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Separations
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Microextraction Techniques for Sample Preparation
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Microextraction Techniques for Sample Preparation

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

Deadline for manuscript submissions: closed (22 October 2020) | Viewed by 15186

Special Issue Editors

Prof. Dr. Wojciech Piekoszewski

E-Mail Website
Guest Editor
Department of Analytical Chemistry, Faculty of Chemistry, Jagiellonian University, 30-387 Krakow, Poland
Interests: plant drugs; natural products; analytical chemistry; extraction techniques; high separation methods; HPLC; LC-MS, GC-MS; capillary electrophoresis; method development; method optimization; method validation
Special Issues, Collections and Topics in MDPI journals
Dr. Katarzyna Madej

E-Mail Website
Guest Editor
Department of Analytical Chemistry, Jagiellonian University, Poland
Interests: Analysis of drugs in biological and environmental materials; Analysis of pesticide residues in food and environmental samples; Sample preparation techniques; Chromatographic and related techniques
Special Issues, Collections and Topics in MDPI journals

Special Issue Information

Dear Colleagues,

Current analysis 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 these features may be realized by so-called microextraction techniques. At present, there are a plethora of such techniques that may be chosen for the solution of a particular analytical problem. As examples of such analytical areas in which these requirements for sample preparation are of particular importance, clinical and forensic analysis can be given. This Special Issue provides main aspects and current advances, as well as future trends in application of microextraction techniques to various analytical fields.

Prof. Dr. Wojciech Piekoszewski
Dr. Katarzyna Madej
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 submissions that pass pre-check are 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 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 2600 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 techniques
  • gas chromatography
  • liquid chromatography
  • miniaturization
  • automatization
  • optimization
  • drug analysis
  • environmental analysis

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Published Papers (4 papers)

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Research

18 pages, 8505 KiB  
Article
Screening Carpet Substrate Interferences in Arson Identification by Solid Phase Microextraction and Gas Chromatography-Mass Spectrometry
by Alyssa Aldrich, Edna Gennarino-Lopez, Gabriel Odugbesi, Kaylandra Woodside and Shokouh Haddadi
Separations 2020, 7(4), 63; https://doi.org/10.3390/separations7040063 - 19 Nov 2020
Cited by 3 | Viewed by 2956
Abstract
The sample analysis and data interpretation is the most challenging step of fire debris analysis, due to the presence of combustion and pyrolysis products in the substrate material. In this study, a headspace solid phase microextraction (HS-SPME) procedure was applied to the extraction [...] Read more.
The sample analysis and data interpretation is the most challenging step of fire debris analysis, due to the presence of combustion and pyrolysis products in the substrate material. In this study, a headspace solid phase microextraction (HS-SPME) procedure was applied to the extraction of combustion and pyrolysis products from three commonly used carpet substrate materials, made of nylon 6,6 and polyesters. Each carpet sample was burned with and without two different ignitable liquids (ILs), i.e., gasoline and kerosene, and the Total Ion Chromatograms (TICs) and Extracted Ion Profiles of characteristic class compounds of ILs were obtained and compared to those of unburned neat ILs, using gas-chromatography mass spectrometry (GC-MS), to study the possible interferences of these substrate materials in fire debris analysis. Full article
(This article belongs to the Special Issue Microextraction Techniques for Sample Preparation)
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10 pages, 810 KiB  
Article
A Simple, Fast, and Green Oil Sample Preparation Method for Determination of Cannabidioloic Acid and Cannabidiol by HPLC-DAD
by Katarzyna Madej, Gabriela Kózka, Maciej Winiarski and Wojciech Piekoszewski
Separations 2020, 7(4), 60; https://doi.org/10.3390/separations7040060 - 29 Oct 2020
Cited by 12 | Viewed by 4578
Abstract
Currently, the medical use of food supplements containing Cannabis sativa has attracted the interest of consumers, as well as the medical and scientific community. With the increasing consumption of these products, there is also a risk of their abuse or discrepancy between the [...] Read more.
Currently, the medical use of food supplements containing Cannabis sativa has attracted the interest of consumers, as well as the medical and scientific community. With the increasing consumption of these products, there is also a risk of their abuse or discrepancy between the actual and declared contents of active substances by the manufacturer in these products. Thus, the development and elaboration of analytical procedures for determination of appropriate phytocannabinoids seems to be important. This work focuses on the development of a simple, fast and environmentally friendly liquid-liquid extraction method combined with fat freezing from an oil sample to isolate two phytocannabinoids: cannabidiol (CBD) and cannabidiolic acid (CBDA). The extraction method was optimized considering efficacy and repeatability of extraction, as well as minimalizing use of organic reagents and sample amount. Under the optimized conditions, extraction recovery for CBD was 97.3–109% and for CBDA was 69.1–69.5% with precision (RSD, %) 5.0–8.4 and 7.1–10.6, respectively. The evaluated main analytical parameters of the developed high pressure liquid chromatography with diode array detector (HPLC-DAD) method for both studied cannabinoids are satisfactory. The usability of the developed method was checked by analysis of real samples of a food supplement–hemp oil enriched with CBD. Full article
(This article belongs to the Special Issue Microextraction Techniques for Sample Preparation)
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12 pages, 1170 KiB  
Article
Novel Room Temperature Ionic Liquid for Liquid-Phase Microextraction of Cannabidiol from Natural Cosmetics
by Susanne Huber, Matthias Harder, Kevin Funck, Kevin Erharter, Michael Popp, Günther K. Bonn and Matthias Rainer
Separations 2020, 7(3), 45; https://doi.org/10.3390/separations7030045 - 26 Aug 2020
Cited by 11 | Viewed by 3468
Abstract
This study presents the synthesis of a novel asymmetric 1,3-di(alkoxy)imidazolium based room temperature ionic liquid, more precisely 1-butoxy-3-ethoxy-2-ethyl-imidazolium bis(trifluoromethane)sulfonimide, and its application as an extraction solvent in liquid-phase microextraction of cannabidiol from natural cosmetics. Quantification was implemented, using a high performance liquid chromatography [...] Read more.
This study presents the synthesis of a novel asymmetric 1,3-di(alkoxy)imidazolium based room temperature ionic liquid, more precisely 1-butoxy-3-ethoxy-2-ethyl-imidazolium bis(trifluoromethane)sulfonimide, and its application as an extraction solvent in liquid-phase microextraction of cannabidiol from natural cosmetics. Quantification was implemented, using a high performance liquid chromatography system coupled to ultraviolet detection. Molecular structure elucidation was performed by nuclear magnetic resonance spectroscopy. The extraction procedure was optimized by means of two different design of experiments. Additionally, a full validation was executed. The established calibration model, ranging from 0.6 to 6.0 mg g−1, was linear with a coefficient of determination of 0.9993. Accuracy and precision were demonstrated on four consecutive days with a bias within −2.6 to 2.3% and a maximum relative standard deviation value of 2.5%. Recoveries, tested for low and high concentration within the calibration range, were 80%. Stability of extracted cannabidiol was proven for three days at room temperature and fourteen days at 4 °C and −20 °C. An autosampler stability for 24 h was validated. Liquid-phase microextraction of cannabidiol from different formulated cream based cosmetics was performed, including four ointments and four creams. The results show that a significantly higher selectivity could be achieved compared to a conventional extraction methods with methanol. Full article
(This article belongs to the Special Issue Microextraction Techniques for Sample Preparation)
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10 pages, 1486 KiB  
Article
Mixed Matrix Membrane Tip Extraction Coupled with UPLC–MS/MS for the Monitoring of Nonsteroidal Anti-Inflammatory Drugs in Water Samples
by Thipashini Ganesan, Nurul Hazirah Mukhtar, Hong Ngee Lim and Hong Heng See
Separations 2020, 7(1), 19; https://doi.org/10.3390/separations7010019 - 13 Mar 2020
Cited by 10 | Viewed by 3634
Abstract
An ultra-performance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS) method, in combination with a mixed matrix membrane microextraction method for the quantification of nonsteroidal anti-inflammatory drugs (NSAIDs) in environmental water samples, is reported. The extraction device was prepared by casting well-dispersed polymeric bonded octadecyl (C [...] Read more.
An ultra-performance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS) method, in combination with a mixed matrix membrane microextraction method for the quantification of nonsteroidal anti-inflammatory drugs (NSAIDs) in environmental water samples, is reported. The extraction device was prepared by casting well-dispersed polymeric bonded octadecyl (C18) particles in a cellulose triacetate matrix solution onto commercially available 200 μL micropipette tips. The membrane formed contains 25% of the adsorbent loading amount and was firmly attached to the inner wall of the membrane tip. The dynamic extraction was performed by withdrawing and dispensing the sample solution through the tip device for effective analyte adsorption, followed by the analyte desorption process into 40 μL of methanol and acetonitrile (1:1) prior to UPLC–MS/MS analysis. NSAIDs—namely diclofenac, ibuprofen, indoprofen, naproxen and sulindac—were chosen as targeted analytes. Several extraction parameters were comprehensively optimized, including sample pH value, ionic strength, dynamic extraction cycle, desorption solvent and desorption time. The optimized conditions demonstrated a linear range from 0.25 to 500 ng L−1, with correlation coefficients (r2) from 0.9988 to 0.9992 and detection limits ranging from 0.08 to 0.40 ng L−1. The recoveries of the spiked water samples were between 92% and 99% and exhibited excellent precision relative to standard deviations (RSDs ≤ 4.9%), and enrichment factors (EFs) were at 201–249 for the developed approach. Full article
(This article belongs to the Special Issue Microextraction Techniques for Sample Preparation)
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