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Solid Phase Microextraction: Going Greener in Sample Preparation-A Themed Honorary Issue to Prof. Janusz Pawliszyn

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

Deadline for manuscript submissions: closed (31 December 2022) | Viewed by 14104

Special Issue Editors


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Guest Editor
Laboratory of Analytical Chemistry, School of Chemistry, Aristotle University of Thessaloniki, 54124 Thessaloniki, Greece
Interests: analytical chemistry; sample preparation; chromatography; HPLC; method validation; method development; separation science; food analysis; bioanalysis; environmental analysis; green analytical chemistry; sorptive extraction; microextraction techniques
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Guest Editor
Laboratory of Pharmaceutical Analysis, Department of Pharmaceutical Technology, School of Pharmacy, Aristotle University of Thessaloniki, 54124 Thessaloniki, Greece
Interests: pharmaceutical analytical chemistry; method development and validation; sample preparation (derivatization, microextraction, etc.); liquid and gas chromatography; capillary electrophoresis; mass spectrometry
Special Issues, Collections and Topics in MDPI journals

Special Issue Information

In recent decades, sample preparation techniques based on microextraction have become—due their valuable features—one of the most thoroughly investigated topics in analytical chemistry. The first “member” of this category was introduced almost three decades ago by J. Pawliszyn in the form of solid-phase microextraction (SPME). To date, numerous novel microextraction techniques and alternatives have been proposed using either solid- or liquid-phase extraction phases.

The use of microextraction has been considered to be beneficial compared to classical approaches offering versatility, reliability, selectivity, sensitivity, automation, fast extractions, sampling convenience (on-site sampling), and environmental sustainability. From the point of view of the concept of Green Analytical Chemistry, environmental sustainability is the most important advantage, since the number of pretreatment steps and also toxic solvents is reduced or even totally eliminated.     

 

Prof. Janusz Pawliszyn is one of the pioneers in the development of microextraction techniques with research experience of over 30 years in this topic. He is internationally recognized for his fundamental contributions to solvent-free techniques, including supercritical fluid, solid phase, and membrane extraction. The breakthrough came in 1989, with the publication of an article describing the application of fused silica fibers for the extraction of organic chemicals from water and their rapid transfer to capillary gas chromatographic columns. The paper heralded the invention of solid-phase microextraction, or—as it is generally known around the world—SPME. The term “SPME” was used for the first time in an article published in ACS Analytical Chemistry in 1990, describing the first practical version of microextraction technology. It took just three years for the technology to be commercialized by Supelco, Inc., and SPME has been one of the most important sample preparation techniques in gas chromatography ever since. Prof. Pawliszyn also developed needle trap technology and membrane extraction with a sorbent interface, sample preparation techniques for monitoring of organic compounds in on-site environments. In the area of analytical separation, he introduced the concept of whole column detection by combining capillary separation with CCD imaging technology. This technology developed by his group formed the foundation of Convergent Bioscience (now “Protein Simple”), a Toronto-based company whose technology is now considered the platinum standard for characterizing proteins and peptides and is widely accepted in the biotech industry.

 

Janusz Pawliszyn was named the 9th most influential person in analytical science across the globe by Analytical Scientist’s 2019 Power List (https://theanalyticalscientist.com/powerlist/2019). He was also recently awarded the 2019 Talanta Medal for his numerous contributions to analytical chemistry and for his pioneering work in solid-phase microextraction (SPME). He is Editor of Analytica Chimica Acta, Trends in Analytical Chemistry and member of the Editorial Boards of the Journal of Separation Science and Journal of Pharmaceutical Analysis. He has published over 650 articles to date and has an H-index of 98.

 

Molecules is pleased to host a Themed Special Issue honoring Prof. Janusz Pawliszyn for his outstanding contribution and achievements in Analytical Chemistry and especially in microextraction techniques.

 

Researchers working on microextraction techniques (solid- or liquid-phase microextraction) and their applications in food, environmental, and biomedical sciences are cordially invited to contribute a research or review article in this Honorary Special Issue and also join us in collectively acknowledging him for his outstanding achievements.

Please note that in the cases of review articles, an additional brief (1–2 pages) description of the topic including a draft index is required. This preliminary step is essential to avoid overlapping of topics.

This Special Issue is supported by the Sample Preparation Task Force and Network, of the European Chemical Society-Division of Analytical Chemistry (https://www.sampleprep.tuc.gr/en/home/).

Prof. Dr. Victoria Samanidou
Dr. Constantinos K. Zacharis
Guest Editors

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Keywords

  • Solid-phase microextraction (direct immersion, headspace sampling, coatings, in-tube extraction, arrow, etc.)
  • Microsolid-phase extraction (μ-SPE)
  • Dispersive microsolid-phase extraction
  • Liquid-phase microextraction (DLLME, single-drop ME, hollow fiber liquid ME, electromembrane-based ME, etc.)
  • Preconcentration
  • Automation
  • Miniaturized designs (chip-based extraction microfluidic devices)
  • Needle trap device
  • Microencapsulation techniques
  • Stir bar sorptive extraction

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Published Papers (5 papers)

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Research

15 pages, 3757 KiB  
Article
Alternative Ecosorbent for the Determination of Trihalomethanes in Aqueous Samples in SPME Mode
by Gustavo Sánchez-Duque, Juan José Lozada-Castro, Emerson Luis Yoshio Hara, Marco Tadeu Grassi, Milton Rosero-Moreano and Jhon Jairo Ríos-Acevedo
Molecules 2022, 27(24), 8653; https://doi.org/10.3390/molecules27248653 - 7 Dec 2022
Cited by 5 | Viewed by 1983
Abstract
A new sorbent material based on modified clay with ionic liquid immobilized into an agarose film was developed as part of this study. It was applied to determine organochlorine pollutants, like disinfection byproducts, through headspace solid-phase microextraction-gas chromatography-electron capture detection (HS-SPME-GC-ECD). The disinfection [...] Read more.
A new sorbent material based on modified clay with ionic liquid immobilized into an agarose film was developed as part of this study. It was applied to determine organochlorine pollutants, like disinfection byproducts, through headspace solid-phase microextraction-gas chromatography-electron capture detection (HS-SPME-GC-ECD). The disinfection byproducts determined in this study were used as model molecules because they were volatile compounds, with proven severe effects on human health. Their presence in aquatic environments is in trace concentrations (from pg L−1 to mg L−1). They are classified as emergent pollutants and their determination is a challenge for analytical chemists. The parameters which affected the extraction efficiency, i.e., number and distance between SPME discs, salt concentration, the temperature of extraction, extraction time, and desorption time, were optimized. A wide linear dynamic range of 10–1000 ng mL−1 and coefficients of determination better than 0.997 were achieved. The limits of detection and the limits of quantitation were found in the ranges of (1.7–3.7) ng mL−1 and (5.6–9.9) ng mL−1, respectively. The precision, expressed as relative standard deviation (RSD), was better than 8%. The developed sorbent exhibits good adsorption affinity. The applicability of the proposed methodology for the analysis of trihalomethanes in environmental and water samples showed recoveries in the range of 86–95%. Finally, the newly created method fully complied with the principles of green chemistry. Due to the fact that the sorbent holder was made of agarose, which is a wholly biodegradable material, sorbent clay is a widespread material in nature. Moreover, the reagents intercalated into the montmorillonite are new green solvents, and during the whole procedure, low amounts of organic solvents were used. Full article
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12 pages, 2466 KiB  
Article
Optimized Solid-Phase Mesh-Enhanced Sorption from Headspace (SPMESH) for Rapid Sub-ng/kg Measurements of 3-Isobutyl-2-methoxypyrazine (IBMP) in Grapes
by Terry L. Bates, Jessica Rafson, Hui Feng, Bruce S. Pan, Benjamin R. J. Mueller, Benjamin Yancey, William Fatigante and Gavin L. Sacks
Molecules 2022, 27(19), 6195; https://doi.org/10.3390/molecules27196195 - 21 Sep 2022
Cited by 3 | Viewed by 2115
Abstract
Parallel extraction of headspace volatiles from multiwell plates using sorbent sheets (HS-SPMESH) followed by direct analysis in real-time high-resolution mass spectrometry (DART-HRMS) can be used as a rapid alternative to solid-phase micro-extraction (SPME) gas-chromatography mass-spectrometry (GC-MS) for trace level volatile analyses. However, an [...] Read more.
Parallel extraction of headspace volatiles from multiwell plates using sorbent sheets (HS-SPMESH) followed by direct analysis in real-time high-resolution mass spectrometry (DART-HRMS) can be used as a rapid alternative to solid-phase micro-extraction (SPME) gas-chromatography mass-spectrometry (GC-MS) for trace level volatile analyses. However, an earlier validation study of SPMESH-DART-MS using 3-isobutyl-2-methoxypyrazine (IBMP) in grape juice showed poor correlation between SPMESH-DART-MS and a gold standard SPME-GC-MS around the compound’s odor detection threshold (<10 ng/kg) in grape juice, and lacked sufficient sensitivity to detect IBMP at this concentration in grape homogenate. In this work, we report on the development and validation of an improved SPMESH extraction approach that lowers the limit of detection (LOD < 0.5 ng/kg), and regulates crosstalk between wells (<0.5%) over a calibration range of 0.5–100 ng/kg. The optimized SPMESH-DART-MS method was validated using Cabernet Sauvignon and Merlot grape samples harvested from commercial vineyards in the central valley of California (n = 302) and achieved good correlation and agreement with SPME-GC-MS (R2 = 0.84) over the native range of IBMP (<0.5–20 ng/kg). Coupling of SPMESH to a lower resolution triple quadrupole (QqQ)-MS via a new JumpShot-HTS DART source also achieved low ng/kg detection limits, and throughput was improved through positioning stage optimizations which reduced time spent on intra-well SPMESH areas. Full article
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13 pages, 3844 KiB  
Communication
Coated Blade Spray-Mass Spectrometry as a New Approach for the Rapid Characterization of Brain Tumors
by Joanna Bogusiewicz, Magdalena Gaca-Tabaszewska, Dominik Olszówka, Karol Jaroch, Jacek Furtak, Marek Harat, Janusz Pawliszyn and Barbara Bojko
Molecules 2022, 27(7), 2251; https://doi.org/10.3390/molecules27072251 - 30 Mar 2022
Cited by 10 | Viewed by 2454
Abstract
Brain tumors are neoplasms with one of the highest mortality rates. Therefore, the availability of methods that allow for the quick and effective diagnosis of brain tumors and selection of appropriate treatments is of critical importance for patient outcomes. In this study, coated [...] Read more.
Brain tumors are neoplasms with one of the highest mortality rates. Therefore, the availability of methods that allow for the quick and effective diagnosis of brain tumors and selection of appropriate treatments is of critical importance for patient outcomes. In this study, coated blade spray-mass spectrometry (CBS-MS), which combines the features of microextraction and fast ionization methods, was applied for the analysis of brain tumors. In this approach, a sword-shaped probe is coated with a sorptive material to enable the extraction of analytes from biological samples. The analytes are then desorbed using only a few microliters of solvent, followed by the insertion of the CBS device into the interface on the mass spectrometer source. The results of this proof-of-concept experiment confirmed that CBS coupled to high-resolution mass spectrometry (HRMS) enables the rapid differentiation of two histologically different lesions: meningiomas and gliomas. Moreover, quantitative CBS-HRMS/MS analysis of carnitine, the endogenous compound, previously identified as a discriminating metabolite, showed good reproducibility with the variation below 10% when using a standard addition calibration strategy and deuterated internal standards for correction. The resultant data show that the proposed CBS-MS technique can be useful for on-site qualitative and quantitative assessments of brain tumor metabolite profiles. Full article
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14 pages, 1167 KiB  
Article
Benefits of Innovative and Fully Water-Compatible Stationary Phases of Thin-Film Microextraction (TFME) Blades
by Łukasz Sobczak, Dominika Kołodziej and Krzysztof Goryński
Molecules 2021, 26(15), 4413; https://doi.org/10.3390/molecules26154413 - 21 Jul 2021
Cited by 5 | Viewed by 2357
Abstract
Octadecyl (C18) groups are arguably the most popular ligands used for preparation of solid phase microextraction (SPME) devices. However, conventional C18-bonded silica particles are not fully compatible with the nearly 100% aqueous composition of typical biological samples (e.g., plasma, [...] Read more.
Octadecyl (C18) groups are arguably the most popular ligands used for preparation of solid phase microextraction (SPME) devices. However, conventional C18-bonded silica particles are not fully compatible with the nearly 100% aqueous composition of typical biological samples (e.g., plasma, saliva, or urine). This study presents the first evaluation of thin-film SPME devices coated with special water-compatible C18-bonded particles. Device performance was assessed by extracting a mixture of 30 model compounds that exhibited various chemical structures and properties, such as hydrophobicity. Additionally, nine unique compositions of desorption solvents were tested. Thin-film SPME devices coated with C18-bonded silica particles with polar end-capping groups (10 µm) were compared with conventional trimethylsilane end-capped C18-bonded silica particles of various sizes (5, 10, and 45 µm) and characteristics. Polar end-capped particles provided the best extraction efficacy and were characterized by the strongest correlations between the efficacy of the extraction process and the hydrophobicity of the analytes. The results suggest that the original features of octadecyl ligands are best preserved in aqueous conditions by polar end-capped particles, unlike with conventional trimethylsilane end-capped particles that are currently used to prepare SPME devices. The benefits associated with this improved type of coating encourage further implementation of microextractraction as greener alternative to the traditional sample preparation methods. Full article
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11 pages, 1386 KiB  
Communication
Systematic Evaluation of Different Coating Chemistries Used in Thin-Film Microextraction
by Jia-Wei Liu, Khaled Murtada, Nathaly Reyes-Garcés and Janusz Pawliszyn
Molecules 2020, 25(15), 3448; https://doi.org/10.3390/molecules25153448 - 29 Jul 2020
Cited by 18 | Viewed by 2703
Abstract
A systematic evaluation of eight different coatings made of solid phase extraction (SPE) and carbon-based sorbents immobilized with polyacrylonitrile in the thin-film microextraction (TFME) format using LC-MS/MS was described. The investigated coatings included graphene, graphene oxide, multi-walled carbon nanotubes (MWCNTs), carboxylated MWCNTs, as [...] Read more.
A systematic evaluation of eight different coatings made of solid phase extraction (SPE) and carbon-based sorbents immobilized with polyacrylonitrile in the thin-film microextraction (TFME) format using LC-MS/MS was described. The investigated coatings included graphene, graphene oxide, multi-walled carbon nanotubes (MWCNTs), carboxylated MWCNTs, as carbon-based coatings, and polystyrene-divinylbenzene (PS-DVB), octadecyl-silica particles (C18), hydrophilic–hydrophobic balance particles (HLB) and phenyl-boronic acid modified particles (PBA), as SPE-based coatings. A total of 24 compounds of diverse moieties and of a wide range of polarities (log P from −2.99 to 6.98) were selected as probes. The investigated coatings were characterized based on their extraction performance toward the selected probes at different pH values and at optimized desorption conditions. In the case of SPE-based coatings, PS-DVB and HLB exhibited a balanced extraction for compounds within a wide range of polarities, and C18 showed superior extraction recoveries for non-polar analytes. Carbon-based coatings showed high affinity for non-polar compounds given that their main driving force for extraction is hydrophobic interactions. Interestingly, among the studied carbon-based coatings, graphene oxide showed the best extraction capabilities toward polar compounds owing to its oxygen-containing groups. Overall, this work provided important insights about the extraction mechanisms and properties of the investigated coatings, facilitating the coating selection when developing new TFME applications. Full article
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