Special Issue "Development of Alternative Green Sample Preparation Techniques"

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

Deadline for manuscript submissions: 15 December 2019.

Special Issue Editor

Dr. Emanuela Gionfriddo
E-Mail Website
Guest Editor
Department of Chemistry and Biochemistry, The University of Toledo, OH, USA
Interests: sample preparation, green extraction techniques, automation, microextraction, food analysis, environmental analysis, bio-clinical analysis

Special Issue Information

Dear Colleagues,

It is without doubt that sample preparation often poses the ultimate challenge to any analytical method development process, whether for targeted or non-targeted analyses in complex matrices.

Recently, trends in the development of newer sample preparation techniques have shifted toward greener and faster approaches, guaranteeing minimal consumption of organic solvents, promoting the production of reusable extraction devices, enhancement of analysis throughput through automated systems, use of natural sorptive materials, etc.

Considering the great efforts made by many research groups in developing more sustainable and efficient sample preparation protocols for food, environmental and bio-analytical applications, I invite you to contribute to this Special Issue of Separations, dedicated to the “Development of Alternative Green Sample Preparation Techniques”, with original research articles and reviews.

With your rich expertise in the field of analytical chemistry, I believe that your contribution to this Special Issue will definitely have a significant impact on the entire scientific research community.

Dr. Emanuela Gionfriddo
Guest Editor

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

  • Green sample preparation
  • Automation
  • Food analysis
  • Environmental analysis
  • Bio-clinical analysis
  • Targeted and untargeted analysis
  • Microextraction

Published Papers (7 papers)

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Research

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Open AccessArticle
Automation of µ-SPE (Smart-SPE) and Liquid-Liquid Extraction Applied for the Analysis of Chemical Warfare Agents
Separations 2019, 6(4), 49; https://doi.org/10.3390/separations6040049 - 09 Oct 2019
Abstract
Existing autosamplers are frequently applied only for subjecting the samples to the instruments for injection. In our study, we have set up a TriPlusRSH autosampler mounted on a GC-FID-MS/MS system using the new Method Composer and Script Editor software to automatize all necessary [...] Read more.
Existing autosamplers are frequently applied only for subjecting the samples to the instruments for injection. In our study, we have set up a TriPlusRSH autosampler mounted on a GC-FID-MS/MS system using the new Method Composer and Script Editor software to automatize all necessary sample preparation steps and subsequent injection of samples in the field of chemical disarmament. Those include but are not limited to: liquid-liquid extraction, drying steps, solvent exchange, and µ-SPE. Tedious and error prone off-line steps are eliminated. In particular, when investigating highly toxic substances like chemical warfare agents or anticancer drugs, automation can help to minimize health risks for lab personnel. The setup engaged features brand new prototype equipment, e.g., a centrifuge to assist in phase separation for liquid-liquid extraction. Efficiency and accuracy of the automated methods were carefully evaluated and proven to outperform the respective manual steps after optimization, e.g., the processing time is up to 60% faster and recovery rates are doubled. The developed workflows can easily be adapted to other sample preparation protocols, e.g., determination of octanol/water partition coefficients, and be used amongst different instruments and chromatography data handling systems. Full article
(This article belongs to the Special Issue Development of Alternative Green Sample Preparation Techniques)
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Open AccessFeature PaperArticle
A Bottom-Up Approach for Data Mining in Bioaromatization of Beers Using Flow-Modulated Comprehensive Two-Dimensional Gas Chromatography/Mass Spectrometry
Separations 2019, 6(4), 46; https://doi.org/10.3390/separations6040046 - 25 Sep 2019
Abstract
In this study, we report the combination of comprehensive two-dimensional gas chromatography (GC×GC) with multivariate pattern recognition through template matching for the assignment of the contribution of Brazilian Ale 02 yeast strain to the aroma profile of beer compared with the traditional Nottingham [...] Read more.
In this study, we report the combination of comprehensive two-dimensional gas chromatography (GC×GC) with multivariate pattern recognition through template matching for the assignment of the contribution of Brazilian Ale 02 yeast strain to the aroma profile of beer compared with the traditional Nottingham yeast. Volatile organic compounds (VOC) from two beer samples, which were fermented with these yeast strains were sampled using headspace solid-phase microextraction (HS-SPME). The aroma profiles from both beer samples were obtained using GC×GC coupled to a fast scanning quadrupole mass spectrometer. Data processing performed through multiway principal components analysis succeeded in separating both beer samples based on yeast strain. The execution of a simple and reliable procedure succeeded and identified 46 compounds as relevant for sample classification. Furthermore, the bottom-up approach spotted compounds found exclusively in the beer sample fermented with the Brazilian yeast, highlighting the bioaromatization properties introduced to the aroma profile by this yeast strain. Full article
(This article belongs to the Special Issue Development of Alternative Green Sample Preparation Techniques)
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Open AccessFeature PaperArticle
Determination of Hydrophilic UV Filters in Real Matrices Using New-Generation Bar Adsorptive Microextraction Devices
Separations 2019, 6(4), 45; https://doi.org/10.3390/separations6040045 - 25 Sep 2019
Abstract
In the present contribution, new-generation bar adsorptive microextraction devices combined with microliquid desorption, followed by high-performance liquid chromatography–diode array detection (BAµE-µLD/HPLC–DAD) are proposed for the determination of two very polar ultraviolet (UV) filters (2-phenylbenzimidazole-5-sulfonic acid (PBS) and 5-benzoyl-4-hydroxy-2-methoxybenzenesulfonic acid (BZ4)) in aqueous media. [...] Read more.
In the present contribution, new-generation bar adsorptive microextraction devices combined with microliquid desorption, followed by high-performance liquid chromatography–diode array detection (BAµE-µLD/HPLC–DAD) are proposed for the determination of two very polar ultraviolet (UV) filters (2-phenylbenzimidazole-5-sulfonic acid (PBS) and 5-benzoyl-4-hydroxy-2-methoxybenzenesulfonic acid (BZ4)) in aqueous media. Different sorbents were evaluated as BAµE coating phases, in which polystyrene–divinylbenzene polymer showed the best selectivity for the analysis of both UV filters, with average extraction efficiency of 61.8 ± 9.1% for PBS and 69.5 ± 4.8% for BZ4. The validated method showed great reproducibility for the analysis of PBS and BZ4 UV filters, providing suitable limits of detection (0.04 µg L−1 and 0.20 µg L−1), as well as good linear dynamic ranges (0.16–16.0 and 0.8–80.0 µg L−1), respectively. The proposed methodology was applied for monitoring the target analytes in several real matrices, including tap, sea, and estuarine waters, as well as wastewater samples. Despite some matrix effects being observed for some real samples, good selectivity and linearity were obtained. The present contribution showed an innovative analytical cycle that includes the use of disposable devices, which make BAµE much more user-friendly and suitable for the routine work, being a remarkable analytical alternative for trace analysis of priority compounds in real matrices. Full article
(This article belongs to the Special Issue Development of Alternative Green Sample Preparation Techniques)
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Open AccessArticle
Optimised Extraction of Trypsin Inhibitors from Defatted Gac (Momordica cochinchinensis Spreng) Seeds for Production of a Trypsin Inhibitor-Enriched Freeze Dried Powder
Separations 2019, 6(1), 8; https://doi.org/10.3390/separations6010008 - 05 Feb 2019
Abstract
The seeds of the Gac fruit, Momordica cochinchinensis Spreng, are rich in trypsin inhibitors (TIs) but their optimal extraction and the effects of freeze drying are not established. This study aims to (1) compare aqueous solvents (DI water, 0.1 M NaCl, 0.02 M [...] Read more.
The seeds of the Gac fruit, Momordica cochinchinensis Spreng, are rich in trypsin inhibitors (TIs) but their optimal extraction and the effects of freeze drying are not established. This study aims to (1) compare aqueous solvents (DI water, 0.1 M NaCl, 0.02 M NaOH and ACN)/water/FA, 25:24:1) for extracting TIs from defatted Gac seed kernel powder, (2) to optimise the extraction in terms of solvent, time and material to solvent ratio and (3) to produce a TI-enriched freeze-dried powder (FD-TIP) with good characteristics. Based on the specific TI activity (TIA), the optimal extraction was 1 h using a ratio of 2.0 g of defatted powder in 30 mL of 0.05 M NaCl. The optimisation improved the TIA and specific TIA by 8% and 13%, respectively. The FD-TIP had a high specific TIA (1.57 ± 0.17 mg trypsin/mg protein), although it also contained saponins (43.6 ± 2.3 mg AE/g) and phenolics (10.5 ± 0.3 mg GAE/g). The FD-TIP was likely stable during storage due to its very low moisture content (0.43 ± 0.08%) and water activity (0.18 ± 0.07) and its ability to be easily reconstituted in water due to its high solubility index (92.4 ± 1.5%). Therefore, the optimal conditions for the extraction of TIs from defatted Gac seed kernel powder followed by freeze drying gave a high quality powder in terms of its highly specific TIA and physical properties. Full article
(This article belongs to the Special Issue Development of Alternative Green Sample Preparation Techniques)
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Review

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Open AccessReview
Development, Optimization and Applications of Thin Film Solid Phase Microextraction (TF-SPME) Devices for Thermal Desorption: A Comprehensive Review
Separations 2019, 6(3), 39; https://doi.org/10.3390/separations6030039 - 05 Aug 2019
Abstract
Through the development of solid phase microextraction (SPME) technologies, thin film solid phase microextraction (TF-SPME) has been repeatedly validated as a novel sampling device well suited for various applications. These applications, encompassing a wide range of sampling methods such as onsite, in vivo [...] Read more.
Through the development of solid phase microextraction (SPME) technologies, thin film solid phase microextraction (TF-SPME) has been repeatedly validated as a novel sampling device well suited for various applications. These applications, encompassing a wide range of sampling methods such as onsite, in vivo and routine analysis, benefit greatly from the convenience and sensitivity TF-SPME offers. TF-SPME, having both an increased extraction phase volume and surface area to volume ratio compared to conventional microextraction techniques, allows high extraction rates and enhanced capacity, making it a convenient and ideal sampling tool for ultra-trace level analysis. This review provides a comprehensive discussion on the development of TF-SPME and the applications it has provided thus far. Emphasis is given on its application to thermal desorption, with method development and optimization for this desorption method discussed in detail. Moreover, a detailed outlook on the current progress of TF-SPME development and its future is also discussed with emphasis on its applications to environmental, food and fragrance analysis. Full article
(This article belongs to the Special Issue Development of Alternative Green Sample Preparation Techniques)
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Open AccessReview
Alternative Green Extraction Phases Applied to Microextraction Techniques for Organic Compound Determination
Separations 2019, 6(3), 35; https://doi.org/10.3390/separations6030035 - 16 Jul 2019
Abstract
The use of green extraction phases has gained much attention in different fields of study, including in sample preparation for the determination of organic compounds by chromatography techniques. Green extraction phases are considered as an alternative to conventional phases due to several advantages [...] Read more.
The use of green extraction phases has gained much attention in different fields of study, including in sample preparation for the determination of organic compounds by chromatography techniques. Green extraction phases are considered as an alternative to conventional phases due to several advantages such as non-toxicity, biodegradability, low cost and ease of preparation. In addition, the use of greener extraction phases reinforces the environmentally-friendly features of microextraction techniques. Thus, this work presents a review about new materials that have been used in extraction phases applied to liquid and sorbent-based microextractions of organic compounds in different matrices. Full article
(This article belongs to the Special Issue Development of Alternative Green Sample Preparation Techniques)
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Open AccessReview
Metal-Organic Frameworks in Green Analytical Chemistry
Separations 2019, 6(3), 33; https://doi.org/10.3390/separations6030033 - 27 Jun 2019
Cited by 1
Abstract
Metal-organic frameworks (MOFs) are porous hybrid materials composed of metal ions and organic linkers, characterized by their crystallinity and by the highest known surface areas. MOFs structures present accessible cages, tunnels and modifiable pores, together with adequate mechanical and thermal stability. Their outstanding [...] Read more.
Metal-organic frameworks (MOFs) are porous hybrid materials composed of metal ions and organic linkers, characterized by their crystallinity and by the highest known surface areas. MOFs structures present accessible cages, tunnels and modifiable pores, together with adequate mechanical and thermal stability. Their outstanding properties have led to their recognition as revolutionary materials in recent years. Analytical chemistry has also benefited from the potential of MOF applications. MOFs succeed as sorbent materials in extraction and microextraction procedures, as sensors, and as stationary or pseudo-stationary phases in chromatographic systems. To date, around 100 different MOFs form part of those analytical applications. This review intends to give an overview on the use of MOFs in analytical chemistry in recent years (2017–2019) within the framework of green analytical chemistry requirements, with a particular emphasis on possible toxicity issues of neat MOFs and trends to ensure green approaches in their preparation. Full article
(This article belongs to the Special Issue Development of Alternative Green Sample Preparation Techniques)
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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.

Title: Modern approaches to preparation of body fluids for determination of bioactive compounds
Authors: Katarzyna Madej 1, Wojciech Piekoszewski 1,2
Affiliation:Department of Analytical Chemistry, Faculty of Chemistry, Jagiellonian University, Krakow 30-387, Poland
2 Department of Food Science and Technology, School of Biomedicine, Far Eastern Federal University, Vladivostok, Russia
Abstract: The current clinical and forensic toxicological analysis of body fluids requires a modern approach to sample preparation characterized by high selectivity and enrichment capability, suitability for micro-samples, simplicity and speed, the possibility of automation and miniaturization, as well as the use of small amounts of reagents, especially toxic solvents. Most of the above mentioned features may be realized by so called microextraction techniques which cover liquid phase techniques (e.g. single drop microextraction, SDME; dispersive liquid liquid microextraction, DLLME; hollow fiber liquid phase microextraction, HF-LPME) and solid phase extraction techniques (solid phase microextraction, SPME; microextraction in packed syringes, MEPS; disposable pipette tips extraction, DPX). Some other extraction methodologies like dispersive solid phase extraction (d-SPE) or magnetic solid phase extraction (MSPE) can be easily miniaturized. This review briefly describes selected extraction methods, and then presents the latest advances in methods for preparing body fluids for the determination of bioactive compounds, in combination with chromatographic analysis. The development perspectives of the analytical area we are interested in are also indicated.
Keywords: microextraction techniques; body fluids; bioactive compounds; clinical and forensic analysis

 

Tentative tittle: Metal-organic frameworks, materials with endless applications in analytical chemistry? How green are they?
Authors: Priscilla Rocío-Bautista1,2,3, Iván Taima-Mancera1,3, Verónica Pino1,*, Jorge Pasán3
Affiliation: 1.Departament of Chemistry, Analytical Division, University of La Laguna, Tenerife, 38206 Spain
2.Department of Pure and Applies Sciences, University of Urbino, Urbino, 61029 Italy
3.Physics Department, X Ray and Molecular Materials Lab (MATMOL), University of La Laguna, Tenerife, 38206 Spain
Tentative Abstract: Metal-organic frameworks (MOFs) are porous hybrid materials composed by metal ions and organic linkers, characterized by their crystallinity and by the highest surface areas known. They have accessible cages, tunnels and modifiable pores, together with adequate mechanical and thermal stability. Their outstanding properties have promoted them as revolutionary materials in recent years. The number of applications of these materials grows exponentially in the scientific community. Thus, they have been included in photovoltaic applications, with purification purposes, for the storage and separation of gases, as sensors, in catalysis, biomedicine… Analytical chemistry has also benefited from the potential of MOFs applications. MOFs have been used successfully as sorbent materials in extraction and microextraction procedures, as sensors, and as stationary phases in chromatographic systems. To date, around 100 different MOFs have been described in analytical applications. This review intends to give an overview of MOFs in analytical chemistry and their future, with particular emphasis on possible toxicity issues of MOFs and trends to ensure green approaches in their preparation.
Keywords: metal-organic frameworks; application; analytical chemistry; sorbent materials; stationary phases; sensors

Title: SPME-Arrow: A Robust Sample Preparation Tool for Hunting Molecules in Complex Matrices
Authors: Jason S. Herrington, German A. Gomez-Rios, Gary Stidsen, David S. Bell
Abstract: In this manuscript, the fundamental and operational aspects behind SPME-Arrow are concisely reviewed. Special emphasis is placed on method development as well as troubleshooting issues potentially encountered when using this technology by non-experienced users. Likewise, we cover a series of applications in environmental, food and forensic analysis; and list other paths that can be explored by existing and new users. Finally, the future direction section focuses on novel interfaces of SPME-Arrow with analytical instrumentation, as well as recent developments in coating materials for SPME-Arrow geometry.

Title: Automation of µ-SPE (Smart-SPE) and Liquid-Liquid Extraction Applied for the Analysis of Chemical Warfare Agents
Authors: Marc André Althoff 1, Andreas Bertsch 2 and Manfred Metzulat 2,*
Affilitions: 1. Department of Chemistry, Ludwig-Maximilian University (LMU), Butenandtstrasse 5-13 (Haus D), D-81377 Munich, Germany; [email protected]
2. Chemistry Section, Science Department, Chemical Defense, Safety and Environmental Protection School, Mühlenweg 12, D-87527 Sonthofen, Germany; [email protected]
*Correspondence: [email protected]
Abstract: Existing autosamplers are frequently applied only for subjecting the samples to the instruments for injection. In our study, we have set up a TriPlusRSH autosampler mounted on a GC-FID-MS/MS system using the new Method Composer and Script Editor software to automatize all necessary sample preparation steps and subsequent injection of samples in the field of chemical disarmament. Those include but are not limited to: liquid-liquid extraction, drying steps, solvent exchange and µ-SPE. Tedious and error prone off-line steps are eliminated. Especially, when investigating highly toxic substances, automation can help to minimize health risks for lab personnel. The setup engaged features brand new prototype equipment, e.g. a centrifuge to assist in phase separation for liquid-liquid extraction. Efficiency and accuracy of the automated methods were carefully evaluated and proven to outperform the respective manual steps after optimization. The developed workflows can easily be adapted to other sample preparation protocols, e.g. determination of octanol/water partition coefficients, and be used amongst different instruments and chromatography data handling systems.
Keywords: automation, sample handling, sample preparation, chemical warfare agent, SPE, LLE

Title: Advancements in Low-Invasive Biological Surface Sampling and Emerging Applications
Authors: Atakan Arda Nalbant and Ezel Boyaci
Affiliation: Middle East Technical University, Ankara, Turkey
Abstract: Biological surfaces such as skin and ocular surface provide a plethora of information about the underlying biological activity of the organism but pose unique problems arising from their innate complexity, constant exposure to the surrounding elements and the general requirements of any used sampling method to be non- or low-invasive. Therefore, it is challenging but also rewarding to develop novel analytical tools that are suitable for direct sampling from biological surfaces. In this context, microextraction based technologies come forward as versatile, low-invasive, fast, and reliable sampling and sample preparation tools that are applicable for in vivo and in situ sampling from biologically relevant surfaces. This review aims to address recent developments in microextraction based in vivo and in situ sampling methods that introduce new ways and improve upon existing ones of sampling from biological surfaces. Directions for the development of future technology and potential areas of applications such as clinical, bioanalytical and doping analyses will also be discussed. These advancements include various types of hydrogels and PDMS patches/microarrays, and other wearable microextraction devices used mainly in skin sampling.

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