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Separations
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Advances in Solid-Phase Microextraction
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Advances in Solid-Phase Microextraction

A special issue of Separations (ISSN 2297-8739).

Deadline for manuscript submissions: closed (20 October 2019) | Viewed by 41089

Printed Edition Available!
A printed edition of this Special Issue is available here.

Special Issue Editors

Dr. Attilio Naccarato

E-Mail Website1 Website2
Guest Editor
Department of Chemistry and Chemical Technologies, University of Calabria, Arcavacata, Italy
Interests: analytical chemistry; sample preparation; microextraction techniques; method optimization; environmental analytical chemistry
Special Issues, Collections and Topics in MDPI journals
Prof. Dr. Antonio Tagarelli

E-Mail Website
Guest Editor
Department of Chemistry and Chemical Technologies, University of Calabria, 87036 Arcavacata, Rende CS, Italy
Interests: sample preparation; microextraction techniques; gas chromatography; mass spectrometry; chemometrics; experimental design; derivatization; environmental analysis; analytical clinical chemistry
Special Issues, Collections and Topics in MDPI journals

Special Issue Information

Dear Colleagues,

Analysis imposes substantial challenges, especially when dealing with analytes present at trace levels in complex matrices. Although modern instrumentation has simplified analyses and makes them more reliable, its use is only the last step of the whole analytical process. On the other hand, sample preparation still represents the bottleneck in many analytical methods and often requires the use of extensive protocols before instrumental analysis.

Solid-phase microextraction (SPME) is a well-established sample-prep technique for simultaneous extraction and pre-concentration of compounds from a variety of matrices. Given the simplicity, versatility, and availability of different formats, SPME addresses several challenges associated with the traditional sample preparation approaches and allows for a substantial streamlining of the analytical workflow.

In this Special Issue we would like to invite colleagues to contribute original research papers and review articles addressing recent advances in the applications of solid-phase microextraction.

Dr. Attilio Naccarato
Prof. Antonio Tagarelli
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. 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

  • solid-phase microextraction (SPME)
  • microextraction techniques
  • sample preparation
  • chromatographic techniques

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Published Papers (7 papers)

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Editorial

Jump to: Research, Review

4 pages, 196 KiB  
Editorial
Advances in Solid-Phase Microextraction
by Attilio Naccarato and Antonio Tagarelli
Separations 2020, 7(2), 34; https://doi.org/10.3390/separations7020034 - 12 Jun 2020
Viewed by 2900
Abstract
Analysis imposes substantial challenges, especially when dealing with analytes present at trace levels in complex matrices [...] Full article
(This article belongs to the Special Issue Advances in Solid-Phase Microextraction)

Research

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17 pages, 1180 KiB  
Article
Low-Cost Quantitation of Multiple Volatile Organic Compounds in Air Using Solid-Phase Microextraction
by Olga P. Ibragimova, Nassiba Baimatova and Bulat Kenessov
Separations 2019, 6(4), 51; https://doi.org/10.3390/separations6040051 - 1 Nov 2019
Cited by 11 | Viewed by 4796
Abstract
Current standard approaches for quantitation of volatile organic compounds (VOCs) in outdoor air are labor-intensive and/or require additional equipment. Solid-phase microextraction (SPME) is a simpler alternative; however, its application is often limited by complex calibration, the need for highly pure gases and the [...] Read more.
Current standard approaches for quantitation of volatile organic compounds (VOCs) in outdoor air are labor-intensive and/or require additional equipment. Solid-phase microextraction (SPME) is a simpler alternative; however, its application is often limited by complex calibration, the need for highly pure gases and the lack of automation. Earlier, we proposed the simple, automated and accurate method for quantitation of benzene, toluene, ethylbenzene and xylenes (BTEX) in air using 20 mL headspace vials and standard addition calibration. The aim of present study was to expand this method for quantitation of >20 VOCs in air. Twenty-five VOCs were chosen for the method development. Polydimethylsiloxane/divinylbenzene (PDMS/DVB) fiber provided better combination of detection limits and relative standard deviations of calibration slopes than other studied fibers. Optimal extraction time was 10 min. For quantification of all analytes except n-undecane, crimp top vials with samples should not stand on the autosampler tray for >8 h, while 22 most stable analytes can be quantified during 24 h. The developed method was successfully tested for automated quantification of VOCs in outdoor air samples collected in Almaty, Kazakhstan. Relative standard deviations (RSDs) of the responses of 23 VOCs were below 15.6%. Toluene-to-benzene concentration ratios were below 1.0 in colder days, indicating that most BTEX originated from non-transport-related sources. Full article
(This article belongs to the Special Issue Advances in Solid-Phase Microextraction)
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12 pages, 7452 KiB  
Article
Exploring New Extractive Phases for In-Tube Solid Phase Microextraction Coupled to Miniaturized Liquid Chromatography
by Pascual Serra-Mora, Paola García-Narbona, Jorge Verdú-Andrés, Rosa Herráez-Hernández and Pilar Campíns-Falcó
Separations 2019, 6(1), 12; https://doi.org/10.3390/separations6010012 - 25 Feb 2019
Cited by 11 | Viewed by 3132
Abstract
In-tube solid-phase microextraction (IT-SPME) coupled on-line to miniaturized liquid chromatography (LC) has emerged as a powerful tool to address a variety of analytical problems. However, in order to expand its applicability, the development of new sorbents that enhance the efficiency and specificity of [...] Read more.
In-tube solid-phase microextraction (IT-SPME) coupled on-line to miniaturized liquid chromatography (LC) has emerged as a powerful tool to address a variety of analytical problems. However, in order to expand its applicability, the development of new sorbents that enhance the efficiency and specificity of the extraction is highly desirable. In this respect, the employment of capillary columns coated with sorbents functionalized with nanoparticles (NPs) replacing the loop of the injection valve (in-valve IT-SPME) is one of the most attractive options. In this work, polymers of tetraethyl orthosilicate (TEOS) and trimethoxyethylsilane (MTEOS) modified with SiO2 and TiO2 NPs have been synthetized and used for the extraction of a variety of water pollutants, using both Capillary-LC and Nano-LC. Compounds with different chemical structures and polarities such as the artificial sweetener saccharine, the polycyclic aromatic hydrocarbons (PAHs) naphthalene and fluoranthene, and some phenylurea and organophosphorous herbicides have been used as target analytes. The extraction efficiencies found with the synthetized capillaries have been compared to those obtained with commercially available capillaries coated with polydiphenyl-polydimethylsiloxane (PDMS), nitroterephthalic acid modified polyetilenglicol (FFAP), and polystyrene-divinylbenzene (PS-DVB) phases. The results obtained in this preliminary study showed that, although PS-DVB phase has the strongest affinity for compounds with two or more aromatic rings, the extraction with TEOS-MTEOS coatings modified with NPs is the best option for a majority of the tested compounds. Examples of application are given. Full article
(This article belongs to the Special Issue Advances in Solid-Phase Microextraction)
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Review

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28 pages, 3791 KiB  
Review
Recent Advances in In Vivo SPME Sampling
by Nicolò Riboni, Fabio Fornari, Federica Bianchi and Maria Careri
Separations 2020, 7(1), 6; https://doi.org/10.3390/separations7010006 - 15 Jan 2020
Cited by 14 | Viewed by 6013
Abstract
In vivo solid-phase microextraction (SPME) has been recently proposed for the extraction, clean-up and preconcentration of analytes of biological and clinical concern. Bioanalysis can be performed by sampling exo- or endogenous compounds directly in living organisms with minimum invasiveness. In this context, innovative [...] Read more.
In vivo solid-phase microextraction (SPME) has been recently proposed for the extraction, clean-up and preconcentration of analytes of biological and clinical concern. Bioanalysis can be performed by sampling exo- or endogenous compounds directly in living organisms with minimum invasiveness. In this context, innovative and miniaturized devices characterized by both commercial and lab-made coatings for in vivo SPME tissue sampling have been proposed, thus assessing the feasibility of this technique for biomarker discovery, metabolomics studies or for evaluating the environmental conditions to which organisms can be exposed. Finally, the possibility of directly interfacing SPME to mass spectrometers represents a valuable tool for the rapid quali- and quantitative analysis of complex matrices. This review article provides a survey of in vivo SPME applications focusing on the extraction of tissues, cells and simple organisms. This survey will attempt to cover the state-of- the-art from 2014 up to 2019. Full article
(This article belongs to the Special Issue Advances in Solid-Phase Microextraction)
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22 pages, 1517 KiB  
Review
Returning to Nature for the Design of Sorptive Phases in Solid-Phase Microextraction
by Gabriela Mafra, María Teresa García-Valverde, Jaime Millán-Santiago, Eduardo Carasek, Rafael Lucena and Soledad Cárdenas
Separations 2020, 7(1), 2; https://doi.org/10.3390/separations7010002 - 29 Dec 2019
Cited by 54 | Viewed by 5875
Abstract
Green analytical chemistry principles aim to minimize the negative impact of analytical procedures in the environment, which can be considered both at close (to ensure the safety of the analysts) and global (to conserve our natural resources) levels. These principles suggest, among other [...] Read more.
Green analytical chemistry principles aim to minimize the negative impact of analytical procedures in the environment, which can be considered both at close (to ensure the safety of the analysts) and global (to conserve our natural resources) levels. These principles suggest, among other guidelines, the reduction/minimization of the sample treatment and the use of renewable sources when possible. The first aspect is largely fulfilled by microextraction, which is considered to be among the greenest sample treatment techniques. The second consideration is attainable if natural products are used as raw materials for the preparation of new extraction phases. This strategy is in line with the change in our production system, which is being gradually moved from a linear model (take–make–dispose) to a circular one (including reusing and recycling as key terms). This article reviews the potential of natural products as sorbents in extraction and microextraction techniques from the synergic perspectives of two research groups working on the topic. The article covers the use of unmodified natural materials and the modified ones (although the latter has a less green character) to draw a general picture of the usefulness of the materials. Full article
(This article belongs to the Special Issue Advances in Solid-Phase Microextraction)
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44 pages, 2119 KiB  
Review
Recent Applications and Newly Developed Strategies of Solid-Phase Microextraction in Contaminant Analysis: Through the Environment to Humans
by Attilio Naccarato and Antonio Tagarelli
Separations 2019, 6(4), 54; https://doi.org/10.3390/separations6040054 - 6 Nov 2019
Cited by 30 | Viewed by 5270
Abstract
The present review aims to describe the recent and most impactful applications in pollutant analysis using solid-phase microextraction (SPME) technology in environmental, food, and bio-clinical analysis. The covered papers were published in the last 5 years (2014–2019) thus providing the reader with information [...] Read more.
The present review aims to describe the recent and most impactful applications in pollutant analysis using solid-phase microextraction (SPME) technology in environmental, food, and bio-clinical analysis. The covered papers were published in the last 5 years (2014–2019) thus providing the reader with information about the current state-of-the-art and the future potential directions of the research in pollutant monitoring using SPME. To this end, we revised the studies focused on the investigation of persistent organic pollutants (POPs), pesticides, and emerging pollutants (EPs) including personal care products (PPCPs), in different environmental, food, and bio-clinical matrices. We especially emphasized the role that SPME is having in contaminant surveys following the path that goes from the environment to humans passing through the food web. Besides, this review covers the last technological developments encompassing the use of novel extraction coatings (e.g., metal-organic frameworks, covalent organic frameworks, PDMS-overcoated fiber), geometries (e.g., Arrow-SPME, multiple monolithic fiber-SPME), approaches (e.g., vacuum and cold fiber SPME), and on-site devices. The applications of SPME hyphenated with ambient mass spectrometry have also been described. Full article
(This article belongs to the Special Issue Advances in Solid-Phase Microextraction)
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29 pages, 3934 KiB  
Review
Metal–Organic Frameworks as Key Materials for Solid-Phase Microextraction Devices—A Review
by Adrián Gutiérrez-Serpa, Idaira Pacheco-Fernández, Jorge Pasán and Verónica Pino
Separations 2019, 6(4), 47; https://doi.org/10.3390/separations6040047 - 2 Oct 2019
Cited by 89 | Viewed by 11933
Abstract
Metal–organic frameworks (MOFs) have attracted recently considerable attention in analytical sample preparation, particularly when used as novel sorbent materials in solid-phase microextraction (SPME). MOFs are highly ordered porous crystalline structures, full of cavities. They are formed by inorganic centers (metal ion atoms or [...] Read more.
Metal–organic frameworks (MOFs) have attracted recently considerable attention in analytical sample preparation, particularly when used as novel sorbent materials in solid-phase microextraction (SPME). MOFs are highly ordered porous crystalline structures, full of cavities. They are formed by inorganic centers (metal ion atoms or metal clusters) and organic linkers connected by covalent coordination bonds. Depending on the ratio of such precursors and the synthetic conditions, the characteristics of the resulting MOF vary significantly, thus drifting into a countless number of interesting materials with unique properties. Among astonishing features of MOFs, their high chemical and thermal stability, easy tuneability, simple synthesis, and impressive surface area (which is the highest known), are the most attractive characteristics that makes them outstanding materials in SPME. This review offers an overview on the current state of the use of MOFs in different SPME configurations, in all cases covering extraction devices coated with (or incorporating) MOFs, with particular emphases in their preparation. Full article
(This article belongs to the Special Issue Advances in Solid-Phase Microextraction)
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