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Special Issue "Solid-Phase Microextraction"

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

Deadline for manuscript submissions: 31 December 2018

Special Issue Editors

Guest Editor
Dr. Constantinos K. Zacharis

Analytical Development Laboratory, Research and Development API Operations, Pharmathen SA, 9th klm Thessaloniki-Thermi, Thessaloniki 57001, Greece
E-Mail
Interests: pharmaceutical analytical chemistry; food analytical chemistry; method development and validation; sample preparation (derivatization, microextraction, etc.); liquid and gas chromatography; capillary electrophoresis
Guest Editor
Assist. Prof. Paraskevas D. Tzanavaras

Laboratory of Analytical Chemistry, Department of Chemistry, Aristotle University of Thessaloniki, Greece
Website | E-Mail
Phone: +30 2310997721
Interests: flow injection analysis; sequential injection analysis; separation techniques (HPLC, CE); post-column derivatization; microextraction

Special Issue Information

Dear Colleagues,

Almost twenty-five years after its introduction, fiber solid phase microextraction (SPME) is undoubtedly a mature sample preparation technique, with numerous applications in various scientific fields. Due to its versatility, reliability, low cost, and sampling convenience (on-site sampling), SPME has been widely used in combination with separation techniques (LC, GC, CE) in academic research and routine analysis as well. As a result of its impact, it has been introduced in several official methods. On-going research and new trends on SPME covers various aspects including, but not limited to, the manufacturing of new fiber coating materials, new designs (in-needle, in-tube, in-tube, etc.), incorporation of SPME in automated systems, etc.

The present Special Issue aims to cover the latest research trends and applications on to SPME. Researchers working on, but not limited, fiber coating technology, on-line automated SPME and their applications in food, enviromental and biomedical sciences are cordially invited to contribute a research or review article in this Special Issue.

Dr. Constantinos K. Zacharis
Dr. Paraskevas D. Tzanavaras
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. Molecules 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 1800 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
  • headspace solid phase microextraction
  • on-fiber derivatization
  • on-site sampling
  • in-needle SPME
  • in-tube SPME
  • multiple extraction
  • automation
  • SPME coupling to various analytical systems-Instrumentation

Published Papers (4 papers)

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Research

Open AccessFeature PaperArticle Analysis of Contact Traces of Cannabis by In-Tube Solid-Phase Microextraction Coupled to Nanoliquid Chromatography
Molecules 2018, 23(9), 2359; https://doi.org/10.3390/molecules23092359
Received: 12 August 2018 / Revised: 6 September 2018 / Accepted: 13 September 2018 / Published: 15 September 2018
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Abstract
Because of its inherent qualities, in-tube solid-phase microextraction (IT-SPME) coupled on-line to nanoliquid chromatography (nanoLC) can be a very powerful tool to address the new challenges of analytical laboratories such as the analysis of traces of complex samples. This is the case of
[...] Read more.
Because of its inherent qualities, in-tube solid-phase microextraction (IT-SPME) coupled on-line to nanoliquid chromatography (nanoLC) can be a very powerful tool to address the new challenges of analytical laboratories such as the analysis of traces of complex samples. This is the case of the detection of contact traces of drugs, especially cannabis. The main difficulties encountered in the analysis of traces of cannabis plants on surfaces are the low amount of sample available (typically < 1 mg), the complexity of the matrix, and the low percentages of cannabinoic compounds in the samples. In this work, a procedure is described for the detection of residues of cannabis on different surfaces based on the responses obtained by IT-SPME coupled to nanoLC with UV diode array detection (DAD) for the cannabinoids Δ9-tetrahydrocannabinol (THC), cannabidiol (CBD), and cannabinol (CBN); the proposed conditions can also be applied for quantitative purposes through the measurement of the percentage of THC, the most abundant cannabinoid in plants. The method is based on collecting the suspected drug samples with cotton swabs, followed by the extraction of the target compounds by ultrasound assisted extraction. The extracts are then separated and processed by IT-SPME-nanoLC. The proposed approach has been applied to the detection of traces of cannabis in different kind of items (plastic bags, office paper, aluminum foil, cotton cloths, and hand skin). Sample amounts as low as 0.08 mg have been collected and analysed for THC. The selectivity and effect of the storage conditions on the levels of THC have also been evaluated. The percentages of THC in the samples typically ranged from 0.6% to 2.8%, which means that amounts of this compound as low as 1–2 µg were adequately detected and quantified. For the first time, the reliability of IT-SPME-nanoLC for the analysis of complex matrices such as cannabis plant extracts has been demonstrated. Full article
(This article belongs to the Special Issue Solid-Phase Microextraction)
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Open AccessArticle High-Throughput Analysis of Selected Urinary Hydroxy Polycyclic Aromatic Hydrocarbons by an Innovative Automated Solid-Phase Microextraction
Molecules 2018, 23(8), 1869; https://doi.org/10.3390/molecules23081869
Received: 22 June 2018 / Revised: 16 July 2018 / Accepted: 26 July 2018 / Published: 26 July 2018
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Abstract
High-throughput screening of samples is the strategy of choice to detect occupational exposure biomarkers, yet it requires a user-friendly apparatus that gives relatively prompt results while ensuring high degrees of selectivity, precision, accuracy and automation, particularly in the preparation process. Miniaturization has attracted
[...] Read more.
High-throughput screening of samples is the strategy of choice to detect occupational exposure biomarkers, yet it requires a user-friendly apparatus that gives relatively prompt results while ensuring high degrees of selectivity, precision, accuracy and automation, particularly in the preparation process. Miniaturization has attracted much attention in analytical chemistry and has driven solvent and sample savings as easier automation, the latter thanks to the introduction on the market of the three axis autosampler. In light of the above, this contribution describes a novel user-friendly solid-phase microextraction (SPME) off- and on-line platform coupled with gas chromatography and triple quadrupole-mass spectrometry to determine urinary metabolites of polycyclic aromatic hydrocarbons 1- and 2-hydroxy-naphthalene, 9-hydroxy-phenanthrene, 1-hydroxy-pyrene, 3- and 9-hydroxy-benzoantracene, and 3-hydroxy-benzo[a]pyrene. In this new procedure, chromatography’s sensitivity is combined with the user-friendliness of N-tert-butyldimethylsilyl-N-methyltrifluoroacetamide on-fiber SPME derivatization using direct immersion sampling; moreover, specific isotope-labelled internal standards provide quantitative accuracy. The detection limits for the seven OH-PAHs ranged from 0.25 to 4.52 ng/L. Intra-(from 2.5 to 3.0%) and inter-session (from 2.4 to 3.9%) repeatability was also evaluated. This method serves to identify suitable risk-control strategies for occupational hygiene conservation programs. Full article
(This article belongs to the Special Issue Solid-Phase Microextraction)
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Open AccessArticle Discrimination of Aroma Characteristics for Cubeb Berries by Sensomics Approach with Chemometrics
Molecules 2018, 23(7), 1627; https://doi.org/10.3390/molecules23071627
Received: 14 June 2018 / Revised: 28 June 2018 / Accepted: 2 July 2018 / Published: 4 July 2018
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Abstract
The dried cubeb berries are widely used as medicinal herb and spicy condiment with special flavor. However, there is a significant definition discrepancy for cubeb berries. In this study, an efficient analytical method to characterize and discriminate two popular cubeb fruits (Litsea
[...] Read more.
The dried cubeb berries are widely used as medicinal herb and spicy condiment with special flavor. However, there is a significant definition discrepancy for cubeb berries. In this study, an efficient analytical method to characterize and discriminate two popular cubeb fruits (Litsea cubeba and Piper cubeba) was established. The aroma profiles of cubeb berries were evaluated by different extraction methods including hydro-distillation, simultaneous distillation/extraction, and solid-phase micro-extraction followed by gas chromatography-mass spectrometry-olfactometry (GC-MS-O). In total, 90 volatile compounds were identified by HD, SDE, and SPME combined with GC-MS. Principal component analysis was further applied and discriminated ambiguous cubeb berries by their unique aromas: Litsea cubeba was characterized by higher level of d-limonene (“fruit, citrus”), citral (“fruit, lemon”) and dodecanoic acid; α-cubebene (“herb”) was identified as a marker compound for Piper cubeba with higher camphor (“camphoraceous”), and linalool (“flower”). Flavor fingerprint combined with PCA could be applied as a promising method for identification of cubeb fruits and quality control for food and medicinal industries. Full article
(This article belongs to the Special Issue Solid-Phase Microextraction)
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Graphical abstract

Open AccessArticle Analysis of the Volatile Profile of Core Chinese Mango Germplasm by Headspace Solid-Phase Microextraction Coupled with Gas Chromatography-Mass Spectrometry
Molecules 2018, 23(6), 1480; https://doi.org/10.3390/molecules23061480
Received: 9 May 2018 / Revised: 8 June 2018 / Accepted: 13 June 2018 / Published: 19 June 2018
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Abstract
Despite abundant published research on the volatile characterization of mango germplasm, the aroma differentiation of Chinese cultivars remains unclear. Using headspace solid phase microextraction (HS-SPME) coupled with gas chromatography–mass spectrometry (GC-MS), the composition and relative content of volatiles in 37 cultivars representing the
[...] Read more.
Despite abundant published research on the volatile characterization of mango germplasm, the aroma differentiation of Chinese cultivars remains unclear. Using headspace solid phase microextraction (HS-SPME) coupled with gas chromatography–mass spectrometry (GC-MS), the composition and relative content of volatiles in 37 cultivars representing the diversity of Chinese mango germplasm were investigated. Results indicated that there are distinct differences in the components and content of volatile compounds among and within cultivars. In total, 114 volatile compounds, including 23 monoterpenes, 16 sesquiterpenes, 29 non-terpene hydrocarbons, 25 esters, 11 aldehydes, five alcohols and five ketones, were identified. The total volatile content among cultivars ranged from 211 to 26,022 μg/kg fresh weight (FW), with 123-fold variation. Terpene compounds were the basic background volatiles, and 34 cultivars exhibited abundant monoterpenes. On the basis of hierarchical cluster analysis (HCA) and principal component analysis (PCA), terpinolene and α-pinene were important components constituting the aroma of Chinese mango cultivars. Most obviously, a number of mango cultivars with high content of various aroma components were observed, and they can serve as potential germplasms for both breeding and direct use. Full article
(This article belongs to the Special Issue Solid-Phase Microextraction)
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Graphical abstract

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