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Early Career Stars in Separation Analysis of Natural Products and...
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Early Career Stars in Separation Analysis of Natural Products and Pharmaceuticals

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 (15 March 2023) | Viewed by 18350

Special Issue Editors

Dr. Irina Ielciu

E-Mail Website
Guest Editor
Department of Pharmaceutical Botany, Iuliu Haţieganu University of Medicine and Pharmacy, 400337 Cluj-Napoca, Romania
Interests: extraction; pharmaceutical development; natural product chemistry; Pharmacokinetics; medicinal plants; flavonoids; polyphenols; alkaloids; antioxidant; antimicrobial; antidiabetic; hepatoprotection; antispastic
Special Issues, Collections and Topics in MDPI journals
Dr. Arnaud Delobel

E-Mail Website
Guest Editor
Quality Assistance sa, Technoparc de Thudinie 2, 6536 Thuin, Belgium
Interests: mass spectrometry; proteins; liquid chromatography; monoclonal antibodies; drugs

Special Issue Information

Dear Colleagues,

“Early Career Stars in Analysis of Natural Products and Pharmaceuticals” is a Special Issue aimed at early career researchers in Analysis of Natural Products and Pharmaceuticals (students and scholars who are at the undergraduate, graduate, or post-graduate level—up to 10 years post-doctoral degree).

Due to COVID-19 pandemic, many Early Career investigators have faced extra challenges in their uphill battle to establish their careers in science. In order to support the such researchers' career, we built a special issue aimed at early career researchers. The special issue aims to provide an international platform for exchanging ideas and presenting the latest achievements in the areas of Separations.

Dr. Irina Ielciu
Dr. Arnaud Delobel
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

  • natural products
  • pharmaceuticals
  • separation techniques
  • chemical analysis

Published Papers (7 papers)

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Research

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23 pages, 3085 KiB  
Article
Capillary Zone Electrophoresis with Light-Emitting Diode-Induced Fluorescence Detection for the Analysis of Monoclonal Antibodies: Detector Optimization through Design of Experiments and Comparison to UV Detection
by Holger Zagst, Sophie Hartung, Dina-Mareike Menges, Antonia Wittmann and Hermann Wätzig
Separations 2023, 10(5), 320; https://0-doi-org.brum.beds.ac.uk/10.3390/separations10050320 - 21 May 2023
Cited by 1 | Viewed by 1470
Abstract
Capillary zone electrophoresis (CZE) is an important technique for the analysis of monoclonal antibodies (mAbs). A recently released light-emitting diode (LED)-induced fluorescence (LEDIF) detector equipped with a 275 nm LED for the detection of proteins through their native fluorescence was used in this [...] Read more.
Capillary zone electrophoresis (CZE) is an important technique for the analysis of monoclonal antibodies (mAbs). A recently released light-emitting diode (LED)-induced fluorescence (LEDIF) detector equipped with a 275 nm LED for the detection of proteins through their native fluorescence was used in this study and compared to results obtained using the predominant detection mode, the measurement of the absorption of ultraviolet light (UV detection). This was accomplished using an established CZE method for the analysis of three mAbs: NISTmAb, matuzumab, and Intact Mass Check Standard (Waters). For this purpose, the detector’s settings were first optimized using a design of experiments approach. Three factors, rise time, photomultiplier high voltage supply, and acquisition frequency, were optimized by means of a D-optimal design. The optimal settings were then used for the investigation of signal-to-noise ratios (S/Ns), linearity, and precision. LEDIF detection offered a similar separation quality, up to 12 times higher S/Ns, and lower limits of detection compared to UV detection. Repeatability was excellent, with relative standard deviations (RSDs) of approximately 1% for percentage areas. For intermediate precision, RSDs of <2% (n = 3 × 10) were typically achieved. Overall, LEDIF detection was found to be an excellent and easily optimizable alternative to UV detection. Full article
(This article belongs to the Special Issue Early Career Stars in Separation Analysis of Natural Products and Pharmaceuticals)
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14 pages, 2699 KiB  
Article
LC–MS/MS Coupled with Chemometric Analysis as an Approach for the Differentiation of Fritillariae cirrhosae Bulbus and Fritillariae pallidiflorae Bulbus
by Xiaomu Zhu, Ting Zhou, Shu Wang, Bengui Ye, Rajeev K. Singla, Devesh Tewari, Atanas G. Atanasov, Dongdong Wang and Simei Liu
Separations 2023, 10(2), 75; https://0-doi-org.brum.beds.ac.uk/10.3390/separations10020075 - 21 Jan 2023
Viewed by 1668
Abstract
Fritillariae cirrhosae bulbus (FCB) is one of the most important traditional Chinese medicines (TCM) for the treatment of cough and phlegm. Due to increasing demand and the complexity of FCB’s botanical origin, various substitutes have appeared in the market, resulting in a major [...] Read more.
Fritillariae cirrhosae bulbus (FCB) is one of the most important traditional Chinese medicines (TCM) for the treatment of cough and phlegm. Due to increasing demand and the complexity of FCB’s botanical origin, various substitutes have appeared in the market, resulting in a major challenge to distinguish FCB and its substitutes (F. pallidiflorae bulbus, FPB). Therefore, discriminating FCB from FPB has becoming an urgent necessity. In this study, an ultra-high-performance liquid chromatography–electrospray ionization–tandem mass spectrometry (UPLC–ESI–MS/MS) method was developed for the simultaneous quantification of nine steroidal alkaloids (imperialine-3-β-D-glucoside, imperialine, verticine, verticinone, peimisine, yibeinoside A, delavine, delavinone, ebeidinone) within 8 min. According to the composition and content of the above nine compounds, multivariate chemometric analyses were applied for the classification of FCB and FPB. The quantitative results showed that there were both similarities and differences in the content of nine steroidal alkaloids between FCB and FPB, and it was difficult to directly distinguish these two species. Fortunately, with the aid of chemometric analyses, FCB and FPB were successfully differentiated by partial least squares discrimination analysis (PLS-DA) and orthogonal partial least squares discrimination analysis (OPLS-DA) models based on the nine alkaloids’ content. Moreover, four compounds (yibeinoside A, ebeiedinone, delavinone and imperialine) were discovered as potential markers for the identification and differentiation of FCB and FPB. Additionally, compared to other studies, this work collected a large number of samples (49 batches of FCB and 17 batches of FPB) to ensure the reliability of the results. In conclusion, this work established a new approach for the authentication of FCB based on its active components, which provides a good reference for the quality control of FCB and will help us to understand the chemical composition differences between FCB and its adulterants further. Full article
(This article belongs to the Special Issue Early Career Stars in Separation Analysis of Natural Products and Pharmaceuticals)
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18 pages, 4170 KiB  
Article
Parameter Effects and Optimisation in Supercritical Fluid Extraction of Phenolic Compounds from Labisia pumila
by Shazana Azfar Radzali, Masturah Markom and Noorashikin Md Saleh
Separations 2022, 9(12), 385; https://0-doi-org.brum.beds.ac.uk/10.3390/separations9120385 - 22 Nov 2022
Cited by 5 | Viewed by 3472
Abstract
Labisia pumila, locally referred to as kacip fatimah, is one of the important herbs utilised in traditional medicine. Nonetheless, to the best of the researchers’ knowledge, the optimum application of Supercritical Fluid Extraction (SFE) has not been reported for Labisia pumila (L. pumila) [...] Read more.
Labisia pumila, locally referred to as kacip fatimah, is one of the important herbs utilised in traditional medicine. Nonetheless, to the best of the researchers’ knowledge, the optimum application of Supercritical Fluid Extraction (SFE) has not been reported for Labisia pumila (L. pumila) extraction and the understanding of this study may offer preliminary insight into the preparation of standardised extracts of L. pumila enriched with natural antioxidants prior to commercialisation at the industrial level. Response surface methodology (RSM) was used to optimise supercritical carbon dioxide extraction (SC-CO2) of functional phenolic compounds from L. pumila leaves. The factors studied were pressure, temperature, percentage of ethanol in co-solvent, and co-solvent concentration. The results demonstrated that the percentage of ethanol in co-solvent, temperature, and co-solvent concentration in the supercritical mixture had significant effects on the extraction of L. pumila. Based on the RSM results, the optimal SC-CO2 extraction conditions were at 283 bar, 32 °C, 78% (v/v) of ethanol-water in co-solvent, and 16% (v/v) of co-solvent concentration, which allowed the recovery of 14.051 ± 0.76% (g/g) of extraction yield, 1.2650 ± 0.10% (g/g) of gallic acid, 0.441 ± 0.29% (g/g) of methyl gallate, and 1.382 ± 0.37% (g/g) of caffeic acid. The experimental values were in agreement with the one predicted by RSM models, confirming the suitability of the model for optimisation of the extraction conditions. Full article
(This article belongs to the Special Issue Early Career Stars in Separation Analysis of Natural Products and Pharmaceuticals)
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9 pages, 1296 KiB  
Communication
Boosting the Liquid Chromatography Separation of Complex Bispecific Antibody Products by Using the Multi-Isocratic Elution Mode
by Amarande Murisier, Valentina D’Atri, Vincent Larraillet, Sebastian Pirner and Davy Guillarme
Separations 2022, 9(9), 243; https://0-doi-org.brum.beds.ac.uk/10.3390/separations9090243 - 04 Sep 2022
Cited by 3 | Viewed by 1932
Abstract
In reversed-phase liquid chromatography (RPLC), the selectivity between major species and minor variants of protein biopharmaceutical products is always limited. Unfortunately, the stationary phase chemistry, type of mobile phase (organic modifier and salts) and temperature only have a very limited impact on selectivity. [...] Read more.
In reversed-phase liquid chromatography (RPLC), the selectivity between major species and minor variants of protein biopharmaceutical products is always limited. Unfortunately, the stationary phase chemistry, type of mobile phase (organic modifier and salts) and temperature only have a very limited impact on selectivity. Therefore, instead of using a linear elution gradient, we evaluated a recently developed strategy, named the multi-isocratic elution mode, to improve the chromatographic resolution. In this contribution, a generic workflow involving the use of an Excel spreadsheet is provided for the rapid and successful development of multi-isocratic elution methods, without the need to use HPLC modeling software. This simple strategy was then successfully applied to very complex biopharmaceutical products; these included one reduced mAb-cytokine fusion protein and a mAb-domain-fusion (C-terminal) protein sample, containing numerous minor variants that were poorly separated from the major species. The addition of several isocratic steps during the chromatographic run provides a clear added value in terms of chromatographic selectivity for several variants, simplifying characterization of the sample with advanced MS tools. In addition to these advantages, some of the limitations of the multi-isocratic elution mode were also highlighted; these included the need to use a highly precise pumping device (preferably, a binary pumping system) and the need to prepare highly accurate mobile phases. Full article
(This article belongs to the Special Issue Early Career Stars in Separation Analysis of Natural Products and Pharmaceuticals)
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11 pages, 1083 KiB  
Article
Comparison of Supercritical Fluid Chromatography Hyphenated to an Ultraviolet Detector and Gas Chromatography Hyphenated to a Flame Ionization Detector for Qualitative and Quantitative Analysis of Citrus Essential Oils
by Cyrille Santerre, Eldra Delannay, Pilar Franco, Nadine Vallet and David Touboul
Separations 2022, 9(7), 183; https://0-doi-org.brum.beds.ac.uk/10.3390/separations9070183 - 20 Jul 2022
Cited by 5 | Viewed by 2738
Abstract
A comparison between the classical gas chromatography (GC) technique with supercritical fluid chromatography (SFC) technology was performed using an essential oil of Citrus limon (lemon) as a model, considering its wide use in the cosmetic world. For the qualitative part, the signal annotation [...] Read more.
A comparison between the classical gas chromatography (GC) technique with supercritical fluid chromatography (SFC) technology was performed using an essential oil of Citrus limon (lemon) as a model, considering its wide use in the cosmetic world. For the qualitative part, the signal annotation was achieved by mass spectrometry using either an electron ionization (EI) or an atmospheric pressure photoionization (APPI) source. For the quantitative part, GC was hyphenated to a flame ionization detector (GC-FID) and SFC to an ultraviolet detector (SFC-UV). The assay of the major component of citrus oil, i.e., limonene, was carried out by SFC-UV. The similar results obtained between GC-FID and SFC-UV allows SFC-UV to be considered as an alternative to GC-FID for Citrus oil characterization. Then, analyses of an essential oil collection from Citrus fruits were achieved to confirm the potential use of SFC-UV for oil classification in the context of quality control of raw materials in cosmetics. Full article
(This article belongs to the Special Issue Early Career Stars in Separation Analysis of Natural Products and Pharmaceuticals)
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15 pages, 2426 KiB  
Article
Phytochemical Characterization and Heavy Metal and Thermal Analyses of Saussurea hypoleuca Root and Evaluation of Its Anthelmintic and Antioxidant Activity In Vitro and In Silico
by Sameh S. Elhady, Numera Arshad, Saiqa Ishtiaq, Roula Bayram, Adnan Amin, Hanin A. Bogari, Reda F. A. Abdelhameed, Fadia S. Youssef and Mohamed L. Ashour
Separations 2022, 9(6), 138; https://0-doi-org.brum.beds.ac.uk/10.3390/separations9060138 - 30 May 2022
Cited by 1 | Viewed by 1770
Abstract
Phytochemical characterization of the ethyl acetate fraction of Saussurea hypoleuca root extract resulted in the isolation of oleic acid (1) and luteolin (2), which were isolated for the first time from Saussurea hypoleuca root. A heavy metal analysis of [...] Read more.
Phytochemical characterization of the ethyl acetate fraction of Saussurea hypoleuca root extract resulted in the isolation of oleic acid (1) and luteolin (2), which were isolated for the first time from Saussurea hypoleuca root. A heavy metal analysis of the root powder performed using atomic absorption spectroscopy showed that the contents of iron, cadmium, lead, zinc, nickel, and copper were within the certified limits according to the WHO guidelines. Differential scanning calorimetry (DSC) revealed its crystalline and amorphous nature; meanwhile, standardization of the root with UHPLC revealed the presence of 14.79 ± 0.015 µg/mL of luteolin. Both the total methanol extract and the ethyl acetate fraction of the plant root held significant anthelmintic activity. Oleic acid and luteolin exhibited potent antioxidant activity, evidenced by their IC50 values, which were equal to 47.0 and 119.8 µg/mL, respectively, in a 2,2-diphenyl-1-picrylhydrazyl (DPPH) scavenging assay. In silico studies showed that luteolin exerted the highest fitting within the binding sites of NADPH oxidase (Nox). For myeloperoxidase (MP), oleic acid revealed the best fitting in its active sites. The results of ADMET (absorption, distribution, metabolism, excretion, and toxicity) and TOPKAT (toxicity prediction) protocols revealed acceptable pharmacodynamic and pharmacokinetic characteristics, in addition to reasonable toxicity characteristics for both compounds. Thus, they can be incorporated into pharmaceutical dosage forms to combat oxidative stress. Full article
(This article belongs to the Special Issue Early Career Stars in Separation Analysis of Natural Products and Pharmaceuticals)
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Review

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21 pages, 460 KiB  
Review
Hypericum spp.—An Overview of the Extraction Methods and Analysis of Compounds
by Valentin Ion, Irina Ielciu, Anca-Gabriela Cârje, Daniela Lucia Muntean, Gianina Crişan and Ramona Păltinean
Separations 2022, 9(1), 17; https://0-doi-org.brum.beds.ac.uk/10.3390/separations9010017 - 14 Jan 2022
Cited by 5 | Viewed by 4491
Abstract
The Hypericum genus contains one of the few genera of flowering plants that contains a species with authorization for marketing as a traditional medicine, H. perforatum. Due to the fact that this is a large genus, comprising numerous species, a large amount [...] Read more.
The Hypericum genus contains one of the few genera of flowering plants that contains a species with authorization for marketing as a traditional medicine, H. perforatum. Due to the fact that this is a large genus, comprising numerous species, a large amount of interest has been shown over the years in the study of its various pharmacological activities. The chemical composition of these species is quite similar, containing compounds belonging to the class of phloroglucinol derivatives, naphthodianthrones, phenols, flavonoids and essential oils. Taking all of this into consideration, the present study aims to offer an overview of the species of the genus from the point of view of their extraction techniques and analysis methods. An extensive study on the scientific literature was performed, and it revealed a wide range of solvents and extraction methods, among which ethanol and methanol, together with maceration and ultrasonication, are the most frequent. Regarding analysis methods, separation and spectral techniques are the most employed. Therefore, the present study provides necessary data for future studies on the species of the genus, offering a complete overview and a possible basis for their development. Full article
(This article belongs to the Special Issue Early Career Stars in Separation Analysis of Natural Products and Pharmaceuticals)
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