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Advances in Electromigration and Chromatographic Techniques: A Special Issue in Honor of Dr. Salvatore Fanali on the Occasion of His 40th Year of Activity in the Field of Separation Science

A special issue of Molecules (ISSN 1420-3049). This special issue belongs to the section "Analytical Chemistry".

Deadline for manuscript submissions: closed (28 February 2022) | Viewed by 20670

Special Issue Editor

Department of Chemistry, Sapienza University, 00185 Rome, Italy
Interests: liquid chromatography; mass spectrometry; development of original extraction procedures (e.g., SPE prototypes, evaluation of last-generation materials as sorbents for SPE and liquid ionic/deep eutectic solvents for DLLME); development and validation of LC methods; LC-DAD-MS/MS profiling of organic micronutrients in foods and biological fluids
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Special Issue Information

Dear colleagues,

2020 will be an important year for our friend and colleague Dr. Salvatore Fanali (Verona University, Italy), because he will be celebrating his 40th year of activity in the field of Separation Science. We all know Salvatore’s valuable contributions to this field. His studies started at the “Istituto di Chromatografia”, CNR, Rome, applying paper and thin-layer chromatography to the separation of inorganic compounds. Later on, he investigated paper electrophoresis for the separation of different types of compounds, also including enantiomers. After the development of capillary separation techniques, he devoted his scientific activity to the development of capillary electrophoresis (CE) and was one of the pioneers in the field of chiral separation utilizing cyclodextrins or their derivatives, glycopeptide antibiotics, and other chiral selectors. Afterwards, his studies included capillary/nano-Liquid chromatography, micellar electrokinetic chromatography (MEKC), high-performance liquid chromatography (HPLC), and sample preparation. Hyphenation of capillary/nanotechniques with mass spectrometry (MS) was done, also preparing a laboratory-made ESI interface. Last but not least, all types of capillary columns were packed by him or his co-workers to study molecular recognition, new stationary phases, and separation method optimization. As demonstrated by the large number of scientific publications available in the literature, numerous young and senior researchers have had the opportunity to cooperate with him,

As Guest Editor of Molecules, I would like to celebrate his long and excellent career in the field of separation science by preparing a Special Issue on “Advances in Electromigration and Chromatographic Techniques” dedicated to Dr. Salvatore.

The journal is pleased to be publishing a commemorative issue in honor of our eminent colleague. Submission of review or original research papers, dealing with all aspects of Electrophoresis and Chromatography, including fundamental developments, column technology, miniaturization, sample preparation, applications of these techniques to drug, chiral, food, and environment analysis, are highly welcome.

I hope that you will accept this invitation and celebrate Dr. Salvatore and his outstanding contribution to separation science. 

Prof. Dr. Alessandra Gentili
Guest Editor

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Keywords

  • Capillary and nanoliquid chromatography
  • Electromigration methods
  • Chiral separations
  • Synthesis of new chiral stationary phases
  • Sample preparation
  • Food analysis
  • Forensic analysis
  • Biomedical analysis

Published Papers (7 papers)

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Research

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17 pages, 2657 KiB  
Article
Hybrid Materials Formed with Green Metal-Organic Frameworks and Polystyrene as Sorbents in Dispersive Micro-Solid-Phase Extraction for Determining Personal Care Products in Micellar Cosmetics
by Patricia I. Napolitano-Tabares, Adrián Gutiérrez-Serpa, Ana I. Jiménez-Abizanda, Francisco Jiménez-Moreno, Jorge Pasán and Verónica Pino
Molecules 2022, 27(3), 813; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules27030813 - 26 Jan 2022
Cited by 5 | Viewed by 2892
Abstract
Hybrid materials based on polystyrene (PS) and green metal-organic frameworks (MOFs) were synthesized, characterized, and evaluated as potential sorbents in dispersive micro-solid-phase extraction (µ-dSPE). Among the resulting materials, the hybrid PS/DUT-67(Zr) was selected as the adequate extraction material for the monitoring of six [...] Read more.
Hybrid materials based on polystyrene (PS) and green metal-organic frameworks (MOFs) were synthesized, characterized, and evaluated as potential sorbents in dispersive micro-solid-phase extraction (µ-dSPE). Among the resulting materials, the hybrid PS/DUT-67(Zr) was selected as the adequate extraction material for the monitoring of six personal care products in micellar cosmetic samples, combining the µ-dSPE method with ultra-high performance liquid chromatography (UHPLC) coupled to ultraviolet/visible detection (UV/Vis). Univariate studies and a factorial design were performed in the optimization of the microextraction procedure. The compromise optimum extraction conditions included 20 mg of PS/DUT-67(Zr) for 10 mL of sample, 2 min of extraction time, and two desorption steps using 100 µL of acetonitrile and 5 min assisted by vortex in each one. The validated μ-dSPE-UHPLC-UV/Vis method presented limits of detection and quantification down to 3.00 and 10.0 μg·L−1, respectively. The inter-day precision values were lower than 23.5 and 21.2% for concentration levels of 75 μg·L−1 and 650 μg·L−1, respectively. The hydrophobicity of the resulting PS/DUT-67(Zr) material was crucial for the improvement of its extraction capacity in comparison with its unitary components, showing the advantages of combining MOFs with other materials, getting new sorbents with interesting properties. Full article
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16 pages, 1680 KiB  
Article
Chiral Nano-Liquid Chromatography and Dispersive Liquid-Liquid Microextraction Applied to the Analysis of Antifungal Drugs in Milk
by Chiara Dal Bosco, Flavia Bonoli, Alessandra Gentili, Chiara Fanali and Giovanni D’Orazio
Molecules 2021, 26(23), 7094; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules26237094 - 24 Nov 2021
Cited by 6 | Viewed by 1700
Abstract
A novel chromatographic application in chiral separation by using the nano-LC technique is here reported. The chiral recognition of 12 antifungal drugs was obtained through a 75 µm I.D. fused-silica capillary, which was packed with a CSP-cellulose 3,5-dichlorophenylcarbamate (CDCPC), by means of a [...] Read more.
A novel chromatographic application in chiral separation by using the nano-LC technique is here reported. The chiral recognition of 12 antifungal drugs was obtained through a 75 µm I.D. fused-silica capillary, which was packed with a CSP-cellulose 3,5-dichlorophenylcarbamate (CDCPC), by means of a lab-made slurry packing procedure. The mobile phase composition and the experimental conditions were optimized in order to find the optimum chiral separation for some selected racemic mixtures of imidazole and triazole derivatives. Some important parameters, such as retention faction, enantioresolution, peak efficiency, and peak shape, were investigated as a function of the mobile phase (pH, water content, type and concentration of both the buffer and the organic modifier, and solvent dilution composition). Within one run lasting 25 min, at a flow rate of approximately 400 nL min−1, eight couples of enantiomers were baseline-resolved and four of them were separated in less than 25 min. The method was then applied to milk samples, which were pretreated using a classical dispersive liquid–liquid microextraction technique preceded by protein precipitation. Finally, the DLLME-nano-LC–UV method was validated in a matrix following the main FDA guidelines for bioanalytical methods. Full article
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14 pages, 1805 KiB  
Article
Application of a Low Transition Temperature Mixture for the Dispersive Liquid–Liquid Microextraction of Illicit Drugs from Urine Samples
by Valeria Gallo, Pierpaolo Tomai, Valerio Di Lisio, Chiara Dal Bosco, Paola D’Angelo, Chiara Fanali, Giovanni D’Orazio, Ilaria Silvestro, Yolanda Picó and Alessandra Gentili
Molecules 2021, 26(17), 5222; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules26175222 - 28 Aug 2021
Cited by 14 | Viewed by 2403
Abstract
The use of psychoactive substances is a serious problem in today’s society and reliable methods of analysis are necessary to confirm their occurrence in biological matrices. In this work, a green sample preparation technique prior to HPLC-MS analysis was successfully applied to the [...] Read more.
The use of psychoactive substances is a serious problem in today’s society and reliable methods of analysis are necessary to confirm their occurrence in biological matrices. In this work, a green sample preparation technique prior to HPLC-MS analysis was successfully applied to the extraction of 14 illicit drugs from urine samples. The isolation procedure was a dispersive liquid–liquid microextraction based on the use of a low transition temperature mixture (LTTM), composed of choline chloride and sesamol in a molar ratio 1:3 as the extracting solvent. This mixture was classified as LTTM after a thorough investigation carried out by FTIR and DSC, which recorded a glass transition temperature at −71 °C. The extraction procedure was optimized and validated according to the main Food and Drug Administration (FDA) guidelines for bioanalytical methods, obtaining good figures of merit for all parameters: the estimated lower limit of quantitation (LLOQ) values were between 0.01 µg L−1 (bk-MMBDB) and 0.37 µg L−1 (PMA); recoveries, evaluated at very low spike levels (in the ng-µg L−1 range), spanned from 55% (MBDB) to 100% (bk-MMBDB and MDPV); finally, both within-run and between-run precisions were lower than 20% (LLOQ) and 15% (10xLLOQ). Full article
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15 pages, 1326 KiB  
Article
Fast and Sensitive Screening of Oxandrolone and Its Major Metabolite 17-Epi-Oxandrolone in Human Urine by UHPLC—MS/MS with On-Line SPE Sample Pretreatment
by Jaroslav Galba, Juraj Piešťanský, Andrej Kováč, Dominika Olešová, Ondrej Cehlár, Martin Kertys, Petr Kozlík, Petra Chaľová, Barbora Tirčová, Kristián Slíž and Peter Mikuš
Molecules 2021, 26(2), 480; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules26020480 - 18 Jan 2021
Cited by 2 | Viewed by 3851
Abstract
Oxandrolone, a synthetic testosterone analog, is used for the treatment of several diseases associated with weight loss. Unfortunately, oxandrolone is abused by many athletes and bodybuilders due to its strong anabolic effect. We have developed and validated a highly sensitive and rapid on-line [...] Read more.
Oxandrolone, a synthetic testosterone analog, is used for the treatment of several diseases associated with weight loss. Unfortunately, oxandrolone is abused by many athletes and bodybuilders due to its strong anabolic effect. We have developed and validated a highly sensitive and rapid on-line SPE-UHPLC-MS/MS method for the determination of oxandrolone and simultaneous identification of its major metabolite 17-epi-oxandrolone in urine matrices. Enrichment of the analytes via an integrated solid-phase extraction was achieved using an Acquity UPLC BEH C18 Column. Subsequently, the chromatographic separation of the on-line preconcentrated sample fraction was achieved using an Acquity HSS T3 C18 Column. For the structural identification of these analytes, a high-resolution mass spectrometer Synapt-G2Si coupled to the Acquity M-class nano-LC system with ionKey source was used. A highly sensitive determination of oxandrolone was achieved using a tandem quadrupole mass spectrometer XEVO TQD. The method was successfully validated in the linear range of oxandrolone from 81.63 pg·mL−1 (limit of quantification, LOQ) to 5000 pg·mL−1 in the human urine matrix. It was applied to the analysis of real urine samples obtained from a healthy volunteer after the oral administration of one dose (10 mg) of oxandrolone. Concentration vs. time dependence was tested in the time interval of 4 h–12 days (after oral administration) to demonstrate the ability of the method to detect the renal elimination of oxandrolone from the human body. Favorable performance parameters along with successful application indicate the usefulness of the proposed method for its routine use in antidoping control labs. Full article
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10 pages, 6300 KiB  
Article
The Effect of Enantiomer Elution Order on the Determination of Minor Enantiomeric Impurity in Ketoprofen and Enantiomeric Purity Evaluation of Commercially Available Dexketoprofen Formulations
by Kenan Can Tok, Mehmet Gumustas, Giorgi Jibuti, Halit Sinan Suzen, Sibel A. Ozkan and Bezhan Chankvetadze
Molecules 2020, 25(24), 5865; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules25245865 - 11 Dec 2020
Cited by 10 | Viewed by 2453
Abstract
In a recent study, opposite enantiomer elution order was observed for ketoprofen enantiomers on two amylose-phenylcarbamate-based chiral columns with the same chemical composition of the chiral selector but in one case with coated while in the other with an immobilized chiral selector. In [...] Read more.
In a recent study, opposite enantiomer elution order was observed for ketoprofen enantiomers on two amylose-phenylcarbamate-based chiral columns with the same chemical composition of the chiral selector but in one case with coated while in the other with an immobilized chiral selector. In the present study, the influence of this uncommon effect on method validation parameters for the determination of minor enantiomeric impurity in dexketoprofen was studied. The validated methods with two alternative elution orders for enantiomers were applied for the evaluation of enantiomeric impurity in six marketed dexketoprofen formulations from various vendors. In most of these formulations except one the content of enantiomeric impurity exceeded 0.1% (w/w). Full article
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Review

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38 pages, 968 KiB  
Review
Deep Eutectic Solvents Application in Food Analysis
by Cecilia Ortega-Zamora, Javier González-Sálamo and Javier Hernández-Borges
Molecules 2021, 26(22), 6846; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules26226846 - 13 Nov 2021
Cited by 17 | Viewed by 3339
Abstract
Current trends in Analytical Chemistry are focused on the development of more sustainable and environmentally friendly procedures. However, and despite technological advances at the instrumental level having played a very important role in the greenness of the new methods, there is still work [...] Read more.
Current trends in Analytical Chemistry are focused on the development of more sustainable and environmentally friendly procedures. However, and despite technological advances at the instrumental level having played a very important role in the greenness of the new methods, there is still work to be done regarding the sample preparation stage. In this sense, the implementation of new materials and solvents has been a great step towards the development of “greener” analytical methodologies. In particular, the application of deep eutectic solvents (DESs) has aroused great interest in recent years in this regard, as a consequence of their excellent physicochemical properties, general low toxicity, and high biodegradability if they are compared with classical organic solvents. Furthermore, the inclusion of DESs based on natural products (natural DESs, NADESs) has led to a notable increase in the popularity of this new generation of solvents in extraction techniques. This review article focuses on providing an overview of the applications and limitations of DESs in solvent-based extraction techniques for food analysis, paying especial attention to their hydrophobic or hydrophilic nature, which is one of the main factors affecting the extraction procedure, becoming even more important when such complex matrices are studied. Full article
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23 pages, 4494 KiB  
Review
Progress in the Enantioseparation of β-Blockers by Chromatographic Methods
by Yiwen Yang, Yehui Wang, Zongbi Bao, Qiwei Yang, Zhiguo Zhang and Qilong Ren
Molecules 2021, 26(2), 468; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules26020468 - 17 Jan 2021
Cited by 9 | Viewed by 3038
Abstract
β-adrenergic antagonists (β-blockers) with at least one chiral center are an exceedingly important class of drugs used mostly to treat cardiovascular diseases. At least 70 β-blockers have been investigated in history. However, only a few β-blockers, e.g., timolol, are clinically marketed as an [...] Read more.
β-adrenergic antagonists (β-blockers) with at least one chiral center are an exceedingly important class of drugs used mostly to treat cardiovascular diseases. At least 70 β-blockers have been investigated in history. However, only a few β-blockers, e.g., timolol, are clinically marketed as an optically pure enantiomer. Therefore, the separation of racemates of β-blockers is essential both in the laboratory and industry. Many approaches have been explored to obtain the single enantiomeric β-blocker, including high performance liquid chromatography, supercritical fluid chromatography and simulated moving bed chromatography. In this article, a review is presented on different chromatographic methods applied for the enantioseparation of β-blockers, covering high performance liquid chromatography (HPLC), supercritical fluid chromatography (SFC) and simulated moving bed chromatography (SMB). Full article
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