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Separations
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Application of Hyphenated Techniques in Natural Product Analysis
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Application of Hyphenated Techniques in Natural Product Analysis

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 (30 November 2023) | Viewed by 14131

Special Issue Editors

Dr. Adriana Arigò

E-Mail Website
Guest Editor
Department of Pure and Applied Sciences, University of Urbino Carlo Bo, Urbino, Italy
Interests: Analytical Chemistry; Food Chemistry; Liquid Chromatography; Gas Chromatography; Supercritical Fluid Chromatography; Tandem Mass Spectrometry; High-Resolution Mass Spectrometry; Ambient Mass Spectrometry; Real-Time analysis; Method validation; Bioactive Compounds; Nutraceuticals; Food; Essential oils; Pesticides
Special Issues, Collections and Topics in MDPI journals
Dr. Emanuela Trovato

E-Mail Website
Guest Editor
Department of Chemical, Biological, Pharmaceutical and Environmental Sciences, University of Messina, Messina, Italy
Interests: gas chromatography; mass spectrometry; tandem mass spectrometry; food analysis; bioactive compounds; MS libraries; essential oils
Special Issues, Collections and Topics in MDPI journals
Dr. Petr Česla

E-Mail Website
Guest Editor
Department of Analytical Chemistry, Faculty of Chemical Technology, University of Pardubice, Pardubice, Czech Republic
Interests: liquid-phase separation methods – liquid chromatography, capillary electrophoresis; two-dimensional liquid chromatography; chromatographic analysis of naturally occurring samples, mainly secondary plant metabolites
Special Issues, Collections and Topics in MDPI journals

Special Issue Information

Dear Colleagues,

The market for natural products has increased exponentially in the last decade. The awareness of a strict correlation between bioactive compounds contained in foods and plants is the reason for the success of natural bioactive compounds and nutraceuticals. Diets based on nutraceuticals and natural medicaments, such as in traditional medicine, are currently representative of a renewed healthy lifestyle.

In this context, the need to characterize bioactive compounds in natural complex matrices or their commercial product derivatives is mandatory. Advanced analytical methods play a key role in this field, allowing for the deep correlation between compounds and pharmacological activity and safeguarding consumer health by proper quality control protocols, enabling regulatory bodies to act where necessary.

In this contest, hyphenated analytical techniques are still the most resolutive approach when a complete and reliable characterization of complex matrices is required. Despite the great success of recent fast analytical techniques, coupling separative methods with MS provides highly informative results, in terms of quali-quantitative data and validation method parameters.

Research studies focused on the “Application of Hyphenated Techniques in Natural Product Analysis” are welcome in this Special Issue, aimed to highlight the great potential of combined powerful analytical strategies and their wide range of applications.

Dr. Adriana Arigò
Dr. Emanuela Trovato
Dr. Petr Česla
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

  • chromatography
  • supercritical fluid chromatography
  • mass spectrometry
  • tandem mass spectrometry
  • high-resolution mass spectrometry
  • method validation
  • bioactive compounds
  • quality control
  • extraction
  • green chemistry

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Published Papers (4 papers)

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Research

12 pages, 751 KiB  
Article
Comparative Study of Chemical Composition and Cholinesterase Inhibition Potential of Essential Oils Isolated from Artemisia Plants from Croatia
by Olivera Politeo, Ivana Cajic, Anja Simic, Mirko Ruscic and Mejra Bektasevic
Separations 2023, 10(10), 546; https://doi.org/10.3390/separations10100546 - 23 Oct 2023
Viewed by 2377
Abstract
The essential oil (EO) of Artemisia plants contains a large number of bioactive compounds that are widely used. The aim of this study was to analyse the chemical composition of EOs of six Artemisia plants collected in Croatia and to test their cholinesterase [...] Read more.
The essential oil (EO) of Artemisia plants contains a large number of bioactive compounds that are widely used. The aim of this study was to analyse the chemical composition of EOs of six Artemisia plants collected in Croatia and to test their cholinesterase inhibitory potential. GC–MS analysis of the EO of A. absinthium showed that the dominant compounds are cis-sabinyl acetate and cis-epoxy-ocimene; in EO of A. abrotanum, it is borneol; in the EO of A. annua, they are artemisia ketone, camphor and 1,8-cineole; in the EO of A. arborescens, they are camphor and chamazulene; in the EO of A. verlotiorum, they are cis-thujone, 1,8-cineole and trans-thujone; and in the EO of A. vulgaris, they are trans-thujone and trans-epoxy-ocimene. The EO of the five studied Artemisia species from Croatia is rich in monoterpenoid compounds (1,8-cineole, artemisia ketone, cis-thujone, trans-thujone, cis-epoxy-ocimene, camphor, borneol and cis-sabinyl acetate). The EO of A. arborescens is also rich in chamazulene. The results also showed that the tested EOs have moderate cholinesterase inhibition potential, especially the EOs of A. annua, A. vulgaris and A. abrotanum. This is the first analysis of the chemical composition of the EOs of four Artemisia plants and the first analysis of cholinesterase potential for plants collected in Croatia. Full article
(This article belongs to the Special Issue Application of Hyphenated Techniques in Natural Product Analysis)
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13 pages, 2539 KiB  
Article
Rhaphiolepis indica Fruit Extracts for Control Fusarium solani and Rhizoctonia solani, the Causal Agents of Bean Root Rot
by Ahmed A. Heflish, Said I. Behiry, Abdulaziz A. Al-Askar, Yiming Su, Ahmed Abdelkhalek and Mohamed K. Gaber
Separations 2023, 10(7), 369; https://doi.org/10.3390/separations10070369 - 23 Jun 2023
Cited by 5 | Viewed by 1803
Abstract
Numerous strategies have been suggested to reduce dependence on synthetic products, such as physical, microbial, and natural methods. Among the natural remedies, plant extracts have emerged as a popular option owing to their eco-friendly character, ease of degradation, and harmless nature to humans. [...] Read more.
Numerous strategies have been suggested to reduce dependence on synthetic products, such as physical, microbial, and natural methods. Among the natural remedies, plant extracts have emerged as a popular option owing to their eco-friendly character, ease of degradation, and harmless nature to humans. In our study, we used the acetone and hexane extracts of Rhaphiolepis indica fruit to combat two fungal pathogens that were isolated from infected bean plants and showed root rot symptoms. The two pathogens were confirmed to be pathogenic by pathogenicity assays conducted in vivo. The morphological and molecular identification by ITS-region sequencing revealed that the two isolates were Rhizoctonia solani and Fusarium solani, and they were assigned accession numbers OQ880457 and OQ820158, respectively. Our data showed that both hexane and acetone extracts caused a significant decrease in the linear growth of F. solani at all concentrations used (1%, 2%, and 3%), compared to the control. However, at a concentration of 3%, the hexane extract caused much greater inhibition than the acetone extract. For R. solani, the hexane extract, shows a significant inhibition percentage at all concentrations, which further increases to 85.24% at 3% concentration. The HPLC of both extracts indicated the presence and absence of phenolic and flavonoid compounds. The obtained results revealed that five acetonic phenolic extract compounds were ferulic, p-coumaric, gallic, p-OH benzoic, and cinnamic, with concentrations of 5.31, 10.36, 7.24, 6.08, and 0.89 mg/mL, respectively. On the other hand, the five hexanoic phenolic compounds were catechol, caffeic, chlorogenic, p-OH benzoic, and cinnamic acids, with concentrations of 3.66, 5.14, 0.69, 6.31, and 13.47 mg/mL, respectively. The identified acetonic flavonoid extract compounds, namely rutin, chrysin, quercetin, kaempferol, chrysoeriol, 7-OH flavone, and naringin, had respective concentrations of 5.36, 10.23, 4.32, 15.33, 1.06, 0.087, and 0.069 mg/mL, respectively. In contrast, it was observed that the seven hexanoic flavonoid extracts comprised of rutin, quercetin, kampferol, luteolin, chrysoeriol, 7-OH flavone, and catechin exhibited concentrations of 5.36, 7.15, 18.20, 6.04, 2.04, 10.24, and 13.43 mg/mL, respectively. The results of the study suggest that plant extracts may be a useful natural remedy for combating fungal pathogens and reducing dependence on synthetic products. Full article
(This article belongs to the Special Issue Application of Hyphenated Techniques in Natural Product Analysis)
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16 pages, 1093 KiB  
Article
Antimicrobial Efficacy and HPLC Analysis of Polyphenolic Compounds in a Whole-Plant Extract of Eryngium campestre
by Abdulaziz A. Al-Askar, Shimaa Bashir, Abdallah E. Mohamed, Omaima A. Sharaf, Rokaia Nabil, Yiming Su, Ahmed Abdelkhalek and Said I. Behiry
Separations 2023, 10(6), 362; https://doi.org/10.3390/separations10060362 - 18 Jun 2023
Cited by 11 | Viewed by 2659
Abstract
Due to the constant increase in the number of plant diseases and the lack of available treatments, there has been a growing interest in plant extracts over the past few decades. Numerous studies suggest that plant extract molecules possess valuable antimicrobial activities, particularly [...] Read more.
Due to the constant increase in the number of plant diseases and the lack of available treatments, there has been a growing interest in plant extracts over the past few decades. Numerous studies suggest that plant extract molecules possess valuable antimicrobial activities, particularly against fungi and bacteria. This suggests that these biomaterials could potentially serve as attractive therapeutic options for the treatment of phytopathogen infections. In the present study, we investigated and analyzed the methanolic extract of Eryngium campestre L. whole plant extract using HPLC. The analysis revealed the presence of several polyphenolic constituents, with benzoic acid, catechol, quercetin, vanillic acid, resveratrol, naringenin, and quinol being the most abundant. The amounts of these constituents were determined to be 2135.53, 626.728, 579.048, 356.489, 323.41, 153.038, and 128.77 mg/kg, respectively. Furthermore, we isolated and identified different plant fungal and bacterial isolates from symptomatic potato plants, which were accessioned as Rhizoctonia solani (OQ880458), Fusarium oxysporum (OQ820156) and Fusarium solani (OQ891085), Ralstonia solanacearum (OQ878653), Dickeya solani (OQ878655), and Pectobacterium carotovorum (OQ878656). The antifungal activity of the extract was assessed using fungal growth inhibitions (FGI) at concentrations of 100, 200, and 300 µg/mL. The results showed that at the lowest concentration tested (100 µg/mL), the extract exhibited the highest effectiveness against R. solani with an FGI of 78.52%, while it was least effective against F. solani with an FGI of 61.85%. At the highest concentration tested, the extract demonstrated the highest effectiveness against R. solani and F. oxysporum, with FGIs of 88.89% and 77.04%, respectively. Additionally, the extract displayed a concentration-dependent inhibitory effect on all three bacterial pathogens. At the highest concentration tested (3000 µg/mL), the extract was able to inhibit the growth of all three bacterial pathogens, although the inhibition zone diameter varied. Among the bacterial pathogens, D. solani exhibited the highest sensitivity to the extract, as it showed the largest inhibition zone diameter at most of the extract concentrations. These findings highlight the potential of the E. campestre extract as a source of natural antimicrobial agents for controlling various plant pathogens. Consequently, it offers a safer alternative to the currently employed protective methods for plant disease management. Full article
(This article belongs to the Special Issue Application of Hyphenated Techniques in Natural Product Analysis)
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11 pages, 1188 KiB  
Article
Quantitation of Ecdysterone and Targeted Analysis of WADA-Prohibited Anabolic Androgen Steroids, Hormones, and Metabolic Modulators in Ecdysterone-Containing Dietary Supplements
by Zoltán Pálinkás, Dániel Békési and Margita Utczás
Separations 2023, 10(4), 242; https://doi.org/10.3390/separations10040242 - 5 Apr 2023
Cited by 6 | Viewed by 6669
Abstract
The aim of our research was to perform a comprehensive study of ecdysterone (ECD)-containing dietary supplements (DSs). Two analytical methods were optimised according to the expected concentration of the target compounds: quantitation of ECD by liquid chromatography (LC) coupled to diode array detector [...] Read more.
The aim of our research was to perform a comprehensive study of ecdysterone (ECD)-containing dietary supplements (DSs). Two analytical methods were optimised according to the expected concentration of the target compounds: quantitation of ECD by liquid chromatography (LC) coupled to diode array detector (DAD), and limit test for 47 World Anti-Doping Agency prohibited by LC coupled with tandem mass spectrometer (MS/MS). For quantitation of ECD, the method was fully validated with outstanding performance characteristics (LOD: 35 µg·g−1, LOQ: 115 µg·g−1, CV% < 5%), resulting in significantly lower LOD and shorter runtime than published previously. For limit tests, a chromatographic method was developed to obtain excellent separation, while MS/MS parameters were optimised to allow the lowest possible reporting limit (RL: 0.6–10 ng·g−1 or mL−1). Twenty-one ecdysterone-containing DSs from ten brands were analysed. In all cases, the measured ECD content was much lower than labelled, and 20% of the samples contained a prohibited substance. The concentration of ecdysterone and contaminations varied randomly from batch to batch. The developed methods help to prevent the use of contaminated or useless DSs. Full article
(This article belongs to the Special Issue Application of Hyphenated Techniques in Natural Product Analysis)
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