4 by co-precipitation assisted hydrothermal method from precursor salts, underwent gentle mechanical agitation. Homogenization of the nanopowder precursors was performed by zirconia ball milling for 2 h. The final material was obtained after annealing at 500 °C for 3.5 h. Structural and morphological characterization of the synthesized material has been achieved employing X-ray diffraction (XRD), Fourier transform infra-red (FTIR) spectroscopy, Brunauer–Emmett–Teller (BET) N2 adsorption–desorption analysis, Scanning electron microscopy-coupled Energy dispersive X-ray spectroscopy (SEM-EDS), Transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), and UV-Vis diffuse reflectance spectroscopy (UV-vis DRS) for optical characterization. The 0.05 wt.% CuWO4-TiO2 catalyst was investigated for its photocatalytic activity over carbamazepine (CBZ), achieving a degradation of almost 100% after 2 h irradiation. A comparison with pure TiO2 prepared under those same conditions was made. The effect of pH, chemical scavengers, H2O2 as well as contaminant ion effects (anions, cations), and humic acid (HA) was investigated, and their related influences on the photocatalyst efficiency towards CBZ degradation highlighted accordingly. Full article
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Article
Influence of Citrus Flavor Addition in Brewing Process: Characterization of the Volatile and Non-Volatile Profile to Prevent Frauds and Adulterations
Separations 2021, 8(2), 18; https://doi.org/10.3390/separations8020018 - 12 Feb 2021
Cited by 7 | Viewed by 2301
Abstract
In the last few years, the flavored beer market has increased significantly. In particular, consumers showed a growing interest in citrus-flavored beers. Citrus fruits contain, among other class of compounds, terpenes and terpenoids and oxygenated heterocyclic compounds. The absence of a specific legislation [...] Read more.
In the last few years, the flavored beer market has increased significantly. In particular, consumers showed a growing interest in citrus-flavored beers. Citrus fruits contain, among other class of compounds, terpenes and terpenoids and oxygenated heterocyclic compounds. The absence of a specific legislation concerning beer flavored production and ingredients reported on the labels makes these beers subject to possible adulterations. Solid phase micro extraction (SPME) followed by gas chromatographic–mass spectrometry (GC-MS) and gas chromatographic-flame ionization detector (GC-FID) analysis of the volatile profile together with the characterization of the oxygen heterocyclic compounds through high performance liquid chromatography coupled to tandem mass spectrometry (HPLC-MS/MS) demonstrated to be a powerful analytical strategy for quality control. In this study, we combined the volatile and non-volatile profiles of “citrus flavored mainstream beers”, in order to evaluate the authenticity and determine markers to prevent food frauds. The changes in the aroma composition of the unflavored types after the addition of peel, or citrus essential oil were also evaluated. The linear retention index (LRI) system was used for both techniques; in particular, its application in liquid chromatography is still limited and represents a novelty. The coupling of the high sensitivity of the HPLC MS/MS method with the LRI system, it has made possible for the first time a reliable identification and an accurate quantification of furocoumarins in citrus-flavored beers. Full article
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Article
Hydrophilic Interaction Liquid Chromatography to Characterize Nutraceuticals and Food Supplements Based on Flavanols and Related Compounds
Separations 2021, 8(2), 17; https://doi.org/10.3390/separations8020017 - 09 Feb 2021
Cited by 5 | Viewed by 2116
Abstract
Purified extracts from different types of berries and medicinal plants are increasingly used as raw materials for the production of nutraceuticals and dietary supplements, mainly due to their high content in bioactive substances. This is, for instance, the case of phenolic compounds such [...] Read more.
Purified extracts from different types of berries and medicinal plants are increasingly used as raw materials for the production of nutraceuticals and dietary supplements, mainly due to their high content in bioactive substances. This is, for instance, the case of phenolic compounds such as flavonoids, which exhibit a wide range of beneficial properties, including antioxidant, anti-inflammatory, antineoplastic and antimicrobial activities. This paper tackles the characterization of several kinds of nutraceuticals based on hydrophilic interaction liquid chromatography (HILIC) with fluorescence detection (FLD). The study focused on the determination of flavanols and related compounds such as condensed tannins. Analytes were recovered by solvent extraction using methanol:water:hydrochloric acid (70:29:1 v:v:v) as the extraction solvent under sonication for 30 min at 55 °C. Experimental design with response surface methodology was used to optimize the HILIC separation to achieve good resolution of the main components, using acetonitrile:acetic acid (99:1 v/v) (solvent A) and methanol:water:acetic acid, (95:3:2 v/v/v) (solvent B) as the components of the mobile phase. For the assessment of the elution gradient, factors under study were solvent B percentage and gradient time. The best conditions were achieved with 10% solvent B as the initial percentage and 30 min of linear gradient to reach 25% solvent B. Principal component analysis and partial least square-discriminant analysis were used to characterize and compare the compositional features of dietary supplements based on both targeted and non-targeted approaches. Results revealed that the sample distribution relied on the oligomeric nature of descriptors. Full article
(This article belongs to the Special Issue Advances in Food and Biological Samples Analysis)
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LC-MS Phytochemical Screening, In Vitro Antioxidant, Antimicrobial and Anticancer Activity of Microalgae Nannochloropsis oculata Extract
Separations 2020, 7(4), 54; https://doi.org/10.3390/separations7040054 - 08 Oct 2020
Cited by 15 | Viewed by 3088
Abstract
Nowadays, marine microalgae are recognized to be a considerably novel and rich origin of bioactive moieties utilized in the sectors of nutraceuticals and pharmaceuticals. In the present study, Nannochloropsis oculata extract (AME) was associated with a wide variety of pharmacological studies such as [...] Read more.
Nowadays, marine microalgae are recognized to be a considerably novel and rich origin of bioactive moieties utilized in the sectors of nutraceuticals and pharmaceuticals. In the present study, Nannochloropsis oculata extract (AME) was associated with a wide variety of pharmacological studies such as in vitro antioxidant, antibacterial, and antifungal and anticancer activity (MDA-MB-231) in cancer cells through in vitro models. In the study, the chemical composition and structure of the bioactive compounds found in the AME extract were studied using the LC-MS technique. The results of the anticancer activity showed a decrease in the percentage of cell viability of the MDA-MB-231 cells in a concentration- and time-dependent manner (400 μg/mL at 24 h, 300 μg/mL at 48 h, and 200 μg/mL at 72 h). We have also observed morphological changes in the cells that could be associated with treatment with AME extract. Our observation of the AME extract-treated MDA-MB231 cells under light microscopy showed that when the concentration increased, the number of cells began to decrease. As far as LC-MS analysis is concerned, it showed the presence of the bioactive molecules was terpenoids along with carotenoids, polyphenolic and fatty acids. The result revealed that the AME extract exhibited noteworthy in vitro free radical scavenging potential, with an IC50 value of 52.10 ± 0.85 µg/L in DPPH assay, 122.84 ± 2.32 µg/mL in H2O2 assay and, 96.95 ± 1.68 µg/mL in ABTS assay. The activity was found to be highly significant against bacteria (Gram-positive and negative) and moderately significant against fungal strain with minimum inhibitory concentration (MIC) and minimum bactericidal concentration (MBC)/minimum fungicidal concentration (MFC) values between 15.63 and 500 µg/mL. Full article
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Article
Pigments Content (Chlorophylls, Fucoxanthin and Phycobiliproteins) of Different Commercial Dried Algae
Separations 2020, 7(2), 33; https://doi.org/10.3390/separations7020033 - 11 Jun 2020
Cited by 48 | Viewed by 6279
Abstract
Algae are a complex, polyphyletic group of organisms, affordable and naturally rich in nutrients, but also valuable sources of structurally diverse bioactive substances such as natural pigments. The aim of this work was to evaluate the polar and non-polar pigment contents of different [...] Read more.
Algae are a complex, polyphyletic group of organisms, affordable and naturally rich in nutrients, but also valuable sources of structurally diverse bioactive substances such as natural pigments. The aim of this work was to evaluate the polar and non-polar pigment contents of different commercial dried algae (brown: Himanthalia elongata, Undaria pinnatifida, Laminaria ochroleuca; red: Porphyra spp.; and a blue-green microalga: Spirulina spp.). The pigment extraction was carried out using different solvents (100% methanol, 100% methanol acid free, 100% ethanol, 90% acetone, N,N-dimethylformamide, dimethyl sulfoxide-water (4:1, v/v) and pH 6.8 phosphate buffer), selected according to their affinity for each class of pigments. Acetone proved to be an efficient solvent to extract chlorophylls from brown and red algae, but not from Spirulina spp. Porphyra spp. presented considerably higher levels of all pigments compared to brown algae, although Spirulina spp. presented significantly higher (p < 0.05) levels of chlorophylls, carotenoids and phycobiliproteins, compared to all macroalgae. The content of fucoxanthin extracted from the three brown algae was highly correlated to the carotenoid content. Within this group, Himanthalia elongata presented the highest fucoxanthin/total carotenoids ratio. Although the yield of extraction depended on the solvent used, the algae studied herein are an interesting source of pigments of great value for a wide range of applications. Full article
(This article belongs to the Special Issue Extraction and Isolation of Natural Products)
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Review

Review
Recent Advances on the Development of Chemosensors for the Detection of Mercury Toxicity: A Review
Separations 2021, 8(10), 192; https://doi.org/10.3390/separations8100192 - 18 Oct 2021
Cited by 4 | Viewed by 1497
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
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Review
Magnetic Ionic Liquids in Sample Preparation: Recent Advances and Future Trends
Separations 2021, 8(9), 153; https://doi.org/10.3390/separations8090153 - 13 Sep 2021
Cited by 4 | Viewed by 1551
Abstract
In the last decades, a myriad of materials has been synthesized and utilized for the development of sample preparation procedures. The use of their magnetic analogues has gained significant attention and many procedures have been developed using magnetic materials. In this context, the [...] Read more.
In the last decades, a myriad of materials has been synthesized and utilized for the development of sample preparation procedures. The use of their magnetic analogues has gained significant attention and many procedures have been developed using magnetic materials. In this context, the benefits of a new class of magnetic ionic liquids (MILs), as non-conventional solvents, have been reaped in sample preparation procedures. MILs combine the advantageous properties of ionic liquids along with the magnetic properties, creating an unsurpassed combination. Owing to their unique nature and inherent benefits, the number of published reports on sample preparation with MILs is increasing. This fact, along with the many different types of extraction procedures that are developed, suggests that this is a promising field of research. Advances in the field are achieved both by developing new MILs with better properties (showing either stronger response to external magnetic fields or tunable extractive properties) and by developing and/or combining methods, resulting in advanced ones. In this advancing field of research, a good understanding of the existing literature is needed. This review aims to provide a literature update on the current trends of MILs in different modes of sample preparation, along with the current limitations and the prospects of the field. The use of MILs in dispersive liquid–liquid microextraction, single drop microextraction, matrix solid-phase dispersion, etc., is discussed herein among others. Full article
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Review
Analytical Methods for Extraction and Identification of Primary and Secondary Metabolites of Apple (Malus domestica) Fruits: A Review
Separations 2021, 8(7), 91; https://doi.org/10.3390/separations8070091 - 25 Jun 2021
Cited by 7 | Viewed by 2822
Abstract
Apples represent a greater proportion of the worldwide fruit supply, due to their availability on the market and to the high number of existing cultivar varieties and apple-based products (fresh fruit, fruit juice, cider and crushed apples). Several studies on apple fruit metabolites [...] Read more.
Apples represent a greater proportion of the worldwide fruit supply, due to their availability on the market and to the high number of existing cultivar varieties and apple-based products (fresh fruit, fruit juice, cider and crushed apples). Several studies on apple fruit metabolites are available, with most of them focusing on their healthy properties’ evaluation. In general, the metabolic profile of apple fruits strongly correlates with most of their peculiar characteristics, such as taste, flavor and color. At the same time, many bioactive molecules could be identified as markers of a specific apple variety. Therefore, a complete description of the analytical protocols commonly used for apple metabolites’ characterization and quantification could be useful for researchers involved in the identification of new phytochemical compounds from different apple varieties. This review describes the analytical methods published in the last ten years, in order to analyze the most important primary and secondary metabolites of Malus domestica fruits. In detail, this review gives an account of the spectrophotometric, chromatographic and mass spectrometric methods. A discussion on the quantitative and qualitative analytical shortcomings for the identification of sugars, fatty acids, polyphenols, organic acids, carotenoids and terpenes found in apple fruits is reported. Full article
(This article belongs to the Special Issue New Analytical Techniques in Plant Active Components Analysis)
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Review
The Use of Ferrofluids in Analytical Sample Preparation: A Review
Separations 2021, 8(4), 47; https://doi.org/10.3390/separations8040047 - 09 Apr 2021
Cited by 5 | Viewed by 2244
Abstract
Ferrofluids (FFs) constitute a type of tunable magnetic material, formed by magnetic nanoparticles suspended in a liquid carrier. The astonishing magnetic properties of these materials and their liquid nature have led to their extended use in different applications, including fields such as magnetochemistry, [...] Read more.
Ferrofluids (FFs) constitute a type of tunable magnetic material, formed by magnetic nanoparticles suspended in a liquid carrier. The astonishing magnetic properties of these materials and their liquid nature have led to their extended use in different applications, including fields such as magnetochemistry, optics, and biomedicine, among others. Recently, FFs have been incorporated as extractant materials in magnetic-driven analytical sample preparation procedures, thus, permitting the development of different applications. FF-based extraction takes advantage of both the magnetic susceptibility of the nanoparticles and the properties of the liquid carrier, which are responsible for a wide variety of interactions with analytes and ultimately are a key factor in achieving better extraction performance. This review article classifies existing FFs in terms of the solvent used as a carrier (organic solvents, water, ionic liquids, deep eutectic solvents, and supramolecular solvents) while overviewing the most relevant analytical applications in the last decade. Full article
(This article belongs to the Special Issue Development of Analytical Methods Based on Microextraction Techniques)
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Review
Recent Applications of Solid Phase Microextraction Coupled to Liquid Chromatography
Separations 2021, 8(3), 34; https://doi.org/10.3390/separations8030034 - 20 Mar 2021
Cited by 8 | Viewed by 1720
Abstract
Solid phase microextraction (SPME) is one of the most popular sample preparation methods which can be applied to organic compounds allowing the simultaneous extraction and pre-concentration of analytes from the sample matrix. It is based on the partitioning of the analyte between the [...] Read more.
Solid phase microextraction (SPME) is one of the most popular sample preparation methods which can be applied to organic compounds allowing the simultaneous extraction and pre-concentration of analytes from the sample matrix. It is based on the partitioning of the analyte between the extracting phase, generally immobilized on a fiber substrate, and the matrix (water, air, etc.), and has numerous advantages such as rapidity, simplicity, low cost, ease of use and automation, and absence of toxic solvents. Fiber SPME has been widely used in combination with various analytical instrumentation even if most of the work has been done coupling the extraction technique with gas and liquid chromatography (GC and LC). This manuscript presents an overview of the recent works (from 2010 to date) of solid phase microextraction coupled to liquid chromatography (SPME-LC) relevant to analytical applications performed using commercially available fibers or lab-made fibers already developed in previous papers, and to improved instrumental systems and approaches. Full article
Review
Ion Mobility–Mass Spectrometry for Bioanalysis
Separations 2021, 8(3), 33; https://doi.org/10.3390/separations8030033 - 16 Mar 2021
Cited by 8 | Viewed by 2233
Abstract
This paper aims to cover the main strategies based on ion mobility spectrometry (IMS) for the analysis of biological samples. The determination of endogenous and exogenous compounds in such samples is important for the understanding of the health status of individuals. For this [...] Read more.
This paper aims to cover the main strategies based on ion mobility spectrometry (IMS) for the analysis of biological samples. The determination of endogenous and exogenous compounds in such samples is important for the understanding of the health status of individuals. For this reason, the development of new approaches that can be complementary to the ones already established (mainly based on liquid chromatography coupled to mass spectrometry) is welcomed. In this regard, ion mobility spectrometry has appeared in the analytical scenario as a powerful technique for the separation and characterization of compounds based on their mobility. IMS has been used in several areas taking advantage of its orthogonality with other analytical separation techniques, such as liquid chromatography, gas chromatography, capillary electrophoresis, or supercritical fluid chromatography. Bioanalysis is not one of the areas where IMS has been more extensively applied. However, over the last years, the interest in using this approach for the analysis of biological samples has clearly increased. This paper introduces the reader to the principles controlling the separation in IMS and reviews recent applications using this technique in the field of bioanalysis. Full article
(This article belongs to the Special Issue Advances in Food and Biological Samples Analysis)
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Review
Overview of Sample Preparation and Chromatographic Methods to Analysis Pharmaceutical Active Compounds in Waters Matrices
Separations 2021, 8(2), 16; https://doi.org/10.3390/separations8020016 - 09 Feb 2021
Cited by 8 | Viewed by 3199
Abstract
In the environment, pharmaceutical residues are a field of particular interest due to the adverse effects to either human health or aquatic and soil environment. Because of the diversity of these compounds, at least 3000 substances were identified and categorized into 49 different [...] Read more.
In the environment, pharmaceutical residues are a field of particular interest due to the adverse effects to either human health or aquatic and soil environment. Because of the diversity of these compounds, at least 3000 substances were identified and categorized into 49 different therapeutic classes, and several actions are urgently required at multiple steps, the main ones: (i) occurrence studies of pharmaceutical active compounds (PhACs) in the water cycle; (ii) the analysis of the potential impact of their introduction into the aquatic environment; (iii) the removal/degradation of the pharmaceutical compounds; and, (iv) the development of more sensible and selective analytical methods to their monitorization. This review aims to present the current state-of-the-art sample preparation methods and chromatographic analysis applied to the study of PhACs in water matrices by pinpointing their advantages and drawbacks. Because it is almost impossible to be comprehensive in all PhACs, instruments, extraction techniques, and applications, this overview focuses on works that were published in the last ten years, mainly those applicable to water matrices. Full article
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Review
Analysis of Monoclonal Antibodies by Capillary Electrophoresis: Sample Preparation, Separation, and Detection
Separations 2021, 8(1), 4; https://doi.org/10.3390/separations8010004 - 04 Jan 2021
Cited by 14 | Viewed by 5678
Abstract
Therapeutic monoclonal antibodies (mAbs) are dominating the biopharmaceutical field due to the fact of their high specificity in the treatment of diverse diseases. Nevertheless, mAbs are very complex glycoproteins exhibiting several macro- and microheterogeneities that may affect their safety, quality, and efficacy. This [...] Read more.
Therapeutic monoclonal antibodies (mAbs) are dominating the biopharmaceutical field due to the fact of their high specificity in the treatment of diverse diseases. Nevertheless, mAbs are very complex glycoproteins exhibiting several macro- and microheterogeneities that may affect their safety, quality, and efficacy. This complexity is very challenging for mAbs development, formulation, and quality control. To tackle the quality issue, a combination of multiple analytical approaches is necessary. In this perspective, capillary electrophoresis has gained considerable interest over the last decade due to the fact of its complementary features to chromatographic approaches. This review provides an overview of the strategies of mAbs and derivatives analysis by capillary electrophoresis hyphenated to ultraviolet, fluorescence, and mass spectrometry detection. The main sample preparation approaches used for mAb analytical characterization (i.e., intact, middle-up/down, and bottom-up) are detailed. The different electrophoretic modes used as well as integrated analysis approaches (sample preparation and separation) are critically discussed. Full article
(This article belongs to the Special Issue Electrophoretic Methodologies for Protein Analysis)
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Review
Role of Ionic Liquids in Composites in Analytical Sample Preparation
Separations 2020, 7(3), 37; https://doi.org/10.3390/separations7030037 - 06 Jul 2020
Cited by 18 | Viewed by 3672
Abstract
Ionic liquids (ILs) are a group of non-conventional salts with melting points below 100 °C. Apart from their negligible vapor pressure at room temperature, high thermal stability, and impressive solvation properties, ILs are characterized by their tunability. Given such nearly infinite combinations of [...] Read more.
Ionic liquids (ILs) are a group of non-conventional salts with melting points below 100 °C. Apart from their negligible vapor pressure at room temperature, high thermal stability, and impressive solvation properties, ILs are characterized by their tunability. Given such nearly infinite combinations of cations and anions, and the easy modification of their structures, ILs with specific properties can be synthesized. These characteristics have attracted attention regarding their use as extraction phases in analytical sample preparation methods, particularly in liquid-phase extraction methods. Given the liquid nature of most common ILs, their incorporation in analytical sample preparation methods using solid sorbents requires the preparation of solid derivatives, such as polymeric ILs, or the combination of ILs with other materials to prepare solid IL-based composites. In this sense, many solid composites based on ILs have been prepared with improved features, including magnetic particles, carbonaceous materials, polymers, silica materials, and metal-organic frameworks, as additional materials forming the composites. This review aims to give an overview on the preparation and applications of IL-based composites in analytical sample preparation in the period 2017–2020, paying attention to the role of the IL material in those composites to understand the effect of the individual components in the sorbent. Full article
(This article belongs to the Special Issue Recent Advances on Ionic Liquid Uses in Separation Techniques)
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Review
Hunting Molecules in Complex Matrices with SPME Arrows: A Review
Separations 2020, 7(1), 12; https://doi.org/10.3390/separations7010012 - 15 Feb 2020
Cited by 25 | Viewed by 5409
Abstract
Thirty years since the invention and public disclosure of solid phase microextraction (SPME), the technology continues evolving and inspiring several other green extraction technologies amenable for the collection of small molecules present in complex matrices. In this manuscript, we review the fundamental and [...] Read more.
Thirty years since the invention and public disclosure of solid phase microextraction (SPME), the technology continues evolving and inspiring several other green extraction technologies amenable for the collection of small molecules present in complex matrices. In this manuscript, we review the fundamental and operational aspects of a novel SPME geometry that can be used to “hunt” target molecules in complex matrices: the SPME Arrow. In addition, a series of applications in environmental, food, cannabis and forensic analysis are succinctly covered. Finally, special emphasis is placed on novel interfaces to analytical instrumentation, as well as recent developments in coating materials for the SPME Arrow. Full article
(This article belongs to the Special Issue Development of Alternative Green Sample Preparation Techniques)
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Review
Evolution of Environmentally Friendly Strategies for Metal Extraction
Separations 2020, 7(1), 4; https://doi.org/10.3390/separations7010004 - 06 Jan 2020
Cited by 27 | Viewed by 6007
Abstract
The demand for the recovery of valuable metals and the need to understand the impact of heavy metals in the environment on human and aquatic life has led to the development of new methods for the extraction, recovery, and analysis of metal ions. [...] Read more.
The demand for the recovery of valuable metals and the need to understand the impact of heavy metals in the environment on human and aquatic life has led to the development of new methods for the extraction, recovery, and analysis of metal ions. With special emphasis on environmentally friendly approaches, efforts have been made to consider strategies that minimize the use of organic solvents, apply micromethodology, limit waste, reduce costs, are safe, and utilize benign or reusable materials. This review discusses recent developments in liquid- and solid-phase extraction techniques. Liquid-based methods include advances in the application of aqueous two- and three-phase systems, liquid membranes, and cloud point extraction. Recent progress in exploiting new sorbent materials for solid-phase extraction (SPE), solid-phase microextraction (SPME), and bulk extractions will also be discussed. Full article
(This article belongs to the Special Issue Development of Alternative Green Sample Preparation Techniques)
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Review
Returning to Nature for the Design of Sorptive Phases in Solid-Phase Microextraction
Separations 2020, 7(1), 2; https://doi.org/10.3390/separations7010002 - 29 Dec 2019
Cited by 29 | Viewed by 4016
Abstract
Green analytical chemistry principles aim to minimize the negative impact of analytical procedures in the environment, which can be considered both at close (to ensure the safety of the analysts) and global (to conserve our natural resources) levels. These principles suggest, among other [...] Read more.
Green analytical chemistry principles aim to minimize the negative impact of analytical procedures in the environment, which can be considered both at close (to ensure the safety of the analysts) and global (to conserve our natural resources) levels. These principles suggest, among other guidelines, the reduction/minimization of the sample treatment and the use of renewable sources when possible. The first aspect is largely fulfilled by microextraction, which is considered to be among the greenest sample treatment techniques. The second consideration is attainable if natural products are used as raw materials for the preparation of new extraction phases. This strategy is in line with the change in our production system, which is being gradually moved from a linear model (take–make–dispose) to a circular one (including reusing and recycling as key terms). This article reviews the potential of natural products as sorbents in extraction and microextraction techniques from the synergic perspectives of two research groups working on the topic. The article covers the use of unmodified natural materials and the modified ones (although the latter has a less green character) to draw a general picture of the usefulness of the materials. Full article
(This article belongs to the Special Issue Advances in Solid-Phase Microextraction)
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Review
Metal–Organic Frameworks as Key Materials for Solid-Phase Microextraction Devices—A Review
Separations 2019, 6(4), 47; https://doi.org/10.3390/separations6040047 - 02 Oct 2019
Cited by 56 | Viewed by 7833
Abstract
Metal–organic frameworks (MOFs) have attracted recently considerable attention in analytical sample preparation, particularly when used as novel sorbent materials in solid-phase microextraction (SPME). MOFs are highly ordered porous crystalline structures, full of cavities. They are formed by inorganic centers (metal ion atoms or [...] Read more.
Metal–organic frameworks (MOFs) have attracted recently considerable attention in analytical sample preparation, particularly when used as novel sorbent materials in solid-phase microextraction (SPME). MOFs are highly ordered porous crystalline structures, full of cavities. They are formed by inorganic centers (metal ion atoms or metal clusters) and organic linkers connected by covalent coordination bonds. Depending on the ratio of such precursors and the synthetic conditions, the characteristics of the resulting MOF vary significantly, thus drifting into a countless number of interesting materials with unique properties. Among astonishing features of MOFs, their high chemical and thermal stability, easy tuneability, simple synthesis, and impressive surface area (which is the highest known), are the most attractive characteristics that makes them outstanding materials in SPME. This review offers an overview on the current state of the use of MOFs in different SPME configurations, in all cases covering extraction devices coated with (or incorporating) MOFs, with particular emphases in their preparation. Full article
(This article belongs to the Special Issue Advances in Solid-Phase Microextraction)
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Review
Metal-Organic Frameworks in Green Analytical Chemistry
Separations 2019, 6(3), 33; https://doi.org/10.3390/separations6030033 - 27 Jun 2019
Cited by 40 | Viewed by 7525
Abstract
Metal-organic frameworks (MOFs) are porous hybrid materials composed of metal ions and organic linkers, characterized by their crystallinity and by the highest known surface areas. MOFs structures present accessible cages, tunnels and modifiable pores, together with adequate mechanical and thermal stability. Their outstanding [...] Read more.
Metal-organic frameworks (MOFs) are porous hybrid materials composed of metal ions and organic linkers, characterized by their crystallinity and by the highest known surface areas. MOFs structures present accessible cages, tunnels and modifiable pores, together with adequate mechanical and thermal stability. Their outstanding properties have led to their recognition as revolutionary materials in recent years. Analytical chemistry has also benefited from the potential of MOF applications. MOFs succeed as sorbent materials in extraction and microextraction procedures, as sensors, and as stationary or pseudo-stationary phases in chromatographic systems. To date, around 100 different MOFs form part of those analytical applications. This review intends to give an overview on the use of MOFs in analytical chemistry in recent years (2017–2019) within the framework of green analytical chemistry requirements, with a particular emphasis on possible toxicity issues of neat MOFs and trends to ensure green approaches in their preparation. Full article
(This article belongs to the Special Issue Development of Alternative Green Sample Preparation Techniques)
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Review
Chromatographic Techniques in the Research Area of Lithium Ion Batteries: Current State-of-the-Art
Separations 2019, 6(2), 26; https://doi.org/10.3390/separations6020026 - 13 May 2019
Cited by 35 | Viewed by 7249
Abstract
Lithium ion batteries (LIBs) are widely used in numerous application areas, including portable consumer electronics, medicine, grid storage, electric vehicles and hybrid electric vehicles. One major challenge during operation and storage is the degradation of the cell constituents, which is called aging. This [...] Read more.
Lithium ion batteries (LIBs) are widely used in numerous application areas, including portable consumer electronics, medicine, grid storage, electric vehicles and hybrid electric vehicles. One major challenge during operation and storage is the degradation of the cell constituents, which is called aging. This phenomenon drastically reduces both storage lifetime and cycle lifetime. Due to numerous aging effects, originating from both the individual LIB cell constituents as well as their interactions, a wide variety of instruments and methods are necessary for aging investigations. In particular, chromatographic methods are frequently applied for the analysis of the typically used liquid non-aqueous battery electrolytes based on organic solvents or ionic liquids. Moreover, chromatographic methods have also been recently used to investigate the composition of electrode materials. In this review, we will give an overview of the current state of chromatographic methods in the context of LIB cell research. Full article
(This article belongs to the Special Issue Analytic Techniques for Lithium Ion Batteries Analysis)
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Review
Total and Free Fatty Acids Analysis in Milk and Dairy Fat
Separations 2019, 6(1), 14; https://doi.org/10.3390/separations6010014 - 05 Mar 2019
Cited by 41 | Viewed by 14325
Abstract
Dairy fat is one of the most complex natural fats because of its fatty acid (FA) composition. Ruminant dairy fat contains more than 400 different FA varying in carbon chain length, and degree, position and configuration of unsaturation. The following article reviews the [...] Read more.
Dairy fat is one of the most complex natural fats because of its fatty acid (FA) composition. Ruminant dairy fat contains more than 400 different FA varying in carbon chain length, and degree, position and configuration of unsaturation. The following article reviews the different methods available to analyze FA (both total and free) in milk and dairy products. The most widely used methodology for separating and analyzing dairy FA is gas chromatography, coupled to a flame ionization detector (CG-FID). Alternatively, gas chromatography coupled to a mass spectrometer (GC-MS) is also used. After lipid extraction, total FA (TFA) are commonly converted into their methyl esters (fatty acid methyl esters, FAME) prior to chromatographic analysis. In contrast, free FA (FFA) can be analyzed after conversion to FAME or directly as FFA after extraction from the product. One of the key questions when analyzing FAME from TFA is the selection of a proper column for separating them, which depends mainly on the objective of the analysis. Quantification is best achieved by the internal standard method. Recently, near-infrared spectroscopy (NIRS), Raman spectroscopy (RS) and nuclear magnetic resonance (NMR) have been reported as promising techniques to analyze FA in milk and dairy products. Full article
(This article belongs to the Special Issue Separation Techniques for Dairy Analysis)
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Review
Recent Advances in Hydrophobic Deep Eutectic Solvents for Extraction
Separations 2019, 6(1), 9; https://doi.org/10.3390/separations6010009 - 12 Feb 2019
Cited by 96 | Viewed by 14467
Abstract
In the over 1,800 articles published since their inception in 2001, most deep eutectic solvents (DES) synthesized have been hydrophilic. The low cost, low toxicity, and bioavailability of DES make the solvent ‘green’ and sustainable for diverse applications. Conversely, the hydrophilicity of DES [...] Read more.
In the over 1,800 articles published since their inception in 2001, most deep eutectic solvents (DES) synthesized have been hydrophilic. The low cost, low toxicity, and bioavailability of DES make the solvent ‘green’ and sustainable for diverse applications. Conversely, the hydrophilicity of DES limits their practical application to only polar compounds, which is a major drawback of the solvent. For the past three years, hydrophobic deep eutectic solvents (HDES) have emerged as an alternative extractive media capable of extracting non-polar organic and inorganic molecules from aqueous environments. Due to the infancy of HDES, for the first time, this mini-review summarizes the recent developmental advances in HDES synthesis, applications, challenges, and future perspectives of the solvent. In the future, it is believed HDES will replace the majority of toxic organic solvents used for analytical purposes. Full article
(This article belongs to the Special Issue Recent Advances on Ionic Liquid Uses in Separation Techniques)
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