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State of the Art in Separation Science
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State of the Art in Separation Science

A topical collection in Separations (ISSN 2297-8739). This collection belongs to the section "Chromatographic Separations".

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A printed edition of this Special Issue is available here.

Editor

Prof. Dr. Victoria Samanidou

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

Topical Collection Information

Dear Colleagues,

The term “Separation techniques” refers to a group of analytical techniques used to separate the components of a homogenous mixture that are further detected, identified and quantitatively determined.

Though separation can involve distillation and evaporation, typically in analytical chemistry, separation techniques include all types of chromatographic and electrophoretic techniques, such as:

  • Gas Chromatography (GC)
  • Liquid Chromatography (LC)
  • High Performance Liquid Chromatography (HPLC)
  • LC-MS
  • LC-MS/MS
  • LC-NMR
  • 2D LC
  • 2D GC
  • GC-MS
  • Capillary Electrochromatography (CEC)
  • Supercritical Fluid Chromatography (SFC)
  • Affinity Electrophoresis
  • Capillary Electrophoresis
  • Gel Electrophoresis
  • Immunoelectrophoresis
  • Isoelectric Focusing ((IEF)
  • Isotachophoresis (ITP)

Significant advances have been made in the last few decades, including in instrumentation as well as the materials used in stationary or mobile phases. All these advances are following the principles of Green Analytical Chemistry. Therefore, automation, speed and safety are of great importance.

Two-dimensional techniques as well as hyphenated with spectroscopic techniques have improved the feature characteristics of established separation techniques making them the best analytical tool in the analysis of any kind of sample derived from various chemistry sectors as well other scientific fields such as food science, veterinary medicine, biology, dentistry, archeology, forensics, pharmaceutical chemistry, medicine, environmental science etc. To that end major advances in separation science have led to significant findings in the above mentioned scientific fields.

The questions that arise are: What is the state of the art in Separation Sciences? What advances have been reported recently? Last but not least, what are the future perspectives?

The aim of this Topical Collection is to have the answers to these questions addressed by the experts in the field, who are invited to contribute with a research or review article.

Prof. Dr. Victoria Samanidou
Collection Editor

Manuscript Submission Information

Manuscripts should be submitted online at www.mdpi.com by registering and logging in to this website. Once you are registered, click here to go to the submission form. Manuscripts can be submitted until the deadline. All submissions that pass pre-check are peer-reviewed. Accepted papers will be published continuously in the journal (as soon as accepted) and will be listed together on the collection website. Research articles, review articles as well as short communications are invited. For planned papers, a title and short abstract (about 100 words) can be sent to the Editorial Office for announcement on this website.

Submitted manuscripts should not have been published previously, nor be under consideration for publication elsewhere (except conference proceedings papers). All manuscripts are thoroughly refereed through a single-blind peer-review process. A guide for authors and other relevant information for submission of manuscripts is available on the Instructions for Authors page. Separations is an international peer-reviewed open access monthly journal published by MDPI.

Please visit the Instructions for Authors page before submitting a manuscript. The Article Processing Charge (APC) for publication in this open access journal is 2600 CHF (Swiss Francs). Submitted papers should be well formatted and use good English. Authors may use MDPI's English editing service prior to publication or during author revisions.

Keywords

  • Gas Chromatography (GC)
  • Liquid Chromatography (LC)
  • High Performance Liquid Chromatography (HPLC)
  • LC-MS
  • LC-MS/MS
  • LC-NMR
  • 2D LC
  • 2D GC
  • GC-MS
  • Capillary electrochromatography
  • Supercritical Fluid Chromatography
  • Affinity electrophoresis
  • Capillary electrophoresis
  • Gel electrophoresis
  • Immunoelectrophoresis
  • Isoelectric focusing
  • Isotachophoresis

Published Papers (11 papers)

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2023

Jump to: 2022, 2021

27 pages, 465 KiB  
Review
Organic Solvent Nanofiltration and Data-Driven Approaches
by Pieter-Jan Piccard, Pedro Borges, Bart Cleuren, Jef Hooyberghs and Anita Buekenhoudt
Separations 2023, 10(9), 516; https://doi.org/10.3390/separations10090516 - 19 Sep 2023
Cited by 1 | Viewed by 2022
Abstract
Organic solvent nanofiltration (OSN) is a membrane separation method that has gained much interest due to its promising ability to offer an energy-lean alternative for traditional thermal separation methods. Industrial acceptance, however, is held back by the slow process of membrane screening based [...] Read more.
Organic solvent nanofiltration (OSN) is a membrane separation method that has gained much interest due to its promising ability to offer an energy-lean alternative for traditional thermal separation methods. Industrial acceptance, however, is held back by the slow process of membrane screening based on trial and error for each solute-solvent couple to be separated. Such time-consuming screening is necessary due to the absence of predictive models, caused by a lack of fundamental understanding of the complex separation mechanism complicated by the wide variety of solute and solvent properties, and the importance of all mutual solute-solvent-membrane affinities and competing interactions. Recently, data-driven approaches have gained a lot of attention due to their unprecedented predictive power, significantly outperforming traditional mechanistic models. In this review, we give an overview of both mechanistic models and the recent advances in data-driven modeling. In addition to other reviews, we want to emphasize the coherence of all mechanistic models and discuss their relevance in an increasingly data-driven field. We reflect on the use of data in the field of OSN and its compliance with the FAIR principles, and we give an overview of the state of the art of data-driven models in OSN. The review can serve as inspiration for any further modeling activities, both mechanistic and data-driven, in the field. Full article
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2022

Jump to: 2023, 2021

9 pages, 1429 KiB  
Article
An Integrated Chromatographic Strategy for the Large-Scale Extraction of Ergosterol from Tulasnellaceae sp.
by Ze Wang, Qi Wang, Jinkui Zhang, Pengcheng Lin and Jun Dang
Separations 2022, 9(7), 176; https://doi.org/10.3390/separations9070176 - 17 Jul 2022
Cited by 1 | Viewed by 2044
Abstract
A reliable chromatographic strategy is crucial for the extraction of target compounds from natural sources as it is related to the preparation efficiency, as well as the purity of the compounds. In this study, medium-pressure normal-phase liquid chromatography and high-pressure reverse-phase liquid chromatography [...] Read more.
A reliable chromatographic strategy is crucial for the extraction of target compounds from natural sources as it is related to the preparation efficiency, as well as the purity of the compounds. In this study, medium-pressure normal-phase liquid chromatography and high-pressure reverse-phase liquid chromatography were combined to prepare and purify ergosterol from Tulasnellaceae sp. of Gymnadenia orchidis. First, Tulasnellaceae sp. was extracted three times (2.0 L and 2 h each time) with ethyl acetate, and the 6.0 L of extract solution was concentrated under reduced pressure to yield 2.2 g of crude sample. Then, the crude sample was pretreated utilizing silica gel medium-pressure liquid chromatography to enrich the target ingredient (586.0 mg). Finally, high-pressure reversed-phase liquid chromatography was used to purify the target compound, and the compound was characterized as ergosterol (purity > 95%) using spectral data. Overall, the simple and reproducible integrated chromatographic strategy developed in this study has the potential for the large-scale purification of steroids for laboratory and even industrial research. To the best of our knowledge, this is also the first report of ergosterol in Tulasnellaceae sp. Full article
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7 pages, 3072 KiB  
Article
Simultaneous Determination of Methyl Nicotinate and Three Salicylic Acid Derivatives in Pain Relief Spray Using HPLC–DAD
by Hazim M. Ali
Separations 2022, 9(4), 93; https://doi.org/10.3390/separations9040093 - 6 Apr 2022
Cited by 3 | Viewed by 3476
Abstract
For the first time, the high-performance liquid chromatography–diode array detector (HPLC–DAD) approach was operated for the simultaneous assessment of methyl nicotinate (MN), methyl salicylate (MS), ethyl salicylate (ES) and 2-hydroxyethyl salicylate (HES) in one pharmaceutical formulation. The limits of detection of MN, HES, [...] Read more.
For the first time, the high-performance liquid chromatography–diode array detector (HPLC–DAD) approach was operated for the simultaneous assessment of methyl nicotinate (MN), methyl salicylate (MS), ethyl salicylate (ES) and 2-hydroxyethyl salicylate (HES) in one pharmaceutical formulation. The limits of detection of MN, HES, MS and ES were found to be 0.0144, 0.0455, 0.0087 and 0.0061 μg/mL. The recovery percentages and relative standard deviations ranged from 93.48 to 102.12% and 0.301 to 6.341% for all active ingredients. Accordingly, the previously described data demonstrate the sensitivity, accuracy and precision of the developed method. Therefore, the investigated approach was effectively applied for the simultaneous assessment of MN, HES, MS and ES in DEEP HEAT Spray. Full article
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10 pages, 1185 KiB  
Article
µQuEChERS Combined with UHPLC-PDA as a State-of-the-Art Analytical Approach for Quantification of Chlorpropham in Potato
by Telma M. Gomes, Rosa Perestrelo and José S. Câmara
Separations 2022, 9(3), 77; https://doi.org/10.3390/separations9030077 - 17 Mar 2022
Cited by 2 | Viewed by 2427
Abstract
Pesticides are chemicals used in agriculture to prevent insects, fungi, weeds, and other pests, from damaging crops. In addition, some types of pesticides are used after harvest as sprout suppressant agents help keeping the quality parameters of crops during storage. Nonetheless, its presence, [...] Read more.
Pesticides are chemicals used in agriculture to prevent insects, fungi, weeds, and other pests, from damaging crops. In addition, some types of pesticides are used after harvest as sprout suppressant agents help keeping the quality parameters of crops during storage. Nonetheless, its presence, even at trace levels, in food products is becoming a big challenge regarding human health. The current work aimed to develop and validate a sensitive and high-throughput analytical approach, based on a state-of-the-art microextraction technique—µQuEChERS, combined with ultra-high performance liquid chromatography equipped with a photodiode array detection system (UHPLC-PDA) to quantify isopropyl-N-(3-chlorophenyl) carbamate (chlorpropham), commonly used as efficient sprout suppressant stored potatoes, in raw and cooked potatoes cultivated in different geographical regions of Madeira Island (Portugal). Good results were obtained in terms of figures of the merit of the method, with correlation coefficients (R2) higher than 0.999 and recoveries between 94.5% to 125%. Method limit of detection (LOD) and limit of quantification (LOQ) were 0.14 μg/Kg and 0.43 μg/Kg, respectively, which are much lower than the accepted and legislated requirements by the European Union, which is 20 μg/Kg for chlorpropham. The concentration of chlorpropham in raw potatoes is significantly higher when compared to cooked samples, which revealed that the thermic treatment during cooking had a significant effect on its degradation. A significant decrease (90%, on average) was observed on chlorpropham levels. Full article
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11 pages, 1081 KiB  
Article
Analysis of Volatiles in Senecio anteuphorbium Essential Oil with a Focus on Its Allelopathic Effect by Means of Gas Chromatography
by Soukaina Ouhaddou, Abdellah Aghraz, Widad Ben Bakrim, Saida Sissi, Mustapha Larhsini, Mohamed Markouk, Khalid Bekkouche, Sara Arrigo, Nicola Cicero, Rosaria Costa and Rossella Vadalà
Separations 2022, 9(2), 36; https://doi.org/10.3390/separations9020036 - 29 Jan 2022
Cited by 8 | Viewed by 3201
Abstract
The present study aimed to investigate Senecio anteuphorbium, an endemic plant growing in West Morocco and widely used in local folk medicine. The essential oil (EO) extracted from the aerial parts was analyzed by gas chromatography and tested for allelopathic activity. The [...] Read more.
The present study aimed to investigate Senecio anteuphorbium, an endemic plant growing in West Morocco and widely used in local folk medicine. The essential oil (EO) extracted from the aerial parts was analyzed by gas chromatography and tested for allelopathic activity. The quantitation of the volatiles was carried out by means of GC-FID with response factors, which were validated through reliable calibration procedures, based on external and internal standardization. This analytical approach allowed to define the real concentration of each constituent (weight%, g/100 g) alongside the conventional relative percent. On the other hand, the identification process was supported by a dual matching based on both mass spectra and retention indices. The essential oil resulted in being rich in sesquiterpenes, with the predominant constituents being bicyclogermacrene (22.75 g/100 g), spathulenol (25.26 g/100 g), epi-γ-eudesmol (6.8 g/100 g), and selina-4,11-diene (5.08 g/100 g). The allelopathic effect was evaluated by studying the inhibition of the germination and growth of Lactuca sativa seeds. A potent allelopathic effect was recorded by the essential oil at a dose of 0.281 mg/mL, with almost a total inhibition of germination. Full article
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23 pages, 3780 KiB  
Review
State of the Art in Separation Processes for Alternative Working Fluids in Clean and Efficient Power Generation
by Odi Fawwaz Alrebei, Abdulkarem I. Amhamed, Muftah H. El-Naas, Mahmoud Hayajnh, Yasmeen A. Orabi, Ward Fawaz, Ahmad S. Al-tawaha and Agustin Valera Medina
Separations 2022, 9(1), 14; https://doi.org/10.3390/separations9010014 - 13 Jan 2022
Cited by 8 | Viewed by 3865
Abstract
Gas turbines must now comply with much stricter emission control regulations. In fact, to combat the greenhouse effect, regulatory authorities have drastically reduced allowable emission levels. For example, in less than 12 years, the United States’ Clean Air Act issued the New Source [...] Read more.
Gas turbines must now comply with much stricter emission control regulations. In fact, to combat the greenhouse effect, regulatory authorities have drastically reduced allowable emission levels. For example, in less than 12 years, the United States’ Clean Air Act issued the New Source Performance Standards (NSPS), which tightened the NOx emission margin of natural gas combustion (from 75 ppm to 10 ppm). On the other hand, despite those efforts, the high demand for energy produced by fossil-fueled gas turbines in power plants has resulted in dramatic increases in anthropogenic CO2 and NOx emitted by gas combustors. Most systems responsible for these undesirable emissions are directly linked to power generation, with gas turbines playing a pivotal role. Yet, gas turbines are still widely used in power plants and will continue to meet the growing demand. Therefore, sequestration and separation techniques such as Carbon Capture and Storage (CCS) and Air Separation Units (ASU) are essential to reduce CO2 and NOx emissions while allowing large amounts of power to be generated from these systems. This paper provides an in-depth examination of the current state of the art in alternative working fluids utilized in the power generation industry (i.e., gas turbines, combustion). In addition, this paper highlights the recent contribution of integrating separation techniques, such as air separation, steam methane reforming, and water-gas shifting, to the power generation industry to facilitate a continuous and adequate supply of alternative working fluids. Full article
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2021

Jump to: 2023, 2022

17 pages, 2207 KiB  
Article
Separation and Disinfection of Contagious Aerosols from the Perspective of SARS-CoV-2
by J. J. H. Brouwers
Separations 2021, 8(10), 190; https://doi.org/10.3390/separations8100190 - 15 Oct 2021
Cited by 3 | Viewed by 2216
Abstract
An assessment was performed on methods of separating and disinfecting airborne droplet nuclei containing viruses, such as SARS-CoV-2. The droplet nuclei originate from evaporating aerosols emitted by the coughing, singing, sneezing, etc. of infected humans. Based on empirical data and theoretical analysis, we [...] Read more.
An assessment was performed on methods of separating and disinfecting airborne droplet nuclei containing viruses, such as SARS-CoV-2. The droplet nuclei originate from evaporating aerosols emitted by the coughing, singing, sneezing, etc. of infected humans. Based on empirical data and theoretical analysis, we successively determined: (i) the particle number distribution of nuclei versus the nucleus diameter, (ii) the statistical distribution of the viral content in the droplet nuclei starting from a uniform random distribution of viruses in the mucus, (iii) the particle number distribution of droplet nuclei containing at least one virus particle, and (iv) the effectiveness of methods for removing and disinfecting nuclei containing one or more virus particles from indoor air; viz., ventilation with fresh air, filtering with porous media, such as HEPA, and centrifugal separation and simultaneous disinfection, particularly with a rotational particle separator (RPS). Indoor aerosol removal with RPS supplemented with HEPA to arrest tiny volumes of very small particles was found to be the most effective. It is as good as particle removal through ventilation with clean air over long periods of time. An RPS facilitates direct elimination of viruses in the collected nuclei by flushing with a disinfection liquid. The components of an RPS are recyclable. Combining HEPA with an RPS extends the service time of HEPA by almost two orders of magnitude compared to the relatively short service time of stand-alone HEPA filters. Full article
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11 pages, 2032 KiB  
Article
Quantitation of Acetyl Hexapeptide-8 in Cosmetics by Hydrophilic Interaction Liquid Chromatography Coupled to Photo Diode Array Detection
by Vasiliki Raikou, Eleni Kalogria, Athanasia Varvaresou, Efthimios Tsirivas and Irene Panderi
Separations 2021, 8(8), 125; https://doi.org/10.3390/separations8080125 - 18 Aug 2021
Cited by 6 | Viewed by 5962
Abstract
Bioactive peptides are gaining more and more popularity in the research and development of cosmetic products with anti-aging effect. Acetyl hexapeptide-8 is a hydrophilic peptide incorporated in cosmetics to reduce the under-eye wrinkles and the forehead furrows. Hydrophilic interaction liquid chromatography (HILIC) is [...] Read more.
Bioactive peptides are gaining more and more popularity in the research and development of cosmetic products with anti-aging effect. Acetyl hexapeptide-8 is a hydrophilic peptide incorporated in cosmetics to reduce the under-eye wrinkles and the forehead furrows. Hydrophilic interaction liquid chromatography (HILIC) is the separation technique of choice for analyzing peptides. In this work, a rapid HILIC method coupled to photodiode array detection operated at 214 nm was developed, validated and used to determine acetyl-hexapeptide-8 in cosmetics. Chromatography was performed on a Xbridge® HILIC BEH analytical column using as mobile phase a 40 mM ammonium formate water solution (pH 6.5)-acetonitrile mixture 30:70, v/v at flow rate 0.25 mL min−1. The assay was linear over the concentration range 20 to 30 μg mL−1 for the cosmetic formulations and 0.004 to 0.007% (w/w) for the cosmetic cream. The limits of quantitation for acetyl hexapeptide-8 were 1.5 μg mL−1 and 0.002% (w/w) for the assay of cosmetic formulations and cosmetic creams, respectively. The method was applied to the analysis of cosmetic formulations and anti-wrinkle cosmetic creams. Full article
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14 pages, 1439 KiB  
Article
Simultaneous Determination of Seven Bioactive Constituents from Salvia miltiorrhiza in Rat Plasma by HPLC-MS/MS: Application to a Comparative Pharmacokinetic Study
by Yanli Zhang, Weiliang Cui, Xianghong Liu, Ning Wang, Wenru Kong, Junyu Sui, Huifen Li and Shuqi Wang
Separations 2021, 8(7), 93; https://doi.org/10.3390/separations8070093 - 29 Jun 2021
Cited by 1 | Viewed by 2832
Abstract
The roots of Salvia miltiorrhiza (Danshen) is a precious herbal medicine used to treat cardiovascular diseases. This study establishes a high-performance liquid chromatography-tandem mass spectrometric (HPLC-MS/MS) method to quantify seven bioactive constituents from Danshen in rat plasma simultaneously. Chromatographic separation is performed on [...] Read more.
The roots of Salvia miltiorrhiza (Danshen) is a precious herbal medicine used to treat cardiovascular diseases. This study establishes a high-performance liquid chromatography-tandem mass spectrometric (HPLC-MS/MS) method to quantify seven bioactive constituents from Danshen in rat plasma simultaneously. Chromatographic separation is performed on an Agilent Eclipse Plus C18 column (150 mm × 2.1 mm, 5 μm), utilizing a gradient of acetonitrile and 0.2% formic acid aqueous solution as the mobile phase, at a flow rate of 0.6 mL/min. We conduct a tandem mass spectrometric detection with electrospray ionization (ESI) interface via multiple reaction monitoring (MRM) in both positive and negative ionization mode. Our results show that a linear relationship is established for each analyte of interest over the concentration range of 0.5–300 ng/mL with r ≥ 0.9976. The validated method is successfully used to compare the pharmacokinetic properties of crude and wine-processed Danshen extract orally administered to rats. Cmax of tanshinone IIA, Cmax, and AUC0-t of dihydrotanshinone I decrease significantly (p < 0.05) in the wine-processed group. No significant changes for other compounds are observed. These results might provide meaningful information for the further application of wine-processed Danshen and understanding of wine-processing mechanisms. Full article
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14 pages, 3262 KiB  
Article
Identification of Abnormal Proteins in Plasma from Gout Patients by LC-MS/MS
by Lijin Shen, Hanyang Dong, Zhenchang Guo, Guijin Zhai and Kai Zhang
Separations 2021, 8(6), 85; https://doi.org/10.3390/separations8060085 - 16 Jun 2021
Cited by 4 | Viewed by 4090
Abstract
A high level of uric acid may cause hyperuricemia, which further develops into gout, eventually leading to chronic kidney disease. However, the pathogenic mechanism remains largely unknown. To investigate the cause and block the transformation of hyperuricemia to related diseases, it is important [...] Read more.
A high level of uric acid may cause hyperuricemia, which further develops into gout, eventually leading to chronic kidney disease. However, the pathogenic mechanism remains largely unknown. To investigate the cause and block the transformation of hyperuricemia to related diseases, it is important to discover the alterations in protein levels between gout patients and non-gout individuals. To date, human blood plasma is still the predominant matrices for clinical analysis. Due to the high abundance, the proteins of plasma samples have strong shielding effects on low abundance proteins, thus, the information on low abundance protein expression is always masked, while the low abundance proteins of human plasma are often of great significance for the diagnosis and treatment of diseases. Therefore, it is very important to separate and analyze the plasma proteins. High-performance liquid chromatography (LC) tandem mass spectrometry (MS)-based proteomics has been developed as a powerful tool to investigate changes in the human plasma proteome. Here, we used LC-MS/MS to detect the differential proteins in the plasmas from simple gout patients, gout with kidney damage patients, and non-gout individuals. We identified 32 obviously differential proteins between non-gout and gout subjects and 10 differential proteins between simple gout and gout with kidney damage patients. These differential proteins were further analyzed to characterize their localization and functions. Additionally, the correlation analysis showed multiple relationships between the abnormal plasma proteins and clinical biochemical indexes, particularly for the immune-inflammatory response proteins. Furthermore, inflammation factors gelsolin (GSN) were confirmed. Our results offer a view of plasma proteins for studying biomarkers of gout patients. Full article
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10 pages, 3047 KiB  
Article
Revisiting Chiral Recognition Mechanism on Chicken Alpha 1-Acid Glycoprotein: Location of Chiral Binding Sites and Insight into Chiral Binding Mechanism
by Jun Haginaka, Taku Yamashita, Hirofumi Tsujino and Mitsuhiro Arisawa
Separations 2021, 8(6), 73; https://doi.org/10.3390/separations8060073 - 23 May 2021
Cited by 4 | Viewed by 2985
Abstract
Chiral stationary phases based on chicken alpha 1-acid glycoprotein (cAGP) have been used for enantioseparations of various compounds. However, the chiral binding sites and mechanism have not been clarified yet. Based on chromatographic properties of native and W26-modified cAGP columns and docking simulations [...] Read more.
Chiral stationary phases based on chicken alpha 1-acid glycoprotein (cAGP) have been used for enantioseparations of various compounds. However, the chiral binding sites and mechanism have not been clarified yet. Based on chromatographic properties of native and W26-modified cAGP columns and docking simulations of studied compounds into the generated model structure of cAGP, the chiral binding sites were located on cAGP and the chiral binding mechanism was discussed. On cAGP, there existed a binding cavity lined with H25, W26, Y47, R128, T129, D161 and E168, which contribute electrostatic or hydrogen bonding interactions. Benzoin and chlorpheniramine enantiomers interacted with cAGP at almost the same sites a little away from W26, while propranolol enantiomers docked, slightly shifting toward H25 and W26. Furthermore, in addition to hydrophobic interactions, ionic interactions between amino groups of chlorpheniramine enantiomers and a carboxyl group of D161 or E168 played an important role in the chiral recognition, while hydrophobic interactions and hydrogen bonding interactions worked for the chiral recognition of benzoin and propranolol enantiomers. Full article
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