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Recent Advances and Future Trends in Sample Preparation II

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

Deadline for manuscript submissions: closed (31 July 2023) | Viewed by 2766

Special Issue Editors


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Guest 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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Guest Editor
Department of Chemistry, Sapienza University, P.le Aldo Moro 5, 00185 Rome, Italy
Interests: eco-friendly synthesis of new sorbent materials and neoteric solvents for green sample preparation; development of sustainable sample preparation techniques; liquid chromatography; mass spectrometry; organic micronutrient profiling of foods and biological fluids; analysis of emerging contaminants in foodstuffs; environmental and biological samples
Special Issues, Collections and Topics in MDPI journals

Special Issue Information

Dear Colleagues,

This Special Issue is dedicated to highlighting the most recent advancements and trends within the framework of sample preparation, which is considered the most delicate stage of an analytical method, as it is easily prone to errors and takes up to more than 50% of the analysis time. Sample preparation is a fundamental step to remove interfering compounds and to enrich the final extract, i.e., to maximize selectivity and sensitivity of a method. It is well known that there are two main families of extraction techniques: (i) direct solvent extraction, which, depending on the sample’s nature, can be classified as liquid–liquid extraction (LLE) or solid–liquid extraction (SLE); and (ii) solid-phase extraction (SPE), which is mediated by microparticle sorbents packed into a cartridge, embedded on disks, or dispersed in the extraction media. In all cases, the main trends, of which the scientific community has frantically been working on, include simplification, speediness, waste and cost reduction, miniaturization, automation, low environmental impact, operator safety, and recycling. In recent decades, the necessity of meeting the requirements of green chemistry has led to the development of a plethora of microextraction techniques, which are the miniaturized versions of LLE and SPE, and to the design of eco-friendly solvents such as deep eutectic solvents (DESs) and low-transition-temperature mixtures (LTTMs). Important advances have been made for SPE in studying novel formats, conceiving more efficient work modes, and developing ground-breaking sorbents. Breakthroughs are also expected in sorbent chemistry, where special attention is paid to the use of low-cost, natural materials from renewables.

The aim of the current Special Issue is to cover emerging and promising research trends within all sectors of sample preparation. Reviews of the recent literature and original research papers are welcome. Areas to be covered may include the following:

  • Development and application of neoteric solvents (subcritical water, supercritical fluids, ionic liquids, deep eutectic solvents, and low-transition-temperature mixtures) as extractants;
  • Improvement and application of liquid-phase microextraction techniques (dispersive liquid–liquid microextraction, hollow-fiber liquid-phase microextraction, mixed-micelle cloud point extraction, etc.);
  • Development of novel sorbents (micro- and nanoparticle-based materials, nanosponges, dendrimers, membranes, nanomaterials, magnetic particles or devices, etc.) for SPE applications;
  • Development of SPE devices that are innovative in terms of format, operational mode, miniaturization, and green features;
  • Applications of original extraction procedures in environmental chemistry, food chemistry, and clinical chemistry.

We warmly welcome our colleagues to submit their original contributions to this Special Issue in order to provide significant updates that are appealing to readers.

Prof. Dr. Alessandra Gentili
Dr. Chiara Dal Bosco
Guest Editors

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 special issue 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. Molecules is an international peer-reviewed open access semimonthly 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 2700 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

  • sample preparation
  • liquid–liquid extraction
  • liquid–solid extraction
  • solid-phase extraction
  • solid-phase microextraction techniques
  • liquid-phase microextraction techniques
  • green solvents
  • ionic liquids
  • deep eutectic solvents
  • low-transition-temperature mixtures
  • SPE sorbents
  • nanosponges
  • nanomaterials
  • membranes
  • applications to real samples

Published Papers (2 papers)

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Research

14 pages, 1414 KiB  
Article
Preparation of Novel Solid Phase Extraction Sorbents for Polycyclic Aromatic Hydrocarbons (PAHs) in Aqueous Media
by Deogratius T. Maiga, Rose W. Kibechu, Bhekie B. Mamba, Titus A. M. Msagati and Terence T. Phadi
Molecules 2023, 28(16), 6129; https://doi.org/10.3390/molecules28166129 - 18 Aug 2023
Cited by 1 | Viewed by 806
Abstract
In this study, functionalized mesoporous silica was prepared and characterized as a stationary phase using various analytical and solid-state techniques, including a Fourier-transform infrared (FTIR) spectrometer, thermogravimetric analysis, and nitrogen sorption. The results confirmed the successful synthesis of the hybrid stationary phase. The [...] Read more.
In this study, functionalized mesoporous silica was prepared and characterized as a stationary phase using various analytical and solid-state techniques, including a Fourier-transform infrared (FTIR) spectrometer, thermogravimetric analysis, and nitrogen sorption. The results confirmed the successful synthesis of the hybrid stationary phase. The potential of the prepared hybrid mesoporous silica as a solid-phase extraction (SPE) stationary phase for separating and enriching polycyclic aromatic hydrocarbons (PAHs) in both spiked water samples and real water samples was evaluated. The analysis involved extracting the PAHs from the water samples using solid-phase extraction and analyzing the extracts using a two-dimensional gas chromatograph coupled to a time-of-flight mass spectrometer (GC × GC-TOFMS). The synthesized sorbent exhibited outstanding performance in extracting PAHs from both spiked water samples and real water samples. In the spiked water samples, the recoveries of the PAHs ranged from 79.87% to 95.67%, with relative standard deviations (RSDs) ranging from 1.85% to 8.83%. The limits of detection (LOD) for the PAHs were in the range of 0.03 µg/L to 0.04 µg/L, while the limits of quantification (LOQ) ranged from 0.05 µg/L to 3.14 µg/L. Furthermore, all the calibration curves showed linearity, with correlation coefficients (r) above 0.98. Additionally, the results from real water samples indicated that the levels of individual PAH detected ranged from 0.57 to 12.31 µg/L with a total of 44.67 µg/L. These findings demonstrate the effectiveness of the hybrid mesoporous silica as a promising stationary phase for solid-phase extraction and sensitive detection of PAHs in water samples. Full article
(This article belongs to the Special Issue Recent Advances and Future Trends in Sample Preparation II)
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18 pages, 4616 KiB  
Article
Impact of Sample Preparation Methods on Single-Cell X-ray Microscopy and Light Elemental Analysis Evaluated by Combined Low Energy X-ray Fluorescence, STXM and AFM
by Lucia Merolle, Lorella Pascolo, Luisa Zupin, Pietro Parisse, Valentina Bonanni, Gianluca Gariani, Sasa Kenig, Diana E. Bedolla, Sergio Crovella, Giuseppe Ricci, Stefano Iotti, Emil Malucelli, George Kourousias and Alessandra Gianoncelli
Molecules 2023, 28(4), 1992; https://doi.org/10.3390/molecules28041992 - 20 Feb 2023
Cited by 3 | Viewed by 1644
Abstract
Background: Although X-ray fluorescence microscopy is becoming a widely used technique for single-cell analysis, sample preparation for this microscopy remains one of the main challenges in obtaining optimal conditions for the measurements in the X-ray regime. The information available to researchers on sample [...] Read more.
Background: Although X-ray fluorescence microscopy is becoming a widely used technique for single-cell analysis, sample preparation for this microscopy remains one of the main challenges in obtaining optimal conditions for the measurements in the X-ray regime. The information available to researchers on sample treatment is inadequate and unclear, sometimes leading to wasted time and jeopardizing the experiment’s success. Many cell fixation methods have been described, but none of them have been systematically tested and declared the most suitable for synchrotron X-ray microscopy. Methods: The HEC-1-A endometrial cells, human spermatozoa, and human embryonic kidney (HEK-293) cells were fixed with organic solvents and cross-linking methods: 70% ethanol, 3.7%, and 2% paraformaldehyde; in addition, HEK-293 cells were subjected to methanol/ C3H6O treatment and cryofixation. Fixation methods were compared by coupling low-energy X-ray fluorescence with scanning transmission X-ray microscopy and atomic force microscopy. Results: Organic solvents lead to greater dehydration of cells, which has the most significant effect on the distribution and depletion of diffusion elements. Paraformaldehyde provides robust and reproducible data. Finally, the cryofixed cells provide the best morphology and element content results. Conclusion: Although cryofixation seems to be the most appropriate method as it allows for keeping cells closer to physiological conditions, it has some technical limitations. Paraformaldehyde, when used at the average concentration of 3.7%, is also an excellent alternative for X-ray microscopy. Full article
(This article belongs to the Special Issue Recent Advances and Future Trends in Sample Preparation II)
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