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Separations
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Separations in Biomedical Analysis
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Separations in Biomedical Analysis

A special issue of Separations (ISSN 2297-8739). This special issue belongs to the section "Bioanalysis/Clinical Analysis".

Deadline for manuscript submissions: closed (31 December 2021) | Viewed by 18384

Special Issue Editor

Prof. Dr. Igor Clarot

E-Mail Website
Guest Editor
Université de Lorraine, Vandœuvre-lès-Nancy, EA 3452 CITHFOR, France
Interests: drug quality control; nanoparticles; bioanalysis, capillary electrophoresis; chromatography; analytical method devlopment; sample treatment; method validation; analytical chemistry

Special Issue Information

Dear Colleagues,

Separation methodologies are essential to biomedical sciences. Biomedical analysis covers a fairly broad field from the characterization of drugs to the monitoring of active substances and related metabolites in biological fluids. The field is booming with the emergence of innovative separation methods focusing on new separation methods/supports and/or new methods of sample processing.

The target of this Special Issue is to present the state-of-the-art and the development of innovative separation methods for biomedical analysis in various fields, such as quality control, biochemistry, medical chemistry biotechnology, molecular biology, cell biology, and related disciplines.

Prof. Dr. Igor Clarot
Guest Editor

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

  • biomedical analysis
  • drug characterization, drug monitoring
  • PK/PD, biological matrices
  • innovative development
  • metabolization
  • chromatography
  • electrophoresis
  • miniaturization

Published Papers (6 papers)

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Editorial

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5 pages, 228 KiB  
Editorial
Separation Methods in Biomedical Analysis, a Booming Field
by Arnaud Pallotta, Ariane Boudier, Jérémie Gouyon and Igor Clarot
Separations 2022, 9(2), 51; https://0-doi-org.brum.beds.ac.uk/10.3390/separations9020051 - 11 Feb 2022
Cited by 1 | Viewed by 2107
Abstract
Many scientific endeavors are dependent upon the accurate quantification of drugs and endogenous substances, such as pharmacokinetics [...] Full article
(This article belongs to the Special Issue Separations in Biomedical Analysis)

Research

Jump to: Editorial

14 pages, 2719 KiB  
Article
GC-MS Method for Quantification and Pharmacokinetic Study of Four Volatile Compounds in Rat Plasma after Oral Administration of Commiphora myrrh (Nees) Engl. Resin and In Vitro Cytotoxic Evaluation
by Ali S. Alqahtani, Rashed N. Herqash, Faleh Alqahtani, Syed Rizwan Ahamad, Fahd A. Nasr and Omar M. Noman
Separations 2021, 8(12), 239; https://0-doi-org.brum.beds.ac.uk/10.3390/separations8120239 - 07 Dec 2021
Cited by 2 | Viewed by 2513
Abstract
A rapid, simple, and sensitive gas chromatography–tandem mass spectrometry (GC–MS) method was established and validated for simultaneous determination of four volatile compounds, namely curzerene, methoxyfuranodiene, β-elemene, and α-pinene in rat plasma samples after oral administration of the resin extract of Commiphora myrrh [...] Read more.
A rapid, simple, and sensitive gas chromatography–tandem mass spectrometry (GC–MS) method was established and validated for simultaneous determination of four volatile compounds, namely curzerene, methoxyfuranodiene, β-elemene, and α-pinene in rat plasma samples after oral administration of the resin extract of Commiphora myrrh using limonene as an internal standard (IS). Liquid-liquid extraction using hexane and ethyl acetate (1:1) mixture as an extracting agent was used for the samples extraction procedure. The GC–MS system was operated under selective ion monitoring (SIM) mode using Perkin Elmer Elite 5MS column (30 m × 0.25 mm × 0.25 µm film thickness). Specificity, linearity, precision, accuracy, extraction recovery, and stability were used to validate the developed method. The assay showed good linearity (r2 ≥ 0.998), and the lowest limits of quantification (LLOQ) were 3.97–21.38 ng/mL for the four analytes. This assay was successfully applied to pharmacokinetic studies of the four volatile compounds in rat plasma. The antiproliferative activity of these volatile compounds was evaluated against lung carcinoma (A549) and colon (LoVo) cell lines, were each compound caused variable inhibition on cells proliferation and methoxyfuranodiene exerted the strong antiproliferative activity against both cell line according to IC50 values. Full article
(This article belongs to the Special Issue Separations in Biomedical Analysis)
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12 pages, 727 KiB  
Article
Monitoring of Gold Biodistribution from Nanoparticles Using a HPLC-Visible Method
by Thomas Chaigneau, Arnaud Pallotta, Fatima Zahra Benaddi, Lucie Sancey, Said Chakir, Ariane Boudier and Igor Clarot
Separations 2021, 8(11), 215; https://0-doi-org.brum.beds.ac.uk/10.3390/separations8110215 - 12 Nov 2021
Cited by 2 | Viewed by 1594
Abstract
There is intensive research using gold nanoparticles for biomedical purposes, which have many advantages such as ease of synthesis and high reactivity. Their possible small size (<10 nm) can lead to the crossing of biological membranes and then to problematic dissemination and storage [...] Read more.
There is intensive research using gold nanoparticles for biomedical purposes, which have many advantages such as ease of synthesis and high reactivity. Their possible small size (<10 nm) can lead to the crossing of biological membranes and then to problematic dissemination and storage in organs that must be controlled and evaluated. In this work, a simple isocratic HPLC method was developed and validated to quantify the gold coming from nanoparticles in different biological samples. After a first carbonization step at 900 °C, the nanoparticles were oxidized by dibroma under acidic conditions, leading to tetrachloroaurate ions that could form ion pairs when adding rhodamine B. Finally, ion pairs were extracted and rhodamine B was evaluated to quantify the corresponding gold concentration by reversed-phase HPLC with visible detection. The method was validated for different organs (liver, spleen, lungs, kidneys, or brain) and fluids (plasma and urine) from rats and mice. Lastly, the developed method was used to evaluate the content of gold in organs and fluids after intravenous (IV) injection of nanoparticles. Full article
(This article belongs to the Special Issue Separations in Biomedical Analysis)
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14 pages, 1880 KiB  
Article
Designing Safer Solvents to Replace Methylene Chloride for Liquid Chromatography Applications Using Thin-Layer Chromatography as a Screening Tool
by Apekshya Sharma, Evan Yu, Gregory Morose, David Trung Nguyen and Wan-Ting Chen
Separations 2021, 8(10), 172; https://0-doi-org.brum.beds.ac.uk/10.3390/separations8100172 - 06 Oct 2021
Cited by 8 | Viewed by 6036
Abstract
Methylene chloride, commonly known as dichloromethane (DCM), is a widely used chemical for chromatography separation within the polymer, chemical, and pharmaceutical industries. With the ability to effectively solvate heterocyclic compounds, and properties including a low boiling point, high density, and low cost, DCM [...] Read more.
Methylene chloride, commonly known as dichloromethane (DCM), is a widely used chemical for chromatography separation within the polymer, chemical, and pharmaceutical industries. With the ability to effectively solvate heterocyclic compounds, and properties including a low boiling point, high density, and low cost, DCM has become the solvent of choice for many different applications. However, DCM has high neurotoxicity and is carcinogenic, with exposure linked to damage to the brain and the central nervous system, even at low exposure levels. This research focuses on sustainability and works towards finding safer alternative solvents to replace DCM in pharmaceutical manufacturing. The research was conducted with three active pharmaceutical ingredients (API) widely used in the pharmaceutical industry: acetaminophen, aspirin, and ibuprofen. Thin-layer chromatography (TLC) was used to investigate if an alternative solvent or solvent blend could show comparable separation performance to DCM. The use of the Hansen Solubility Parameter (HSP) theory and solubility testing allowed for the identification of potential alternative solvents or solvent blends to replace DCM. HSP values for the three APIs were experimentally determined and used to identify safer solvents and blends that could potentially replace DCM. Safer solvents or binary solvent blends were down-selected based on their dissolution power, safety, and price. The down-selected solvents (e.g., ethyl acetate) and solvent blends were further evaluated using three chemical hazard classification approaches to find the best fitting nonhazardous replacement to DCM. Several safer solvent blends (e.g., mixtures composed of methyl acetate and ethyl acetate) with adequate TLC performance were identified. Results from this study are expected to provide guidance for identifying and evaluating safer solvents to separate APIs using chromatography. Full article
(This article belongs to the Special Issue Separations in Biomedical Analysis)
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11 pages, 1106 KiB  
Article
Enantioselective Chromatographic Separation and Lipase Catalyzed Asymmetric Resolution of Biologically Important Chiral Amines
by Mohammed Farrag El-Behairy, Rasha M. Hassan and Eirik Sundby
Separations 2021, 8(10), 165; https://0-doi-org.brum.beds.ac.uk/10.3390/separations8100165 - 30 Sep 2021
Cited by 2 | Viewed by 2160
Abstract
Cyanoacetamides are vital synthons in synthetic organic chemistry. However, methods to enantiopure cyanoacetamides have not yet been well explored. In this work, the preparation of cyanoacetamide synthons RS-(1a–4a) or methoxyacetamides RS-(1b–4b) in enantiopure/enriched [...] Read more.
Cyanoacetamides are vital synthons in synthetic organic chemistry. However, methods to enantiopure cyanoacetamides have not yet been well explored. In this work, the preparation of cyanoacetamide synthons RS-(1a–4a) or methoxyacetamides RS-(1b–4b) in enantiopure/enriched form was investigated. Compounds S-1, S-2, R-1b, R-1a, andR-2b were prepared in enantiopure form (ee > 99%) while compounds S-4, R-2a, and R-4a were achieved in ee 9%, 80%, and 76%, respectively. Many baselines enantioselective HPLC separations of amines 1–4, their cyanoacetamides (1a–4a), and methoxyacetamides (1b–4b) were achieved by utilizing diverse mobile-phase compositions and two cellulose-based CSPs (ODH® and LUX-3® columns). Such enantioselective HPLC separations were used to monitor the lipase-catalyzed kinetic resolution of amines RS-(1–4). Full article
(This article belongs to the Special Issue Separations in Biomedical Analysis)
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10 pages, 1115 KiB  
Article
Quantification of Histidine-Containing Dipeptides in Dolphin Serum Using a Reversed-Phase Ion-Pair High-Performance Liquid Chromatography Method
by Momochika Kumagai, Sanae Kato, Nanami Arakawa, Mika Otsuka, Takahisa Hamano, Nobuyuki Kashiwagi, Akira Yabuki and Osamu Yamato
Separations 2021, 8(8), 128; https://0-doi-org.brum.beds.ac.uk/10.3390/separations8080128 - 23 Aug 2021
Cited by 5 | Viewed by 2738
Abstract
The quantification of histidine-containing dipeptides (anserine, carnosine, and balenine) in serum might be a diagnostic tool to assess the health condition of animals. In this study, an existing reversed-phase ion-pair high-performance liquid chromatography (HPLC)–ultraviolet detection method was improved and validated to quantify serum [...] Read more.
The quantification of histidine-containing dipeptides (anserine, carnosine, and balenine) in serum might be a diagnostic tool to assess the health condition of animals. In this study, an existing reversed-phase ion-pair high-performance liquid chromatography (HPLC)–ultraviolet detection method was improved and validated to quantify serum anserine, carnosine, and balenine levels in the dolphin. The serum was deproteinized with trichloroacetic acid and directly injected into the HPLC system. Chromatographic separation of the three histidine-containing dipeptides was achieved on a TSK–gel ODS-80Ts (4.6 mm × 150 mm, 5 µm) analytical column using a mobile phase of 50 mmol/L potassium dihydrogen phosphate (pH 3.4) containing 6 mmol/L 1-heptanesulfonic acid and acetonitrile (96:4). The standard curve ranged from 0.1 µmol/L to 250 µmol/L. The average accuracy of the intra- and inter-analysis of anserine, carnosine, and balenine was 97–106%. The relative standard deviations of total precision (RSDr) of anserine, carnosine, and balenine in dolphin serum were 5.9%, 4.1%, and 2.6%, respectively. The lower limit of quantification of these compounds was 0.11–0.21 µmol/L. These results indicate that the improved method is reliable and concise for the simultaneous determination of anserine, carnosine, and balenine in dolphin serum, and may be useful for evaluation of health conditions in dolphins. Furthermore, this method can also be applied to other biological samples. Full article
(This article belongs to the Special Issue Separations in Biomedical Analysis)
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