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Solid-Phase Microextraction II
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Solid-Phase Microextraction II

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

Deadline for manuscript submissions: closed (31 December 2020) | Viewed by 23702

Special Issue Editors

Dr. Constantinos K. Zacharis

E-Mail Website
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
Dr. Paraskevas D. Tzanavaras

E-Mail Website
Guest Editor
Laboratory of Analytical Chemistry, School of Chemistry, Aristotle University of Thessaloniki, 54124 Thessaloniki, Greece
Interests: automation; sequential injection analysis; separation techniques (HPLC, CE); post-column derivatization; microextraction
Special Issues, Collections and Topics in MDPI journals

Special Issue Information

Dear Colleagues,

Following the great success of the first Special Issue of the international journal Molecules dedicated to solid phase microextraction (SPME), which hosted 15 high-quality articles from colleagues all around the world (URL https://www.mdpi.com/journal/molecules/special_issues/Solid_phase_microextraction), in cooperation with the editors of the journal, we have decided to edit a second Special Issue on the same topic.
Solid phase microextraction (SPME) is a mature and advantageous 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 cover 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.
This second Special Issue on SPME still aims to cover the latest research trends and applications in this research field. Researchers working on—but not limited to—fiber coating technology, online automated SPME, and their applications in food, environmental, and biomedical sciences are cordially invited to contribute a research or review article.

Dr. Constantinos K. Zacharis
Assist. Prof. 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

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Published Papers (5 papers)

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Research

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14 pages, 270 KiB  
Article
Volatile Compounds Content, Physicochemical Parameters, and Antioxidant Activity of Beers with Addition of Mango Fruit (Mangifera Indica)
by Alan Gasiński, Joanna Kawa-Rygielska, Antoni Szumny, Anna Czubaszek, Justyna Gąsior and Witold Pietrzak
Molecules 2020, 25(13), 3033; https://doi.org/10.3390/molecules25133033 - 2 Jul 2020
Cited by 54 | Viewed by 5150
Abstract
This study was performed to determine the possibility of using mango fruit (Mangifera indica) in brewing technology. The aim of using the SPME-HS-GC-MS technique was to assess what changes occurred in the volatile composition of mango beers brewed in this study. [...] Read more.
This study was performed to determine the possibility of using mango fruit (Mangifera indica) in brewing technology. The aim of using the SPME-HS-GC-MS technique was to assess what changes occurred in the volatile composition of mango beers brewed in this study. Mango fruit was added to the beer in five different forms to ascertain what kind of preparation should be used to improve beer aroma. Analysis of the volatile components in mango beer showed that beer without mango addition was characterized by the lowest content of volatile compounds (1787.84 µg/100 mL). The addition of mango fruit increased the concentration of compounds, such as α-pinene, β-myrcene, terpinolene, α-terpineol, cis-β-ocimene, caryophyllene, and humulene, in beer. Beer prepared with mango pulp addition was characterized by the highest concentration of volatile components from mango beers (2112.15 µg/100 mL). Furthermore, beers with mango addition were characterized by a higher polyphenol content (up to 44% higher than control beer) and antioxidant activity than control beer and were evaluated by a trained panel as having a better taste and aroma than beer without fruit addition. Full article
(This article belongs to the Special Issue Solid-Phase Microextraction II)
12 pages, 3685 KiB  
Article
Preliminary Study on the Differences in Hydrocarbons Between Phosphine-Susceptible and -Resistant Strains of Rhyzopertha dominica (Fabricius) and Tribolium castaneum (Herbst) Using Direct Immersion Solid-Phase Microextraction Coupled with GC-MS
by Ihab Alnajim, Manjree Agarwal, Tao Liu, Beibei Li, Xin Du and Yonglin Ren
Molecules 2020, 25(7), 1565; https://doi.org/10.3390/molecules25071565 - 29 Mar 2020
Cited by 7 | Viewed by 2764
Abstract
Phosphine resistance is a worldwide issue threatening the grain industry. The cuticles of insects are covered with a layer of lipids, which protect insect bodies from the harmful effects of pesticides. The main components of the cuticular lipids are hydrocarbon compounds. In this [...] Read more.
Phosphine resistance is a worldwide issue threatening the grain industry. The cuticles of insects are covered with a layer of lipids, which protect insect bodies from the harmful effects of pesticides. The main components of the cuticular lipids are hydrocarbon compounds. In this research, phosphine-resistant and -susceptible strains of two main stored-grain insects, T. castaneum and R. dominica, were tested to determine the possible role of their cuticular hydrocarbons in phosphine resistance. Direct immersion solid-phase microextraction followed by gas chromatography-mass spectrometry (GC-MS) was applied to extract and analyze the cuticular hydrocarbons. The results showed significant differences between the resistant and susceptible strains regarding the cuticular hydrocarbons that were investigated. The resistant insects of both species contained higher amounts than the susceptible insects for the majority of the hydrocarbons, sixteen from cuticular extraction and nineteen from the homogenized body extraction for T. castaneum and eighteen from cuticular extraction and twenty-one from the homogenized body extraction for R. dominica. 3-methylnonacosane and 2-methylheptacosane had the highest significant difference between the susceptible and resistant strains of T. castaneum from the cuticle and the homogenized body, respectively. Unknown5 from the cuticle and 3-methylhentriacontane from the homogenized body recorded the highest significant differences in R. dominica. The higher hydrocarbon content is a key factor in eliminating phosphine from entering resistant insect bodies, acting as a barrier between insects and the surrounding phosphine environment. Full article
(This article belongs to the Special Issue Solid-Phase Microextraction II)
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12 pages, 1326 KiB  
Article
Determination of Volatile Compounds in Nut-Based Milk Alternative Beverages by HS-SPME Prior to GC-MS Analysis
by Natalia Manousi and George A. Zachariadis
Molecules 2019, 24(17), 3091; https://doi.org/10.3390/molecules24173091 - 26 Aug 2019
Cited by 37 | Viewed by 5071
Abstract
A reliable Headspace-Solid Phase Microextraction (HS-SPME) method was developed for the determination of polar volatile components of commercial nut-based milk alternative drinks prior to Gas Chromatography–Mass Spectrometry (GC-MS) analysis. Under the optimum extraction conditions, a divinylbenzene (DVB)/Carboxen™ CAR)/polydimethylsiloxane (PDMS) fiber was used and [...] Read more.
A reliable Headspace-Solid Phase Microextraction (HS-SPME) method was developed for the determination of polar volatile components of commercial nut-based milk alternative drinks prior to Gas Chromatography–Mass Spectrometry (GC-MS) analysis. Under the optimum extraction conditions, a divinylbenzene (DVB)/Carboxen™ CAR)/polydimethylsiloxane (PDMS) fiber was used and 2 mL of sample was heated at 60 °C for 40 min under stirring, without salt addition. Ten compounds from different chemical classes (heptane, a-pinene, toluene, 2-methylpyrazine, 3-heptanone, heptanal, 2-octanone, 1-heptanol, benzaldehyde and 1-octanol) were chosen as model analytes for quantification. Limits of detection and limits of quantification were found to be 0.33–1.67 ng g−1 and 1–5 ng g−1, accordingly. Good linearity, precision and accuracy were obtained as well as a wide linear range. The proposed method was successfully applied to various beverages including almond milk, walnut milk, peanut milk and almond chocolate milk. More than 70 volatile compounds were detected in the different samples. Most of the detected volatiles were aldehydes, ketones and alcohols. This technique can be used for the determination of volatile compounds in nut-based beverages, to detect compositional changes during storage and technological treatment used for their production. Full article
(This article belongs to the Special Issue Solid-Phase Microextraction II)
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15 pages, 723 KiB  
Article
Determination of Various Drying Methods’ Impact on Odour Quality of True Lavender (Lavandula angustifolia Mill.) Flowers
by Jacek Łyczko, Klaudiusz Jałoszyński, Mariusz Surma, José Miguel García-Garví, Ángel A. Carbonell-Barrachina and Antoni Szumny
Molecules 2019, 24(16), 2900; https://doi.org/10.3390/molecules24162900 - 9 Aug 2019
Cited by 27 | Viewed by 4083
Abstract
True lavender flowers (Lavandula angustifolia Mill.) is a critical source of essential oils and a flavouring agent used in numerous industries like foods, cosmetics and pharmaceuticals. Its main volatile constituents are linalool and linalyl acetate, which are commonly considered as main odour-active [...] Read more.
True lavender flowers (Lavandula angustifolia Mill.) is a critical source of essential oils and a flavouring agent used in numerous industries like foods, cosmetics and pharmaceuticals. Its main volatile constituents are linalool and linalyl acetate, which are commonly considered as main odour-active constituents (OACs). Nevertheless, the quality of true lavender flowers is highly dependent on its post-harvest treatment, mainly the preservation method. Recognising that drying is the most frequently used preservation method, the influence of various drying methods, including convective drying (CD) at 50, 60 and 70 °C, vacuum-microwave drying (VMD) with powers 240, 360 and 480 W and combined convective pre-drying at 60 °C followed by vacuum-microwave finish-drying with power 480 W (CPD-VMFD), on the quality of true lavender flowers was verified. The evaluation of influence was carried out by HS-SPME(HS, solid-phase microextraction), GC-MS, GC-MS-O (gas chromatography–mass spectrometry–olfactometry) techniques. Moreover, the sensory panel has assessed the sample odour quality. As a result, the optimal drying methods regarding the requirements for products were established. Overall, for total essential oil recovery, CD at 50 °C is the optimal drying method, while for odour quality concerning the sensory panel evaluation, VMD with power 360 W combined CPD-VMFD and CD at 50 °C is the optimal drying method. Full article
(This article belongs to the Special Issue Solid-Phase Microextraction II)
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Review

Jump to: Research

32 pages, 3211 KiB  
Review
Bioanalytical HPLC Applications of In-Tube Solid Phase Microextraction: A Two-Decade Overview
by Natalia Manousi, Paraskevas D. Tzanavaras and Constantinos K. Zacharis
Molecules 2020, 25(9), 2096; https://doi.org/10.3390/molecules25092096 - 30 Apr 2020
Cited by 34 | Viewed by 5839
Abstract
In-tube solid phase microextraction is a cutting-edge sample treatment technique offering significant advantages in terms of miniaturization, green character, automation, and preconcentration prior to analysis. During the past years, there has been a considerable increase in the reported publications, as well as in [...] Read more.
In-tube solid phase microextraction is a cutting-edge sample treatment technique offering significant advantages in terms of miniaturization, green character, automation, and preconcentration prior to analysis. During the past years, there has been a considerable increase in the reported publications, as well as in the research groups focusing their activities on this technique. In the present review article, HPLC bioanalytical applications of in-tube SPME are discussed, covering a wide time frame of twenty years of research reports. Instrumental aspects towards the coupling of in-tube SPME and HPLC are also discussed, and detailed information on materials/coatings and applications in biological samples are provided. Full article
(This article belongs to the Special Issue Solid-Phase Microextraction II)
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