Pharmaceutical and Biomedical Applications in Separation Techniques: Recent Trends and Developments

Topic Information

Dear Colleagues,

The analysis of pharmaceuticals, drugs and their metabolites, and biomolecules (proteins, peptides, oligonucleotides, etc.) from different matrices (plasma, serum, oral fluid, urine, etc.) is of great interest to academia and industry. The development of new and green extraction methodologies and validated analytical methods of separation and analysis is therefore of the utmost importance.

Chromatographic techniques such as liquid and gas chromatography are the most frequently used analytical techniques. In addition to these, miniaturized techniques such as capillary electrophoresis, nano-liquid chromatography, and lab-on-a-chip devices are also of great interest; hyphenated detection techniques improve the state of the art of conventional analytical instrumentation. Furthermore, with the further evolution of the classical techniques, instrumental methodologies such as ultra-performance liquid chromatography, supercritical fluid chromatography, capillary electrochromatography, and 2D and 3D systems have seen significant enhancement.

This topic aims to put together original research papers and review articles that demonstrate the recent advances in separation techniques, including all aspects of extraction methodologies, method development, analytical method validation, and application to the various matrices. We therefore encourage authors to submit analyses of chiral and achiral pharmaceuticals, drugs, impurities from pharmaceutical dosage forms, newly developed drug delivery systems, biological media (therapeutic drug monitoring, etc.), environmental samples, targeted and untargeted omics (metabolomics, proteomics, lipidomics, etc.), and substances of abuse.

Dr. Mehmet Gumustas
Prof. Dr. Emirhan Nemutlu
Prof. Dr. Sibel A. Ozkan
Topic Editors

Keywords

Participating Journals

Journal Name	Impact Factor	CiteScore	Launched Year	First Decision (median)	APC
Metabolites metabolites	3.5	5.7	2011	16.1 Days	CHF 2700
Molecules molecules	4.2	7.4	1996	15.1 Days	CHF 2700
Pharmaceuticals pharmaceuticals	4.3	6.1	2004	13.9 Days	CHF 2900
Pharmaceutics pharmaceutics	4.9	7.9	2009	15.5 Days	CHF 2900
Separations separations	2.5	3.0	2014	15.1 Days	CHF 2600

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Published Papers (6 papers)

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All Metabolites Molecules Pharmaceuticals Pharmaceutics Separations

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19 pages, 3742 KiB  

Open AccessArticle

Comparison of Secondary Metabolite Extraction Methods in Hamelia patens Jacq. and Their Inhibitory Effect on Fusarium oxysporum f. sp. radicis-lycopersici

by Daniel Jafet Valle Ortiz, Dolores Guadalupe Aguila Muñoz, María del Carmen Cruz López, Diana Verónica Cortés Espinosa, Martha Rosales Castro and Fabiola Eloísa Jiménez Montejo

Metabolites 2025, 15(1), 23; https://doi.org/10.3390/metabo15010023 - 6 Jan 2025

Viewed by 1243

Abstract

Background: Hamelia patens Jacq. (HP) is widely recognized in traditional medicine for its antimicrobial properties, which are attributed to secondary metabolites such as phenolic compounds, alkaloids, and terpenes. Fusarium oxysporum f. sp. radicis-lycopersici (Fo), a phytopathogenic fungus affecting economically important crops, is [...] Read more.

Background: Hamelia patens Jacq. (HP) is widely recognized in traditional medicine for its antimicrobial properties, which are attributed to secondary metabolites such as phenolic compounds, alkaloids, and terpenes. Fusarium oxysporum f. sp. radicis-lycopersici (Fo), a phytopathogenic fungus affecting economically important crops, is managed with fungicides like benzimidazoles and azoles. Excessive use of these compounds has led to resistance and environmental contamination, highlighting the need for sustainable alternatives. This study aimed to optimize the extraction of secondary metabolites from HP leaves and flowers, evaluate their antifungal activity, and assess the impact of extraction methods and plant parts on chemical composition and efficacy. Methods: Three extraction methods were employed: consecutive maceration (CM) using solvents of ascending polarity; total maceration (TM), which is a single-step methanol-based method; and ultrasound-assisted maceration (UAM) employing ultrasonic waves with methanol. Extracts were characterized by quantifying total phenols (TP), condensed tannins (TC), flavonoids (Fl), alkaloids (TA), sterols (TS), and saponins (S) using colorimetric assays and UPLC-MS. Multivariate analyses, including PCA, PLS-DA, OPLS-DA, and Pearson correlation, evaluated the relationships between the chemical profiles and antifungal activity. Results: Leaf extracts exhibited higher flavonoid and tannin contents than flower extracts. CMML showed the highest antifungal activity (IC₅₀ 3.7% w/v), which was associated with elevated levels of these compounds. Significant correlations linked antifungal activity with rutin (HP21) and kaempferol-3-O-β-rutinoside (HP29). Conclusions: Methanolic extracts of HP exhibited significant antifungal activity against Fo. These findings highlight the importance of optimizing extraction methods and selecting specific plant parts to enhance bioactive compound efficacy, offering a sustainable approach to pathogen management. Full article

(This article belongs to the Topic Pharmaceutical and Biomedical Applications in Separation Techniques: Recent Trends and Developments)

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12 pages, 2428 KiB  

Open AccessArticle

Ligand Screening of Membrane Proteins Embedded in Nanodiscs: How to Manage Non-Specific Interactions in Weak Affinity Chromatography?

by François-Xavier Vidal, Adrien Deloche, Gabrielle Zeder-Lutz, Maria Hideux, Renaud Wagner, Vincent Dugas and Claire Demesmay

Molecules 2024, 29(12), 2814; https://doi.org/10.3390/molecules29122814 - 13 Jun 2024

Cited by 1 | Viewed by 1685

Abstract

Miniaturized weak affinity chromatography is emerging as an interesting alternative to conventional biophysical tools for performing fragment-screening studies in the context of fragment-based drug discovery. In order to push back the analytical limits, it is necessary not only to control non-specific interactions with [...] Read more.

Miniaturized weak affinity chromatography is emerging as an interesting alternative to conventional biophysical tools for performing fragment-screening studies in the context of fragment-based drug discovery. In order to push back the analytical limits, it is necessary not only to control non-specific interactions with chromatographic support, but also to adapt this methodology by comparing the results obtained on an affinity column to a control column. The work presented in this study focused on fragment screening that targets a model membrane protein, the adenosine A2A receptor, embedded in nanodiscs (NDs) as biomimetic membranes. By studying the retention behavior of test fragment mixtures on supports modified with different types of NDs, we were able to determine the contribution of ND-related non-specific interactions, in particular the electrostatic effect of anionic phospholipids and the hydrophobic effect of neutral phospholipids. Different strategies for the preparation of control columns (empty NDs, orthosteric site blocking) were investigated and are presented for the first time. With these two types of control columns, the screening enabled the identification of two new fragments of AA_2AR, which were confirmed by competition experiments and whose K_d values, estimated directly during the screening or after the competition experiments in frontal mode, were in good agreement. Full article

(This article belongs to the Topic Pharmaceutical and Biomedical Applications in Separation Techniques: Recent Trends and Developments)

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18 pages, 4412 KiB  

Open AccessArticle

In Vitro Wound Healing Potential of a Fibroin Film Incorporating a Cannabidiol/2-Hydroxypropyl-β-cyclodextrin Complex

by Thamonphat Klinsang, Pensri Charoensit, Preeyawass Phimnuan, Kunlathida Luangpraditkun, Gareth M. Ross, Céline Viennet, Sukunya Ross and Jarupa Viyoch

Pharmaceutics 2023, 15(12), 2682; https://doi.org/10.3390/pharmaceutics15122682 - 27 Nov 2023

Cited by 7 | Viewed by 2091

Abstract

This study aimed to develop a film dressing prepared by incorporating a complex of cannabidiol and 2-hydroxypropyl-β-cyclodextrin (CBD/HP-β-CD) into a fibroin-based film and to investigate its wound healing capabilities. The fibroin from silkworm cocoons exhibited a total protein content of 96.34 ± 0.14% [...] Read more.

This study aimed to develop a film dressing prepared by incorporating a complex of cannabidiol and 2-hydroxypropyl-β-cyclodextrin (CBD/HP-β-CD) into a fibroin-based film and to investigate its wound healing capabilities. The fibroin from silkworm cocoons exhibited a total protein content of 96.34 ± 0.14% w/w and a molecular weight range of 25 to 245 kDa. Fourier-transform infrared spectroscopy (FTIR) revealed the presence of characteristic amide peaks (I, II, and III) in the isolated fibroin. The CBD/HP-β-CD complex, prepared with a molar ratio of 1:2 (CBD to HP-β-CD), had 81.5 ± 1.2% w/w CBD content, as determined by high-performance liquid chromatography (HPLC). X-ray diffraction (XRD) and FTIR analyses demonstrated successful encapsulation of CBD’s hydrophobic aromatic rings by HP-β-CD. Blending the fibroin solution with the CBD/HP-β-CD complex produced a transparent, slightly yellowish film. Mechanical testing revealed a tensile strength of 48.67 ± 2.57 MPa and a % elongation at a break of 1.71 ± 0.21%. XRD and FTIR analyses showed distinctive crystalline and chemical structures of the film. In subsequent in vitro experiments with normal human dermal fibroblasts, the film demonstrated potential for wound healing. An increase in cell division (G2/M phase) was observed compared to the fibroin film without the CBD/HP-β-CD complex. Additionally, fibroblasts treated with the film exhibited enhanced cell migration in a scratch assay and increased expression of vascular endothelial growth factor protein compared to the control group. Overall, these findings underscore the film’s potential for enhancing wound healing outcomes. Full article

(This article belongs to the Topic Pharmaceutical and Biomedical Applications in Separation Techniques: Recent Trends and Developments)

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13 pages, 1689 KiB  

Open AccessArticle

OMNI: Gas Chromatograph Captures Seven Common PET Radiotracer Analytes in under 5 Minutes

by Camry Vonyae’ A’Keen, Jakub Mroz, Simon Kunta Joseph, Jairo Baquero, Melchor V. Cantorias and Patrick Carberry

Pharmaceuticals 2023, 16(11), 1623; https://doi.org/10.3390/ph16111623 - 17 Nov 2023

Viewed by 1522

Abstract

A novel gas chromatography method was developed using automatic injections to identify and quantify the amount of residual solvents or analytes in samples of fluorine-18 and carbon-11 radiopharmaceuticals. This approach evaluates seven analytes in less than 5 versus 13 min of acquisition time. [...] Read more.

A novel gas chromatography method was developed using automatic injections to identify and quantify the amount of residual solvents or analytes in samples of fluorine-18 and carbon-11 radiopharmaceuticals. This approach evaluates seven analytes in less than 5 versus 13 min of acquisition time. The method additionally includes a 3 min bakeout to aid in the removal and carry-over of higher-boiling impurities. Chromatographic parameters such as column temperature, hold time, column pressure, flow rate, and split ratios were adjusted and optimized to analyze radioactive drug samples containing analytes which include methanol, ethanol, acetone, acetonitrile, triethylamine, N,N-dimethylformamide, and dimethyl sulfoxide. The relative standard deviation for each solvent was determined to be no greater than 1.6%. The method limit of detection (LOD) and limit of quantification (LOQ) were between 0.053 and 0.163 and 0.000 (5.791 × 10⁻⁶) and 0.520 mg/mL, respectively. This GC technique, using flame ionization detection (FID), was validated and is currently employed for the routine quality control of all approved IND and RDRC PET radiopharmaceuticals at our center. Full article

(This article belongs to the Topic Pharmaceutical and Biomedical Applications in Separation Techniques: Recent Trends and Developments)

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15 pages, 3776 KiB  

Open AccessArticle

Interface-Based Design of High-Affinity Affibody Ligands for the Purification of RBD from Spike Proteins

by Siyuan Song and Qinghong Shi

Molecules 2023, 28(17), 6358; https://doi.org/10.3390/molecules28176358 - 30 Aug 2023

Cited by 7 | Viewed by 2155

Abstract

The outbreak of coronavirus disease 2019 (COVID-19) has sparked an urgent demand for advanced diagnosis and vaccination worldwide. The discovery of high-affinity ligands is of great significance for vaccine and diagnostic reagent manufacturing. Targeting the receptor binding domain (RBD) from the spike protein [...] Read more.

The outbreak of coronavirus disease 2019 (COVID-19) has sparked an urgent demand for advanced diagnosis and vaccination worldwide. The discovery of high-affinity ligands is of great significance for vaccine and diagnostic reagent manufacturing. Targeting the receptor binding domain (RBD) from the spike protein of severe acute respiratory syndrome-coronavirus 2, an interface at the outer surface of helices on the Z domain from protein A was introduced to construct a virtual library for the screening of Z_RBD affibody ligands. Molecular docking was performed using HADDOCK software, and three potential Z_RBD affibodies, Z_RBD-02, Z_RBD-04, and Z_RBD-07, were obtained. Molecular dynamics (MD) simulation verified that the binding of Z_RBD affibodies to RBD was driven by electrostatic interactions. Per-residue free energy decomposition analysis further substantiated that four residues with negative-charge characteristics on helix α1 of the Z domain participated in this process. Binding affinity analysis by microscale thermophoresis showed that Z_RBD affibodies had high affinity for RBD binding, and the lowest dissociation constant was 36.3 nmol/L for Z_RBD-07 among the three potential Z_RBD affibodies. Herein, Z_RBD-02 and Z_RBD-07 affibodies were selected for chromatographic verifications after being coupled to thiol-activated Sepharose 6 Fast Flow (SepFF) gel. Chromatographic experiments showed that RBD could bind on both Z_RBD SepFF gels and was eluted by 0.1 mol/L NaOH. Moreover, the Z_RBD-07 SepFF gel had a higher affinity for RBD. This research provided a new idea for the design of affibody ligands and validated the potential of affibody ligands in the application of RBD purification from complex feedstock. Full article

(This article belongs to the Topic Pharmaceutical and Biomedical Applications in Separation Techniques: Recent Trends and Developments)

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12 pages, 279 KiB  

Open AccessFeature PaperReview

Measurement of Steroids in the Placenta, Maternal Serum, and Fetal Serum in Humans, Rats, and Mice: A Technical Note

by Hayley R. Price, Cecilia Jalabert, Désirée R. Seib, Chunqi Ma, Dickson Lai, Kiran K. Soma and Abby C. Collier

Separations 2023, 10(4), 221; https://doi.org/10.3390/separations10040221 - 23 Mar 2023

Cited by 2 | Viewed by 2106

Abstract

Steroid hormones are vital for a successful pregnancy. The placenta is attached to the uterine wall and is the major organ of communication between the mother and the fetus through the umbilical cord and the transfer of compounds (including the production and actions [...] Read more.

Steroid hormones are vital for a successful pregnancy. The placenta is attached to the uterine wall and is the major organ of communication between the mother and the fetus through the umbilical cord and the transfer of compounds (including the production and actions of steroids) across the villous placenta. Therefore, a correct understanding and measurement of steroid levels across the maternal–placental–fetal interface is essential. We have experience spanning more than two decades and have published more than 40 papers using a variety of methods to assess circulating and placental steroid levels. In this review, we discuss various methods for steroid detection and quantitation, as well as their advantages and disadvantages. This document provides technical guidance for best practices that, in our estimation, can assist researchers in more easily and correctly performing these studies. Critical methodological considerations, including tissue collection, tissue processing, and analytical factors (sensitivity, selectivity, matrix effects, and internal standards), are covered. We highlight important differences between human and rodent tissues as they relate to steroid levels in pregnancy and the interpretation of results, and provide guidance for best practices in future studies. Full article

(This article belongs to the Topic Pharmaceutical and Biomedical Applications in Separation Techniques: Recent Trends and Developments)

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