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New Materials in Microextraction Techniques

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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 (31 March 2020) | Viewed by 20562

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Prof. Dr. Rafael Lucena

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Guest Editor

School of Pharmacy, National and Kapodistrian University of Athens, 157 71 Athens, Greece
Interests: sample preparation; microextraction; nanoparticles and ionic liquid
Special Issues, Collections and Topics in MDPI journals

Prof. Dr. Soledad Cárdenas

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Departamento de Química Analítica, Instituto Universitario de Investigación en Química Fina y Nanoquímica, Universidad de Córdoba, Campus de Rabanales, Edificio Marie Curie, E-14071 Córdoba, España
Interests: sample preparation; microextraction; nanoparticles and ionic liquid

Dr. Guillermo Lasarte Aragonés

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Guest Editor

Instituto Universitario de Nanoquímica (IUNAN), University of Cordoba, 14071 Cordoba, Spain
Interests: microextraction; switchable solvents; biorecognition (DNA, peptides and hybrid materials) to improve the Analytical Process

Special Issue Information

Dear Colleagues,

Sample preparation has been the focus of continuous research over the last two decades. Microextraction techniques, originated in this evolution, are powerful tools for analysists and they are applied, not only in research laboratories, but also in routine ones. Microextraction techniques, among other characteristics, are based on the reduction of the amount/volume of the extractant phases. In this scenario, the efficiency and selectivity of the applied materials are key. Additionally, the environmental and safety connotations of the novel extractant phases are deeply considered in the new developments.

The present Special Issue is focused on new materials, including sorbents and solvents, in microextraction techniques. The description of novel sorptive materials is warmly encouraged. In addition, the application of novel, but already proposed, materials (e.g., nanoparticles, composites, ionic liquids or switchable solvents) is welcome if they are applied for the resolution of new/important analytical problems in different fields.

Prof. Dr. Rafael Lucena
Prof. Dr. Soledad Cárdenas
Dr. Guillermo Lasarte Aragonés
Guest Editors

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Keywords

microextraction
polymers
nanoparticles
new solvents

Published Papers (6 papers)

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Research

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12 pages, 1412 KiB

Open AccessArticle

Application of Switchable Hydrophobicity Solvents for Extraction of Emerging Contaminants in Wastewater Samples

by Guillermo Lasarte-Aragonés, Alejandro Álvarez-Lueje, Ricardo Salazar and Carla Toledo-Neira

Molecules 2020, 25(1), 86; https://doi.org/10.3390/molecules25010086 - 25 Dec 2019

Cited by 15 | Viewed by 2545

Abstract

In the present work, the effectiveness of switchable hydrophobicity solvents (SHSs) as extraction solvent (N,N-Dimethylcyclohexylamine (DMCA), N,N-Diethylethanamine (TEA), and N,N-Benzyldimethylamine (DMBA)) for a variety of emerging pollutants was evaluated. Different pharmaceutical products (nonsteroidal anti-inflammatory drugs (NSAIDs), hormones, and triclosan) were selected as target analytes, covering a range of hydrophobicity (LogP) of 3.1 to 5.2. The optimized procedure was used for the determination of the target pharmaceutical analytes in wastewater samples as model analytical problem. Absolute extraction recoveries were in the range of 51% to 103%. The presented method permits the determination of the target analytes at the low ng mL⁻¹ level, ranging from 0.8 to 5.9 (except for Triclosan, 106 ng mL⁻¹) with good precision (relative standard deviation lower than 6%) using high-pressure liquid chromatography (HPLC) combined with ultraviolet (DAD) and fluorescence (FLR) detection. The microextraction alternative resulted in a fast, simple, and green method for a wide variety of analytes in environmental water sample. The results suggest that this type of solvent turns out to be a great alternative for the determination of different analytes in relatively complex water samples. Full article

(This article belongs to the Special Issue New Materials in Microextraction Techniques)

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13 pages, 1475 KiB

Open AccessArticle

Magnetic Polyamide Nanocomposites for the Microextraction of Benzophenones from Water Samples

by Hoda Ghambari, Emilia M. Reyes-Gallardo, Rafael Lucena, Mohammad Saraji and Soledad Cárdenas

Molecules 2019, 24(5), 953; https://doi.org/10.3390/molecules24050953 - 08 Mar 2019

Cited by 6 | Viewed by 2399

Abstract

In this article, the influence of the monomers on the extraction efficiency and the effect of the addition of surfactants during the synthesis have also been considered. The sorption capacity of the resulting nanocomposites has been evaluated, in the dispersive micro-solid phase extraction format, by determining that of six benzophenones in water using ultra performance liquid chromatography (UPLC) combined with photodiode array detection. Under the optimum conditions, the limits of detection were in the range of 0.5–4.3 ng/mL and the repeatability, expressed as the relative standard deviation (RSD), varied between 1.5% and 5.6%. The proposed method has been applied for the analysis of real water samples, providing relative recoveries in the interval of 84–105% Full article

(This article belongs to the Special Issue New Materials in Microextraction Techniques)

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17 pages, 3000 KiB

Open AccessFeature PaperArticle

Application of a Pillared-Layer Zn-Triazolate Metal-Organic Framework in the Dispersive Miniaturized Solid-Phase Extraction of Personal Care Products from Wastewater Samples

by Providencia González-Hernández, Ana B. Lago, Jorge Pasán, Catalina Ruiz-Pérez, Juan H. Ayala, Ana M. Afonso and Verónica Pino

Molecules 2019, 24(4), 690; https://doi.org/10.3390/molecules24040690 - 15 Feb 2019

Cited by 20 | Viewed by 3812

Abstract

The pillared-layer Zn-triazolate metal-organic framework (CIM-81) was synthesized, characterized, and used for the first time as a sorbent in a dispersive micro-solid phase extraction method. The method involves the determination of a variety of personal care products in wastewaters, including four preservatives, four UV-filters, and one disinfectant, in combination with ultra-high performance liquid chromatography and UV detection. The CIM-81 MOF, constructed with an interesting mixed-ligand synthetic strategy, demonstrated a better extraction performance than other widely used MOFs in D-µSPE such as UiO-66, HKUST-1, and MIL-53(Al). The optimization of the method included a screening design followed by a Doehlert design. Optimum conditions required 10 mg of CIM-81 MOF in 10 mL of the aqueous sample at a pH of 5, 1 min of agitation by vortex and 3 min of centrifugation in the extraction step; and 1.2 mL of methanol and 4 min of vortex in the desorption step, followed by filtration, evaporation and reconstitution with 100 µL of the initial chromatographic mobile phase. The entire D-µSPE-UHPLC-UV method presented limits of detection down to 0.5 ng·mL⁻¹; intra-day and inter-day precision values for the lowest concentration level (15 ng·mL⁻¹)-as a relative standard deviation (in %)-lower than 8.7 and 13%, respectively; average relative recovery values of 115%; and enrichment factors ranging from ~3.6 to ~34. The reuse of the CIM-81 material was assessed not only in terms of maintaining the analytical performance but also in terms of its crystalline stability. Full article

(This article belongs to the Special Issue New Materials in Microextraction Techniques)

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14 pages, 1636 KiB

Open AccessArticle

Solvent Bar Micro-Extraction of Heavy Metals from Natural Water Samples Using 3-Hydroxy-2-Naphthoate-Based Ionic Liquids

by Philip Pirkwieser, José A. López-López, Wolfgang Kandioller, Bernhard K. Keppler, Carlos Moreno and Franz Jirsa

Molecules 2018, 23(11), 3011; https://doi.org/10.3390/molecules23113011 - 17 Nov 2018

Cited by 14 | Viewed by 3581

Abstract

Developments in the liquid micro-extraction of trace metals from aqueous phases have proven to be limited when extended from pure water to more complex and demanding matrices such as sea water or wastewater treatment effluents. To establish a system that works under such matrices, we successfully tested three task-specific ionic liquids, namely trihexyltetradecyl- phosphonium-, methyltrioctylphosphonium- and methyltrioctylammonium 3-hydroxy-2-naphthoate in two-phase solvent bar micro-extraction (SBME) experiments. We describe the influence of pH, organic additives, time, stirring rate and volume of ionic liquid for multi-elemental micro-extraction of Cu, Ag, Cd and Pb from various synthetic and natural aqueous feed solutions. Highest extraction for all metals was achieved at pH 8.0. Minimal leaching of the ionic liquids into the aqueous phase was demonstrated, with values < 30 mg L⁻¹ DOC in all cases. Sample salinities of up to 60 g L⁻¹ NaCl had a positive effect on the extraction of Cd, possibly due to an efficient extraction mechanism of the present chlorido complexes. In metal-spiked natural feed solutions, the selected SBME setups showed unchanged stability under all conditions tested. We could efficiently (≥85%) extract Cu and Ag from drinking water and achieved high efficacies for Ag and Cd from natural sea water and hypersaline water, respectively. The method presented here proves to be a useful tool for an efficient SBME of heavy metals from natural waters without the need to pretreat or modify the sample. Full article

(This article belongs to the Special Issue New Materials in Microextraction Techniques)

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Review

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25 pages, 666 KiB

Open AccessReview

Use of Nanomaterial-Based (Micro)Extraction Techniques for the Determination of Cosmetic-Related Compounds

by José Grau, Juan L. Benedé and Alberto Chisvert

Molecules 2020, 25(11), 2586; https://doi.org/10.3390/molecules25112586 - 02 Jun 2020

Cited by 8 | Viewed by 3243

Abstract

The high consumer demand for cosmetic products has caused the authorities and the industry to require rigorous analytical controls to assure their safety and efficacy. Thus, the determination of prohibited compounds that could be present at trace level due to unintended causes is increasingly important. Furthermore, some cosmetic ingredients can be percutaneously absorbed, further metabolized and eventually excreted or bioaccumulated. Either the parent compound and/or their metabolites can cause adverse health effects even at trace level. Moreover, due to the increasing use of cosmetics, some of their ingredients have reached the environment, where they are accumulated causing harmful effects in the flora and fauna at trace levels. To this regard, the development of sensitive analytical methods to determine these cosmetic-related compounds either for cosmetic control, for percutaneous absorption studies or for environmental surveillance monitoring is of high interest. In this sense, (micro)extraction techniques based on nanomaterials as extraction phase have attracted attention during the last years, since they allow to reach the desired selectivity. The aim of this review is to provide a compilation of those nanomaterial-based (micro)extraction techniques for the determination of cosmetic-related compounds in cosmetic, biological and/or environmental samples spanning from the first attempt in 2010 to the present. Full article

(This article belongs to the Special Issue New Materials in Microextraction Techniques)

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31 pages, 3842 KiB

Open AccessFeature PaperReview

New Advanced Materials and Sorbent-Based Microextraction Techniques as Strategies in Sample Preparation to Improve the Determination of Natural Toxins in Food Samples

by Natalia Casado, Judith Gañán, Sonia Morante-Zarcero and Isabel Sierra

Molecules 2020, 25(3), 702; https://doi.org/10.3390/molecules25030702 - 06 Feb 2020

Cited by 40 | Viewed by 4397

Abstract

Natural toxins are chemical substances that are not toxic to the organisms that produce them, but which can be a potential risk to human health when ingested through food. Thus, it is of high interest to develop advanced analytical methodologies to control the occurrence of these compounds in food products. However, the analysis of food samples is a challenging task because of the high complexity of these matrices, which hinders the extraction and detection of the analytes. Therefore, sample preparation is a crucial step in food analysis to achieve adequate isolation and/or preconcentration of analytes and provide suitable clean-up of matrix interferences prior to instrumental analysis. Current trends in sample preparation involve moving towards “greener” approaches by scaling down analytical operations, miniaturizing the instruments and integrating new advanced materials as sorbents. The combination of these new materials with sorbent-based microextraction technologies enables the development of high-throughput sample preparation methods, which improve conventional extraction and clean-up procedures. This review gives an overview of the most relevant analytical strategies employed for sorbent-based microextraction of natural toxins of exogenous origin from food, as well as the improvements achieved in food sample preparation by the integration of new advanced materials as sorbents in these microextraction techniques, giving some relevant examples from the last ten years. Challenges and expected future trends are also discussed. Full article

(This article belongs to the Special Issue New Materials in Microextraction Techniques)

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