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Recent Advances and Future Trends in Sample Preparation

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

Deadline for manuscript submissions: closed (15 September 2022) | Viewed by 23107

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Special Issue Editors

Prof. Dr. Alessandra Gentili

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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
Special Issues, Collections and Topics in MDPI journals

Dr. Chiara Dal Bosco

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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, being easily prone to errors and taking 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 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 on which the scientific community has frantically been working are simplification, speediness, waste and cost reduction, miniaturization, automation, low environmental impact, operator safety, and recycling. In the last 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 (DES) and low-transition-temperature mixtures (LTTM). 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 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.

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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 (8 papers)

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Research

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14 pages, 5120 KiB

Open AccessArticle

Multi-Residue Analysis of Chemical Additives in Edible Vegetable Oils Using QuEChERS Extraction Method Followed by Supercritical Fluid Chromatography

by Yaping Gan and Yan Zhu

Molecules 2022, 27(5), 1681; https://doi.org/10.3390/molecules27051681 - 03 Mar 2022

Cited by 3 | Viewed by 2094

Abstract

Since the quality and safety of food highly depend on its preservation and protection, the use of food packaging materials increases the risk of chemical contamination of the packaged food by migration. Herein, we focused on antioxidants, photoinitiators, UV absorbers and plasticizers which are extensive additives used in food packaging materials. In the present study, a rapid, simple, green and reliable method was developed and validated for the determination of twelve chemical additives in edible vegetable oils using SFC together with a modified QuEChERS procedure. Under the optimum conditions, twelve additives were separated within 10 min, and the consumption of the organic solvent was significantly reduced, which improved the environmentally friendliness. The performance of the developed method was evaluated. Good linearity (r > 0.999) was obtained in the range of 0.20–20.0 µg/mL and 0.50–20.0 µg/mL, respectively. The limits of detection and limits of quantification of the twelve additives in vegetable oils were 0.05–0.15 µg/mL and 0.15–0.50 µg/mL, respectively. Recoveries of all the chemical additives for the spiked samples were between 60.9% and 106.4%, with relative standard deviations (RSD) lower than 9.9%. The results demonstrated that the proposed method was efficient, reliable and robust for the routine analysis of additives in edible vegetable oils and can be an alternative to the multi-residue analysis of chemical additives for other packaged foods. Full article

(This article belongs to the Special Issue Recent Advances and Future Trends in Sample Preparation)

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13 pages, 1455 KiB

Open AccessArticle

Hydrophobic Eutectic Solvent-Based Dispersive Liquid-Liquid Microextraction Applied to the Analysis of Pesticides in Wine

by Chiara Dal Bosco, Francesca Mariani and Alessandra Gentili

Molecules 2022, 27(3), 908; https://doi.org/10.3390/molecules27030908 - 28 Jan 2022

Cited by 13 | Viewed by 1899

Abstract

A green solvent-based DLLME/HPLC-MS method for the determination of 19 pesticides in wine samples has been developed. The extractant solvent is a hydrophobic eutectic mixture composed of L-menthol and butylated hydroxytoluene in a molar ratio of 3:1. The endogenous ethanol of wine has been used as dispersive solvent, in order to avoid the solidification of the extracts under 19 °C. The mobile phase composition, the elution gradient and the sample injection volume were optimized in order to make this hydrophobic mixture compatible with conventional reversed phase chromatography and electrospray ionization. The method was validated in matrix, using a wine free from the target compounds. Average recovery as high as 80%, precision between 3 and 14%, and limits of detection and quantification much lower than the maximum residue levels (MRLs) for grapes and wines fixed by the EU regulation, make this multiresidue method fitted for the purpose, with the further advantages of being quick, cheap and in compliance with the green analytical chemistry. From the analysis of 11 commercial wines it was found that just in a bio sample the target compounds were not detectable or lower than quantification limit; as for the other samples, the most widespread and abundant pesticides were methoxyfenozide and boscalid, but their levels were much lower than the relative MRLs. Full article

(This article belongs to the Special Issue Recent Advances and Future Trends in Sample Preparation)

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15 pages, 20098 KiB

Open AccessArticle

Greener Monolithic Solid Phase Extraction Biosorbent Based on Calcium Cross-Linked Starch Cryogel Composite Graphene Oxide Nanoparticles for Benzo(a)pyrene Analysis

by Aree Choodum, Nareumon Lamthornkit, Chanita Boonkanon, Tarawee Taweekarn, Kharittha Phatthanawiwat, Wilasinee Sriprom, Wadcharawadee Limsakul, Laemthong Chuenchom and Worawit Wongniramaikul

Molecules 2021, 26(20), 6163; https://doi.org/10.3390/molecules26206163 - 13 Oct 2021

Cited by 13 | Viewed by 2097

Abstract

Benzo(a)pyrene (BaP) has been recognized as a marker for the detection of carcinogenic polycyclic aromatic hydrocarbons. In this work, a novel monolithic solid-phase extraction (SPE) sorbent based on graphene oxide nanoparticles (GO) in starch-based cryogel composite (GO-Cry) was successfully prepared for BaP analysis. Rice flour and tapioca starch (gel precursors) were gelatinized in limewater (cross-linker) under alkaline conditions before addition of GO (filler) that can increase the ability to extract BaP up to 2.6-fold. BaP analysis had a linear range of 10 to 1000 µgL⁻¹ with good linearity (R² = 0.9971) and high sensitivity (4.1 ± 0.1 a.u./(µgL⁻¹)). The limit of detection and limit of quantification were 4.21 ± 0.06 and 14.04 ± 0.19 µgL⁻¹, respectively, with excellent precision (0.17 to 2.45%RSD). The accuracy in terms of recovery from spiked samples was in the range of 84 to 110% with no significant difference to a C₁₈ cartridge. GO-Cry can be reproducibly prepared with 2.8%RSD from 4 lots and can be reused at least 10 times, which not only helps reduce the analysis costs (~0.41USD per analysis), but also reduces the resultant waste to the environment. Full article

(This article belongs to the Special Issue Recent Advances and Future Trends in Sample Preparation)

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13 pages, 1047 KiB

Open AccessArticle

Simultaneous Quantification of 25 Fentanyl Derivatives and Metabolites in Oral Fluid by Means of Microextraction on Packed Sorbent and LC–HRMS/MS Analysis

by Flaminia Vincenti, Camilla Montesano, Svetlana Pirau, Adolfo Gregori, Fabiana Di Rosa, Roberta Curini and Manuel Sergi

Molecules 2021, 26(19), 5870; https://doi.org/10.3390/molecules26195870 - 28 Sep 2021

Cited by 7 | Viewed by 1794

Abstract

Fentanyl and fentalogs’ intake as drugs of abuse is experiencing a great increase in recent years. For this reason, there are more and more cases in which it is important to recognize and quantify these molecules and related metabolites in biological matrices. Oral fluid (OF) is often used to find out if a subject has recently used a psychoactive substance and if, therefore, the person is still under the effect of psychotropics. Given its difficulty in handling, good sample preparation and the development of instrumental methods for analysis are essential. In this work, an analytical method is proposed for the simultaneous determination of 25 analytes, including fentanyl, several derivatives and metabolites. OF was collected by means of passive drool; sample pretreatment was developed in order to be fast, simple and possibly semi-automated by exploiting microextraction on packed sorbent (MEPS). The analysis was performed by means of LC–HRMS/MS obtaining good identification and quantification of all the analytes in less than 10 min. The proposed method was fully validated according to the Scientific Working Group for Forensic Toxicology (SWGTOX) international guidelines. Good results were obtained in terms of recoveries, matrix effect and sensitivity, showing that this method could represent a useful tool in forensic toxicology. The presented method was successfully applied to the analysis of proficiency test samples. Full article

(This article belongs to the Special Issue Recent Advances and Future Trends in Sample Preparation)

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15 pages, 2687 KiB

Open AccessArticle

A Novel Glass Fiber Coated with Sol–Gel Poly-Diphenylsiloxane Sorbent for the On-Line Determination of Toxic Metals Using Flow Injection Column Preconcentration Platform Coupled with Flame Atomic Absorption Spectrometry

by Eleni Lazaridou, Abuzar Kabir, Kenneth G. Furton and Aristidis Anthemidis

Molecules 2021, 26(1), 9; https://doi.org/10.3390/molecules26010009 - 22 Dec 2020

Cited by 9 | Viewed by 2664

Abstract

A novel simple and sensitive, time-based flow injection solid phase extraction system was developed for the automated determination of metals at low concentration. The potential of the proposed scheme, coupled with flame atomic absorption spectrometry (FAAS), was demonstrated for trace lead and chromium(VI) determination in environmental water samples. The method, which was based on a new sorptive extraction system, consisted of a microcolumn packed with glass fiber coated with sol–gel poly (diphenylsiloxane) (sol–gel PDPS), which is presented here for the first time. The analytical procedure involves the on-line chelate complex formation of target species with ammonium pyrrolidine dithiocarbamate (APDC), retention onto the hydrophobic sol–gel sorbent coated surface of glass fibers, and finally elution with methyl isobutyl ketone prior to atomization. All main chemical and hydrodynamic factors, which affect the complex formation, retention, and elution of the metal, were optimized thoroughly. Furthermore, the tolerance to potential interfering ions appearing in environmental samples was also explored. Enhancement factors of 215 and 70, detection limits (3 s) of 1.1 μg·L⁻¹ and 1.2 μg·L⁻¹, and relative standard deviations (RSD) of 3.0% (at 20.0 μg·L⁻¹) and 3.2% (at 20.0 μg·L⁻¹) were obtained for lead and chromium(VI), respec tively, for 120 s preconcentration time. The trueness of the developed method was estimated by analyzing certified reference materials and spiked environmental water samples. Full article

(This article belongs to the Special Issue Recent Advances and Future Trends in Sample Preparation)

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Review

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59 pages, 879 KiB

Open AccessReview

A Review of In Situ Methods—Solid Phase Adsorption Toxin Tracking (SPATT) and Polar Organic Chemical Integrative Sampler (POCIS) for the Collection and Concentration of Marine Biotoxins and Pharmaceuticals in Environmental Waters

by Naghmeh Kamali, Feras Abbas, Mary Lehane, Michael Griew and Ambrose Furey

Molecules 2022, 27(22), 7898; https://doi.org/10.3390/molecules27227898 - 15 Nov 2022

Cited by 2 | Viewed by 1705

Abstract

Solid Phase Adsorption Toxin Tracking (SPATT) and Polar Organic Chemical Integrative Sampler (POCIS) are in situ methods that have been applied to pre-concentrate a range of marine toxins, pesticides and pharmaceutical compounds that occur at low levels in marine and environmental waters. Recent research has identified the widespread distribution of biotoxins and pharmaceuticals in environmental waters (marine, brackish and freshwater) highlighting the need for the development of effective techniques to generate accurate quantitative water system profiles. In this manuscript, we reviewed in situ methods known as Solid Phase Adsorption Toxin Tracking (SPATT) and Polar Organic Chemical Integrative Sampler (POCIS) for the collection and concentration of marine biotoxins, freshwater cyanotoxins and pharmaceuticals in environmental waters since the 1980s to present. Twelve different adsorption substrates in SPATT and 18 different sorbents in POCIS were reviewed for their ability to absorb a range of lipophilic and hydrophilic marine biotoxins, pharmaceuticals, pesticides, antibiotics and microcystins in marine water, freshwater and wastewater. This review suggests the gaps in reported studies, outlines future research possibilities and guides researchers who wish to work on water contaminates using Solid Phase Adsorption Toxin Tracking (SPATT) and Polar Organic Chemical Integrative Sampler (POCIS) technologies. Full article

(This article belongs to the Special Issue Recent Advances and Future Trends in Sample Preparation)

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20 pages, 2290 KiB

Open AccessReview

Current Sample Preparation Methodologies for Determination of Catecholamines and Their Metabolites

by Nian Shi, Xinmiao Bu, Manyu Zhang, Bin Wang, Xinli Xu, Xuezhong Shi, Dilshad Hussain, Xia Xu and Di Chen

Molecules 2022, 27(9), 2702; https://doi.org/10.3390/molecules27092702 - 22 Apr 2022

Cited by 6 | Viewed by 5885

Abstract

Catecholamines (CAs) and their metabolites play significant roles in many physiological processes. Changes in CAs concentration in vivo can serve as potential indicators for the diagnosis of several diseases such as pheochromocytoma and paraganglioma. Thus, the accurate quantification of CAs and their metabolites in biological samples is quite important and has attracted great research interest. However, due to their extremely low concentrations and numerous co-existing biological interferences, direct analysis of these endogenous compounds often suffers from severe difficulties. Employing suitable sample preparation techniques before instrument detection to enrich the target analytes and remove the interferences is a practicable and straightforward approach. To date, many sample preparation techniques such as solid-phase extraction (SPE), and liquid-liquid extraction (LLE) have been utilized to extract CAs and their metabolites from various biological samples. More recently, several modern techniques such as solid-phase microextraction (SPME), liquid–liquid microextraction (LLME), dispersive solid-phase extraction (DSPE), and chemical derivatizations have also been used with certain advanced features of automation and miniaturization. There are no review articles with the emphasis on sample preparations for the determination of catecholamine neurotransmitters in biological samples. Thus, this review aims to summarize recent progress and advances from 2015 to 2021, with emphasis on the sample preparation techniques combined with separation-based detection methods such capillary electrophoresis (CE) or liquid chromatography (LC) with various detectors. The current review manuscript would be helpful for the researchers with their research interests in diagnostic analysis and biological systems to choose suitable sample pretreatment and detection methods. Full article

(This article belongs to the Special Issue Recent Advances and Future Trends in Sample Preparation)

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24 pages, 1066 KiB

Open AccessReview

Deep Eutectic Solvents as Promising Green Solvents in Dispersive Liquid–Liquid Microextraction Based on Solidification of Floating Organic Droplet: Recent Applications, Challenges and Future Perspectives

by Asmaa Kamal El-Deen and Kuniyoshi Shimizu

Molecules 2021, 26(23), 7406; https://doi.org/10.3390/molecules26237406 - 06 Dec 2021

Cited by 28 | Viewed by 3628

Abstract

Deep eutectic solvents (DESs) have recently attracted attention as a promising green alternative to conventional hazardous solvents by virtue of their simple preparation, low cost, and biodegradability. Even though the application of DESs in analytical chemistry is still in its early stages, the number of publications on this topic is growing. Analytical procedures applying dispersive liquid–liquid microextraction based on the solidification of floating organic droplets (DLLME-SFOD) are among the more appealing approaches where DESs have been found to be applicable. Herein, we provide a summary of the articles that are concerned with the application of DESs in the DLLME-SFOD of target analytes from diverse samples to provide up-to-date knowledge in this area. In addition, the major variables influencing enrichment efficiency and the microextraction mechanism are fully investigated and explained. Finally, the challenges and future perspectives of applying DESs in DLLME-SFOD are thoroughly discussed and are critically analyzed. Full article

(This article belongs to the Special Issue Recent Advances and Future Trends in Sample Preparation)

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