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Hyphenated Techniques’ Enlightenment in Chemical Analysis: From Complex Matrices of...
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Hyphenated Techniques’ Enlightenment in Chemical Analysis: From Complex Matrices of Plant Extracts and Foods to Human and Human Metabolism

A special issue of Separations (ISSN 2297-8739). This special issue belongs to the section "Chromatographic Separations".

Deadline for manuscript submissions: closed (31 December 2022) | Viewed by 8929

Special Issue Editor

Dr. Constantinos G. Tsiafoulis

E-Mail Website
Guest Editor
1. Laboratory Didaktic Personnel, Lab. of Analytical Chemistry, NMR Centre, Section of Inorganic and Analytical Chemistry, Dept. of Chemistry, University of Ioannina, Ioannina, Greece
2. Collaborative Educational Personnel, School of Natural Sciences and Technology, MSc Program Course “Chemical and Biomolecular Analysis”, Hellenic Open University, Patra, Greece
Interests: chromatography; hyphenated techniques; analytical chemistry; metabolomics
Special Issues, Collections and Topics in MDPI journals

Special Issue Information

Dear Colleagues,

Hyphenated techniques combine powerful analytical systems in order to illustrate the composition of several complex matrices and to reveal their chemical information. Among these are complex matrices from natural plant extracts and foods to the human metabolism.

The development and application of hyphenated techniques and the analytical information obtained provide tools for several scientific fields.

Focusing on either bioactive compounds or safety and originality for several matrices, from plant and food extracts to fluids of the human body, hyphenated techniques are widely applicable in the above fields for a range of approaches from constituent determination to holistic approaches.

The proposed Special Issue focuses mainly on methods based on gas (GC) or liquid chromatography (LC) techniques hyphenated to, mainly, spectroscopic (such as fluorescence spectroscopy, Nuclear Magnetic Resonance spectroscopy (NMR)) and spectrometric techniques (mainly MS) for several matrices: plant extracts, foods and human body fluids.

Review/mini-review articles and original research papers dealing with the above thematic issues are warmly welcomed.

Dr. Constantinos G. Tsiafoulis
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 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

  • hyphenated techniques
  • plant extracts
  • food
  • milk
  • human milk
  • metabolomics

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Published Papers (4 papers)

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Research

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17 pages, 1549 KiB  
Article
Accurate Determination of Pesticide Residues in Milk by Sonication-QuEChERS Extraction and LC-LTQ/Orbitrap Mass Spectrometry
by Ourania Koloka, Vasiliki Boti, Triantafyllos Albanis and Ioannis Konstantinou
Separations 2023, 10(3), 146; https://doi.org/10.3390/separations10030146 - 22 Feb 2023
Cited by 4 | Viewed by 3497
Abstract
A modified, quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction procedure combined with sonication and Ultra-High Performance Liquid Chromatography–Orbitrap-Mass Spectrometry (UHPLC–Orbitrap-MS) was developed as a sensitive and reliable methodology for the determination of multiclass pesticides in full-fat milk. Different amounts of EMR-lipid [...] Read more.
A modified, quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction procedure combined with sonication and Ultra-High Performance Liquid Chromatography–Orbitrap-Mass Spectrometry (UHPLC–Orbitrap-MS) was developed as a sensitive and reliable methodology for the determination of multiclass pesticides in full-fat milk. Different amounts of EMR-lipid sorbent were assayed for the cleanup step in order to achieve both acceptably high recoveries and low co-extractives in the final extracts. Accurate mass measurements of the analyte’s pseudo-molecular ions and tandem MS fragmentation were used to quantify and identify the target pesticides. Analytical performance characteristics of the method, such as linearity, recovery, precision, the limit of detection (LOD) and quantification (LOQ), matrix effects (ME), and expanded uncertainty, have been determined for method validation fulfilling all criteria for its use as a validated routine method. The method was successfully applied to real samples (by local farms and commercial), revealing the presence of carbendazim in one milk sample at a concentration level below the maximum residue limits. Full article
(This article belongs to the Special Issue Hyphenated Techniques’ Enlightenment in Chemical Analysis: From Complex Matrices of Plant Extracts and Foods to Human and Human Metabolism)
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12 pages, 966 KiB  
Article
Method Development and Validation for Simultaneous Analysis of Eleven Components for Quality Control of Geumgwesingihwan Using HPLC–DAD and UPLC–MS/MS
by Chang-Seob Seo and Mee-Young Lee
Separations 2022, 9(8), 213; https://doi.org/10.3390/separations9080213 - 10 Aug 2022
Cited by 2 | Viewed by 1805
Abstract
Geumgwesingihwan (GGSGH) is an oriental herbal formula made by adding Achyranthes bidentate Blume and Plantago asiatica L. to Yukmijiwhanghwan. It has been used for the treatment of edema since ancient times. The purpose of this study is to develop and validate a method [...] Read more.
Geumgwesingihwan (GGSGH) is an oriental herbal formula made by adding Achyranthes bidentate Blume and Plantago asiatica L. to Yukmijiwhanghwan. It has been used for the treatment of edema since ancient times. The purpose of this study is to develop and validate a method for simultaneous quantification of 11 components: gallic acid (1), 5-(hydroxymethyl)furfural (2), geniposidic acid (3), morroniside (4), loganin (5), paeoniflorin (6), acteoside (7), cornuside (8), benzoic acid (9), benzoylpaeoniflorin (10), and paeonol (11), using high-performance liquid chromatography with a diode array detector (HPLC–DAD) and ultra-performance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS). Compounds 1–11 were separated on a Capcell Pak UG 80 C18 column (250 mm × 4.6 mm, 5 μm) using a mobile phase of a distilled water–acetonitrile system, both containing 0.1% formic acid. In UPLC–MS/MS, compounds 1–11 were separated on an Acquity UPLC BEH C18 column (100 mm × 2.1 mm, 1.7 µm) using a mobile phase of a distilled water–acetonitrile system containing 1.0% acetic acid. Using these methods, samples of GGSGH were determined to contain 0.13–2.87 mg/g (HPLC–DAD) and not detected–4.60 mg/g (UPLC–MS/MS) of compounds 1–11. The developed HPLC–DAD assays for simultaneous determination of all analytes were validated with respect to linearity, limits of detection and quantification, recovery, and precision. The established HPLC assay will be used to obtain basic data for quality evaluation of GGSGH and related oriental herbal formulas. Full article
(This article belongs to the Special Issue Hyphenated Techniques’ Enlightenment in Chemical Analysis: From Complex Matrices of Plant Extracts and Foods to Human and Human Metabolism)
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15 pages, 3754 KiB  
Article
Anti-Osteoporotic Effect of Viscozyme-Assisted Polysaccharide Extracts from Portulaca oleracea L. on H2O2-Treated MC3T3-E1 Cells and Zebrafish
by Yunhua Fu, Xuan Hu, Dongyue Zhou, Xue Li, Xingyu Tao, Di Yang, Fei Zheng, Yulin Dai and Hao Yue
Separations 2022, 9(5), 128; https://doi.org/10.3390/separations9050128 - 20 May 2022
Cited by 5 | Viewed by 2262
Abstract
This study aims to screen and characterize the protective effect of polysaccharides from Portulaca oleracea L. (POP) against H2O2-stimulated osteoblast apoptosis in vivo and in vitro. The enzymes viscozyme, celluclast, α-amylase, and β-glucanase were used to extract POPs. Among [...] Read more.
This study aims to screen and characterize the protective effect of polysaccharides from Portulaca oleracea L. (POP) against H2O2-stimulated osteoblast apoptosis in vivo and in vitro. The enzymes viscozyme, celluclast, α-amylase, and β-glucanase were used to extract POPs. Among all enzyme-assisted POPs, the first participating fraction of viscozyme extract POP (VPOP1) exhibited the highest antioxidant activity. Hoechst 33342 and acridine orange/ethidium bromide staining and flow cytometry of MC3T3 cells revealed that VPOP1 inhibited apoptosis in a dose-dependent manner. Moreover, VPOP1 increased the expression levels of heme oxygenase-1 (HO-1) and NADPH quinine oxidoreductase 1 (NQO1) and decreased the expression levels of nuclear factor (erythroid-derived 2)-like 2 (Nrf2) and Kelch-like ECH-associated protein 1 (Keap1) in H2O2-induced cells compared with their controls. The results of an in vivo experiment show that VPOP1 significantly reduced reactive oxygen species generation and lipid peroxidation in zebrafish at 72 h post-fertilization and promoted bone growth at 9 days post-fertilization. Furthermore, VPOP1 was identified via 1-phenyl-3-methyl-5-pyrazolone derivatization as an acidic heteropolysaccharide comprising mannose and possessing a molecular weight of approximately 7.6 kDa. Collectively, VPOP1 was selected as a potential anti-osteoporotic functional food because of its protective activity against H2O2-induced damage in vitro and in vivo. Full article
(This article belongs to the Special Issue Hyphenated Techniques’ Enlightenment in Chemical Analysis: From Complex Matrices of Plant Extracts and Foods to Human and Human Metabolism)
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Review

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28 pages, 1405 KiB  
Review
Hyphenated Techniques and NMR Methods for Possible Organochlorinated Pesticides Occurrence in Human and Animal Milk
by Eleni D. Thanou and Constantinos G. Tsiafoulis
Separations 2024, 11(10), 282; https://doi.org/10.3390/separations11100282 - 29 Sep 2024
Viewed by 744
Abstract
Although not expected to be used due to restrictions raised on their usage, Persisted Organic Pollutants (POP) such as organochlorinated pesticides (OCPs) can be found in several matrices, even nowadays. The lack of biodegradation and, furthermore, their persistence in the environment result in [...] Read more.
Although not expected to be used due to restrictions raised on their usage, Persisted Organic Pollutants (POP) such as organochlorinated pesticides (OCPs) can be found in several matrices, even nowadays. The lack of biodegradation and, furthermore, their persistence in the environment result in the possible occurrence of these lipophilic toxins in several matrices, from environmental samples and foods to human milk. The current review focuses on the usage of hyphenated techniques for the determination and monitoring of OCPs in several matrices, such as milk—both animal and human milk. The lipid matrix of milk and dairy products favors the possible bioaccumulation of the above pollutants, and the complex matrix of the dairy products is a challenge for method development. Additionally, spectroscopic methods—mainly Nuclear Magnetic Resonance (NMR)-based metabolomics—for biomonitoring of OCPs persistence, bioaccumulation, and effect of possible exposure, along with NMR usage in several methods developed, are also presented and discussed. Finally, we introduce and present the metabolomic approach for OCPs and other POPs in lipid matrices. Full article
(This article belongs to the Special Issue Hyphenated Techniques’ Enlightenment in Chemical Analysis: From Complex Matrices of Plant Extracts and Foods to Human and Human Metabolism)
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