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Special Issue "Control and Optimization of Extractive Methodologies and Analysis of Natural Products"

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A special issue of Processes (ISSN 2227-9717). This special issue belongs to the section "Separation Processes".

Deadline for manuscript submissions: 31 August 2023 | Viewed by 15651

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Prof. Dr. Ofelia Anjos

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Instituto Politécnico de Castelo Branco, Quinta da Senhora de Mércules, 6001-909 Castelo Branco, Portugal
Interests: spectroscopic techniques; chromatographic techniques; food engineering; forest science and technology
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Prof. Dr. Eugenia Gallardo

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1. Centro de Investigação em Ciências da Saúde, Universidade da Beira Interior (CICS-UBI), 6201-506 Covilhã, Portugal
2. Laboratório de Farmaco-Toxicologia, UBIMedical, Universidade da Beira Interior (CICS-UBI), 6201-506 Covilhã, Portugal
Interests: toxicology; analytical method development; recreational drugs; natural psychoactive substances; therapeutic drug monitoring; sample preparation; alternative samples; miniaturized extraction procedures
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Prof. Dr. Raquel P. F. Guiné

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CERNAS Research Centre and Department of Food Industry, Polytechnic Institute of Viseu, 3504-510 Viseu, Portugal
Interests: food chemistry; food engineering; nutrition; sustainable agriculture; food science
Special Issues, Collections and Topics in MDPI journals

Special Issue Information

Dear Colleagues,

The interest in biobased compounds extracted from natural sources or recirculated materials has increased in recent decades due to the circular economy and their potential application as active ingredients in several industries (i.e., food and pharmaceutical, cosmetics and wellness).

The optimization and validation of extraction techniques are critical in the quality and quantity of the analytes obtained from a matrix, and represent an early and fundamental step in natural products’ isolation and application.

It is of great interest to isolate and study bioactive natural products from different parts of trees, shrubs, plants, foods, or industrial food wastes in order to identify potential bioactive properties—namely, antioxidant, anti-inflammatory, and anti-carcinogenic activities.

This Issue intends to provide an overview of innovative techniques for the extraction, isolation, and analysis of natural products that could have several applications. Presenting a vast scope, this Special Issue welcomes full papers, short communications, and review articles on , but not limited to, extract optimization and comparative studies of extraction techniques, and the analysis of qualitative and quantitative composition using chromatographic or spectroscopic techniques. Additionally, evaluations of the biological effects of natural compounds are encouraged, as are comparative studies investigating quality in terms of the variability of natural sources.

Furthermore, papers dealing with bioinformatic tools and mathematical models of extracts’ mechanisms of action are welcome.

This Issue should serve as a text for academia, or as a reference tool for researchers—particularly those working in the fields of phytochemistry, natural product chemistry, food, medicinal chemistry, toxicology, and health, as well as industry professionals.

Prof. Dr. Ofelia Anjos
Prof. Dr. Eugenia Gallardo
Prof. Dr. Raquel P. F. Guiné
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 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. Processes 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 2000 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.

Published Papers (13 papers)

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Research

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Open AccessArticle

Application of Plant Surfactants as Cleaning Agents in Shampoo Formulations

Káren G. O. Bezerra

Hugo M. Meira

Bruno O. Veras

Thayza C. M. Stamford

and

Processes 2023, 11(3), 879; https://doi.org/10.3390/pr11030879 - 15 Mar 2023

Viewed by 407

Abstract

With the increased demand for sustainable, hypoallergenic products, plant surfactants are a promising, eco-friendly option for cleaning products due to their low toxicity or even the absence of toxicity. In the present study, surfactant-rich extracts from Chenopodium quinoa, Glycine max, and Malpighia emarginata were assessed for their stability, antioxidant capacity, toxic potential, and cleaning potential in shampoo formulations. The surfactants in the extracts were isolated and characterized by NMR, UV-Vis, and FTIR spectroscopy. The results demonstrated that the extracts remained stable within the temperature and pH ranges tested. The antioxidant properties were also determined. In the analysis of irritation potential, G. max and C. quinoa exhibited low toxicity and no toxicity, respectively. The cleaning potential analysis confirmed that the extracts could be used as primary surfactants. Seven shampoo formulations were developed, which showed potential to reduce surface tension to the range of 27.1–31.7 mN/m and interfacial tension to the range of 5.4–7.3 mN/m. The wettability, percentage of solids, density, pH, and dirt dispersion of the formulas were within standard ranges, and the sebum removal capacity of the seven formulations was similar to or even better than that of a commercial shampoo. Full article

(This article belongs to the Special Issue Control and Optimization of Extractive Methodologies and Analysis of Natural Products)

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Open AccessArticle

Production of Extracellular Lipase by Bacillus halotolerans from Oil-Contaminated Soil in a Pilot-Scale Submerged Bioreactor

Mater H. Mahnashi

Veeranna S. Hombalimath

Ibrahim Ahmed Shaikh

Uday M. Muddapur

Shivalingsarj V. Desai

Mohammed Merae Alshahrani

Muhanad Alhujaily

Amer Al Ali

Basheerahmed Abdulaziz Mannasaheb

Ahmed Abdullah Al Awadh

and

Aejaz Abdullatif Khan

Processes 2022, 10(8), 1548; https://doi.org/10.3390/pr10081548 - 07 Aug 2022

Viewed by 907

Abstract

Microbial lipases are the biocatalyst of choice for the present and future because of their characteristics, including their ability to remain active as an enzyme throughout a broad pH, temperature, and substrate range. The goal of the current investigation was to find novel sources of substrates and isolates from soil contaminated by oil for the synthesis of lipase. On tributyrin media, 10 lipolytic bacterial strains that were isolated from oil-contaminated soil were grown. Using the zone of clearance, it was possible to identify the isolates with the highest activity. Following phylogenetic tree analysis, molecular characterization of the 16S rRNA sequence of the bacterial isolates revealed that it was Bacillus halotolerans (VSH 09). The enzyme was purified to near homogeneity. The enzyme activity was found to be optimum at a pH of 7.0 and a temperature of 35 °C. While Ni²⁺ and Cu²⁺ had no effect, the presence of Mg²⁺ and Ca²⁺ exhibited the highest levels of enzyme activity. At 1%, tributyrin as a substrate exhibited its highest level of activity. The molecular weight, as determined by SDS-PAGE, was found to be 38 kDa. The kinetics of the enzyme were found to be 41.66 and 9.37 mg/mL for V_max and K_m, respectively. The high yield of lipase produced by this method suggests that it holds potential for production on a large scale and could be used for various biotechnological applications. Full article

(This article belongs to the Special Issue Control and Optimization of Extractive Methodologies and Analysis of Natural Products)

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Open AccessEditor’s ChoiceArticle

Overview of Different Modes and Applications of Liquid Phase-Based Microextraction Techniques

José S. Câmara

Rosa Perestrelo

Basit Olayanju

Cristina V. Berenguer

Abuzar Kabir

and

Jorge A. M. Pereira

Processes 2022, 10(7), 1347; https://doi.org/10.3390/pr10071347 - 11 Jul 2022

Cited by 1 | Viewed by 1219

Abstract

Liquid phase-based microextraction techniques (LPµETs) have attracted great attention from the scientific community since their invention and implementation mainly due to their high efficiency, low solvent and sample amount, enhanced selectivity and precision, and good reproducibility for a wide range of analytes. This review explores the different possibilities and applications of LPμETs including dispersive liquid–liquid microextraction (DLLME) and single-drop microextraction (SDME), highlighting its two main approaches, direct immersion-SDME and headspace-SDME, hollow-fiber liquid-phase microextraction (HF-LPME) in its two- and three-phase device modes using the donor–acceptor interactions, and electro membrane extraction (EME). Currently, these LPμETs are used in very different areas of interest, from the environment to food and beverages, pharmaceutical, clinical, and forensic analysis. Several important potential applications of each technique will be reported, highlighting its advantages and drawbacks. Moreover, the use of alternative and efficient “green” extraction solvents including nanostructured supramolecular solvents (SUPRASs, deep eutectic solvents (DES), and ionic liquids (ILs)) will be discussed. Full article

(This article belongs to the Special Issue Control and Optimization of Extractive Methodologies and Analysis of Natural Products)

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Open AccessArticle

Green Extraction of Date Palm Fruits via Ultrasonic-Assisted Approach: Optimizations and Antioxidant Enrichments

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Processes 2022, 10(6), 1049; https://doi.org/10.3390/pr10061049 - 24 May 2022

Viewed by 908

Abstract

Background: Green extraction involves using green solvents, such as water, to reduce energy consumption, avoid health and environmental hazards and induce the quality and quantity of the extract. Date palm fruits are a vital source of food and medicinal activities, as they contain a high diversity of phytochemicals, mainly phenolic and flavonoid compounds. The main aim of this study is to investigate the use of water as a green solvent, when assisted by different ultrasonic frequencies, in the extraction of four different cultivars of date palm fruits, by evaluating the phenolic and flavonoid composition as well as the antioxidant capacity of the extract. Methods: Four date palm fruits’ cultivars (Agwa, Anbarah, Khalas, and Reziz) were extracted using conventional methods (by water and ethanol) and by ultrasonic means, using two frequencies, 28 and 40 kHz, and applying temperatures (30, 45, and 60 °C), also measuring extraction times (20, 40, 60 min.). Response surface methodology was used for the statistical analysis, applying three factors (temperature, time, and ultrasonic frequency), four responses (total phenolic content, total flavonoid content, FRAP, and ABTS), and four cultivars (categories). Results: Conventional water extraction obtained minimal phenolic and flavonoid compounds (up to 52% of ethanol extraction). This percent improved to reach 60% when heat was utilized. The application of ultrasonic frequencies significantly enhanced the extraction of phenolics/flavonoids and the antioxidant ability of the extract to nearly 90% and 80%, respectively. The use of 40 kHz ultrasonic power managed to extract more phenolic and flavonoid components; however, the antioxidant capacities of the extract were less than when the 28 kHz power was utilized. Agwa and Khalas demonstrated themselves to be the best cultivars for ultrasonic-assisted extraction, depending on the results of the optimized responses. Conclusion: This study could be implemented in the industry to produce date palm fruits’ enriched extracts with phenolic and flavonoid components and/or antioxidants. Full article

(This article belongs to the Special Issue Control and Optimization of Extractive Methodologies and Analysis of Natural Products)

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Open AccessArticle

A New LC-MS Method for Evaluating the Efficacy of Pesticide Residue Removal from Fruit Surfaces by Washing Agents

Magdalena Zarębska

Zofia Hordyjewicz-Baran

Tomasz Wasilewski

Ewa Zajszły-Turko

and

Natalia Stanek

Processes 2022, 10(4), 793; https://doi.org/10.3390/pr10040793 - 18 Apr 2022

Viewed by 1350

Abstract

Modern agriculture uses pesticides to improve the quality and quantity of crops. However, pesticide residues can remain on agricultural products, posing very serious risks to human health and life. It is recommended to wash fruits and vegetables before consumption. To assess the removal efficacy of pesticide residue, a sensitive and reliable method based on ultrahigh-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) was developed and optimized for the simultaneous determination of four pesticide residues (acetamiprid, boscalid, pyraclostrobin, and pendimethalin). Isotope-labeled standards were used to validate the method in terms of recovery, linearity, matrix effects, precision, and sensitivity. The mean recovery values for both low-quality control (LQC) and high-quality control (HQC) transitions were in the range of 89–105%, and the intra-day precision was less than 13.7%. The limits of detection (LOD) and quantification (LOQ) were 0.003 mg/kg and 0.01 mg/kg, respectively. The proposed method is suitable for evaluating the quality of detergents for removing pesticide residues from fruit surfaces. Full article

(This article belongs to the Special Issue Control and Optimization of Extractive Methodologies and Analysis of Natural Products)

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Open AccessArticle

Extraction and Purification of (E)-Resveratrol from the Bark of Conifer Species

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Processes 2022, 10(4), 647; https://doi.org/10.3390/pr10040647 - 26 Mar 2022

Viewed by 1399

Abstract

(E)-Resveratrol is a naturally occurring polyphenolic compound in plants with a variety of widely studied health benefits. The bark of Northern American, Canadian, and Northern European conifer species, which is an underutilized by-product generated by forest industries, is a source of (E)-resveratrol, providing a potential value-added product for these industries. Bark may serve as a good alternative to the invasive plant Japanese knotweed (Polygonum cuspidatum), which currently is the leading commercial source of (E)-resveratrol. This work describes a method to extract and purify (E)-resveratrol from conifer bark with high yield and high purity and investigates the relationship between the amount of (E)-resveratrol and the total phenolic contents in the bark of common conifer species. In this work, barks of four conifer species were extracted and the total phenolic contents were determined by Folin–Cicoalteu’s assay. The (E)-resveratrol content was determined by HPLC-MS. A purification method that utilizes solvent extraction and column chromatography was developed to isolate (E)-resveratrol in high yield from black spruce (Picea mariana) bark. The quantitative analysis of bark samples suggests the presence of (E)-resveratrol in black spruce (Picea mariana) and Norway spruce (Picea abies), in comparable amounts to Japanese knotweed. Based on HPLC-MS and HPLC-UV analyses, the purification method isolates the compound with a yield of 84% and purity of 99%. Hence, our method extracts and isolates (E)-resveratrol from conifer bark in high purity and high yield. The results do not support any correlation between the total phenolic content and the amount of (E)-resveratrol. Full article

(This article belongs to the Special Issue Control and Optimization of Extractive Methodologies and Analysis of Natural Products)

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Open AccessArticle

Simultaneous Optimization of Extraction Yield, Phenolic Compounds and Antioxidant Activity of Moroccan Propolis Extracts: Improvement of Ultrasound-Assisted Technique Using Response Surface Methodology

Abderrazak Aboulghazi

Meryem Bakour

Mouhcine Fadil

and

Badiaa Lyoussi

Processes 2022, 10(2), 297; https://doi.org/10.3390/pr10020297 - 02 Feb 2022

Cited by 8 | Viewed by 1775

Abstract

Propolis has given rise to refreshing interest in recent years in the field of conventional medicine. Its extraction represents an important process that requires optimal conditions, which strongly affect the yield of extraction, total polyphenols, flavonoid content, and radical scavenging capacity markers. The objective of the present study was to optimize the ultrasound-assisted extraction conditions of Moroccan propolis. The studied responses were the extraction yield, total polyphenols, flavonoid contents (TPC, TFC), and antioxidant activity of the extract evaluated by DPPH-IC₅₀ and FRAP-EC₅₀ assays. The response surface methodology (RSM) and specifically the Box–Behnken design (BBD) were used, taking into account three variables: sonication time (min), solvent/propolis ratio (mL/g), and ethanol concentration (%). After the realization of experiments and data analysis, optimal response values were 15.39%, 192 mg GAE/g of propolis,45.15 mg QEq/g, 29.8 µg/mL, and 128.3 µmol Fe²⁺/g for extraction yield, TPC, TFC, DPPH-IC₅₀, and FRAP-EC₅₀, respectively. Besides, optimal ultrasound extraction conditions were 15 min for sonication time, 30 mL/g for solvent/propolis ratio, and 40% for ethanol concentration. All obtained experimental values were in good agreement with the predicted values, suggesting that using an experimental design in the ultrasound-assisted extraction process and optimization was prudently chosen. Full article

(This article belongs to the Special Issue Control and Optimization of Extractive Methodologies and Analysis of Natural Products)

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Open AccessArticle

Property Determination, FA Composition and NMR Characterization of Palm Oil, Used Palm Oil and Their Methyl Esters

Omojola Awogbemi

Daramy Vandi Von Kallon

Victor Sunday Aigbodion

and

Vuyisa Mzozoyana

Processes 2022, 10(1), 11; https://doi.org/10.3390/pr10010011 - 22 Dec 2021

Cited by 3 | Viewed by 1695

Abstract

The search for a cost-effective, environmentally friendly and sustainable feedstock for biodiesel production has attracted attention among researchers. After frying, palm oil may become thermally degraded and unsuitable for consumption. In the current effort, neat palm oil (NPO), waste palm oil earlier utilized for frying fish and chips (WPO_FC) and waste palm oil previously utilized to fry sausage and chips (WPO_SC) were transesterified into waste palm oil methyl ester, namely, WPOME_FC and WPOME_SC, respectively. The PO, WPOs and their ester derivatives were subjected to physicochemical properties, fatty acid (FA) compositions and ¹H and ¹³C nuclear magnetic resonance (NMR) analyses. The thermal degradation, transesterification process and the foods the palm oil was used to fry affected the density, kinematic viscosity, acid value, pH, iodine value and FA profile of the samples. The outcome of the characterization reveals that the ¹H and ¹³C NMR spectra of NPO, WPO_FC and WPO_SC show clear similarity, but NPO exhibits different intensities from that of the WPO samples. The absence of the peaks between δ 4.6 ppm and 5.0 ppm in the ¹H NMR spectrum signifies the complete transformation of triglycerides in the WPO samples into biodiesel. The ¹³C NMR spectrum indicates the presence of ester carbonyl carbon (C=O) in WPOME_FC and WPOME_SC, peculiar to ester, at a chemical shift ranging from 174.8 ppm to 174.9 ppm. Full article

(This article belongs to the Special Issue Control and Optimization of Extractive Methodologies and Analysis of Natural Products)

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Review

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Open AccessFeature PaperReview

Miniaturized Solid Phase Extraction Techniques Applied to Natural Products

André R. T. S. Araújo

Ofélia Anjos

and

Eugenia Gallardo

Processes 2023, 11(1), 243; https://doi.org/10.3390/pr11010243 - 11 Jan 2023

Cited by 1 | Viewed by 713

Abstract

Natural products are increasingly becoming part of our daily lives through their use in industry, food, as therapeutic agents, etc. To evaluate their possible applications, it is essential to characterize them chemically to explore their potential. Different techniques may be used to characterize natural products, including microextraction techniques. These techniques have been gaining popularity due to the advantages associated with their low use of organic solvents and the small amount of sample used relative to more classical sample preparation techniques. Their application in the extraction of compounds from natural products is still scarce. This manuscript intends to review the most used solid-based miniaturized sample preparation techniques applied to determining compounds in natural products. The main applications of these methodologies will be discussed, with a particular focus on natural product analysis, as well as their advantages and disadvantages over traditionally used sample preparation techniques. Full article

(This article belongs to the Special Issue Control and Optimization of Extractive Methodologies and Analysis of Natural Products)

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Open AccessFeature PaperReview

Extraction, Isolation, and Purification of Value-Added Chemicals from Lignocellulosic Biomass

Tanmay Chaturvedi

Laura Sini Sofia Hulkko

Malthe Fredsgaard

and

Mette Hedegaard Thomsen

Processes 2022, 10(9), 1752; https://doi.org/10.3390/pr10091752 - 02 Sep 2022

Cited by 2 | Viewed by 1311

Abstract

This review covers the operating conditions for extracting top value-added chemicals, such as levulinic acid, lactic acid, succinic acid, vanillic acid, 3-hydroxypropionic acid, xylitol, 2,5-furandicarboxylic acid, 5-hydroxymethyl furfural, chitosan, 2,3-butanediol, and xylo-oligosaccharides, from common lignocellulosic biomass. Operating principles of novel extraction methods, beyond pretreatments, such as Soxhlet extraction, ultrasound-assisted extraction, and enzymatic extraction, are also presented and reviewed. Post extraction, high-value biochemicals need to be isolated, which is achieved through a combination of one or more isolation and purification steps. The operating principles, as well as a review of isolation methods, such as membrane filtration and liquid–liquid extraction and purification using preparative chromatography, are also discussed. Full article

(This article belongs to the Special Issue Control and Optimization of Extractive Methodologies and Analysis of Natural Products)

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Open AccessReview

A Systematic Review on Waste as Sustainable Feedstock for Bioactive Molecules—Extraction as Isolation Technology

Adrian Drescher

and

Marlene Kienberger

Processes 2022, 10(8), 1668; https://doi.org/10.3390/pr10081668 - 22 Aug 2022

Viewed by 988

Abstract

In today’s linear economy, waste streams, environmental pollution, and social–economic differences are increasing with population growth. The need to develop towards a circular economy is obvious, especially since waste streams are composed of valuable compounds. Waste is a heterogeneous and complex matrix, the selective isolation of, for example, polyphenolic compounds, is challenging due to its energy efficiency and at least partially its selectivity. Extraction is handled as an emerging technology in biorefinery approaches. Conventional solid liquid extraction with organic solvents is hazardous and environmentally unfriendly. New extraction methods and green solvents open a wider scope of applications. This research focuses on the question of whether these methods and solvents are suitable to replace their organic counterparts and on the definition of parameters to optimize the processes. This review deals with the process development of agro-food industrial waste streams for biorefineries. It gives a short overview of the classification of waste streams and focuses on the extraction methods and important process parameters for the isolation of secondary metabolites. Full article

(This article belongs to the Special Issue Control and Optimization of Extractive Methodologies and Analysis of Natural Products)

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Open AccessReview

Potential Applications of the Cytisus Shrub Species: Cytisus multiflorus, Cytisus scoparius, and Cytisus striatus

and

Processes 2022, 10(7), 1287; https://doi.org/10.3390/pr10071287 - 30 Jun 2022

Viewed by 873

Abstract

Cytisus spp. is present throughout the Portuguese territory. Although most of these species are considered native in Portugal, at least one species has already been reported as invasive in other parts of the world. Different measures of control have been investigated, and the application of herbicides is the most commonly used. This review gathers information about the biochemical profile and analytical methods used for the evaluation of the potential bioactivities of three species of the genus Cytisus, better known as brooms, which were used in traditional medicine through the production of infusions and decoctions for the treatment of several health problems, mainly due to their high value of phenolic compounds. However, little research has been conducted on its biological activities as a potential antioxidant, anti-inflammatory, and antimicrobial agent. Furthermore, one species (Cytisus striatus) has not been subjected to extensive research in identifying chemical compounds and evaluating their potential bioactivities. This species (known as the Portuguese broom) has a great expression in one of the forest typologies with a considerable percentage in Portugal. This research work is essential to encourage a scientific and sustainable valorisation of Cytisus spp. (namely C. striatus), which will consequently contribute to forest cleaning and management to reduce the risk of wildfires. Full article

(This article belongs to the Special Issue Control and Optimization of Extractive Methodologies and Analysis of Natural Products)

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Open AccessEditor’s ChoiceReview

Isolation and Analysis of Carotenoids in Hungary from Zechmeister until Today

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Processes 2022, 10(4), 707; https://doi.org/10.3390/pr10040707 - 05 Apr 2022

Viewed by 847

Abstract

László Zechmeister, one of the most important pioneers of carotenoid chemistry, died 50 years ago. He founded a carotenoid research group in Pécs (Hungary), which is the only place in the world where carotenoid research has been conducted continuously over the past 95 years. This review presents the life of Zechmeister and gives a summary about the evolution of the methods of analysis, isolation, and structure elucidation of carotenoids from the 1930s until today, based on the results of the research group founded by Zechmeister. Full article

(This article belongs to the Special Issue Control and Optimization of Extractive Methodologies and Analysis of Natural Products)

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