Special Issue "Advances in Solid-Phase Microextraction"

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

Deadline for manuscript submissions: 20 October 2019.

Special Issue Editors

Dr. Attilio Naccarato
E-Mail Website
Guest Editor
Institute of Atmospheric Pollution Research - Italian National Research Council, Italy
Interests: sample preparation; analytical separations; mass spectrometry; gas chromatography; inductively coupled plasma mass spectrometry; microextraction techniques; microextraction by packed sorbent (MEPS); solid-phase microextraction (SPME); food analysis; environmental analysis; bioclinical analysis
Prof. Antonio Tagarelli
E-Mail Website
Guest Editor
Department of Chemistry and Chemical Technologies, University of Calabria, Italy
Interests: sample preparation, microextraction techniques, gas chromatography, mass spectrometry, chemometrics, experimental design, derivatization, environmental analysis, analytical clinical chemistry

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 papers will be 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 quarterly 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 1000 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

Published Papers (2 papers)

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Research

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Open AccessArticle
Exploring New Extractive Phases for In-Tube Solid Phase Microextraction Coupled to Miniaturized Liquid Chromatography
Separations 2019, 6(1), 12; https://doi.org/10.3390/separations6010012 - 25 Feb 2019
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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Open AccessReview
Metal–Organic Frameworks as Key Materials for Solid-Phase Microextraction Devices—A Review
Separations 2019, 6(4), 47; https://doi.org/10.3390/separations6040047 - 02 Oct 2019
Cited by 1
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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Planned Papers

The below list represents only planned manuscripts. Some of these manuscripts have not been received by the Editorial Office yet. Papers submitted to MDPI journals are subject to peer-review.

Paper Title: New extractive phases for in-tube solid phase microextraction coupled to miniaturized liquid chromatography
Authors: Pascual Serra-Mora, Paola García-Narbona, Jorge Verdú-Andrés, Rosa Herráez-Hernández*, Pilar Campíns-Falcó *
Affiliation: MINTOTA Research Group, Department of Analytical Chemistry, Faculty of Chemistry, University of Valencia, Dr Moliner 50, 46100 Burjassot, Valencia, Spain
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 selectivity of the extraction is highly desirable. In this respect, the employment of capillary columns coated with sorbents functionalized with nanoparticles (NPs) in replacement of the loop of the injection valve (in-valve IT-SPME) is one of the most attractive options. In this work, different polymers of tetraethyl-orthosilicate (TEOS) and trimethoxyethylsilane (MTEOS) modified with SiO2 and TiO2 NPs have been synthetized and used for IT-SPME of a variety of water pollutants, using both capillary-LC and nano-LC. Compounds with different chemical structures and polarities such as polycyclic aromatic hydrocarbons (PAHs), and phenylurea and organophosphorous herbicides have been used as target analytes. The extraction efficiencies found with the synthetized capillaries have been compared with those obtained with commercially available capillaries coated with polydimethylsiloxane (PDMS), nitroterephthalic acid modified polyetilenglicol (FFAP) and polystyrene-divinylbenzene (PS-DVB) phases. The results obtained showed that, although PS-DVB phase has the strongest affinity for PAHs, TEOS-MTEOS coatings modified with NPs is the best option for a majority of the tested compounds, providing limits of detection ≤ 2 µg/L for most of them. Examples of application are given.

Title: Metal-Organic Fameworks: Highly Ordered Tnable Materials in SolidPhase Microextraction – A review
Authors: Adrián Gutiérrez-Serpa 1, Idaira Pacheco-Fernández 1, Jorge Pasán 2, Verónica Pino *,1,3
Affiliation:
1 Departamento de Química, Unidad Departamental de Química Analítica, Universidad de La Laguna (ULL), La Laguna (Tenerife), 38206, Spain
2 Departamento de Física, Laboratorio de Rayos X y Materiales Moleculares, Universidad de La Laguna, La Laguna (Tenerife), Spain
3 University Institute of Tropical Diseases and Public Health, Universidad de La Laguna (ULL), La Laguna, Tenerife, 38206 Spain
Correspondence: [email protected]; (+34) 922318990
Abstract: In the past few years, metal-organic frameworks (MOFs) have attracted considerable attention in analytical sample preparation, particularly when used as novel coatings in solid-phase microextraction (SPME). MOFs are highly ordered porous crystalline three-dimensional 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 and outstanding 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 promising materials in SPME. This review offers an overview on the current state of the use of MOFs as coatings in the different SPME configurations, their preparation and applicability to real complex samples analysis, together with an analytical performance comparison with commercially available SPME coatings.
Keywords: solid-phase microextraction, metal-organic framework, crystalline nanostructures, nanomaterials, analytical chemistry, coatings

Title: Low-Cost Quantitation of Multiple Volatile Organic Compounds in Ar Using Solid-Phase Microextraction
Authors: Olga P. Ibragimova, Nassiba Baimatova, Bulat Kenessov*
Affiliation: Al-Farabi Kazakh National University, Center of Physical Chemical Methods of Research and Analysis, Almaty, Kazakhstan
Correspondence: ; Tel: +7727-2390624; Fax: +7727-2923731
Abstract: Current standard approaches for quantification of volatile organic compounds (VOCs) in air are labor-intensive and require additional equipment. Solid-phase microextraction (SPME) is a simpler alternative, however, there are only methods for simultaneous quantification of few VOCs. The aim of this study was to develop simple, automated and accurate method for quantitation of >20 VOCs in 20-mL ambient air samples using SPME and gas chromatography-mass spectrometry. Twenty-six VOCs were chosen for the method development. It has been proven that air samples can be stored in 20-mL crimp vials during 48 h without significant losses of all chosen analytes. The fiber selection was made to achieve desired detection limits and relative standard deviations of slopes of calibration plots <10% for the greatest number of analytes. Extraction and desorption time were optimized for greatest responses of chosen analytes. The developed method was tested for automated quantification of VOCs in outdoor air samples collected in Almaty, Kazakhstan.

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