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Chromatographic and Electrophoretic Separation Methods in Pharmaceutical Analysis

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A special issue of Molecules (ISSN 1420-3049). This special issue belongs to the section "Analytical Chemistry".

Deadline for manuscript submissions: closed (30 June 2023) | Viewed by 16973

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Prof. Dr. Gabriel Hancu

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Pharmaceutical and Therapeutical Chemistry Department, Faculty of Pharmacy, George Emil Palade University of Medicine, Pharmacy, Science and Technology of Târgu Mureș, 38 Gheorghe Marinescu Street, 540142 Targu Mureș, Romania
Interests: drug analysis; chirality; chiral separation; separation techniques; capillary electrophoresis; high performance liquid chromatography
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Prof. Dr. Aura Rusu

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Pharmaceutical and Therapeutical Chemistry Department, Faculty of Pharmacy, George Emil Palade University of Medicine, Pharmacy, Science and Technology of Târgu Mureș, 38 Gheorghe Marinescu Street, 540142 Targu Mureș, Romania
Interests: pharmaceutical chemistry; medicinal chemistry; drug design; antibacterial agents; metal complexes; drug analysis; capillary electrophoresis; patient–pharmacist communication
Special Issues, Collections and Topics in MDPI journals

Dr. Andreea Pricopie

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Department of Biochemistry and Chemistry of Environmental Factors, Faculty of Pharmacy, University of Medicine, Pharmacy, Science and Technology "George Emil Palade" of Targu Mures, Targu Mures, Romania
Interests: organic chemical synthesis; antibiotherapy; drug design and development; antimicrobial activity evaluation; pharmaceutical chemistry; biochemistry

Special Issue Information

Dear Colleagues,

Modern pharmaceutical research is strongly linked to pharmaceutical analysis, as the development of new innovative methods of analysis is becoming both a necessity and a challenge for analysts. The process of drug development necessitates the use of accurate analytical methods allowing researchers to evaluate drug molecules in a precise and straightforward manner. A pharmaceutical analysis is used to provide reliable data to help not just drug discovery and development, but also postmarket surveillance. The analytical analysis of bulk drug materials, intermediates, drug formulations, contaminants, and degradation products, as well as biological samples containing pharmaceutical substances and their metabolites, is critical in pharmaceutical research. Analytical techniques for the quantitative and qualitative analysis of pharmaceutical substances have been included in compendial monographs, with the goal of characterizing the quality of bulk pharmaceutical materials by defining active component concentration limits. Analytical techniques play an important role throughout the drug development process, from understanding the physical and chemical stability of the drug, assessing the stability of the drug molecules, quantifying impurities, to identifying those impurities that are above the established threshold and evaluating the toxicity profiles of these impurities or pharmacokinetic studies. Consequently, it is important to identify the best analytical solutions for method development when it comes to quantitative and qualitative pharmaceutical analysis. The current Special Issue highlights the role of various analytical techniques in the analysis of pharmaceuticals, focusing on the applications of high-performance liquid chromatography (HPLC) and capillary electrophoresis (CE). Although HPLC is the most common technique for separating complicated mixtures of chemicals, CE today can be considered an interesting alternative and, sometimes, a complementary method in the drug analysis. Over the last 10 years, new technologies have continually developed; furthermore, the employment of more established approaches is being aided by gradual advances in technology and protocol. Combination approaches, high-throughput technologies, chemometrics, miniaturization, and nanotechnology have all developed and are currently employed in modern pharmaceutical analysis. The quest for novel medications continues as researchers combine available analytical methods, develop new technologies, and find new uses for the existing technology.

This Special Issue focuses on original research papers covering the development and application of chromatographic and electrophoretic methods in modern pharmaceutical analysis. Additionally, review papers presenting an in-depth analysis of the state-of-the-art of the topic are also eligible. Scientists focusing on this domain are encouraged to submit their research results for publication in this Special Issue.

Dr. Gabriel Hancu
Prof. Dr. Aura Rusu
Dr. Andreea Pricopie
Guest Editors

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Keywords

pharmaceutical analysis
high-performance liquid chromatography
capillary electrophoresis
separation technology
purity control
chiral analysis
biomedical analysis

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Published Papers (8 papers)

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Research

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11 pages, 921 KiB

Open AccessArticle

Quantitative Insight into PCA Formation following Different Chlorhexidine Activation Methods in Endodontic Treatment

by Barbara Czopik, Aneta Woźniakiewicz, Natalia Świętoniowska, Joanna Zarzecka and Michał Woźniakiewicz

Molecules 2023, 28(16), 6159; https://doi.org/10.3390/molecules28166159 - 21 Aug 2023

Viewed by 1370

Abstract

The aim of the study was a quantitative analysis of p-chloroaniline (PCA) formation during 2% CHX activation with US and MDI methods in a root canal-like environment with the HPLC-DAD method and, thus, a safety assessment of US and MDI agitation of CHX in endodontic treatment. Two percent CHX was activated with the US method using ISO 30 and 35 K-file, and the MDI method using ISO 30.06 and 35.06 GP cones for 15, 30, 60, and 90 s. PCA concentration was assessed with the HPLC-DAD method. PCA concentration was also assessed for 2% CHX after 0, 3, 18, and 21 days of storage in ambient conditions. PCA was detected in all samples in all methods of activation. The concentration of PCA was dependent on time of activation in US ISO 30 and ISO 35 group (p < 0.05). In the MDI ISO 30.06 and ISO 35.06 groups, a similar trend was observed but without statistical significance (p > 0.05). PCA was detected in shelf-stored 2% CHX and the concentration was related to the time of storage. PCA is released after CHX activation with US and MDI, but mean concentrations are not higher than those observed from self-degradation of shelf-stored 2% CHX. Full article

(This article belongs to the Special Issue Chromatographic and Electrophoretic Separation Methods in Pharmaceutical Analysis)

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13 pages, 3045 KiB

Open AccessArticle

Chiral Separation of Oxazolidinone Analogs by Capillary Electrophoresis Using Anionic Cyclodextrins as Chiral Selectors: Emphasis on Enantiomer Migration Order

by Zoltán-István Szabó, Francisc Boda, Béla Fiser, Máté Dobó, Levente Szőcs and Gergő Tóth

Molecules 2023, 28(11), 4530; https://doi.org/10.3390/molecules28114530 - 2 Jun 2023

Viewed by 1362

Abstract

Comparative chiral separations of enantiomeric pairs of four oxazolidinone and two related thio-derivatives were performed by capillary electrophoresis, using cyclodextrins (CDs) as chiral selectors. Since the selected analytes are neutral, the enantiodiscrimination capabilities of nine anionic CD derivatives were determined, in 50 mM phosphate buffer pH = 6. Unanimously, the most successful chiral selector was the single isomeric heptakis-(6-sulfo)-β-cyclodextrin (HS-β-CD), which resulted in the highest enantioresolution values out of the CDs applied for five of the six enantiomeric pairs. The enantiomer migration order (EMO) was the same for two enantiomeric pairs, irrespective of the CD applied. However, several examples of EMO reversals were obtained in the other cases. Interestingly, changing from randomly substituted, multi-component mixtures of sulfated-β-CD to the single isomeric chiral selector, enantiomer migration order reversal occurred for two enantiomeric pairs and similar observations were made when comparing heptakis-(2,3-di-O-methyl-6-O-sulfo)-β-CD, (HDMS-β-CD) with HS-β-CD. In several cases, cavity-size-dependent, and substituent-dependent EMO reversals were also observed. Minute differences in the structure of the analytes were also responsible for several cases of EMO reversal. The present study offers a complex overview of the chiral separation of structurally related oxazolidinones, and thio-analogs, highlighting the importance of the adequate choice of chiral selector in this group of compounds, where enantiomeric purity is of utmost importance. Full article

(This article belongs to the Special Issue Chromatographic and Electrophoretic Separation Methods in Pharmaceutical Analysis)

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16 pages, 3001 KiB

Open AccessArticle

Toxicity of the 3,4-Methylenedioxymethamphetamine and Its Enantiomers to Daphnia magna after Isolation by Semipreparative Chromatography

by Ana Rita Costa, Virgínia M. F. Gonçalves, Bruno B. Castro, João Soares Carrola, Ivan Langa, Ariana Pereira, Ana Rita Carvalho, Maria Elizabeth Tiritan and Cláudia Ribeiro

Molecules 2023, 28(3), 1457; https://doi.org/10.3390/molecules28031457 - 2 Feb 2023

Cited by 7 | Viewed by 2707

Abstract

MDMA (3,4-methylenedioxymethamphetamine) is a chiral psychoactive recreational drug sold in illicit markets as racemate. Studies on the impact of MDMA on aquatic organisms are scarce. While enantioselectivity in toxicity in animals and humans has been reported, none is reported on aquatic organisms. This study aimed to investigate the ecotoxicological effects of MDMA and its enantiomers in Daphnia magna. For that, enantiomers (enantiomeric purity > 97%) were separated by liquid chromatography using a homemade semipreparative chiral column. Daphnids were exposed to three concentrations of (R,S)-MDMA (0.1, 1.0 and 10.0 µg L⁻¹) and two concentrations of (R)- and (S)-enantiomers (0.1 and 1.0 µg L⁻¹) over the course of 8 days. Morphophysiological responses were dependent on the substance form and daphnia development stage, and they were overall not affected by the (R)-enantiomer. Changes in swimming behaviour were observed for both the racemate and its enantiomers, but enantioselective effects were not observed. Reproductive or biochemical changes were not observed for enantiomers whereas a significant decrease in acetylcholinesterase and catalase activity was noted at the highest concentration of (R,S)-MDMA (10 µg L⁻¹). Overall, this study showed that sub-chronic exposure to MDMA racemate and its enantiomers can interfere with morphophysiological and swimming behaviour of D. magna. In general, the (R)-enantiomer demonstrated less toxicity than the (S)-enantiomer. Full article

(This article belongs to the Special Issue Chromatographic and Electrophoretic Separation Methods in Pharmaceutical Analysis)

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12 pages, 1007 KiB

Open AccessArticle

A Novel Validated UHPLC Method for the Estimation of Rosuvastatin and Its Complete Impurity Profile in Tablet Formulations

by Francesca Romana Mammone, Leo Zanitti, Michela Puxeddu, Giuseppe La Regina, Romano Silvestri, Anna Borioni and Roberto Cirilli

Molecules 2023, 28(1), 431; https://doi.org/10.3390/molecules28010431 - 3 Jan 2023

Cited by 5 | Viewed by 2296

Abstract

A key step in the development of medicinal products is the research and validation of selective and sensitive analytical methods for the control of impurities from synthesis and degradation. As most impurities are similar in structure to the drug substance, the achievement of chemo-selective conditions is usually challenging. Herein, a direct and highly selective ultra-high-performance liquid chromatographic method for determining the assay and related substances content in medicinal products containing rosuvastatin calcium salt (RSV) is presented. RSV is used to treat high cholesterol levels and prevent heart attacks and strokes. The most engaging feature of this method was the baseline separation of all organic related substances listed in the European Pharmacopoeia (EP) monograph for the RSV tablets, achieved for the first time in less than 15 min using the Acquity BEH C18 (100 mm × 2.1 mm, 1.7 μm) column under reversed-phase isocratic conditions. The mobile phase adopted for the chemo-selective analysis does not contain buffers but instead contains trifluoroacetic as an acid additive. The chromatographic method was validated according to the guidelines of the International Conference on Harmonization (ICH) and proved to be linear, precise and accurate for determining the content of RSV and related chiral substances in tablet formulations. Full article

(This article belongs to the Special Issue Chromatographic and Electrophoretic Separation Methods in Pharmaceutical Analysis)

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17 pages, 3987 KiB

Open AccessArticle

User-Driven Strategy for In Silico Screening of Reversed-Phase Liquid Chromatography Conditions for Known Pharmaceutical-Related Small Molecules

by Thomas Van Laethem, Priyanka Kumari, Bruno Boulanger, Philippe Hubert, Marianne Fillet, Pierre-Yves Sacré and Cédric Hubert

Molecules 2022, 27(23), 8306; https://doi.org/10.3390/molecules27238306 - 28 Nov 2022

Cited by 3 | Viewed by 1537

Abstract

In the pharmaceutical field, and more precisely in quality control laboratories, robust liquid chromatographic methods are needed to separate and analyze mixtures of compounds. The development of such chromatographic methods for new mixtures can result in a long and tedious process even while using the design of experiments methodology. However, developments could be accelerated with the help of in silico screening. In this work, the usefulness of a strategy combining response surface methodology (RSM) followed by multicriteria decision analysis (MCDA) applied to predictions from a quantitative structure–retention relationship (QSRR) model is demonstrated. The developed strategy shows that selecting equations for the retention time prediction models based on the pKa of the compound allows flexibility in the models. The MCDA developed is shown to help to make decisions on different criteria while being robust to the user’s decision on the weights for each criterion. This strategy is proposed for the screening phase of the method lifecycle. The strategy offers the possibility to the user to select chromatographic conditions based on multiple criteria without being too sensitive to the importance given to them. The conditions with the highest desirability are defined as the starting point for further optimization steps. Full article

(This article belongs to the Special Issue Chromatographic and Electrophoretic Separation Methods in Pharmaceutical Analysis)

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21 pages, 2022 KiB

Open AccessFeature PaperArticle

Effect of Culture Conditions on Fatty Acid Profiles of Bacteria and Lipopolysaccharides of the Genus Pseudomonas—GC-MS Analysis on Ionic Liquid-Based Column

by Emerencia Mező, Fruzsina Hartmann-Balogh, Ibolya Madarászné Horváth, Anita Bufa, Tamás Marosvölgyi, Béla Kocsis and Lilla Makszin

Molecules 2022, 27(20), 6930; https://doi.org/10.3390/molecules27206930 - 15 Oct 2022

Cited by 7 | Viewed by 2064

Abstract

The profiling of bacterial fatty acids is a well-established technique in identifying and classifying bacteria. Cultivation conditions may affect the biosynthesis, thereby, changing the fatty acid profile in bacteria. The effect of the culture conditions on the fatty acid components of Pseudomonas aeruginosa PAO1, Pseudomonas aeruginosa ATCC 27853, Pseudomonas aeruginosa polyresistant and Pseudomonas putida all are aligned to the genus Pseudomonas. The fatty acids in the lipopolysaccharides of Pseudomonas aeruginosa PAO1 were also examined. The effects of the cultivation conditions were followed by using agar and blood agar media at the characteristic temperatures, 25 °C, 37 °C and 42 °C, respectively, and an analysis was made during the 1st, 3rd and 5th day following inoculation. In addition to quantitative differences, we also experienced qualitative differences in the fatty acid profiles which detect newly appearing fatty acids, due to changes in environmental factors. The application of ionic liquid-based column unveils new possibilities for the analyses of fatty acids in GC-MS experiments for bacterial fatty acid profiling. The validation results (response linearity, limit of detection, limit of quantification, system suitability, intraday and interday repeatability and accuracy) show the high separation efficiency of the ionic liquid-based column in the analyses. Full article

(This article belongs to the Special Issue Chromatographic and Electrophoretic Separation Methods in Pharmaceutical Analysis)

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13 pages, 1788 KiB

Open AccessArticle

Chiral Discrimination of Mexiletine Enantiomers by Capillary Electrophoresis Using Cyclodextrins as Chiral Selectors and Experimental Design Method Optimization

by Melania Cârcu-Dobrin, Gabriel Hancu, Lajos Attila Papp and Ibolya Fülöp

Molecules 2022, 27(17), 5603; https://doi.org/10.3390/molecules27175603 - 31 Aug 2022

Cited by 3 | Viewed by 1527

Abstract

Mexiletine (MXL) is a class IB antiarrhythmic agent, acting as a non-selective voltage-gated sodium channel blocker, used in therapy as a racemic mixture R,S-MXL hydrochloride. The aim of the current study was the development of a new, fast, and efficient method for the chiral separation of MXL enantiomers using capillary electrophoresis (CE) and cyclodextrins (CDs) as chiral selectors (CSs). After an initial CS screening, using several neutral and charged CDs, at four pH levels, heptakis-2,3,6-tri-O-methyl-β-CD (TM-β-CD), a neutral derivatized CD, was chosen as the optimum CS for the enantioseparation. For method optimization, an initial screening fractional factorial design was applied to identify the most significant parameters, followed by a face-centered central composite design to establish the optimal separation conditions. The best results were obtained by applying the following optimized electrophoretic conditions: 60 mM phosphate buffer, pH 5.0, 50 mM TM-β-CD, temperature 20 °C, applied voltage 30 kV, hydrodynamic injection 50 mbar/s. MXL enantiomers were baseline separated with a resolution of 1.52 during a migration time of under 5 min; S-MXL was the first migrating enantiomer. The method’s analytical performance was verified in terms of precision, linearity, accuracy, and robustness (applying a Plackett–Burman design). The developed method was applied for the determination of MXL enantiomers in pharmaceuticals. A computer modeling of the MXL-CD complexes was applied to characterize host–guest chiral recognition. Full article

(This article belongs to the Special Issue Chromatographic and Electrophoretic Separation Methods in Pharmaceutical Analysis)

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Review

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13 pages, 1700 KiB

Open AccessReview

Applications of Capillary Electrophoresis for the Determination of Cannabinoids in Different Matrices

by Nicoleta Mirela Blebea, Gabriel Hancu, Robert Alexandru Vlad and Andreea Pricopie

Molecules 2023, 28(2), 638; https://doi.org/10.3390/molecules28020638 - 8 Jan 2023

Cited by 5 | Viewed by 3031

Abstract

Cannabinoids, terpenophenolic chemicals found only in cannabis, are primarily responsible for cannabis pharmacologic effects; nearly 150 distinct cannabinoids have been identified thus far. Among these, the main psychoactive molecule, tetrahydrocannabinol (THC), and the non-psychoactive counterpart, cannabidiol (CBD) are distinguishable. In the past decade, a CBD-containing pharmaceutical preparation was approved by Food and Drug Administration (FDA) for the treatment of drug-resistant epileptic seizures in children, and research trials for a variety of additional medical conditions for which CBD has been suggested as a therapy are being conducted. Additionally, the number of “CBD-containing” dietary supplements, largely available online, is increasing rapidly. Consequently, the necessity for the development of qualitative and quantitative methodologies for the analysis of the bioactive components of Cannabis is rising because of the increase in the production of therapeutic cannabis products. One of the analytical methods with good potential in cannabinoids analysis is capillary electrophoresis (CE). It has advantages related to high separation efficiency, relatively short analysis time, and the small consumption of analytes and reagents which generates relatively lower operational costs than other methods. This review focuses on the use of CE techniques to examine biological matrices and plant materials for the presence of cannabinoids and other bioactive compounds found in cannabis. The advantages, drawbacks, and applicability of the various electromigration approaches are also assessed. The article provides an overview of the “state of the art” and the latest trends in CE-based methods for the determination of cannabinoids. Full article

(This article belongs to the Special Issue Chromatographic and Electrophoretic Separation Methods in Pharmaceutical Analysis)

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