Extraction and Analysis of Bioactive Compounds in Crops

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 (20 December 2022) | Viewed by 37984

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Department of Analytical Chemistry, Faculty of Sciences, IVAGRO, University of Cadiz, 11510 Puerto Real, Cádiz, Spain
Interests: agri-food analysis; optimization; method validation; bioactive compounds; green extraction techniques; liquid chromatography; mass spectrometry
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Guest Editor
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
Special Issues, Collections and Topics in MDPI journals

Special Issue Information

Dear Colleagues,

There is a growing interest in the consumption of crops rich in bioactive compounds, which seem to be responsable for a wide range of biological properties associated with an improvement of health, as antioxidant, anticarcinogenic, anti-inflammatory, antiobesity, and so on. Many of these crops and their extracts are used in agri-food, pharmaceutical or agrochemical industries, as well as food supplements or functional products. The development of extraction and analysis methodologies is essential both for quality control and to obtain extracts with the largest amount of bioactive compounds. This Special Issue will focus on the extraction, identification and analysis of bioactive compounds present in crops. We welcome novel research and reviews covering all related topics in extraction methods, identification, separation, determination and analysis of bioactive compounds in crops, the obtaining and the usage of plant extracts, the use of by-products for different industries and quality control of raw material.

Dr. Mercedes Vazquez Espinosa
Prof. Dr. Gerardo Fernández Barbero
Guest Editors

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Keywords

  • Bioactive compounds
  • Secondary metabolites
  • Crop analysis
  • Identification
  • Ultrasound-assisted extraction
  • Microwave-assisted extraction
  • Pressurized liquid extraction
  • Supercritical fluid extraction
  • Quality control
  • By-products valorization

Published Papers (16 papers)

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Research

13 pages, 2660 KiB  
Article
Optimization of a Microwave-Assisted Extraction Method for the Recovery of the Anthocyanins from Jabuticaba By-Products
by Tiago L. C. T. Barroso, Luiz E. N. Castro, Gerardo F. Barbero, Miguel Palma, Ceferino Carrera, Mauricio A. Rostagno and Tânia Forster-Carneiro
Agronomy 2023, 13(2), 556; https://0-doi-org.brum.beds.ac.uk/10.3390/agronomy13020556 - 15 Feb 2023
Cited by 3 | Viewed by 1371
Abstract
In this study, a Box-Behnken Design (BBD) has been used to optimize the recovery of bioactive compounds from jabuticaba (Myrciaria cauliflora) by-products through microwave-assisted extraction (MAE). Thus, the Box-Behnken (BBD) experimental design was followed by a response surface methodology (RSM) that [...] Read more.
In this study, a Box-Behnken Design (BBD) has been used to optimize the recovery of bioactive compounds from jabuticaba (Myrciaria cauliflora) by-products through microwave-assisted extraction (MAE). Thus, the Box-Behnken (BBD) experimental design was followed by a response surface methodology (RSM) that would allow investigating the influence of the four independent variables (temperature, solvent composition, pH, and sample-solvent ratio) that have been considered. The results revealed that temperature and solvent composition (%MeOH) were the most significant factors regarding the yields of anthocyanins obtained from the studied plant matrix. The established optimized conditions and 10-min-extraction time resulted in yields of 9.70 ± 0.28 mg g−1 of total anthocyanins. The method exhibited good repeatability and intermediate precision, with RSD variations lower than 5% for both parameters. The developed process was also able to extract and identify anthocyanins in commercial samples (jabuticaba pulp and jam). The results obtained from the optimized MAE method suggest that this technique is not only efficient for the recovery of anthocyanins from jabuticaba by-products, but it is also beneficial for a circular economy approach. Full article
(This article belongs to the Special Issue Extraction and Analysis of Bioactive Compounds in Crops)
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19 pages, 1982 KiB  
Article
Hop (Humulus lupulus L.) Specialized Metabolites: Extraction, Purification, Characterization in Different Plant Parts and In Vitro Evaluation of Anti-Oomycete Activities against Phytophthora infestans
by Justine Jacquin, Sophie Moureu, Caroline Deweer, Asma Hakem, Anne-Sophie Paguet, Natacha Bonneau, Simon Bordage, Charles Dermont, Sevser Sahpaz, Jérôme Muchembled and Céline Rivière
Agronomy 2022, 12(11), 2826; https://0-doi-org.brum.beds.ac.uk/10.3390/agronomy12112826 - 12 Nov 2022
Cited by 7 | Viewed by 2237
Abstract
Botanicals represent a promising source of metabolites in the search for new biofungicides. In this context, this study aimed at evaluating the in vitro anti-oomycete activity of hop (Humulus lupulus L.) extracts and metabolites against Phytophthora infestans, an oomycete causing late [...] Read more.
Botanicals represent a promising source of metabolites in the search for new biofungicides. In this context, this study aimed at evaluating the in vitro anti-oomycete activity of hop (Humulus lupulus L.) extracts and metabolites against Phytophthora infestans, an oomycete causing late blight disease in Solanaceae. Crude hydro-ethanolic extracts and dichloromethane sub-extracts of different parts (cones, leaves, stems and rhizomes) were characterized by UHPLC-UV–MS and some cone specialized metabolites were purified by CPC and preparative HPLC. A commercial hop cone essential oil was also analyzed by GC–MS. All extracts succeeded in inhibiting mycelial growth and spore germination with morphological alteration of the mycelium. Extracts of leaves showed a significant anti-oomycete activity compared to the extracts of cones, stems, and rhizomes. Moreover, no difference was noticed between the crude hydro-ethanolic extract and the dichloromethane sub-extract activity, except for leaves, with the apolar sub-extract being more active than the crude one. The extracts of cones succeeded in inhibiting more P. infestans than the essential oil, which appeared to be the less active evaluated modality. Some purified prenylated phenolic compounds also inhibited P. infestans although copper sulfate, a mineral fungicide control, was still more active. This study highlights the potential use of hop by-products as biofungicides to manage P. infestans. Full article
(This article belongs to the Special Issue Extraction and Analysis of Bioactive Compounds in Crops)
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12 pages, 1263 KiB  
Article
Ultrasound-Assisted Extraction of Betalains from Opuntia Fruit Pulp of Different Color Varieties
by Mercedes Vázquez-Espinosa, Ana V. González-de-Peredo, Ceferino Carrera, Miguel Palma, Gerardo F. Barbero and María José Aliaño-González
Agronomy 2022, 12(11), 2604; https://0-doi-org.brum.beds.ac.uk/10.3390/agronomy12112604 - 23 Oct 2022
Cited by 3 | Viewed by 1565
Abstract
Betalains are water-soluble pigments that have exhibited important pharmacological properties such as antioxidant, anticancer, antilipidemic and antimicrobial activity. These compounds have been isolated in numerous purple plants or fruits, as is the case of the wild species under the Opuntia genus. The fruits [...] Read more.
Betalains are water-soluble pigments that have exhibited important pharmacological properties such as antioxidant, anticancer, antilipidemic and antimicrobial activity. These compounds have been isolated in numerous purple plants or fruits, as is the case of the wild species under the Opuntia genus. The fruits of these species are often disregarded because of their small size as well as the frequent presence of prickles. Based on this, this research has as its objective the optimization of a method based on ultrasound-assisted extraction to obtain extracts enriched with betalains from a wild Opuntia species (Opuntia dillenii (Ker Gawl.) Haw.). Four variables (%EtOH in the solvent, temperature of extraction, ultrasound amplitude and cycle) were selected using a Box–Behnken design. The quadratic interaction of %EtOH and the interaction of %EtOH–cycle have proven to be influential variables at 95% confidence. The conditions to obtain the highest betalain concentration were 100 mg of pulp with 20 mL (60%:40% EtOH:H2O) solvent at 20 °C at 24% amplitude and 0.2 cycle for 10 min. The suitability and reliability of the method were evaluated with repeatability and intermediate precision tests obtaining CVs <5%. Finally, the developed method has been employed in the analysis of five Opuntia commercial samples and obtained significant antioxidant activity of the extracts, confirming its applicability. Full article
(This article belongs to the Special Issue Extraction and Analysis of Bioactive Compounds in Crops)
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13 pages, 1072 KiB  
Article
New Biodegradable Mulching Films for Strawberry (Fragaria × Ananassa Duch.): Effects on the Volatile Profiles of the Fruit
by Rosaria Cozzolino, Giuseppe Amato, Francesco Siano, Gianluca Picariello, Matteo Stocchero, Luigi Morra, Emiliana Mignoli, Mariarosaria Sicignano, Milena Petriccione and Livia Malorni
Agronomy 2022, 12(10), 2514; https://0-doi-org.brum.beds.ac.uk/10.3390/agronomy12102514 - 15 Oct 2022
Cited by 1 | Viewed by 1463
Abstract
The effects of mulching films on the profiles of volatile organic compounds (VOCs) from two strawberry cultivars, namely Elide and Sabrina, were evaluated by headspace solid-phase micro-extraction coupled to gas chromatography mass spectrometry (HS-SPME/GC-MS). Strawberries were grown on two biodegradable mulching films, named [...] Read more.
The effects of mulching films on the profiles of volatile organic compounds (VOCs) from two strawberry cultivars, namely Elide and Sabrina, were evaluated by headspace solid-phase micro-extraction coupled to gas chromatography mass spectrometry (HS-SPME/GC-MS). Strawberries were grown on two biodegradable mulching films, named N5 and N18, in comparison to black polyethylene (PE). PCA models, separately performed on the VOCs dataset of the two cultivars, showed that the observations for each of the three mulching films lie in corresponding regions of the PCA plot, suggesting that the mulching films represented the main source of data variation, and hence, the variability of the VOCs profile induced by the mulching films overcame the cv-related one. For both the cultivars, a higher number of VOCs with a positive impact on the “sweet” taste sensation and consumers’ preference were positively correlated with strawberries produced on the biodegradable films compared to PE. However, there was an interaction between the type of cultivar and the mulches, as Elide responded better to N18 and N5 mulching films, while Sabrina responded better only to N18. Altogether, these results could contribute to assessing the effects of mulching type on putative volatile markers of the desirable sensory perception and consumers’ acceptability of strawberries. Full article
(This article belongs to the Special Issue Extraction and Analysis of Bioactive Compounds in Crops)
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15 pages, 1555 KiB  
Article
Optimization of an Enzyme-Assisted Extraction Method for the Anthocyanins Present in Açai (Euterpe oleracea Mart.)
by Diego Alavarsa-Cascales, María José Aliaño-González, Miguel Palma, Gerardo F. Barbero and Ceferino Carrera
Agronomy 2022, 12(10), 2327; https://0-doi-org.brum.beds.ac.uk/10.3390/agronomy12102327 - 27 Sep 2022
Cited by 8 | Viewed by 1728
Abstract
Several investigations have proven the presence of anthocyanins in different parts of açai plants. These compounds are responsible for the notable therapeutic properties of açai such as antioxidant, antimicrobial, anti-inflammatory, anticancer, and anticonvulsant. We have therefore optimized an enzyme-assisted extraction method for the [...] Read more.
Several investigations have proven the presence of anthocyanins in different parts of açai plants. These compounds are responsible for the notable therapeutic properties of açai such as antioxidant, antimicrobial, anti-inflammatory, anticancer, and anticonvulsant. We have therefore optimized an enzyme-assisted extraction method for the anthocyanins found in açai, to be subsequently applied in many fields such as agrifood, medicine, or cosmetics. A Plackett–Burman design with seven variables (time of extraction, pH, temperature, agitation, percentage of ethanol in the solvent, amount of sample, and units of enzyme) was employed to determine the predominant extraction variables, of which four were categorized as influential. Subsequently, a Box–Behnken design–response surface methodology made it possible to determine the degree of influence from these variables and their optimal values. The optimal conditions were established as 0.1 g of açai heated up to 60 °C and extracted using 15 mL of solvent with pH 4 and 40% ethanol, 500 units of enzyme per gram of sample, and agitation at 150 rpm for 15 min. The repeatability and intermediate precision of the developed method were confirmed by variation coefficients below 5%. Finally, the developed method was compared against the extensively used maceration and ultrasound-assisted extraction methods. Full article
(This article belongs to the Special Issue Extraction and Analysis of Bioactive Compounds in Crops)
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20 pages, 2663 KiB  
Article
Ultrasound-Assisted Extraction of Total Phenolic Compounds and Antioxidant Activity in Mushrooms
by María José Aliaño-González, Marta Barea-Sepúlveda, Estrella Espada-Bellido, Marta Ferreiro-González, José Gerardo López-Castillo, Miguel Palma, Gerardo F. Barbero and Ceferino Carrera
Agronomy 2022, 12(8), 1812; https://0-doi-org.brum.beds.ac.uk/10.3390/agronomy12081812 - 30 Jul 2022
Cited by 12 | Viewed by 2428
Abstract
The consumption of mushrooms has considerably increased in recent years because of their beneficial nutritional properties due to their essential amino acids, proteins, and dietary fiber content. Recent research has shown that they are also rich in polysaccharides and phenolic compounds. These compounds [...] Read more.
The consumption of mushrooms has considerably increased in recent years because of their beneficial nutritional properties due to their essential amino acids, proteins, and dietary fiber content. Recent research has shown that they are also rich in polysaccharides and phenolic compounds. These compounds exhibit decisive free radical and ROS scavenging power with potential application to the treatment of neurodegenerative disorders. In addition, they present important properties like antioxidant, antiaging, and immune modulation. In the present research, the optimization for the extraction of total phenolic compounds and the antioxidant activity (DPPH and ABTS), based on ultrasound–assisted techniques has been carried out. Five variables (% MeOH in solvent, extraction temperature, amplitude, cycle, and sample:solvent ratio have been selected; both the total phenolic compounds content as well as the antioxidant activity (DPPH and ABTS)) have been considered as the response variables. The optimal conditions, determined by means of a multiresponse optimization method, were established at 0.2 g of sample extracted with 15.3 mL of solvent (93.6% MeOH) at 60 °C for 5 min and using 16.86% amplitude and 0.71 s−1 cycles. A precision study of the optimized method has been performed with deviations lower than 5%, which proves the repeatability and precision of the extraction method. Finally, the extraction method has been applied to wild and commercial mushrooms from Andalusia and Northern Morocco, which has confirmed its suitability for the extraction of the phenolic compounds from mushroom samples, while ensuring maximum antioxidant activity. Full article
(This article belongs to the Special Issue Extraction and Analysis of Bioactive Compounds in Crops)
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13 pages, 1426 KiB  
Article
Evaluation of the Effect of Different Co-Solvent Mixtures on the Supercritical CO2 Extraction of the Phenolic Compounds Present in Moringa oleifera Lam. Leaves
by Beatriz Juliana Yerena-Prieto, Monserrat Gonzalez-Gonzalez, Miguel Ángel García-Alvarado, Lourdes Casas, Miguel Palma, Guadalupe del Carmen Rodríguez-Jimenes, Gerardo F. Barbero and Cristina Cejudo-Bastante
Agronomy 2022, 12(6), 1450; https://0-doi-org.brum.beds.ac.uk/10.3390/agronomy12061450 - 17 Jun 2022
Cited by 3 | Viewed by 2048
Abstract
Supercritical fluid extraction (SFE), using CO2, is a novel, sustainable and very efficient technique for the recovery of highly apolar compounds. However, the recovery of phenolic compounds requires the use of different co-solvent combinations such as water and ethanol to enhance [...] Read more.
Supercritical fluid extraction (SFE), using CO2, is a novel, sustainable and very efficient technique for the recovery of highly apolar compounds. However, the recovery of phenolic compounds requires the use of different co-solvent combinations such as water and ethanol to enhance the recovery of these compounds through the optimization of a number of variables. In this sense, the effect of pressure (100, 150 and 200 bar), temperature (50, 65 and 80 °C), extraction time (30, 60, 90, 120, 150 and 180 min) and the effect of the different percentages of ethanol and water as co-solvents on the composition and phenolic content of moringa leaf extracts were evaluated. Six major flavonoids were identified by ultra-high-performance liquid chromatography coupled to a quadrupole-time-of-flight mass spectrometer (UHPLC-Q-ToF-MS). Pressure and temperature had a significant effect on the phenolic composition of the extracts, as well as on their concentrations. The highest concentration of total flavonoids compounds (TFCs) was obtained by using a mixture of CO2 and water of 50:50 (v/v) at 100 bar, at 65 °C after a 120 min extraction time that produced a concentration of 11.66 mg ± 0.02 mg TFC g−1 sample, which corresponds to 89.0% of the total flavonoids of the sample, obtained by exhaustive extraction. Full article
(This article belongs to the Special Issue Extraction and Analysis of Bioactive Compounds in Crops)
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17 pages, 1938 KiB  
Article
Simultaneous Estimation of Rhein and Aloe-Emodin in Traditional and Ultrasound-Based Extracts of Rheum palmatum L. (Rhubarb) Using Sustainable Reverse-Phase and Conventional Normal-Phase HPTLC Methods
by Mohammed H. Alqarni, Prawez Alam, Faiyaz Shakeel, Aftab Alam, Mohammad A. Salkini and Magdy M. Muharram
Agronomy 2022, 12(6), 1295; https://0-doi-org.brum.beds.ac.uk/10.3390/agronomy12061295 - 28 May 2022
Viewed by 1570
Abstract
The greenness indices of literature analytical procedures for the simultaneous measurement of rhein and aloe-emodin have not been determined. As a consequence, the first goal of this study was to design and validate a sensitive and sustainable reverse-phase high-performance thin-layer chromatography (HPTLC) method [...] Read more.
The greenness indices of literature analytical procedures for the simultaneous measurement of rhein and aloe-emodin have not been determined. As a consequence, the first goal of this study was to design and validate a sensitive and sustainable reverse-phase high-performance thin-layer chromatography (HPTLC) method for the simultaneous estimation of rhein and aloe-emodin in a traditional extract (TE) and ultrasound-based extract (UBE) of commercial Rhubarb and Rhubarb plant extracts in comparison to the conventional normal-phase HPTLC method. The second goal was to determine the greenness indices for both methods using the AGREE approach. For the sustainable reverse-phase HPTLC approach, the method was linear in the 50–1000 ng/spot range for rhein and 25–1000 ng/spot range for aloe-emodin. However, for the conventional normal-phase HPTLC approach, the method was linear in the 50–600 ng/spot range for rhein and 100–600 ng/spot range for aloe-emodin. The limit of detection (LOD) for rhein and aloe-emodin was 16.81 ng/spot and 8.49 ng/spot, respectively, using the sustainable analytical method. However, the LOD for rhein and aloe-emodin was 18.53 ng/spot and 39.42 ng/spot, respectively, using the conventional analytical method. For the simultaneous determination of rhein and aloe-emodin, the sustainable analytical method was more sensitive, accurate, precise, and robust than the conventional analytical method. The amount of rhein and aloe-emodin was higher in the UBE of commercial Rhubarb and Rhubarb plant extract over their TE. For the simultaneous quantification of rhein and aloe-emodin in the TE and UBE of marketed Rhubarb and Rhubarb plant extract, the sustainable analytical method was superior to the conventional analytical method. The AGREE index for the sustainable reverse-phase and conventional normal-phase HPTLC methods was determined to be 0.78 and 0.49, respectively, indicating an excellent greenness profile of the sustainable reverse-phase HPTLC method over the conventional normal-phase HPTLC approach. The sustainable analytical method was found to be superior to the conventional analytical method based on these results. Full article
(This article belongs to the Special Issue Extraction and Analysis of Bioactive Compounds in Crops)
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13 pages, 1279 KiB  
Article
A Simple, Cost-Effective, and Green HPTLC Method for the Estimation of Ascorbic Acid in Solvent and Ultrasound-Assisted Extracts of Phyllanthus emblica, Capsicum annuum, and Psidium guajava
by Ahmed I. Foudah, Prawez Alam, Faiyaz Shakeel, Aftab Alam, Mohammad A. Salkini, Sultan Alshehri, Mohammed M. Ghoneim and Samir A. Ross
Agronomy 2022, 12(5), 1016; https://0-doi-org.brum.beds.ac.uk/10.3390/agronomy12051016 - 23 Apr 2022
Cited by 1 | Viewed by 1923
Abstract
Greener analytical methodologies for the estimation of ascorbic acid (AA) are poorly reported in the literature. Furthermore, the green indexes of the literature’s analytical assays of AA estimation have not been assessed. As a consequence, the aim of this research is to invent [...] Read more.
Greener analytical methodologies for the estimation of ascorbic acid (AA) are poorly reported in the literature. Furthermore, the green indexes of the literature’s analytical assays of AA estimation have not been assessed. As a consequence, the aim of this research is to invent and validate a simple, cost-effective, and green reverse-phase “high-performance thin-layer chromatography (HPTLC)” method for the estimating AA in the solvent extracts (SE) and ultrasound-assisted extracts (UAE) of Phyllanthus emblica, Psidium guajava, and Capsicum annuum. The greener mobile phase for AA estimation was a binary mixture of water and ethanol (70:30, v/v). At a wavelength of 265 nm, the detection of AA was carried out. The greener HPTLC technique was linear in the 25–1200 ng/band range. In addition, the method was simple, cost-effective, accurate, precise, robust, sensitive, and green. The amount of AA was highest in the SE and UAE of P. emblica compared to the SE and UAE of P. guajava and C. annuum. The amount of AA in the SE of P. emblica, P. guajava, and C. annuum was found to be 491.16, 168.91, and 144.30 mg/100 g, respectively. However, the amount of AA in the UAE of P. emblica, P. guajava, and C. annuum was found to be 673.02, 218.71, and 199.30 mg/100 g, respectively. Using the “analytical GREEnness (AGREE)” methodology, the greenness index for the developed method was calculated to be 0.88, showing that the developed method has an excellent green profile. When it came to extracting AA, the UAE method outperformed the SE method. These findings suggested that the developed method might be used to estimate the AA in a variety of vegetable crops, plant-based extracts, and commercial formulations. Furthermore, because of the use of greener solvent systems against the commonly utilized hazardous solvent systems for AA determination, this technique is also safe and sustainable. Full article
(This article belongs to the Special Issue Extraction and Analysis of Bioactive Compounds in Crops)
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13 pages, 1492 KiB  
Article
Partial Purification and Characterization of the Lectins of Two Varieties of Phaseolus coccineus (Ayocote Bean)
by Leopoldo González-Cruz, Carmen Valadez-Vega, José Mayolo Simitrio Juárez-Goiz, Norma Leticia Flores-Martínez, José Luis Montañez-Soto and Aurea Bernardino-Nicanor
Agronomy 2022, 12(3), 716; https://0-doi-org.brum.beds.ac.uk/10.3390/agronomy12030716 - 16 Mar 2022
Cited by 4 | Viewed by 2171
Abstract
In this study, a partial purification and characterization of the lectins from two varieties of Phaseolus coccineus (black and purple ayocote bean) was carried out. A partial purification of the lectins was performed by affinity chromatography on fetuin-agarose. The lectins’ characterization showed that [...] Read more.
In this study, a partial purification and characterization of the lectins from two varieties of Phaseolus coccineus (black and purple ayocote bean) was carried out. A partial purification of the lectins was performed by affinity chromatography on fetuin-agarose. The lectins’ characterization showed that the hemagglutination activity was only inhibited by the fetuin and that the saccharides (mono-, di- and tri-saccharides) do not influence their hemagglutination capacity. A difference in the relative molecular weight between the two Phaseolus varieties was observed, 28.5 kDa for the black variety and 30.6 kDa for the purple variety. In the lectins of both Phaseolus varieties, ions were detected in their structure and influenced their hemagglutination activity, principally to the ion Ca+2; on the other hand, only the lectins of the purple variety of the Phaseolus, had a detectable ion, Cu+2. The lectins showed thermostability in the temperature range of 25 and 70 °C, on the other hand, in the pH range between 3 and 10, the lectins showed hemagglutination activity. According to the obtained results, the structural differences between the lectins obtained from both Phaseolus varieties influence their hemagglutination activity. Full article
(This article belongs to the Special Issue Extraction and Analysis of Bioactive Compounds in Crops)
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16 pages, 3488 KiB  
Article
Dual Response Optimization of Ultrasound-Assisted Oil Extraction from Red Fruit (Pandanus conoideus): Recovery and Total Phenolic Compounds
by Endah Prasetia Susanti, Abdul Rohman and Widiastuti Setyaningsih
Agronomy 2022, 12(2), 523; https://0-doi-org.brum.beds.ac.uk/10.3390/agronomy12020523 - 19 Feb 2022
Cited by 2 | Viewed by 2331
Abstract
Red fruit oil (RFO) is a high-value oil that contains functional compounds, mainly phenolic compounds, providing antioxidant activity. Therefore, an optimal extraction method is essential to recover the RFO and phenolic compounds simultaneously. This research aimed to optimize the ultrasound-assisted extraction (UAE) for [...] Read more.
Red fruit oil (RFO) is a high-value oil that contains functional compounds, mainly phenolic compounds, providing antioxidant activity. Therefore, an optimal extraction method is essential to recover the RFO and phenolic compounds simultaneously. This research aimed to optimize the ultrasound-assisted extraction (UAE) for oil from red fruit using the Box-Behnken design combined with response surface methodology. The studied UAE factors, including sample-to-solvent ratio (1:3, 1:2, and 1:1 g mL−1), extraction temperature (60, 75, and 90 °C), and pulse duty-cycle (0.20, 0.50, and 0.80 s−1). Analysis of variance revealed that the three studied factors significantly influenced the recovered RFO, while the level of total phenolic compounds in the extracts was defined merely by extraction temperature (p < 0.05). These significant factors were then included in the optimization models (R2 > 0.99, lack-of-fit p > 0.05). The proposed UAE setting by the multiresponse optimization was an extraction temperature of 67 °C, a pulse duty-cycle of 0.50 s−1, and a sample-to-solvent ratio of 1:2.5 g mL−1. Subsequently, the extraction kinetic was evaluated, confirming full recovery at 60 min of extraction time. The developed method was then applied to extract six red fruit clones. Mbarugum clones provided high RFO recovery (9.60%), with an uppermost total phenolic compound of (42.63 mg GAE g−1) among the six red fruit clones. Additionally, the resulting RFO showed eminent antioxidant activities, indicated by excellent values of IC50 DPPH (37.69 mg L−1), IC50 FIC (30.43 mg L−1), FRAP reducing power (63.55 mg AAEA g−1), and IC50 ABTS (93.88 mg L−1). In contrast with a wet rendering method, UAE enhanced the RFO recovery by 53.02%, resulting in a higher level of total phenolic compounds. Henceforth, the proposed UAE method is a promising technique to substitute conventional oil production in the food and pharmaceutical industries. Full article
(This article belongs to the Special Issue Extraction and Analysis of Bioactive Compounds in Crops)
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13 pages, 1040 KiB  
Article
Optimization of an Ultrasound-Assisted Extraction Method Applied to the Extraction of Flavonoids from Moringa Leaves (Moringa oleífera Lam.)
by Beatriz Juliana Yerena-Prieto, Monserrat Gonzalez-Gonzalez, Mercedes Vázquez-Espinosa, Ana Velasco González-de-Peredo, Miguel Ángel García-Alvarado, Miguel Palma, Guadalupe del Carmen Rodríguez-Jimenes and Gerardo Fernández Barbero
Agronomy 2022, 12(2), 261; https://0-doi-org.brum.beds.ac.uk/10.3390/agronomy12020261 - 20 Jan 2022
Cited by 21 | Viewed by 2963
Abstract
Interest in phenolic compounds has recently increased due to their potential as antioxidant agents. Moringa leaves (Moringa oleifera) have a high content of phenolic compounds, which presents them as a promising source for the extraction of these compounds. However, it is [...] Read more.
Interest in phenolic compounds has recently increased due to their potential as antioxidant agents. Moringa leaves (Moringa oleifera) have a high content of phenolic compounds, which presents them as a promising source for the extraction of these compounds. However, it is necessary to use analytical techniques to identify and quantify their actual compound content to determine the quality of the raw material and the potential of the final product. Ultrasound assisted extraction is a green, rapid and environmentally friendly extraction technique that produces high quality extracts from natural products. Hence, the aim of this research is to optimize the variables of the ultrasound-assisted extraction (UAE) process for the extraction of moringa leaves using response surface methodology (RSM) to extract the main flavonoids using methanol as the extraction solvent. A Box–Behnken design (BBD) has been used to evaluate the effect of the ultrasound extraction process variables. Finally, the optimal extraction time in the range between 2 and 30 min was determined. The results revealed that the methanol concentration was the most influential variable. The optimal extraction time was established at 15 min. Six of the main flavonoids were quantified by UHPLC-DAD and identified by UHPLC-QToF-MS. The results confirmed that UAE is an efficient method for the extraction and subsequent analysis and quality control of the flavonoids that can be found in moringa leaves. Full article
(This article belongs to the Special Issue Extraction and Analysis of Bioactive Compounds in Crops)
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14 pages, 1664 KiB  
Article
A Greener HPTLC Approach for the Determination of β-Carotene in Traditional and Ultrasound-Based Extracts of Different Fractions of Daucus carota (L.), Ipomea batatas (L.), and Commercial Formulation
by Mohammed H. Alqarni, Prawez Alam, Aftab Alam, Abuzer Ali, Ahmed I. Foudah, Sultan Alshehri, Mohammed M. Ghoneim and Faiyaz Shakeel
Agronomy 2021, 11(12), 2443; https://0-doi-org.brum.beds.ac.uk/10.3390/agronomy11122443 - 30 Nov 2021
Cited by 5 | Viewed by 6214
Abstract
Various analytical approaches for determining β-carotene in vegetable crops and commercial dosage forms have been documented. However, neither the qualitative nor quantitative environmental safety and greener aspects of the literature analytical methodologies of β-carotene analysis have been assessed. As a result, the goal [...] Read more.
Various analytical approaches for determining β-carotene in vegetable crops and commercial dosage forms have been documented. However, neither the qualitative nor quantitative environmental safety and greener aspects of the literature analytical methodologies of β-carotene analysis have been assessed. As a result, the goal of this research is to develop and validate a reversed-phase “high-performance thin-layer chromatography (HPTLC)” approach for determining β-carotene in traditional (TE) and ultrasound-assisted (UBE) extracts of different fractions of Daucus carota (L.), Ipomea batatas (L.), and commercial formulation. The greener mobile phase for β-carotene analysis was a ternary mixture of ethanol, cyclohexane, and ammonia (95:2.5:2.5, v v v−1). The detection of β-carotene was done at a wavelength of 459 nm. In the 25–1000 ng band−1 range, the greener reversed-phase HPTLC approach was linear. Other validation factors for β-carotene analysis, including as accuracy, precision, robustness, and sensitivity, were likewise dependable. The contents of β-carotene were found to be maximum in hexane: acetone (50:50%) fractions of TE and UBE of D. carota and I. batatas compared to their acetone and hexane fractions. The amount of β-carotene in hexane: acetone (50:50%) portions of TE of D. carota, I. batatas and commercial formulation A was estimated to be 10.32, 3.73, and 6.73 percent w w−1, respectively. However, the amount of β-carotene in hexane: acetone (50:50%) portions of UBE of D. carota, I. batatas and commercial formulation A was estimated to be 11.03, 4.43, and 6.89 percent w w−1, respectively. The greenness scale for the proposed HPTLC strategy was calculated as 0.81 using the “analytical GREEnness (AGREE)” method, indicating that the proposed HPTLC methodology has good greenness. The UBE approach for extracting β-carotene outperformed the TE procedure. These results indicated that the greener reversed-phase HPTLC approach can be utilized for the determination of β-carotene in different vegetable crops, plant-based phytopharmaceuticals, and commercial products. In addition, this approach is also safe and sustainable due to the utilization of a greener mobile phase compared to the toxic mobile phases utilized in literature analytical approaches of β-carotene estimation. Full article
(This article belongs to the Special Issue Extraction and Analysis of Bioactive Compounds in Crops)
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14 pages, 2204 KiB  
Article
A Sustainable Reversed-Phase HPTLC Method for the Quantitative Estimation of Hesperidin in Traditional and Ultrasound-Assisted Extracts of Different Varieties of Citrus Fruit Peels and Commercial Tablets
by Ahmed I. Foudah, Faiyaz Shakeel, Prawez Alam, Mohammed H. Alqarni, Maged S. Abdel-Kader and Sultan Alshehri
Agronomy 2021, 11(9), 1744; https://0-doi-org.brum.beds.ac.uk/10.3390/agronomy11091744 - 30 Aug 2021
Cited by 5 | Viewed by 2245
Abstract
Hesperidin (HSP) is a bioactive flavanone glycoside, present abundantly in the variety of citrus fruits. The environmental safety and sustainability of the reported analytical assays of HSP analysis have not been considered in the literature. Hence, a sensitive and sustainable “reversed-phase high-performance thin-layer [...] Read more.
Hesperidin (HSP) is a bioactive flavanone glycoside, present abundantly in the variety of citrus fruits. The environmental safety and sustainability of the reported analytical assays of HSP analysis have not been considered in the literature. Hence, a sensitive and sustainable “reversed-phase high-performance thin-layer chromatography (RP-HPTLC)” method has been developed and validated for HSP analysis in traditional (TE) and ultrasound-based (UBE) extracts of four different varieties of citrus fruit peels and its commercial tablet dosage forms. The binary combination of green solvents such as ethanol-water (50:50, v v−1) was used as the mobile phase. The detection of HSP was performed at 287 nm. The sustainable RP-HPTLC method was linear in 20–2000 ng band−1 range. The studied validation parameters, including accuracy, precision, robustness, sensitivity were acceptable for HSP analysis. The content of HSP in TE of four different varieties of citrus fruits including grapefruit peels (Citrus paradisi), mosambi peels (Citrus limetta), lemon peels (Citrus lemon), and orange peels (Citrus sinensis) was detected as 8.26, 6.94, 5.90, and 6.81% w w−1, respectively. The content of HSP in TE of commercial formulations A and B was detected as 5.31 and 5.55% w w−1, respectively. However, the content of HSP in UBE of grapefruit peels, mosambi peels, lemon peels, and orange peels was detected as 11.41, 8.86, 7.98, and 8.64% w w−1, respectively. The content of HSP in UBE of commercial formulations A and B was detected as 6.72 and 6.92% w w−1, respectively. The greenness score of the sustainable RP-HPTLC method was predicted as 0.83 using analytical GREEnness (AGREE) metric approach, indicated the excellent greenness profile of the RP-HPTLC method. UBE procedure for HSP was superior over its TE procedure. These observations and results suggested that the present RP-HPTLC method can be successfully used for the quantitative estimation of HSP in the variety of citrus fruit peels and its commercial formulations. In addition, this method is simple, rapid, precise, accurate, and economical compared to the reported analytical methods of HSP analysis. It is also safe and sustainable method due to the use of ethanol-water solvents systems, as both the solvents are green solvents compared to the solvents used in reported analytical methods of HSP analysis. Full article
(This article belongs to the Special Issue Extraction and Analysis of Bioactive Compounds in Crops)
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14 pages, 2362 KiB  
Article
How Different Cooking Methods Affect the Phenolic Composition of Sweet Potato for Human Consumption (Ipomea batata (L.) Lam)
by Ceferino Carrera, Cristy Fabiola Zelaya-Medina, Nuria Chinchilla, Marta Ferreiro-González, Gerardo F. Barbero and Miguel Palma
Agronomy 2021, 11(8), 1636; https://0-doi-org.brum.beds.ac.uk/10.3390/agronomy11081636 - 17 Aug 2021
Cited by 5 | Viewed by 2173
Abstract
In recent years, there has been increasing interest in the functional components of sweet potato because of its nutritional and medicinal value. The aim of this study is to analyse how much sweet potato phenolic compounds composition (derived from caffeoylquinic acids) varies as [...] Read more.
In recent years, there has been increasing interest in the functional components of sweet potato because of its nutritional and medicinal value. The aim of this study is to analyse how much sweet potato phenolic compounds composition (derived from caffeoylquinic acids) varies as a result of cooking. Traditional techniques such as: boiling, oven roasting and more recent processing techniques such as microwave cooking were tested. Three sweet potato varieties were cooked for different periods of time and under different conditions. Ultrasound-assisted extraction (UAE) was used to extract the compounds of interest and then, a chemometric tool such as Box-Behnken design (BBD) was successfully used to evaluate and optimise the most influential factors in the extraction, i.e., temperature, solvent composition and sample-to-solvent ratio. The optimal settings for UAE were: solvent 100% methanol, a temperature of 39.4 °C and a mass/volume ratio of 0.5 g per 10 mL solvent. Oven roasting of sweet potatoes resulted in increased levels of caffeoylquinic acids, whereas prolonged cooking times in water resulted in decreasing levels of the same. Full article
(This article belongs to the Special Issue Extraction and Analysis of Bioactive Compounds in Crops)
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11 pages, 1198 KiB  
Article
Optimization of the Microwave-Assisted Extraction of Simple Phenolic Compounds from Grape Skins and Seeds
by Latifa Azaroual, Ali Liazid, Fouad El Mansouri, Jamal Brigui, Ana Ruíz-Rodriguez, Gerardo F. Barbero and Miguel Palma
Agronomy 2021, 11(8), 1527; https://0-doi-org.brum.beds.ac.uk/10.3390/agronomy11081527 - 30 Jul 2021
Cited by 16 | Viewed by 2194
Abstract
A method for the extraction of phenolic compounds from grape seeds and skins using microwave-assisted extraction (MAE) was developed. Optimization of the effects of the extraction parameters in terms of the results of extraction was obtained using the response surface methodology. The parameters [...] Read more.
A method for the extraction of phenolic compounds from grape seeds and skins using microwave-assisted extraction (MAE) was developed. Optimization of the effects of the extraction parameters in terms of the results of extraction was obtained using the response surface methodology. The parameters studied were extraction solvent (methanol, ethanol, acetone, and water), percentage of methanol in water, quantity of sample in relation to volume of extraction solvent (solid:liquid, 10–50 mg mL−1), power (100–500 W), magnetic stirring speed (0–100%), and extraction time (5–20 min). Finally, the repeatability and the intermediate precision of the method were determined. The best conditions proved to be: 65% methanol in water as an optimum extraction solvent; 0.5 g of grape skin or seed in a volume of 25 mL; a power of 500 W with the maximum stirring speed (100%); and an extraction time of 5 min. The phenolic compounds proved to be stable in the optimized extraction conditions. The resulting repeatability and the intermediate precision of the optimized method showed a relative standard deviation below 7%. The new method applied on Napoleon grape allowed for the determination of catechin (453.2 (mg kg−1)), epicatechin (306.3 mg kg−1), caftaric acid (22.37 mg caffeic acid equivalents kg−1), dihydrokaempferol-glycoside (11.13 mg kaempferol equivalents kg−1), quercetin (18.28 mg kg−1), quercetin-3-glucoside (20.09 mg quercetin equivalents kg−1), and kaempferol-3-glucoside (11.10 mg kaempferol equivalents kg−1). Full article
(This article belongs to the Special Issue Extraction and Analysis of Bioactive Compounds in Crops)
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