Extraction and Analysis of Natural Product in Plant

A special issue of Agronomy (ISSN 2073-4395). This special issue belongs to the section "Agricultural Biosystem and Biological Engineering".

Deadline for manuscript submissions: closed (31 December 2020) | Viewed by 61485

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Department of Analytical Chemistry, Faculty of Sciences, IVAGRO, Agrifood Campus of International Excellence (ceiA3), University of Cadiz, 11510 Puerto Real, Cadiz, Spain
Interests: chemometrics; fire investigation; headspace-mass spectrometry electronic nose; ignitable liquids; petroleum-based products; volatile organic compounds; food adulteration; ion mobility spectroscopy; forensic chemistry; food analysis; analytical chemistry; HPLC; GC; UHPLC; MS; extraction techniques
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Special Issue Information

Dear colleagues,

Plants are a source of a large number and amount of natural compounds, many of them with great biological importance as antioxidants, anti-inflammatory, antimicrobial, anti-cancer, etc. For this reason, many of these plants and their extracts, are commonly used in agri-food, pharmaceutical or agrochemical industries. In this sense, the techniques of extraction of natural compounds in plants are used with a double purpose:  (i) to extract compounds for the analysis of the content of natural compounds in plant matrix (quality control of raw material, intermediate products, and final products ); (ii) to extract and obtain extracts rich in these natural compounds to be used for different purposes (food, pharmaceutical or chemical products, etc.).

This special volume will focus on the extraction, identification, analysis and use of natural compounds present in plants, for both, analytical and industrial purposes. We welcome novel research and reviews covering all related topics in extraction methods of natural compounds in plants (ultrasound assisted extraction, microwave assisted extraction, pressurized liquid extraction, supercritical fluid extraction, etc.), identification and analysis of natural compounds in plants, the obtaining and the usage of plant extracts, the use of by-products from the agri-food industry and, the quality control of raw materials, intermediate products and final products of plant origin.

Dr. Gerardo Fernández Barbero
Guest Editor

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Keywords

  • natural products extraction
  • identification
  • analysis
  • ultrasound assisted extraction
  • microwave assisted extraction
  • pressurized liquid extraction
  • supercritical fluid extraction
  • quality control
  • by-products valorization

Published Papers (17 papers)

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Editorial

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4 pages, 197 KiB  
Editorial
Extraction and Analysis of Natural Product in Plant
by Gerardo F. Barbero
Agronomy 2021, 11(3), 415; https://0-doi-org.brum.beds.ac.uk/10.3390/agronomy11030415 - 25 Feb 2021
Cited by 8 | Viewed by 2066
Abstract
Plants are well known for being a major source of natural compounds, many of them generally considered of biological interest for their antioxidant, anti-inflammatory, antimicrobial or anti-cancerogenic properties [...] Full article
(This article belongs to the Special Issue Extraction and Analysis of Natural Product in Plant)

Research

Jump to: Editorial, Review

13 pages, 2124 KiB  
Article
Process Optimization for Ultrasound-Assisted Starch Production from Cassava (Manihot esculenta Crantz) Using Response Surface Methodology
by Widiastuti Setyaningsih, Karmila, Rohmah Nur Fathimah and Muhammad Nur Cahyanto
Agronomy 2021, 11(1), 117; https://0-doi-org.brum.beds.ac.uk/10.3390/agronomy11010117 - 09 Jan 2021
Cited by 12 | Viewed by 3650
Abstract
Ultrasound-assisted extraction (UAE) has been optimized to improve the current cassava starch production by conventional maceration for the extraction method. Evaluation of several extraction parameters disclosed significant effects (p < 0.05) by three studied factors (ultrasound power, x1; pulse duty-cycle, [...] Read more.
Ultrasound-assisted extraction (UAE) has been optimized to improve the current cassava starch production by conventional maceration for the extraction method. Evaluation of several extraction parameters disclosed significant effects (p < 0.05) by three studied factors (ultrasound power, x1; pulse duty-cycle, x2; and solvent to sample ratio, x3). Subsequently, a Box-Behnken design (BBD) in conjunction with response surface methodology (RSM) was employed to optimise the three factors at three levels: x1 (30, 60, 90%), x2 (0.3, 0.6, 0.9 s−1), and x3 (10:1, 20:1, 30:1). The model built for the RSM was validated through the coefficient of determination (R2 > 0.95), prediction error (2.12%), and lack-of-fit (0.71) values. The model validation suggested that the RSM was adequate for the observed data at the 95.0% confidence level. The optimum yield of cassava starch extraction was achieved by applying 90% for ultrasound power, pulse duty-cycle of 1.0 s−1, and solvent to sample ratio of 30:1 with 10 min extraction time. Finally, the UAE produced starch with a purity of 88.36% and a lower viscosity than the commercial sample due to the granules’ size alteration. Hence, apart from speeding up the extraction process, UAE was worthwhile for the starch modification that could maintain the viscosity at a lower value (1920 cP) than the commercial starch (1996 cP) at the highest studied temperature treatment of 70 °C. Full article
(This article belongs to the Special Issue Extraction and Analysis of Natural Product in Plant)
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15 pages, 1373 KiB  
Article
Optimization and Comparison of Ultrasound and Microwave-Assisted Extraction of Phenolic Compounds from Cotton-Lavender (Santolina chamaecyparissus L.)
by Mohammed Aourach, Ana V. González-de-Peredo, Mercedes Vázquez-Espinosa, Haiat Essalmani, Miguel Palma and Gerardo F. Barbero
Agronomy 2021, 11(1), 84; https://0-doi-org.brum.beds.ac.uk/10.3390/agronomy11010084 - 04 Jan 2021
Cited by 20 | Viewed by 3546
Abstract
The interest in natural phenolic compounds has increased because of their attractive use especially as antioxidant and antimicrobial agents in foods. The large content in phenolic compounds of interest in Santolina chamaecyparissus L. (S. chamaecyparissus) makes this plant a target source [...] Read more.
The interest in natural phenolic compounds has increased because of their attractive use especially as antioxidant and antimicrobial agents in foods. The large content in phenolic compounds of interest in Santolina chamaecyparissus L. (S. chamaecyparissus) makes this plant a target source that is worthy of note. In this work, new extraction technologies comprising ultrasound (UAE) and microwave (MAE) assisted extraction of the phenolic compounds in S. chamaecyparissus have been developed, optimized, and compared. Several extraction factors have been optimized based on a Box-Behnken design. Such optimized factors include the percentage of methanol in water (25–75%), the temperature (10–70 °C), the ultrasound amplitude (20–80%), the ultrasound cycle (0.2–1 s), the solvent pH (2–7) and the solvent-sample ratio (5/0.2–15/0.2 mL/g) with regard to UAE, while the percentage of methanol in water (50–100%), the temperature (50–100 °C), the pH (2–7) and the solvent-sample ratio (5/0.2–15/0.2 mL/g) were optimized for MAE. The solvent composition was the most influential parameter both on MAEs (64%) and UAEs (74%). The extraction optimum time was established as 15 min for MAE and 25 min for UAE. Five major phenolic compounds were detected and identified by Ultra-High-Performance Liquid Chromatography—Quadrupole Time of Flight—Mass Spectrometry (UHPLC-QToF-MS) in the extracts: chlorogenic acid, quercetin 3-O-galactoside, quercetin 3-O-glucoside, isoorientin, and cynarin. With the exception of chlorogenic acid, the other four compounds have been identified for the first time in S. chamaecyparissus. The findings have confirmed that MAE is a significantly more efficient extraction method than UAE to extract phenolic compounds from S. chamaecyparissus. Full article
(This article belongs to the Special Issue Extraction and Analysis of Natural Product in Plant)
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20 pages, 5800 KiB  
Article
Bioactive Compounds and Antiradical Activity of the Rosa canina L. Leaf and Twig Extracts
by Małgorzata Kubczak, Ainur B. Khassenova, Bartosz Skalski, Sylwia Michlewska, Marzena Wielanek, Araylim N. Aralbayeva, Maira K. Murzakhmetova, Maria Zamaraeva, Maria Skłodowska, Maria Bryszewska and Maksim Ionov
Agronomy 2020, 10(12), 1897; https://0-doi-org.brum.beds.ac.uk/10.3390/agronomy10121897 - 01 Dec 2020
Cited by 12 | Viewed by 2761
Abstract
It is important to search for new sources of bioactive, natural compounds, because customers are paying more attention to food quality. Fruits and berries from horticultural plants are known to be good sources of agents beneficial for human well-being and could serve as [...] Read more.
It is important to search for new sources of bioactive, natural compounds, because customers are paying more attention to food quality. Fruits and berries from horticultural plants are known to be good sources of agents beneficial for human well-being and could serve as natural preservatives in the food industry. However, more recent research indicates that other plant organs can also be rich in nutrients. Our study focused on characterizing an unexplored source, namely leaf and twig extracts from Rosa canina. The chemical composition of these extracts was analyzed and their in vitro activity measured. HPLC analysis of the content of phenolics, vitamins and amino acids revealed that the leaf and twig extracts were found to be rich in bioactive compounds with potent antioxidant properties. The greatest differences between bioactive phenolic compounds in leaf and twig extracts related mainly to p-coumaric acid, myricetin, ellagic acid, cyanidin, procyanidin and quercetin, whereas salicylic acid levels were similar in both types of extract. Interactions with human serum albumin were investigated, and some conformational changes in protein structure were observed. Further analysis (lipid peroxidation, protein carbonylation, thiol group oxidation, DPPH inhibition and ROS inhibition) confirmed that both leaf and twig extracts exhibited antioxidant and antiradical scavenging activities. Cytotoxicity and hemotoxicity assays confirmed very low toxicity of the extracts towards human cells over the range of concentrations tested. Our results indicate that both extracts could serve as non-toxic sources of bioactive compounds with antiradical properties. Full article
(This article belongs to the Special Issue Extraction and Analysis of Natural Product in Plant)
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11 pages, 1169 KiB  
Article
Comparison of Flavonoid Profiles in Sprouts of Radiation Breeding Wheat Lines (Triticum aestivum L.)
by Ah-Reum Han, Min Jeong Hong, Bomi Nam, Bo-Ram Kim, Hyeon Hwa Park, Inwoo Baek, Yun-Seo Kil, Joo-Won Nam, Chang Hyun Jin and Jin-Baek Kim
Agronomy 2020, 10(10), 1489; https://0-doi-org.brum.beds.ac.uk/10.3390/agronomy10101489 - 01 Oct 2020
Cited by 8 | Viewed by 2449
Abstract
Wheat (Triticum aestivum Linn.; Poaceae), one of the most popular food crops worldwide, contains basic and essential nutrients and various health benefiting phytochemicals. Among them, flavonoids have attracted significant interest owing to their various health-promoting properties. In this study, 35 wheat mutant [...] Read more.
Wheat (Triticum aestivum Linn.; Poaceae), one of the most popular food crops worldwide, contains basic and essential nutrients and various health benefiting phytochemicals. Among them, flavonoids have attracted significant interest owing to their various health-promoting properties. In this study, 35 wheat mutant lines were developed via gamma-irradiated mutation breeding from the original cultivar. The effects of radiation breeding on the endogenous phytochemical production in the sprouts of these mutant lines were investigated using high performance liquid chromatography-diode array detector-electrospray ionization mass spectrometry (HPLC-DAD-ESIMS) with multivariate analysis for the first time in this study. Fourteen characteristic peaks, including eleven flavone C-glycosides, two flavone O-glycosides, and one flavone, were identified. In addition, the contents of three flavone C-glycosides, namely, isoschaftoside, isoorientin, and isoscoparin, in 37 wheat sprout samples from the original cultivar, certificated cultivar, and the mutant lines were determined. A heat map combined with hierarchical clustering showed variation in the relative content for the flavonoids between the 37 wheat sprout samples, clustering into three groups. On principal component analysis scores scatter and loading plots, significant differences in the levels of flavonoids were found between the samples and several markers responsible for group separation were detected. These results provide a scientific reference for the phytochemical variation in wheat mutant lines, thereby aiding in further mutation mechanism studies and for the quality control of the improved wheat cultivars. Full article
(This article belongs to the Special Issue Extraction and Analysis of Natural Product in Plant)
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14 pages, 2027 KiB  
Article
Effects of the Extraction Technology on Pomegranate Juice Quality
by Pietro Catania, Antonio Comparetti, Claudio De Pasquale, Giuseppe Morello and Mariangela Vallone
Agronomy 2020, 10(10), 1483; https://0-doi-org.brum.beds.ac.uk/10.3390/agronomy10101483 - 28 Sep 2020
Cited by 6 | Viewed by 2843
Abstract
Pomegranate juice is a rich source of phenolic components; its consumption has considerably increased throughout the world in recent years, due to its nutraceutical properties. Commercial juice production involves pressing the fruits. The aim of this study was to assess the influence of [...] Read more.
Pomegranate juice is a rich source of phenolic components; its consumption has considerably increased throughout the world in recent years, due to its nutraceutical properties. Commercial juice production involves pressing the fruits. The aim of this study was to assess the influence of the pressing stage on pomegranate juice properties, in terms of value, duration of the applied pressure and juice yield in order to examine the influence of pressure level on volatiles and nutraceutical properties of the juice. Pomegranate fruits cv. Wonderful One were manually harvested and mechanically processed for extracting the juice by means of a shelling machine, a peristaltic pump and a pneumatic press. Chemical analytical determinations were performed on the juice samples corresponding to the different pressure levels applied. They did not show a univocal trend with respect to the increase in pressure; total phenol content values gradually increased as the pressure applied increased, conversely the highest total anthocyanins value was obtained in the first step of the process (552 mg L−1), afterwards a 40% decrease occurred. More than forty Volatile Organic Compounds were identified in the obtained pomegranate juices. The results showed a significant increase in the values in some compounds, particularly for pressure values higher than 0.7 bar, while in others there was a significant decrease as pressure increases. Therefore, the application of different pressure values during pomegranate juice extraction process allowed to obtain products of different quality. Full article
(This article belongs to the Special Issue Extraction and Analysis of Natural Product in Plant)
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13 pages, 2184 KiB  
Article
The Influence of UV on the Production of Free Terpenes in Vitis vinifera cv. Shiraz
by Wen Miao, Jiaqiang Luo, Junda Liu, Kate Howell and Pangzhen Zhang
Agronomy 2020, 10(9), 1431; https://0-doi-org.brum.beds.ac.uk/10.3390/agronomy10091431 - 20 Sep 2020
Cited by 9 | Viewed by 2930
Abstract
Terpenes contribute to the desirable flavour and aroma of grapes and wine. The biosynthesis of these plant secondary metabolites is influenced by both physiological and environmental factors, such as grapevine phenological stage and sunlight exposure. In this study, we investigated the influence of [...] Read more.
Terpenes contribute to the desirable flavour and aroma of grapes and wine. The biosynthesis of these plant secondary metabolites is influenced by both physiological and environmental factors, such as grapevine phenological stage and sunlight exposure. In this study, we investigated the influence of ultraviolet (UV) at different grapevine phenological stages on free terpenes in grape at harvest. Two types of transparent polymer films were applied to grape bunches to eliminate both UV-A and UV-B or only eliminate UV-B, followed by the identification and quantification of terpenes using headspace solid-phase microextraction with gas chromatography–mass spectrometry (HS–SPME–GC–MS) analysis. In all, 27 free terpenes were identified, including eight monoterpenes/monoterpenoids, four norisoprenoids and fifteen sesquiterpenes. Higher concentrations of γ-terpinene, linalool and β-damascenone were observed in grapes with UV-B attenuation compared to the naturally exposed grape bunches. Elevated α-muurolene was observed in UV-attenuated grapes from pre-veraison to harvest, while higher concentrations of γ-cadinene were observed in naturally exposed grapes. The impacts of UV exclusion on grape terpenes at harvest were specific to phenological stages, where applying UV films from veraison to intermediate ripeness reduced the concentrations of key terpenes in grape harvest and UV attenuation from intermediate ripeness to harvest promoted the accumulation of α-muurolene and γ-cadinene. This study provides information for viticulturists to better manage grape terpene composition through UV shading. Full article
(This article belongs to the Special Issue Extraction and Analysis of Natural Product in Plant)
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14 pages, 1279 KiB  
Article
Changes in Capsiate Content in Four Chili Pepper Genotypes (Capsicum spp.) at Different Ripening Stages
by Mercedes Vázquez-Espinosa, Oreto Fayos, Ana V. González-de-Peredo, Estrella Espada-Bellido, Marta Ferreiro-González, Miguel Palma, Ana Garcés-Claver and Gerardo F. Barbero
Agronomy 2020, 10(9), 1337; https://0-doi-org.brum.beds.ac.uk/10.3390/agronomy10091337 - 05 Sep 2020
Cited by 10 | Viewed by 4271
Abstract
Interest in the consumption of the fruits of pepper (Capsicum spp.) is not only due to its organoleptic characteristics, but also due to its bioactive compounds content, which are reported to provide essential benefits to human health. However, the amount and diversity [...] Read more.
Interest in the consumption of the fruits of pepper (Capsicum spp.) is not only due to its organoleptic characteristics, but also due to its bioactive compounds content, which are reported to provide essential benefits to human health. However, the amount and diversity of these compounds in each fruit specimen depend on its genotype and on a number of environmental factors. This work describes the quantitative ultra-high-performance liquid chromatography coupled to photodiode-array (UHPLC-PDA) analysis of the capsinoids content in four varieties of pepper (‘Habanero’, ‘Habanero Roxo’, ‘Bode’, and ‘Malagueta’) grown until different development stages in a greenhouse under controlled conditions. In all the varieties analyzed, capsiate was the only capsinoid found. The accumulation of capsiate, in all the pepper varieties, started from the 10th to the 20th day post-anthesis (dpa), and increased during the first days (between the 20th and the 27th dpa). From that moment a drastic reduction took place until the end of the ripening stage, except for ‘Bode’ peppers, where the capsiate content increased from the first harvest point on the 20th dpa up to the 76th dpa. The capsiate accumulation patterns over the development of the fruit has been related to the capsaicionoids accumulation patterns in the same samples of the four varieties of pepper. According to our results, the content evolution of both families of compounds will vary depending on each fruit’s genotype, as well as on environmental conditions. No clear trends have been established and, therefore, an in-depth analysis under controlled conditions should be carried out. Full article
(This article belongs to the Special Issue Extraction and Analysis of Natural Product in Plant)
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9 pages, 447 KiB  
Communication
Physicochemical and Nutritional Characterization of Winemaking Lees: A New Food Ingredient
by Pau Sancho-Galán, Antonio Amores-Arrocha, Ana Jiménez-Cantizano and Víctor Palacios
Agronomy 2020, 10(7), 996; https://0-doi-org.brum.beds.ac.uk/10.3390/agronomy10070996 - 11 Jul 2020
Cited by 10 | Viewed by 3342
Abstract
Wine lees are defined as the sediment formed at the bottom of the tank or barrel after wine alcoholic fermentation. They have a heterogeneous composition and currently constitute 6% of the byproducts generated by each ton of wine grapes. However, it is the [...] Read more.
Wine lees are defined as the sediment formed at the bottom of the tank or barrel after wine alcoholic fermentation. They have a heterogeneous composition and currently constitute 6% of the byproducts generated by each ton of wine grapes. However, it is the most under-researched of all the byproducts of the winemaking process. Therefore, with the aim of highlighting this byproduct, a physicochemical and nutritional characterization of winemaking lees from three different wine making processes (white, rosé, and red winemaking) was carried out. In addition, the technological properties of these winemaking lees were also analyzed. The lees analyzed in this research demonstrated an interesting nutritional and heterogeneous composition. Moreover, wine lees showed high values of emulsifying capacity. Thus, winemaking lees could be considered, in a preliminary way, as a new ingredient to be included in new food formulations. Full article
(This article belongs to the Special Issue Extraction and Analysis of Natural Product in Plant)
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22 pages, 1458 KiB  
Article
Optimization of Analytical Ultrasound-Assisted Methods for the Extraction of Total Phenolic Compounds and Anthocyanins from Sloes (Prunus spinosa L.)
by Ana V. González-de-Peredo, Mercedes Vázquez-Espinosa, Estrella Espada-Bellido, Marta Ferreiro-González, Ceferino Carrera, Miguel Palma, José Ángel Álvarez, Gerardo F. Barbero and Jesús Ayuso
Agronomy 2020, 10(7), 966; https://0-doi-org.brum.beds.ac.uk/10.3390/agronomy10070966 - 04 Jul 2020
Cited by 18 | Viewed by 2927
Abstract
Prunus spinosa L. is a shrub that produces berries—sloes—with a high content of phenolic compounds and anthocyanins. Numerous consumer products are made from sloes, such as “Pacharán” liquors or jams. For these reasons, it is crucial to design accurate analytical methods for the [...] Read more.
Prunus spinosa L. is a shrub that produces berries—sloes—with a high content of phenolic compounds and anthocyanins. Numerous consumer products are made from sloes, such as “Pacharán” liquors or jams. For these reasons, it is crucial to design accurate analytical methods for the extraction of these bioactive compounds in order to promote their consumption and to improve our health. In this study, an ultrasound-assisted extraction method was developed to extract phenolic compounds and anthocyanins from sloes. Several process variables (methanol composition, pH, temperature, cycle, amplitude, and sample–solvent ratio) were optimized based on a Box–Behnken design. The most influential parameters for the extraction of total phenolic compounds were the cycle, the percentage of methanol, and pH of the extraction solvent, with 0.2 s, 67%, and pH 7 as their optimal values, respectively. For total anthocyanins, all parameters were influential, with 44% methanol at pH 2, 48 °C, 0.2 s cycles, 30% amplitude, and 1.5 g/20 mL ratio as the optimal values for their corresponding variables. Both methods showed high recoveries, short time use, and high precision (RSD < 5%). In addition, the sloe liqueur “Pacharán” and sloe jams were analyzed to demonstrate the applicability of these methods for the extraction of the real matrix. Full article
(This article belongs to the Special Issue Extraction and Analysis of Natural Product in Plant)
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17 pages, 9906 KiB  
Article
Sustainability: Obtaining Natural Dyes from Waste Matrices Using the Prickly Pear Peels of Opuntia ficus-indica (L.) Miller
by Pierpaolo Scarano, Daniele Naviglio, Antonello Prigioniero, Maria Tartaglia, Alessia Postiglione, Rosaria Sciarrillo and Carmine Guarino
Agronomy 2020, 10(4), 528; https://0-doi-org.brum.beds.ac.uk/10.3390/agronomy10040528 - 07 Apr 2020
Cited by 21 | Viewed by 4949
Abstract
In this work, the effect of dyes extracted through the Naviglio method (an eco-innovative solid-liquid extraction technique) was tested, which proved interesting for such an extraction. The dyes extracted from Opuntia ficus-indica (L.) Miller waste were treated to maximize the extraction of the [...] Read more.
In this work, the effect of dyes extracted through the Naviglio method (an eco-innovative solid-liquid extraction technique) was tested, which proved interesting for such an extraction. The dyes extracted from Opuntia ficus-indica (L.) Miller waste were treated to maximize the extraction of the coloring molecules. The extraction method was compared with conventional methods under the same conditions. The results showed that the extracts obtained with the different techniques, in the same extraction conditions (solvent, pH, temperature, time), were richer in the pigments for the extract obtained with the Naviglio method. The stability of the dyes was tested before the staining. A plant-based fiber, cotton, as well as an animal-based fiber, wool, were chosen for the staining tests. For the two types of fiber, two etching methods were used: one with rock alum, a method widely used to fix a color and one with lemon juice, a method used for a long time by rural populations who practiced the coloring of hides and tissues. In addition, the qualitative content of the pigments was also verified with an HPLC profile of the Opuntia ficus-indica (L.) Miller extracts. Ultimately, the results suggest that the Opuntia ficus-indica (L.) Miller fruit can be of great interest as a natural source of dyes and be used for tinctures. Full article
(This article belongs to the Special Issue Extraction and Analysis of Natural Product in Plant)
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14 pages, 1263 KiB  
Article
Extraction of Anthocyanins and Total Phenolic Compounds from Açai (Euterpe oleracea Mart.) Using an Experimental Design Methodology. Part 2: Ultrasound-Assisted Extraction
by María José Aliaño-González, Estrella Espada-Bellido, Marta Ferreiro-González, Ceferino Carrera, Miguel Palma, Jesús Ayuso, José Ángel Álvarez and Gerardo F. Barbero
Agronomy 2020, 10(3), 326; https://0-doi-org.brum.beds.ac.uk/10.3390/agronomy10030326 - 28 Feb 2020
Cited by 23 | Viewed by 3072
Abstract
Two optimized methods for ultrasound-assisted extraction were evaluated for the extraction of two types of acai bioactive compounds: Total anthocyanins (TAs) and total phenolic compounds (TPCs). For the extraction optimization, a Box Behnken factorial design of different variables in the following intervals was [...] Read more.
Two optimized methods for ultrasound-assisted extraction were evaluated for the extraction of two types of acai bioactive compounds: Total anthocyanins (TAs) and total phenolic compounds (TPCs). For the extraction optimization, a Box Behnken factorial design of different variables in the following intervals was used: Methanol-water (25%–75%) for solvent composition, temperatures between 10 and 70 °C, amplitude in the range between 30% and 70% of the maximum amplitude −200 W), extraction solvent pH (2–7), the ratio for sample-solvent (0.5 g:10 mL–0.5 g:20 mL), and cycle between 0.2 and 0.7 s. The extraction kinetics were studied using different periods between 5 and 30 min. TA and TPC were analyzed by UHPLC and the Folin–Ciocalteu method, respectively. Optimized conditions for TA were: 51% MeOH in water, 31 °C temperature, pH 6.38, cycle 0.7 s, 65% amplitude, and 0.5 g:10 mL of sample-solvent ratio. Optimized conditions for the TPC were: 49% MeOH in water, 41 °C temperature, pH 6.98, cycle 0.2 s, 30% amplitude, and 0.5 g:10 mL of sample-solvent ratio. Both methods presented a relative standard deviation below 5% in the precision study. The suitability of the methods was tested in real samples. It was confirmed that these methods are feasible for the extraction of the studied bioactive compounds from different açai matrices. Full article
(This article belongs to the Special Issue Extraction and Analysis of Natural Product in Plant)
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15 pages, 2402 KiB  
Article
Influence of Fruit Ripening on the Total and Individual Capsaicinoids and Capsiate Content in Naga Jolokia Peppers (Capsicum chinense Jacq.)
by Mercedes Vázquez-Espinosa, José Arturo Olguín-Rojas, Oreto Fayos, Ana V. González-de-Peredo, Estrella Espada-Bellido, Marta Ferreiro-González, Carmelo G. Barroso, Gerardo F. Barbero, Ana Garcés-Claver and Miguel Palma
Agronomy 2020, 10(2), 252; https://0-doi-org.brum.beds.ac.uk/10.3390/agronomy10020252 - 08 Feb 2020
Cited by 16 | Viewed by 3838
Abstract
“Naga Jolokia” (Capsicum chinense Jacq.) is a hot pepper variety native to India which has received the attention of the global scientific community due to its high capsaicinoid concentration. The present study evaluated the influence of fruit ripening on the total and [...] Read more.
“Naga Jolokia” (Capsicum chinense Jacq.) is a hot pepper variety native to India which has received the attention of the global scientific community due to its high capsaicinoid concentration. The present study evaluated the influence of fruit ripening on the total and individual capsaicinoids, as well as capsiate content. The aim was to determine the optimal moment to harvest the peppers depending on their pungent properties. Ultrasound-assisted extraction (UAE) using methanol as the extraction solvent and reverse-phase ultra-high-performance liquid chromatography (UHPLC-photodiode array (PDA)) were employed. Capsaicinoids gradually accumulated in the peppers from the moment they started growing until they reached a maximum concentration (7.99 ± 0.11 mg g−1 of fresh weight (FW)) at 33 days postanthesis (dpa). For this reason, based on its content of pungent compounds, as it is one of the main attributes of this variety, the optimal time for collection would be on day 33. From then on, there was a sharp decrease (96.35% of the total concentration) due to the peroxidase enzymes. The evolution of the principal capsaicinoids in “Naga Jolokia” peppers had a different behavior with respect to literature reports. After this investigation, these changes in content can be attributed to each pepper genotype. Capsiate content reached it maximum value at 19 dpa (0.27 ± 0.01 mg g−1 of FW). Then, there was a gradual drop due to the activities of different peroxidases. Given the important biological activity of capsaicinoids and capsinoids, the information described here allows for determining the ideal time to harvest “Naga Jolokia” peppers. Full article
(This article belongs to the Special Issue Extraction and Analysis of Natural Product in Plant)
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17 pages, 1650 KiB  
Article
Extraction of Anthocyanins and Total Phenolic Compounds from Açai (Euterpe oleracea Mart.) Using an Experimental Design Methodology. Part 1: Pressurized Liquid Extraction
by María José Aliaño-González, Marta Ferreiro-González, Estrella Espada-Bellido, Ceferino Carrera, Miguel Palma, José A. Álvarez, Jesús Ayuso and Gerardo F. Barbero
Agronomy 2020, 10(2), 183; https://0-doi-org.brum.beds.ac.uk/10.3390/agronomy10020183 - 28 Jan 2020
Cited by 20 | Viewed by 4452
Abstract
Currently, açai is one of the most important fruits present in the world. Several studies have demonstrated its high content in phenolic compounds and anthocyanins. Both of them are responsible of interesting properties of the fruit such as anti-inflammatory, antioxidant or anticancer. In [...] Read more.
Currently, açai is one of the most important fruits present in the world. Several studies have demonstrated its high content in phenolic compounds and anthocyanins. Both of them are responsible of interesting properties of the fruit such as anti-inflammatory, antioxidant or anticancer. In the present study, two optimized pressurized liquid extraction (PLE) methods have been developed for the extraction of anthocyanins and total phenolic compounds from açai. A full factorial design (Box–Behnken design) with six variables (solvent composition (25–75% methanol-in-water), temperature (50–100 °C), pressure (100–200 atm), purge time (30–90 s), pH (2–7) and flushing (50–150%)) were employed. The percentage of methanol in the extraction solvent was proven to be the most significant variable for the extraction of anthocyanins. In the case of total phenolic compounds, the extraction temperature was the most influential variable. The developed methods showed high precision, with relative standard deviations (RSD) of less than 5%. The applicability of the methods was successfully evaluated in real samples. In conclusion, two rapid and reliable PLE extraction methods to be used for laboratories and industries to determine anthocyanins and total phenolic compounds in açai and its derived products were developed in this work. Full article
(This article belongs to the Special Issue Extraction and Analysis of Natural Product in Plant)
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15 pages, 1589 KiB  
Article
Extraction of Anthocyanins and Total Phenolic Compounds from Açai (Euterpe oleracea Mart.) Using an Experimental Design Methodology. Part 3: Microwave-Assisted Extraction
by María José Aliaño-González, Marta Ferreiro-González, Estrella Espada-Bellido, Ceferino Carrera, Miguel Palma, Jesús Ayuso, Gerardo F. Barbero and José Á. Álvarez
Agronomy 2020, 10(2), 179; https://0-doi-org.brum.beds.ac.uk/10.3390/agronomy10020179 - 27 Jan 2020
Cited by 14 | Viewed by 3801
Abstract
In this work, two methods based on microwave-assisted extraction techniques for the extraction of both anthocyanins and total phenolic compounds from açai have been developed. For that, a full factorial design (Box-Behnken design) has been used to optimize the following four variables: solvent [...] Read more.
In this work, two methods based on microwave-assisted extraction techniques for the extraction of both anthocyanins and total phenolic compounds from açai have been developed. For that, a full factorial design (Box-Behnken design) has been used to optimize the following four variables: solvent composition (25–75% methanol in water), temperature (50–100 °C), pH (2–7), and sample/solvent ratio (0.5 g: 10 mL–0.5 g: 20 mL). The anthocyanins and total phenolic compounds content have been determined by ultra high-pressure liquid chromatography and Folin-Ciocalteu method, respectively. The optimum conditions for the extraction of anthocyanins were 38% MeOH in water, 99.63 °C, pH 3.00, at 0.5 g: 10 mL of ratio, while for the extraction of total phenolic compounds they were 74.16% MeOH in water, 99.14 °C, pH 5.46, at 0.5 g: 20 mL of ratio. Both methods have shown a high repeatability and intermediate precision with a relative standard deviation lower than 5%. Furthermore, an extraction kinetics study was carried out using extraction periods ranging from 2 min until 25 min. The optimized methods have been applied to açai-containing real samples. The results with such real samples have confirmed that both methods are suitable for a rapid and reliable extraction of anthocyanins and total phenolic compounds. Full article
(This article belongs to the Special Issue Extraction and Analysis of Natural Product in Plant)
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18 pages, 5505 KiB  
Article
Response Surface Modeling and Optimization of Polyphenols Extraction from Apple Pomace Based on Nonionic Emulsifiers
by Liubov Skrypnik and Anastasia Novikova
Agronomy 2020, 10(1), 92; https://0-doi-org.brum.beds.ac.uk/10.3390/agronomy10010092 - 09 Jan 2020
Cited by 34 | Viewed by 4307
Abstract
The factors affecting the efficiency of micelle-mediated extraction of phenolic compounds from apple pomace was investigated. Higher extraction efficiency by using as a solvent an aqueous solution of Tween 80 in comparison to Triton X-100, Span 20, Tween 20, 70% ethanol, and water [...] Read more.
The factors affecting the efficiency of micelle-mediated extraction of phenolic compounds from apple pomace was investigated. Higher extraction efficiency by using as a solvent an aqueous solution of Tween 80 in comparison to Triton X-100, Span 20, Tween 20, 70% ethanol, and water was shown. Four independent variables (Tween 80 concentration, time, solvent-to material ratio, and pH) to enhance the recovery of polyphenols from apple pomace was investigated. Applying response surface methodology, the second order polynomial regression equation showing dependence of the yield of polyphenols on the extraction parameters was derived. The adjusted regression coefficient (R2 = 98.73%) and the lack-of-fit test (p > 0.05) showed a good accuracy of the developed model. The difference between observed and predicted values was no more than 3%. The optimal extraction conditions were found to be Tween 80 concentration of 1.14%, time of 65 min, solvent-to-material ratio of 104 mL g−1, pH of 3.8. Under optimal conditions the predicted total phenolic compounds content was 7.75 mg g−1. The obtained apple pomace extracts were characterized in terms of their antioxidant activity. The proposed extraction technology by using Tween 80 aqueous solution as a solvent allows obtaining the extracts with high content of polyphenols which are suitable for the applications in food, cosmetic, and pharmaceutical products requiring a surfactant to stabilize them. Full article
(This article belongs to the Special Issue Extraction and Analysis of Natural Product in Plant)
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Review

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20 pages, 739 KiB  
Review
Bioactive Compounds, Therapeutic Activities, and Applications of Ficus pumila L.
by Zhi-Yong Qi, Jia-Ying Zhao, Fang-Jun Lin, Wan-Lai Zhou and Ren-You Gan
Agronomy 2021, 11(1), 89; https://0-doi-org.brum.beds.ac.uk/10.3390/agronomy11010089 - 05 Jan 2021
Cited by 10 | Viewed by 4201
Abstract
Ficus pumila L. has been used as a functional plant for a long time in East Asia, especially its fruits, as a dietary component in Japan and parts of China. A series of bioactive compounds, including phenolic acids, flavonoids, terpenoids, alcohols, and steroids, [...] Read more.
Ficus pumila L. has been used as a functional plant for a long time in East Asia, especially its fruits, as a dietary component in Japan and parts of China. A series of bioactive compounds, including phenolic acids, flavonoids, terpenoids, alcohols, and steroids, have been extracted from the stems, leaves, flowers, and fruits of Ficus pumila L. Accumulated studies have demonstrated that Ficus pumila L. has multiple therapeutic activities, including antioxidant, anti-inflammatory, antibacterial, antitumor, hypoglycemic, and cardiovascular protective effects. Moreover, Ficus pumila L. has extensive applications, such as in the food industry and ecological city construction. Herein, we summarize the latest knowledge about the bioactive compounds and therapeutic activities of Ficus pumila L., and its applications in the food industry and ecological city construction are also discussed. We hope that this comprehensive review can attract more attention to Ficus pumila L. and be helpful for its further applications. Full article
(This article belongs to the Special Issue Extraction and Analysis of Natural Product in Plant)
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