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Special Issue "Development of Analytical Methodologies for Selective Extraction, Separation, Identification, and Purification of Valuable Compounds"

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

Deadline for manuscript submissions: 31 October 2023 | Viewed by 6733

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Special Issue Editors

Dr. João Miguel F. Rocha

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Laboratory for Process Engineering, Environment, Biotechnology and Energy (LEPABE), Department of Chemical Engineering (DEQ), Faculty of Engineering, University of Porto (FEUP), Porto, Portugal
Interests: food microbiota; chromatography and mass spectrometry; separation processes; valorisation of agro-food by-products; fermentation processes and microbial starter cultures; sourdough and breadmaking
Special Issues, Collections and Topics in MDPI journals

Dr. Kristian Pastor

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Department of Applied and Engineering Chemistry, Faculty of Technology Novi Sad, University of Novi Sad, Novi Sad, Serbia
Interests: food authentication; functional food; gas chromatography; mass spectrometry; chemometrics; machine learning; cereals and pseudocereals; bakery products; edible vegetable oils
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Dr. Nataša Nastić

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Faculty of Technology Novi Sad, University of Novi Sad, Novi Sad, Serbia
Interests: advanced extraction techniques; green technologies; sample preparation; plants; agro-food waste and by-products valorization; bioactive compounds; chromatography and mass spectrometry
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Prof. Dr. Fatih Ozogul

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Department of Seafood Processing Technology, Faculty of Fisheries, Cukurova University, 01330 Balcali, Adana, Turkey
Interests: food technology & microbiology; microbial biotechnology; lactic acid bacteria; probiotics; biogenic amines; histamine; food-borne pathogens; food spoilage bacteria; modified atmosphere & vacuum packaging; food compounds analysis using HPLC, GC, GS-MS; Spectrophotometer; Texture analyses
Special Issues, Collections and Topics in MDPI journals

Special Issue Information

Dear Colleagues,

This is a holistic Special Issue that will cover state-of-the-art of innovative analytical methodologies that can be employed in virtually any research field, from science and engineering to biochemistry, chemistry, and green-chemistry and to (bio)polymers, biology, ecology, environment and pollution, microbiology, agri-food (e.g., dairy, feed, pet food, meat, juices, refrigerants, beer, wine), enzymology, biotechnology, biomedicine, biomaterials, bioengineering, etc. The main focus of this Special Issue is to describe the development and optimization of novel analytical methodologies for the selective extraction, separation, identification, and purification of high-added value compounds or fractions from virtually any matrix, such as from chemicals, agriculture, and industrial by-products and wastes; microbial metabolites from fermentation processes by yeasts, molds and bacteria; or compounds from algae and microalgae. Any type of high-added value compound, such as chemicals, food, cosmetics, pharmaceuticals, nutraceuticals, bioenergy (e.g., biofuel, bioethanol, biobutanol, biohydrogen), and biofertilizers will be considered. Likewise, the application of any type of analytical methodology, such as separation techniques (TLC, HPLC, GLC), mass spectrometry (GC-MSn, LC-MSn, HRMS, etc.), and spectroscopy (NMR, NIR, FT-IR, FTIR-PAS) as well as genomics, proteomics, transcriptomics, metabolomics, and lipidomics approaches are also welcome.

Dr. João Miguel F. Rocha
Dr. Kristian Pastor
Dr. Nataša Nastić
Prof. Dr. Fatih Ozogul
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. Molecules is an international peer-reviewed open access semimonthly 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 2700 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

biotechnology
analytical methodologies
extraction, separation, and purification processes
waste and by-product valorization
bioactive compounds
innovative industrial products and processes
socioeconomically and environmental sustainability
circular economy

Published Papers (6 papers)

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Research

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Open AccessArticle

Study of Brewer’s Spent Grain Environmentally Friendly Processing Ways

Konstantin V. Kobelev

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Molecules 2023, 28(11), 4553; https://doi.org/10.3390/molecules28114553 - 05 Jun 2023

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Abstract

Background: This article is devoted to the study of the effect of electrochemically activated water (catholyte with pH 9.3) on organic compounds of the plant matrix of brewer’s spent grain in order to extract various compounds from it. Methods: Brewer’s spent grain was obtained from barley malt at a pilot plant by mashing the malt followed by filtration and washing of the grain in water and storing it at (0 ± 2) °C in craft bags. For the organic compound quantitative determination, instrumental methods of analysis (HPLC) were used, and the results were subjected to mathematical analysis. Results: The study results showed that at atmospheric pressure, the alkaline properties of the catholyte showed better results compared to aqueous extraction with respect to β-glucan, sugars, nitrogenous and phenolic compounds, and 120 min was the best period for extraction at 50 °C. The excess pressure conditions used (0.5 ÷ 1 atm) revealed an increase in the accumulation of non-starch polysaccharide and nitrogenous compounds, while the level of sugars, furan and phenolic compounds decreased with increasing treatment duration. The waste grain extract ultrasonic treatment used revealed the effectiveness of catholyte in relation to the extraction of β-glucan and nitrogenous fractions; however, sugars and phenolic compounds did not significantly accumulate. The correlation method made it possible to reveal the regularities in the formation of furan compounds under the conditions of extraction with the catholyte: Syringic acid had the greatest effect on the formation of 5-OH-methylfurfural at atmospheric pressure and 50 °C and vanillic acid under conditions of excess pressure. Regarding furfural and 5-methylfurfural, amino acids had a direct effect at excess pressure. It was shown that the content of all furan compounds depends on amino acids with thiol groups and gallic acid; the formation of 5-hydroxymethylfurfural and 5-methylfurfural is influenced by gallic and vanillic acids; the release of furfural and 5-methylfurfural is determined by amino acids and gallic acid; excess pressure conditions promote the formation of furan compounds under the action of gallic and lilac acids. Conclusions: This study showed that a catholyte allows for efficient extraction of carbohydrate, nitrogenous and monophenolic compounds under pressure conditions, while flavonoids require a reduction in extraction time under pressure conditions. Full article

(This article belongs to the Special Issue Development of Analytical Methodologies for Selective Extraction, Separation, Identification, and Purification of Valuable Compounds)

Open AccessArticle

Comparison between Cashew-Based and Petrochemical Hydroxyoximes: Insights from Molecular Simulations

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Molecules 2023, 28(9), 3971; https://doi.org/10.3390/molecules28093971 - 08 May 2023

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Abstract

Solvent extraction has been ubiquitously used to recover valuable metals from wastes such as spent batteries and electrical boards. With increasing demands for energy transition, there is a critical need to improve the recycling rate of critical metals, including copper. Therefore, the sustainability of reagents is critical for the overall sustainability of the process. Yet, the recycling process relies on functional organic compounds based on the hydroxyoxime group. To date, hydroxyoxime extractants have been produced from petrol-based chemical feedstocks. Recently, natural-based cardanol has been used to produce an alternative hydroxyoxime. The natural-based oxime has been employed to recover valuable metals (Ga, Ni, Co) via a liquid/liquid extraction process. The natural compound has a distinctive structure with 15 carbons in the alkyl tail. In contrast, petrol-based hydroxyoximes have only 12 or fewer carbons. However, the molecular advantages of this natural-based compound over the current petrol-based ones remain unclear. In this study, molecular dynamics simulation was employed to investigate the effect of extractant hydrocarbon chains on the extraction of copper ions. Two hydroxyoxime extractants with 12 and 15 carbons in the alkyl chain were found to have similar interactions with Cu²⁺ ions. Yet, a slight molecular binding increase was observed when the carbon chain was increased. In addition, lengthening the carbon chain made the extracting stage easier and the stripping stage harder. The binding would result in a lower pH in the extraction step and a lower pH in the stripping step. The insights from this molecular study would help design the extraction circuit using natural-based hydroxyoxime extractants. A successful application of cashew-based cardanol will improve the environmental benefits of the recycling process. With cashew-producing regions in developing countries, the application also improves these regions’ social and economic sustainability. Full article

(This article belongs to the Special Issue Development of Analytical Methodologies for Selective Extraction, Separation, Identification, and Purification of Valuable Compounds)

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Open AccessArticle

Elagolix Sodium Salt and Its Synthetic Intermediates: A Spectroscopic, Crystallographic, and Conformational Study

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Molecules 2023, 28(9), 3861; https://doi.org/10.3390/molecules28093861 - 03 May 2023

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Abstract

Elagolix sodium salt is the first marketed orally active non-peptide gonadotropin-releasing hormone receptor antagonist (GnRHR-ant) for the management of hormone dependent diseases, such as endometriosis and uterine fibroids. Despite its presence on the market since 2018, a thorough NMR analysis of this drug, together with its synthetic intermediates, is still lacking. Hence, with the aim of filling this literature gap, we here performed a detailed NMR investigation, which allowed the complete assignment of the ¹H, ¹³C, and ¹⁵N NMR signals. These data allowed, with the support of the conformational analysis, the determination of the stereochemical profile of the two atropisomers, detectable in solution. Moreover, these latter were also detected by means of cellulose-based chiral HPLC, starting from a sample prepared through an implemented synthetic procedure with respect to the reported ones. Overall, these results contribute to further understanding of the topic of atropisomerism in drug discovery and could be applied in the design of safe and stable analogs, endowed with improved target selectivity. Full article

(This article belongs to the Special Issue Development of Analytical Methodologies for Selective Extraction, Separation, Identification, and Purification of Valuable Compounds)

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Open AccessArticle

Comparison of Phytochemical Profiles of Wild and Cultivated American Ginseng Using Metabolomics by Ultra-High Performance Liquid Chromatography-High-Resolution Mass Spectrometry

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Molecules 2023, 28(1), 9; https://doi.org/10.3390/molecules28010009 - 20 Dec 2022

Cited by 3 | Viewed by 1294

Abstract

American ginseng (Panax quinquefolius L.) has been recognized as a valuable herb medicine, and ginsenosides are the most important components responsible for the health-beneficial effects. This study investigated the secondary metabolites responsible for the differentiation of wild and cultivated American ginsengs with ultrahigh-performance liquid chromatography-high resolution mass spectrometry (UHPLC-HRMS)-based metabolomic approach. An in-house ginsenoside library was developed to facilitate data processing and metabolite identification. Data visualization methods, such as heatmaps and volcano plots, were utilized to extract discriminated ion features. The results suggested that the ginsenoside profiles of wild and cultivated ginsengs were significantly different. The octillol (OT)-type ginsenosides were present in greater abundance and diversity in wild American ginsengs; however, a wider distribution of the protopanaxadiol (PPD)-and oleanolic acid (OA)-type ginsenosides were found in cultivated American ginseng. Based on the tentative identification and semi-quantification, the amounts of five ginsenosides (i.e., notoginsenoside H, glucoginsenoside Rf, notoginsenoside R1, pseudoginsenoside RT2, and ginsenoside Rc) were 2.3–54.5 fold greater in wild ginseng in comparison to those in their cultivated counterparts, and the content of six ginsenosides (chicusetsusaponin IVa, malonylginsenoside Rd, pseudoginsenoside Rc1, malonylfloralginsenoside Rd6, Ginsenoside Rd, and malonylginsenoside Rb1) was 2.6–14.4 fold greater in cultivated ginseng compared to wild ginseng. The results suggested that the in-house metabolite library can significantly reduce the complexity of the data processing for ginseng samples, and UHPLC-HRMS is effective and robust for identifying characteristic components (marker compounds) for distinguishing wild and cultivated American ginseng. Full article

(This article belongs to the Special Issue Development of Analytical Methodologies for Selective Extraction, Separation, Identification, and Purification of Valuable Compounds)

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Open AccessArticle

Separation of Mandelic Acid by a Reactive Extraction Method Using Tertiary Amine in Different Organic Diluents

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Molecules 2022, 27(18), 5986; https://doi.org/10.3390/molecules27185986 - 14 Sep 2022

Cited by 1 | Viewed by 1036

Abstract

Mandelic acid is a valuable chemical that is commonly used in the synthesis of various drugs, in antibacterial products, and as a skin care agent in cosmetics. As it is an important chemical, various methods are used to synthesize and extract this compound. However, the yields of the used processes is not significant. A dilute aqueous solution is obtained when using several production methods, such as a fermentation, etc. In this study, the reactive extraction of mandelic acid from aqueous solutions using tri-n-octylamine extractant at 298.15 K was investigated. Dimethyl phthalate (DMP), methyl isobutyl ketone (MIBK), 2-octanone, 1-octanol, n-pentane, octyl acetate, and toluene were used as diluents. The batch extraction results of the mandelic acid experiments were obtained for the development of a process design. Calculations of the loading factor (Z), distribution coefficient (D), and extraction efficiency (E%) were based on the experimental data. The highest separation yield was obtained as 98.13% for 0.458 mol.L⁻¹ of tri-n-octylamine concentration in DMP. The overall extraction constants were analyzed for the complex of acid-amine by the Bizek approach, including K₁₁, K₁₂, and K₂₃. Full article

(This article belongs to the Special Issue Development of Analytical Methodologies for Selective Extraction, Separation, Identification, and Purification of Valuable Compounds)

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Review

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Open AccessReview

Betaine as a Functional Ingredient: Metabolism, Health-Promoting Attributes, Food Sources, Applications and Analysis Methods

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Molecules 2023, 28(12), 4824; https://doi.org/10.3390/molecules28124824 - 17 Jun 2023

Viewed by 1116

Abstract

Betaine is a non-essential amino acid with proven functional properties and underutilized potential. The most common dietary sources of betaine are beets, spinach, and whole grains. Whole grains—such as quinoa, wheat and oat brans, brown rice, barley, etc.—are generally considered rich sources of betaine. This valuable compound has gained popularity as an ingredient in novel and functional foods due to the demonstrated health benefits that it may provide. This review study will provide an overview of the various natural sources of betaine, including different types of food products, and explore the potential of betaine as an innovative functional ingredient. It will thoroughly discuss its metabolic pathways and physiology, disease-preventing and health-promoting properties, and further highlight the extraction procedures and detection methods in different matrices. In addition, gaps in the existing scientific literature will be emphasized. Full article

(This article belongs to the Special Issue Development of Analytical Methodologies for Selective Extraction, Separation, Identification, and Purification of Valuable Compounds)

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