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Extraction and Analysis of Chemical Composition from Natural Products and...
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Extraction and Analysis of Chemical Composition from Natural Products and Metabolites

A special issue of Separations (ISSN 2297-8739). This special issue belongs to the section "Analysis of Natural Products and Pharmaceuticals".

Deadline for manuscript submissions: closed (10 November 2024) | Viewed by 8478

Special Issue Editors

Prof. Dr. Aurea Bernardino-Nicanor

E-Mail Website
Guest Editor
Tecnológico Nacional de México-Celaya, Antonio García Cubas Pte #600 esq., Av. Tecnológico, A. P. 57, Celaya 38010, Guanajuato, Mexico
Interests: food; nutraceuticals; macromolecules; vegetable metabolites; biomedicine; natural products; chemical composition
Dr. Leopoldo González Cruz

E-Mail Website
Guest Editor
Tecnológico Nacional de México-Celaya, Antonio García Cubas Pte #600 esq., Av. Tecnológico, A. P. 57, Celaya 38010, Guanajuato, Mexico
Interests: food; antioxidants; vegetables; macromolecules

Special Issue Information

Dear Colleagues,

A recent trend in the food, pharmaceutical, cosmetic and agricultural sectors is the search for novel compounds that contribute to the development of novel products. For this reason, in recent years, plants grown under stress conditions have been included in experiments to produce new drugs that are also natural products or derived from them. In recent years, the separation of metabolites and natural products has made great progress. For this reason, it is important to highlight the recent trend in process optimization and characterization of natural products or metabolites using this new technology. However, the contributions of traditional separation methods are also important when new sources of metabolites or natural products are found. Considering the importance of separation and characterization of metabolites and natural products, it is necessary to consider various extraction and separation techniques, such as microwave and ultrasonic-assisted extraction, molecular distillation methods, supercritical fluid extraction, membrane separation methods and/or chromatographic methods such as preparative high-performance liquid chromatography (HPLC). For these reasons, the aim of this Special Issue is to present new methods for the separation of natural products or metabolites, to report on changes in their nutraceutical value through the separation process and to highlight new potential sources for the separation of natural products and/or metabolites.

We invite you to submit a research article, short communication or review to this Special Issue dedicated to the separation and analysis of the chemical composition of natural products and metabolites.

Prof. Dr. Aurea Bernardino-Nicanor
Dr. Leopoldo González Cruz
Guest Editors

Manuscript Submission Information

Manuscripts should be submitted online at www.mdpi.com by registering and logging in to this website. Once you are registered, click here to go to the submission form. Manuscripts can be submitted until the deadline. All submissions that pass pre-check are peer-reviewed. Accepted papers will be published continuously in the journal (as soon as accepted) and will be listed together on the special issue website. Research articles, review articles as well as short communications are invited. For planned papers, a title and short abstract (about 100 words) can be sent to the Editorial Office for announcement on this website.

Submitted manuscripts should not have been published previously, nor be under consideration for publication elsewhere (except conference proceedings papers). All manuscripts are thoroughly refereed through a single-blind peer-review process. A guide for authors and other relevant information for submission of manuscripts is available on the Instructions for Authors page. Separations is an international peer-reviewed open access monthly journal published by MDPI.

Please visit the Instructions for Authors page before submitting a manuscript. The Article Processing Charge (APC) for publication in this open access journal is 2600 CHF (Swiss Francs). Submitted papers should be well formatted and use good English. Authors may use MDPI's English editing service prior to publication or during author revisions.

Keywords

  • HPLC separation
  • metabolites separation
  • non-conventional separation techniques
  • gas chromatography
  • protein separation
  • pigment separation
  • separation and characterization of carbohydrates

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Published Papers (5 papers)

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Research

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11 pages, 3136 KiB  
Article
Isolation and Hydrolysis of Proteins from Vigna umbellata and the Effect on Their Antioxidant and Anticancer Activities
by Leopoldo González-Cruz, Leonardo Morales-Cerda, Gerardo Teniente-Martínez, Carmen Valadez-Vega and Aurea Bernardino-Nicanor
Separations 2025, 12(3), 55; https://doi.org/10.3390/separations12030055 - 20 Feb 2025
Viewed by 594
Abstract
Rice bean is a legume that is considered to be an important source of protein; it is still poorly understood but can produce peptides with various biological activities. These peptides can be released by enzymes during gastrointestinal passage and have a physiological effect [...] Read more.
Rice bean is a legume that is considered to be an important source of protein; it is still poorly understood but can produce peptides with various biological activities. These peptides can be released by enzymes during gastrointestinal passage and have a physiological effect on cancer cells. Since both the type of legume and the enzyme cocktail used are crucial for the production of peptides against certain cancer cell types, the anticancer effects of Vigna umbellata isolate and hydrolysate against MDA and SiHa cells were investigated in this study. The isolate was obtained via isoelectric precipitation, and the hydrolysate was obtained via pepsin P7012 and pancreatin P1750. The anticancer activity was determined by cell viability via the MTT assay, and a Pearson correlation coefficient was calculated to determine the relationships between the anticancer activity and total phenolic compounds, and the antioxidant activity of the isolated rice bean protein and its hydrolysate. The rice bean hydrolysate had a higher concentration of phenolic compounds than the isolate does, resulting in high antioxidant activity. The inhibition of proliferation in SiHa cells and MDA cells was twofold greater when they were exposed to the hydrolysate than when they were exposed to the isolate, with the IC50 values at a concentration of 1000 μg/mL after 48 h of exposure for both MDA and SiHa cells. Rice bean protein hydrolysate is a good alternative for inhibiting the proliferation of SiHa cells and MDA cells, although further studies are needed. Full article
(This article belongs to the Special Issue Extraction and Analysis of Chemical Composition from Natural Products and Metabolites)
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10 pages, 1179 KiB  
Article
Supercritical Extraction of Ylang Ylang (Cananga odorata) Essential Oil at the Near-Critical Region
by Rodney Mahabir, Sharad Maharaj, Marian J. Watson, David R. McGaw and Cian Coonai
Separations 2024, 11(10), 295; https://doi.org/10.3390/separations11100295 - 13 Oct 2024
Cited by 1 | Viewed by 2445
Abstract
The flowers of the ylang ylang tree contain an essential oil which is utilized in high-quality perfumes. The traditional mode of extraction is by steam distillation but it has been shown that the more modern supercritical fluid extraction (SFE) using carbon dioxide has [...] Read more.
The flowers of the ylang ylang tree contain an essential oil which is utilized in high-quality perfumes. The traditional mode of extraction is by steam distillation but it has been shown that the more modern supercritical fluid extraction (SFE) using carbon dioxide has potential for replacing steam distillation. This technology, however, generally operates under high pressures, up to 500 bar. The work described in this paper examines the possibility of using carbon dioxide at much lower pressures, close to the critical point, i.e., 75 bar and 30 °C. Two series of experiments were therefore carried out under such conditions, the first using carbon dioxide alone and the second utilizing ethanol as a co-solvent, the conditions being chosen by applying the Design of Experiments (DOE) technique over ranges of pressure from 80 to 120 bar and temperatures from 35 to 50 °C. Extraction curves are presented which show the rates of extraction to be significantly increased by the use of the co-solvent, with the measured values being 0.74% to 0.97% with no co-solvent addition, increasing to 0.92% to 1.16% with co-solvent addition. These rates are, however, lower than the rates previously reported at higher pressures, i.e., 0.9 to 1.8%. Better quality oils are, however, produced compared to those at higher pressures, with the major components being benzene benzoate, benzene salicylate, cubebene, and benzyl acetate. It is recommended that an economic study be carried out to evaluate whether it is feasible to utilize this process commercially. Full article
(This article belongs to the Special Issue Extraction and Analysis of Chemical Composition from Natural Products and Metabolites)
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18 pages, 3717 KiB  
Article
The Optimization of the Osborne Extraction Method for the Fractionation and Characterization of Oat Proteins
by Sorel Tchewonpi Sagu, Lara Talea Wiedemann, Kapil Nichani, Andrea Henze and Harshadrai M. Rawel
Separations 2024, 11(9), 271; https://doi.org/10.3390/separations11090271 - 17 Sep 2024
Cited by 4 | Viewed by 2295
Abstract
The growing number of wheat-related allergies worldwide has resulted in a new trend towards gluten-free alternatives. In this context, alternative cereals such as sorghum and oats are attracting new interest. Given the limited data available, the question of whether these cereals are completely [...] Read more.
The growing number of wheat-related allergies worldwide has resulted in a new trend towards gluten-free alternatives. In this context, alternative cereals such as sorghum and oats are attracting new interest. Given the limited data available, the question of whether these cereals are completely safe and gluten-free for allergy sufferers remains open. One of the key steps in protein research is their efficient extraction. In this work, the Osborne sequential extraction method was developed and optimized using the response surface methodology in order to fractionate oat proteins. An optimized desirability of 0.986 was achieved with an extraction time of 4.7 min, a speed of 6, and a sample/solvent ratio of 5. The corresponding optimized responses were 8.7, 4.0, and 5.1% for the extraction yields of the avenin, avenalin, and albumin/globulin fractions, respectively. Further characterization of the extracts was carried out on 24 homogeneous and commercial oat samples via LC-MS/MS, targeting six potentially allergenic proteins. The avenin-E protein featured prominently, with relative contents of 60.7, 32.2, 58.0, and 59.8% in the total extract, avenin, avenalin, and albumin/globulin fractions, respectively, while the Avenin-3, ATI-2, avenin, SSG2, and SSG1 proteins in the total extract showed levels of 16.4, 9.3, 6.6, 4.8, and 2.2%, respectively. The preliminary results of an ELISA performed on the different fractions revealed low levels of gluten (from 1.24 ± 0.14 to 3.61 ± 0.16 mg/kg), which were well below the threshold limit of 20 mg/kg. These results support the hypothesis that oats can be a safe food for people suffering from cereal-related allergies. These results open the door to further studies into the comprehensive characterization of oat proteins. Full article
(This article belongs to the Special Issue Extraction and Analysis of Chemical Composition from Natural Products and Metabolites)
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13 pages, 1880 KiB  
Article
Screening Biogenic Volatile Organic Compounds from Common Portuguese Shrubs Using Headspace–Bar Adsorptive Microextraction (HS-BAµE)
by Jéssica S. R. F. Cerqueira and José M. F. Nogueira
Separations 2024, 11(9), 264; https://doi.org/10.3390/separations11090264 - 9 Sep 2024
Viewed by 1214
Abstract
In this study, headspace–bar adsorptive microextraction (HS-BAµE) combined with gas chromatography–mass spectrometry (GC-MS) was employed to screen the major biogenic volatile organic compounds (BVOCs) emitted by six different Portuguese shrub species (Erica scoparia L., Cistus ladanifer L., Cistus monspeliensis L., Lavandula stoechas [...] Read more.
In this study, headspace–bar adsorptive microextraction (HS-BAµE) combined with gas chromatography–mass spectrometry (GC-MS) was employed to screen the major biogenic volatile organic compounds (BVOCs) emitted by six different Portuguese shrub species (Erica scoparia L., Cistus ladanifer L., Cistus monspeliensis L., Lavandula stoechas L., Thymus villosus L., and Thymus camphoratus). The HS-BAµE/GC-MS methodology was developed, optimized, and validated using five common monoterpenoids (α-pinene, β-pinene, limonene, 1,8-cineole, and thymol) and one sesquiterpenoid (caryophyllene oxide). Under optimized experimental conditions (microextraction-sorbent phase: activated carbon (CN1), 3 h (35 °C); back-extraction: n-C6 (1 h)), good efficiencies (>45%), low analytical thresholds (5.0–15.0 µg/L) and suitable linear dynamic ranges (20.0–120.0 µg/L, r2 > 0.9872) were achieved, as well as acceptable intra and inter-day precisions (RSD ≤ 30.1%). Benchmarking the proposed methodology, HS-BAµE(CN1), against the reference methodology, HS-SPME(PDMS/DVB), revealed comparable analytical responses and demonstrated excellent reproducibility. Among the six shrub species studied, Thymus camphoratus exhibited the highest emissions of BVOCs from its leaves, notably, 1,8-cineole (4136.9 ± 6.3 µg/g), α-pinene (763.9 ± 0.5 µg/g), and β-pinene (259.3 ± 0.5 µg/g). It was also the only species found to release caryophyllene oxide (411.4 ± 0.3 µg/g). The observed levels suggest that these shrub species could potentially serve as fuel sources in the event of forest fires occurring under extreme conditions. In summary, the proposed methodology proved to be a favorable analytical alternative for screening BVOCs in plants. It not only exhibited remarkable performance but also demonstrated user- and eco-friendliness, cost-effectiveness, and ease of implementation. Full article
(This article belongs to the Special Issue Extraction and Analysis of Chemical Composition from Natural Products and Metabolites)
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Review

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19 pages, 2910 KiB  
Review
Techniques and Methods for Fatty Acid Analysis in Lipidomics: Exploring Pinus cembroides Kernels as a Sustainable Food Resource
by Luis Ricardo León-Herrera, Luis Miguel Contreras-Medina, Ana Angélica Feregrino-Pérez, Christopher Cedillo, Genaro Martín Soto-Zarazúa, Miguel Angel Ramos-López, Samuel Tejeda, Eduardo Amador-Enríquez and Enrique Montoya-Morado
Separations 2025, 12(2), 41; https://doi.org/10.3390/separations12020041 - 6 Feb 2025
Viewed by 1217
Abstract
The large-scale conversion of forests to agriculture has caused biodiversity loss, climate change, and disrupted dietary fatty acid balances, with adverse public health effects. Wild edibles like pine nuts, especially Pinus cembroides, provide sustainable solutions by supporting ecosystems and offering economic value. [...] Read more.
The large-scale conversion of forests to agriculture has caused biodiversity loss, climate change, and disrupted dietary fatty acid balances, with adverse public health effects. Wild edibles like pine nuts, especially Pinus cembroides, provide sustainable solutions by supporting ecosystems and offering economic value. However, variability in seed quality limits market potential, and lipidomic studies on P. cembroides remain sparse. This paper underscores the ecological, social, and nutritional value of P. cembroides while advocating for advanced research to enhance its use as a non-timber forest resource in Mexico’s communal areas. It explores various analytical techniques, such as nuclear magnetic resonances (NMR), chromatography coupled with mass spectrometry (HPLC-MS, GC-MS) and GC coupled with flame ionization detector (GC-FID), highlighting extraction methods like derivatization, purification, and thin-layer chromatography. Likewise, some considerations are addressed for the treatment of data obtained in the detection of fatty acids from bioformatics and the evaluation of the data through statistical methods and artificial intelligence and deep learning. These approaches aim to improve fatty acid profiling and seed quality assessments, fostering the species economic viability and supporting sustainable livelihoods in rural communities, encouraging researchers across the country to explore the fatty acid composition of different P. cembroides populations can drive valuable insights into its nutritional and ecological significance. Such efforts can enhance understanding of regional variations, promote sustainable use, and elevate the specie’s economic and scientific value. Full article
(This article belongs to the Special Issue Extraction and Analysis of Chemical Composition from Natural Products and Metabolites)
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