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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 January 2019

Special Issue Editors

Guest Editor
Dr. Constantinos K. Zacharis

- Laboratory of Pharmaceutical Analysis, Department of Pharmaceutical Technology, School of Pharmacy, Aristotle University of Thessaloniki, Greece
- Analytical Development Laboratory, Research and Development API Operations, Pharmathen SA, 9th klm Thessaloniki-Thermi, Thessaloniki 57001, Greece
E-Mail
Interests: pharmaceutical analytical chemistry; method development and validation; sample preparation (derivatization, microextraction, etc); liquid and gas chromatography; capillary electrophoresis; mass spectrometry
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

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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 (10 papers)

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Research

Open AccessArticle GC-MS and HS-SPME-GC×GC-TOFMS Determination of the Volatile Composition of Essential Oils and Hydrosols (By-Products) from Four Eucalyptus Species Cultivated in Tuscany
Molecules 2019, 24(2), 226; https://doi.org/10.3390/molecules24020226
Received: 3 December 2018 / Revised: 31 December 2018 / Accepted: 4 January 2019 / Published: 9 January 2019
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Abstract
Essential oils are widely used as functional ingredients for potential multi-purpose functional uses. Hydrosols, co-products of the distillation of plant material, are used in food and cosmetic industries and in biological agriculture, but their volatile composition is poorly investigated. The volatile fractions of
[...] Read more.
Essential oils are widely used as functional ingredients for potential multi-purpose functional uses. Hydrosols, co-products of the distillation of plant material, are used in food and cosmetic industries and in biological agriculture, but their volatile composition is poorly investigated. The volatile fractions of essential oils and hydrosols from four less-studied 1,8-cineol-rich Eucalyptus species (E. parvula L.A.S. Johnson & K.D. Hill, E. cinerea F. Muell, E. pulverulenta Sims and E. pulverulenta baby blue Sims), cultivated in Tuscany in a system of organic farming, were characterized by solvent dilution (essential oils) or extraction (hydrosols) followed by GC-MS and by HS-SPME-GC×GC-TOFMS analysis. GC-MS analysis showed that essential oils were mainly constituted by oxygenated monoterpenes, particularly 1,8-cineole, with monoterpenes hydrocarbons up to 10.8%. Relative differences in the abundance of minor terpenes as limonene, α-pinene, γ-terpinene, p-cymene, terpinen-4-ol, α-terpineol, and alloaromandrene were pointed out and seem to be suitable for differentiation among EOs of the four different Eucalyptus species. Hydrosols of these species were characterized for the first time: they were mainly constituted by oxygenated monoterpenes (97.6–98.9%), with 1,8-cineole up to 1.6 g/L, while monoterpene and sesquiterpene hydrocarbons were detected only in traces. HS-SPME-GC×GC-TOFMS analysis also allowed providing metabolic profiling of hydrosols for the direct comparison and visualization of volatile components, pointing out the potentially different uses of these products as functional ingredients in food, beverage, and cosmetic industries. Full article
(This article belongs to the Special Issue Solid-Phase Microextraction)
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Open AccessCommunication Quantification of VOC Emissions from Carbonized Refuse-Derived Fuel Using Solid-Phase Microextraction and Gas Chromatography-Mass Spectrometry
Molecules 2018, 23(12), 3208; https://doi.org/10.3390/molecules23123208
Received: 14 November 2018 / Revised: 1 December 2018 / Accepted: 4 December 2018 / Published: 5 December 2018
PDF Full-text (241 KB) | HTML Full-text | XML Full-text | Supplementary Files
Abstract
In this work, for the first time, the volatile organic compound (VOC) emissions from carbonized refuse-derived fuel (CRDF) were quantified on a laboratory scale. The analyzed CRDF was generated from the torrefaction of municipal waste. Headspace solid-phase microextraction (SPME) and gas chromatography-mass spectrometry
[...] Read more.
In this work, for the first time, the volatile organic compound (VOC) emissions from carbonized refuse-derived fuel (CRDF) were quantified on a laboratory scale. The analyzed CRDF was generated from the torrefaction of municipal waste. Headspace solid-phase microextraction (SPME) and gas chromatography-mass spectrometry (GC-MS) was used to identify 84 VOCs, including many that are toxic, e.g., derivatives of benzene or toluene. The highest emissions were measured for nonanal, octanal, and heptanal. The top 10 most emitted VOCs contributed to almost 65% of the total emissions. The VOC mixture emitted from torrefied CRDF differed from that emitted by other types of pyrolyzed biochars, produced from different types of feedstock, and under different pyrolysis conditions. SPME was a useful technology for surveying VOC emissions. Results provide an initial database of the types and relative quantities of VOCs emitted from CRDF. This data is needed for further development of CRDF technology and comprehensive assessment of environmental impact and practical storage, transport, and potential adoption of CRDF as means of energy and resource recovery from municipal waste. Full article
(This article belongs to the Special Issue Solid-Phase Microextraction)
Open AccessArticle Skin Permeation of Solutes from Metalworking Fluids to Build Prediction Models and Test A Partition Theory
Molecules 2018, 23(12), 3076; https://doi.org/10.3390/molecules23123076
Received: 27 October 2018 / Revised: 21 November 2018 / Accepted: 23 November 2018 / Published: 24 November 2018
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Abstract
Permeation of chemical solutes through skin can create major health issues. Using the membrane-coated fiber (MCF) as a solid phase membrane extraction (SPME) approach to simulate skin permeation, we obtained partition coefficients for 37 solutes under 90 treatment combinations that could broadly represent
[...] Read more.
Permeation of chemical solutes through skin can create major health issues. Using the membrane-coated fiber (MCF) as a solid phase membrane extraction (SPME) approach to simulate skin permeation, we obtained partition coefficients for 37 solutes under 90 treatment combinations that could broadly represent formulations that could be associated with occupational skin exposure. These formulations were designed to mimic fluids in the metalworking process, and they are defined in this manuscript using: one of mineral oil, polyethylene glycol-200, soluble oil, synthetic oil, or semi-synthetic oil; at a concentration of 0.05 or 0.5 or 5 percent; with solute concentration of 0.01, 0.05, 0.1, 0.5, 1, or 5 ppm. A single linear free-energy relationship (LFER) model was shown to be inadequate, but extensions that account for experimental conditions provide important improvements in estimating solute partitioning from selected formulations into the MCF. The benefit of the Expanded Nested-Solute-Concentration LFER model over the Expanded Crossed-Factors LFER model is only revealed through a careful leave-one-solute-out cross-validation that properly addresses the existence of replicates to avoid an overly optimistic view of predictive power. Finally, the partition theory that accompanies the MCF approach is thoroughly tested and found to not be supported under complex experimental settings that mimic occupational exposure in the metalworking industry. Full article
(This article belongs to the Special Issue Solid-Phase Microextraction)
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Open AccessArticle Application of Direct Immersion Solid-Phase Microextraction (DI-SPME) for Understanding Biological Changes of Mediterranean Fruit Fly (Ceratitis capitata) During Mating Procedures
Molecules 2018, 23(11), 2951; https://doi.org/10.3390/molecules23112951
Received: 7 October 2018 / Revised: 7 November 2018 / Accepted: 9 November 2018 / Published: 12 November 2018
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Abstract
Samples from three different mating stages (before, during and after mating) of the Mediterranean fruit fly Ceratitis capitata were used in this experiment. Samples obtained from whole insects were subjected to extraction with the two mixtures of solvents (acetonitrile/water (A) and methanol/acetonitrile/water (B))
[...] Read more.
Samples from three different mating stages (before, during and after mating) of the Mediterranean fruit fly Ceratitis capitata were used in this experiment. Samples obtained from whole insects were subjected to extraction with the two mixtures of solvents (acetonitrile/water (A) and methanol/acetonitrile/water (B)) and a comparative study of the extractions using the different solvents was performed. Direct immersion-solid phase microextraction (DI-SPME) was employed, followed by gas chromatographic-mass spectrometry analyses (GC/MS) for the collection, separation and identification of compounds. The method was validated by testing its sensitivity, linearity and reproducibility. The main compounds identified in the three different mating stages were ethyl glycolate, α-farnesene, decanoic acid octyl ester, 2,6,10,15-tetramethylheptadecane, 11-tricosene, 9,12-(Z,Z)-octadecadienoic acid, methyl stearate, 9-(Z)-tricosene, 9,11-didehydro-lumisterol acetate; 1,54-dibromotetrapentacontane, 9-(Z)-hexadecenoic acid hexadecyl ester, 9-(E)-octadecenoic acid and 9-(Z)-hexadecenoic acid octadecyl ester. The novel findings indicated that compound compositions were not significantly different before and during mating. However, new chemical compounds were generated after mating, such as 1-iodododecane, 9-(Z)-tricosene and 11,13-dimethyl-12-tetradecen-1-acetate which were extracted with both (A) and (B) and dodecanoic acid, (Z)-oleic acid, octadecanoic acid and hentriacontane which were extracted with (A) and ethyl glycolate, 9-hexadecenoic acid hexadecyl ester, palmitoleic acid and 9-(E)-octadecenoic acid, which were extracted with solvent (B). This study has demonstrated that DI-SPME is useful in quantitative insect metabolomics by determining changes in the metabolic compounds in response to mating periods. DI-SPME chemical extraction technology might offer analysis of metabolites that could potentially enhance our understanding on the evolution of the medfly. Full article
(This article belongs to the Special Issue Solid-Phase Microextraction)
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Open AccessArticle Volatile Terpenes and Terpenoids from Workers and Queens of Monomorium chinense (Hymenoptera: Formicidae)
Molecules 2018, 23(11), 2838; https://doi.org/10.3390/molecules23112838
Received: 8 October 2018 / Revised: 24 October 2018 / Accepted: 27 October 2018 / Published: 1 November 2018
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Abstract
Twenty-one volatile terpenes and terpenoids were found in Monomorium chinense Santschi (Hymenoptera: Formicidae), a native Chinese ant, by using headspace solid-phase microextraction (HS-SPME) coupled with gas-phase chromatography and mass spectrometry (GC-MS), which makes this ant one of the most prolific terpene producers in
[...] Read more.
Twenty-one volatile terpenes and terpenoids were found in Monomorium chinense Santschi (Hymenoptera: Formicidae), a native Chinese ant, by using headspace solid-phase microextraction (HS-SPME) coupled with gas-phase chromatography and mass spectrometry (GC-MS), which makes this ant one of the most prolific terpene producers in insect. A sesquiterpene with unknown structure (terpene 1) was the main terpene in workers and neocembrene in queens. Terpenes and terpenoids were detected in poison, Dufour’s and mandibular glands of both workers and queens. Worker ants raised on a terpene-free diet showed the same terpene profile as ants collected in the field, indicating that de novo terpene and terpenoid synthesis occurs in M. chinense. Full article
(This article belongs to the Special Issue Solid-Phase Microextraction)
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Open AccessArticle Optimization of Time-Weighted Average Air Sampling by Solid-Phase Microextraction Fibers Using Finite Element Analysis Software
Molecules 2018, 23(11), 2736; https://doi.org/10.3390/molecules23112736
Received: 15 September 2018 / Revised: 9 October 2018 / Accepted: 15 October 2018 / Published: 23 October 2018
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Abstract
Determination of time-weighted average (TWA) concentrations of volatile organic compounds (VOCs) in air using solid-phase microextraction (SPME) is advantageous over other sampling techniques, but is often characterized by insufficient accuracies, particularly at longer sampling times. Experimental investigation of this issue and disclosing the
[...] Read more.
Determination of time-weighted average (TWA) concentrations of volatile organic compounds (VOCs) in air using solid-phase microextraction (SPME) is advantageous over other sampling techniques, but is often characterized by insufficient accuracies, particularly at longer sampling times. Experimental investigation of this issue and disclosing the origin of the problem is problematic and often not practically feasible due to high uncertainties. This research is aimed at developing the model of the TWA extraction process and optimization of TWA air sampling by SPME using finite element analysis software (COMSOL Multiphysics, Burlington, MA, USA). It was established that sampling by porous SPME coatings with high affinity to analytes is affected by slow diffusion of analytes inside the coating, an increase of their concentrations in the air near the fiber tip due to equilibration, and eventual lower sampling rate. The increase of a fiber retraction depth (Z) resulted in better recoveries. Sampling of studied VOCs using 23 ga Carboxen/polydimethylsiloxane (Car/PDMS) assembly at maximum possible Z (40 mm) was proven to provide more accurate results. Alternative sampling configuration based on 78.5 × 0.75 mm internal diameter SPME liner was proven to provide similar accuracy at improved detection limits. Its modification with the decreased internal diameter from the sampling side should provide even better recoveries. The results obtained can be used to develop a more accurate analytical method for determination of TWA concentrations of VOCs in air using SPME. The developed model can be used to simulate sampling of other environments (process gases, water) by retracted SPME fibers. Full article
(This article belongs to the Special Issue Solid-Phase Microextraction)
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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
Cited by 1 | PDF Full-text (2389 KB) | HTML Full-text | XML Full-text
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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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
Cited by 1 | PDF Full-text (1219 KB) | HTML Full-text | XML Full-text
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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