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Chromatography and Extraction Techniques for Chemical Applications

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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: 30 June 2024 | Viewed by 6160

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Special Issue Editors

Dr. Jorge Pereira

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Guest Editor

CQM – Centro de Químcia da Madeira, Universidade da Madeira, 9000 Funchal, Portugal
Interests: food composition in bioactive compounds; food quality and degradation; markers for food origin and authenticity; microextraction; chromatographic analysis; foodomics
Special Issues, Collections and Topics in MDPI journals

Dr. Natalia Casado Navas

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Guest Editor

Departamento de Tecnología Química y Ambiental, Universidad Rey Juan Carlos, 28933 Móstoles, Spain
Interests: contaminants; bioactive compounds; natural toxins; miniaturization; microextraction; sample preparation; liquid chromatography; mass spectrometry; novel sorbents; analytical methods
Special Issues, Collections and Topics in MDPI journals

Special Issue Information

Dear Colleagues,

Chromatography and extraction are essential techniques in the field of chemistry, being combined for the separation and purification of chemical compounds. These methods are widely applied in various industries, including pharmaceuticals, biotechnology, environmental analysis, and food science. Chromatography involves the separation of components of a mixture based on their physical and chemical properties, while extraction involves the removal of one or more components from a mixture using a suitable solvent.

This Special Issue is devoted to emerging technologies and applications in the field of chromatography and extraction techniques for chemical analysis. This includes reviews and original research articles that focus on the development, application, and optimization of chromatography and extraction methods for a wide range of chemical applications. Topics of interest include advances in chromatography and extraction theory, instrumentation, sample preparation, and data analysis, as well as applications in food, medicinal, and environmental analysis. Additionally, contributions in new developments in method development and validation, as well as novel approaches for the determination of trace contaminants, and other topics related to the field are welcomed. This Special Issue offers readers an invaluable resource for furthering the advancement of chromatography and extraction techniques for chemical applications.

Dr. Jorge Pereira
Dr. Natalia Casado Navas
Guest Editors

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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. Molecules is an international peer-reviewed open access semimonthly 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 2700 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

liquid chromatography
gas chromatography
sample preparation
extraction
supercritical fluid extraction
solid-phase extraction
liquid-liquid extraction

Published Papers (6 papers)

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Research

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15 pages, 2794 KiB

Open AccessArticle

The Impact of Water as an Additive on the Elution of Some Basic Organic Compounds in Supercritical Fluid Chromatography

by Muhamad Yahia Kazmouz and Attila Felinger

Molecules 2024, 29(9), 2124; https://doi.org/10.3390/molecules29092124 - 3 May 2024

Viewed by 274

Abstract

In this study, water was used as an additive in the methanol-modified carbon dioxide-based eluent for the elution of some basic organic compounds from a hybrid silica column via supercritical fluid chromatography (SFC). The experiments were applied to sulfonamides, propranolol, and other organic nitrogen compounds involving aromatic rings from different classes of amine, pyrimidine, and purine with different pKa values (the pKa values for the studied analytes range from 4.6 to 10.4). The results revealed different responses to the different percentages of water addition. Adding 1~2% of water to the modifier (methanol) led to a positive effect manifested by more symmetrical peak shapes and reduced retention times for most compounds. The key factor for this improvement in the properties of chromatographic peaks is due to the adsorption of water on the silanol groups of the stationary phase, consequently resembling the phenomena observed in hydrophilic interaction liquid chromatography (HILIC). Moreover, the availability of hydrogen bond acceptor and donor sites in the analyte structure is an important factor to be considered when adding water as an additive to the modifier for improving the chromatographic peaks. However, introducing water in an amount higher than 3% resulted in perturbed chromatographic signals. It was also found that water as an additive alone could not successfully elute propranolol from the hybrid silica column with an acceptable peak shape; thus, the addition of a strong base such as amine salts was also necessary. The proposed use of a particular amount of water in the mobile phase could have a positive effect compared to the same mobile phase without water, improving the chromatographic peak properties of the elution of some basic organic compounds from the hybrid silica column. Full article

(This article belongs to the Special Issue Chromatography and Extraction Techniques for Chemical Applications)

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21 pages, 3636 KiB

Open AccessArticle

Temperature Dependence of the Polar and Lewis Acid–Base Properties of Poly Methyl Methacrylate Adsorbed on Silica via Inverse Gas Chromatography

by Tayssir Hamieh

Molecules 2024, 29(8), 1688; https://doi.org/10.3390/molecules29081688 - 9 Apr 2024

Viewed by 1081

Abstract

The adsorption of polymers on solid surfaces is common in many industrial applications, such as coatings, paints, catalysis, colloids, and adhesion processes. The properties of absorbed polymers commonly vary with temperature. In this paper, inverse gas chromatography at infinite dilution was used to determine the physicochemical characterization of PMMA adsorbed on silica. A new method based on the London dispersion equation was applied with a new parameter associating the deformation polarizability with the harmonic mean of the ionization energies of the solvent. More accurate values of the dispersive and polar interaction energies of the various organic solvents adsorbed on PMMA in bulk phase and PMMA/silica at different recovery fractions were obtained, as well as the Lewis acid–base parameters and the transition temperatures of the different composites. It was found that the temperature and the recovery fraction have important effects on the various physicochemical and thermodynamic properties. The variations in all the interaction parameters showed the presence of three transition temperatures for the different PMMA composites adsorbed on silica with various coverage rates, with a shift in these temperatures for a recovery fraction of 31%. An important variation in the polar enthalpy and entropy of adsorption, the Lewis acid–base parameters and the intermolecular separation distance was highlighted as a function of the temperature and the recovery fraction of PMMA on silica. Full article

(This article belongs to the Special Issue Chromatography and Extraction Techniques for Chemical Applications)

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14 pages, 4880 KiB

Open AccessArticle

Cu(II)-Loaded Polydopamine-Coated Urchin-like Titanate Microspheres as a High-Performance IMAC Adsorbent for Hemoglobin Separation

by Qian Zhang, Linlin Hu, Jianyu Yang, Pengfei Guo, Jinhong Wang and Weifen Zhang

Molecules 2024, 29(7), 1656; https://doi.org/10.3390/molecules29071656 - 7 Apr 2024

Viewed by 452

Abstract

Immobilized metal ion affinity chromatography (IMAC) adsorbents generally have excellent affinity for histidine-rich proteins. However, the leaching of metal ions from the adsorbent usually affects its adsorption performance, which greatly affects the reusable performance of the adsorbent, resulting in many limitations in practical applications. Herein, a novel IMAC adsorbent, i.e., Cu(II)-loaded polydopamine-coated urchin-like titanate microspheres (Cu-PDA-UTMS), was prepared via metal coordination to make Cu ions uniformly decorate polydopamine-coated titanate microspheres. The as-synthesized microspheres exhibit an urchin-like structure, providing more binding sites for hemoglobin. Cu-PDA-UTMS exhibit favorable selectivity for hemoglobin adsorption and have a desirable adsorption capacity towards hemoglobin up to 2704.6 mg g⁻¹. Using 0.1% CTAB as eluent, the adsorbed hemoglobin was easily eluted with a recovery rate of 86.8%. In addition, Cu-PDA-UTMS shows good reusability up to six cycles. In the end, the adsorption properties by Cu-PDA-UTMS towards hemoglobin from human blood samples were analyzed by SDS-PAGE. The results showed that Cu-PDA-UTMS are a high-performance IMAC adsorbent for hemoglobin separation, which provides a new method for the effective separation and purification of hemoglobin from complex biological samples. Full article

(This article belongs to the Special Issue Chromatography and Extraction Techniques for Chemical Applications)

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12 pages, 1694 KiB

Open AccessArticle

HPLC–DAD Analysis, SFE-CO₂ Extraction, and Antibacterial Activity on Bioactive Compounds from Mosla chinensis Maxim

by Ruixi Gao, Bingchen Han, Yanfeng Zeng, Linchuang Shen, Xinqiao Liu, Qiang Wang, Maochuan Liao and Jun Li

Molecules 2023, 28(23), 7724; https://doi.org/10.3390/molecules28237724 - 23 Nov 2023

Viewed by 780

Abstract

Mosla chinensis Maxim is an annual herb with many potential purposes in agricultural, industrial, and pharmaceutical fields. At present, the extract of the whole plant from M. chinensis has been proven to demonstrate antifungal, antioxidant, and anti-inflammatory activities. Previous studies focused on the enzyme pretreatment in hydrodistillation from M. chinensis. However, organic solvent or supercritical fluid carbon dioxide extraction (SFE-CO₂) methods, which are commonly utilized in industry, have seldom been studied and cannot provide multiple evaluations of yield. In this work, we analysed compounds from M. chinensis by HPLC–DAD, discussed n-hexane extraction, and conducted further investigations on SFE-CO₂ through the design of response surface methodology (RSM). The sample obtained from pilot-scale SFE-CO₂ was also tested against nine kinds of microorganisms. Single-factor results revealed that the extraction rates from M. chinensis by steam distillation, n-hexane extraction, and SFE-CO₂ were 1%, 2.09%, and 3.26%, respectively. RSM results showed a significant improvement in extraction rate through optimising pressure and time, and the interaction of both factors was more important than that of temperature–pressure and temperature–time. A pilot-scale test with an extraction rate of 3.34% indicated that the predicted RSM condition was operable. In addition, samples from the pilot-scale SFE-CO₂ showed antibacterial effects against three previously unreported bacteria (Gardnerella vaginalis, methicillin-resistant Staphylococcus aureus, and Propionibacterium acnes). These results fill the gap in previous research and provide more information for the application and development of M. chinensis in the future. Full article

(This article belongs to the Special Issue Chromatography and Extraction Techniques for Chemical Applications)

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12 pages, 927 KiB

Open AccessArticle

Fast and Sensitive Bioanalytical Method for the Determination of Deucravacitinib in Human Plasma Using HPLC-MS/MS: Application and Greenness Evaluation

by Pottabattula Mahesh, M. Akiful Haque, Baher I. Salman, Tarek S. Belal, Adel Ehab Ibrahim and Sami El Deeb

Molecules 2023, 28(14), 5471; https://doi.org/10.3390/molecules28145471 - 17 Jul 2023

Cited by 4 | Viewed by 1806

Abstract

Plaque psoriasis is a common, long-lasting illness that affects the immune system and causes significant negative impacts on a patient’s physical health, well-being, and ability to work effectively. Deucravacitinib (DEU) is the first oral medication used in the treatment of plaque psoriasis, a chronic skin condition that causes red, scaly patches on the skin. DEU is a type of medication called an oral Janus kinase (JAK) inhibitor, which works by blocking specific enzymes that play a role in the inflammation and immune response associated with psoriasis. Therefore, a quick, easy, novel, reliable, sensitive, and straightforward liquid chromatography-tandem mass spectrometry (LC-MS/MS) approach was used to analyze DEU in plasma samples. The LC-MS/MS method for the determination of DEU in human plasma was based on using trimethoprim as an internal standard (IS). The separation of DEU and IS was carried out via liquid–liquid extraction (LLE). The extract was then subjected to the chromatographic system separation using the ACE-C18 column (4.6 × 100 mm, 5 µm). The mobile phase employed consisted of methanol and a solution of 2 mM ammonium formate (80:20 v/v, respectively). The flow rate used was set at 0.9 mL min⁻¹. The creative strategy was performed by running an ABSCIEX API 4000 mass spectrometer with an electron spray ionization source in multiple reaction monitoring (MRM) mode. The ion transitions m/z 426.3 → 358.2 were used for DEU quantitation, while the ion transitions m/z 291.1 → 261.1 were used for trimethoprim quantitation. The accuracy, precision, linearity, recovery, and selectivity of DEU were deemed acceptable when validated for a concentration range between 0.500 and 601.050 ng/mL, utilizing a weighting factor of 1/x². Full article

(This article belongs to the Special Issue Chromatography and Extraction Techniques for Chemical Applications)

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Review

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30 pages, 3088 KiB

Open AccessReview

Sample Preparation Techniques for Growth-Promoting Agents in Various Mammalian Specimen Preceding MS-Analytics

by Laura Klöppner, Lukas Corbinian Harps and Maria Kristina Parr

Molecules 2024, 29(2), 330; https://doi.org/10.3390/molecules29020330 - 9 Jan 2024

Viewed by 1126

Abstract

The misuse of growth-promoting drugs such as beta-2 agonists and steroids is a known problem in farming and sports competitions. Prior to the analysis of biological samples via liquid chromatography (LC)–mass spectrometry (MS) or gas chromatography (GC)–MS, sufficient sample preparation is required to reliably identify or determine the residues of drugs. In practice, broad screening methods are often used to save time and analyze as many compounds as possible. This review was conceptualized to analyze the literature from 2018 until October 2023 for sample preparation procedures applied to animal specimens before LC- or GC-MS analysis. The animals were either used in farming or sports. In the present review, solid phase extraction (SPE) was observed as the dominant sample clean-up technique for beta-2 agonists and steroids, followed by protein precipitation. For the extraction of beta-2 agonists, mixed-mode cation exchanger-based SPE phases were preferably applied, while for the steroids, various types of SPE materials were reported. Furthermore, dispersive SPE-based QuEChERs were utilized. Combinatory use of SPE and liquid–liquid extraction (LLE) was observed to cover further drug classes in addition to beta-2 agonists in broader screening methods. Full article

(This article belongs to the Special Issue Chromatography and Extraction Techniques for Chemical Applications)

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