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Separations
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Analysis and Bioanalysis of Pharmaceuticals: Sample Preparation and Chromatography
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Analysis and Bioanalysis of Pharmaceuticals: Sample Preparation and Chromatography

A special issue of Separations (ISSN 2297-8739). This special issue belongs to the section "Chromatographic Separations".

Deadline for manuscript submissions: 20 May 2024 | Viewed by 1911

Special Issue Editors

Dr. Anne Marie Ciobanu

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Guest Editor
Drug Control Department, Faculty of Pharmacy, "Carol Davila" University of Medicine and Pharmacy, 020956 Bucharest, Romania
Interests: pharmaceutical analysis; bioanalysis of medicines and drugs of abuse; chromatography; spectrophotometry; methods validation; medicines stability studies; quality control of pharmaceutical products and dietary supplements
Prof. Dr. Daniela Baconi

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Guest Editor
Department of Toxicology, Faculty of Pharmacy, “Carol Davila” University of Medicine and Pharmacy, 020956 Bucharest, Romania
Interests: analytical testing of medicines; drugs of abuse; natural products; bioanalytical methods; chromatography (HPLTC, GC-MS, HPLC, LC-MS); spectrophotometry; food safety; environmental toxicology
Prof. Dr. George Traian Alexandru Burcea-Dragomiroiu

E-Mail Website
Guest Editor
Drug Control Department, Faculty of Pharmacy, "Carol Davila" University of Medicine and Pharmacy, 020956 Bucharest, Romania
Interests: pharmaceutical analysis; biopharmacy; pharmaceutical industry; chromatography; spectrophotometry; methods validation; medicines stability
Dr. Carmen Lidia Chitescu

E-Mail Website
Guest Editor
Faculty of Medicine and Pharmacy, "Dunărea de Jos" University of Galaţi, Galaţi, Romania
Interests: extraction and chemical profiling of bioactive compounds from vegetal matters; emerging contaminant residue analysis in environmental and biological matrices; food safety; analytical investigations; HPLC, LC-HRMS/MS; method validation

Special Issue Information

Dear Colleagues,

It is widely recognized that pharmaceutical analysis plays a pivotal role not only in the quality control of pharmaceutical products but also in the development of original or generic formulations. Simultaneously, pharmaceutical bioanalysis stands out as an indispensable tool in pharmacokinetic and therapeutic drug monitoring studies. In both pharmaceutical analysis and bioanalysis, chromatography is a predominant analytical technique that has been widely practiced for decades.

Innovative breakthroughs, including ultra-performance thin-layer chromatography (HPTLC), ultra-high-pressure liquid chromatography (UHPLC), and hyphenated techniques like gas chromatography–mass spectrometry (GC-MS) and liquid chromatography–mass spectrometry (LC–MS) or two-dimensional liquid chromatography (2D-LC), chiral separations, core–shell columns, and novel stationary phases, have collectively improved chromatography, permitting faster speed, higher resolution, greater sensitivity, and increased precision.

Unquestionably, sample preparation also constitutes a critical facet of the analytical process. Recent advances introduced by the development of novel technologies and sorbents have substantially enhanced the performance of sample preparation techniques.

This Special Issue is dedicated to original research publications applying optimized extraction techniques to molecules of significant biopharmaceutical interest from various matrices and their quantification using chromatographic techniques coupled with sensitive detectors. Moreover, the scope extends to review papers that present an exhaustive examination of the state of the art in chromatographic analysis and bioanalysis concerning specific active pharmaceutical ingredients.

Dr. Anne Marie Ciobanu
Prof. Dr. Daniela Baconi
Prof. Dr. George Traian Alexandru Burcea-Dragomiroiu
Dr. Carmen Lidia Chitescu
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

  • chromatography
  • drug analysis
  • sample preparation
  • method validation
  • biological matrices
  • extraction
  • liquid chromatography
  • gas chromatography
  • pharmaceuticals
  • sample preparation
  • high-performance thin-layer chromatography

Published Papers (2 papers)

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Research

14 pages, 5548 KiB  
Article
Changes in the Serum and Tissue Levels of Free and Conjugated Sialic Acids, Neu5Ac, Neu5Gc, and KDN in Mice after the Oral Administration of Edible Bird’s Nests: An LC–MS/MS Quantitative Analysis
by Meng-Hua Wang, Zhi-Fan Wang, Man Yuan, Chun-Guo Yang, Dong-Liang Wang and Shu-Qi Wang
Separations 2024, 11(4), 107; https://doi.org/10.3390/separations11040107 - 01 Apr 2024
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Abstract
Edible bird’s nests have a variety of biological activities, the main components of which are sialic acids. Sialic acids are a group of nine-carbon N-acetylated derivatives of neuraminic acid containing a keto group at position C2 and play important roles in many biological [...] Read more.
Edible bird’s nests have a variety of biological activities, the main components of which are sialic acids. Sialic acids are a group of nine-carbon N-acetylated derivatives of neuraminic acid containing a keto group at position C2 and play important roles in many biological processes. To verify whether the oral administration of edible bird’s nests would change the content and distribution of sialic acid components in vivo, a liquid chromatography–mass spectrometry method for the quantitative analysis of sialic acid levels in serum and tissues was developed. In the negative ion mode, the mobile phases consist of 0.1% formic acid in water (A) and acetonitrile (v/v) (B). Isocratic elution was performed with 60% B for 0−15 min. The chromatographic separation was performed on a Morphling HILIC Amide column (2.1 mm × 150 mm, 5 μm) at a flow rate of 0.5 mL min−1. The results showed that the correlation coefficients of the typical calibration curves were all higher than 0.995, exhibiting good linearity. The levels of free and conjugated forms of N-glycolylneuraminic acid (Neu5Gc), N-acetylneuraminic acid (Neu5Ac), and 2-keto-3-deoxy-D-glycero-D-galactonononic acid (KDN) in the serum and different tissues were simultaneously detected after the oral administration of the edible bird’s nests at a daily dose of 300 and 700 mg Kg−1 for seven days in mice. Our study found that the oral administration of edible bird’s nests can significantly increase the concentration of total sialic acids (Neu5Gc + Neu5Ac + KDN) in serum and spleen and lungs tissues, which may be related to the anti-inflammatory and immune function of edible bird’s nest, but further studies are needed to verify this. Neu5Ac was the dominant sialic acid in brain tissue, and Neu5Gc was the dominant sialic acid in serum and other tissues, including heart, liver, spleen, lungs, and kidney. Moreover, we found that the forms of Neu5Ac and Neu5Gc were mainly conjugated in all groups except liver tissue. In conclusion, the method we established had good linearity and accuracy; it allowed the analytes to be effectively separated from the matrix and endogenous substances in serum or tissues, so it could effectively detect the distribution and concentration of free and conjugated forms of sialic acids in serum and tissues, which was beneficial to the research and exploitation of edible bird’s nests and sialic acids. Full article
(This article belongs to the Special Issue Analysis and Bioanalysis of Pharmaceuticals: Sample Preparation and Chromatography)
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14 pages, 1692 KiB  
Article
Development and Validation of HPLC-FLD Analysis of Perampanel in MEPS-Processed Rat Plasma Sample
by Ayah Nader Abu-shark, Ashok K. Shakya, Safwan M. Al-Adwan and Rajashri R. Naik
Separations 2024, 11(2), 55; https://doi.org/10.3390/separations11020055 - 08 Feb 2024
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Abstract
Perampanel, a novel α-amino-3-hydroxy-5-methyl-4-isoxazolepropionic acid (AMPA) receptor antagonist, is registered for the adjunctive treatment of patients (aged ≥ 12 years) with refractory partial-onset seizures. A simple high-performance liquid chromatographic method fluorescence detection (HPLC-FLD) was developed to analyze perampanel in rats’ plasma and validated [...] Read more.
Perampanel, a novel α-amino-3-hydroxy-5-methyl-4-isoxazolepropionic acid (AMPA) receptor antagonist, is registered for the adjunctive treatment of patients (aged ≥ 12 years) with refractory partial-onset seizures. A simple high-performance liquid chromatographic method fluorescence detection (HPLC-FLD) was developed to analyze perampanel in rats’ plasma and validated for bioanalytical purposes. Rats’ plasma (50 µL) was processed by microextraction packed sorbent (MEPS). The analytes were separated using a Hypersil Gold octadecyl silane column (250 × 4.6 mm internal diameter, 5 μm particle size) with isocratic elution. A mobile phase consisting of acetonitrile–methanol–water (275:275:450, v/v/v; containing 50 µL triethylamine and pH adjusted to 3.25 with orthophosphoric acid) was used in this analysis. The flow rate was 1.25 mL/min. Analytes were monitored at an excitation wavelength of 285 nm and an emission wavelength of 430 nm. The linearity range for this validated method was from 3.75 to 300 ng/mL. No endogenous peaks were found in the elution of analytes in drug-free rats’ plasma. Intra- and inter-batch reproducibility studies demonstrated accuracy and precision within the acceptance criteria. The results indicate that the present method is simple, selective, reproducible, and suitable for the analysis of perampanel in small volume samples. The robustness of the method was accessed using MODDE® design of experiments software version 12.5. Full article
(This article belongs to the Special Issue Analysis and Bioanalysis of Pharmaceuticals: Sample Preparation and Chromatography)
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