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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: 10 July 2025 | Viewed by 14003

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

E-Mail Website
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

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Published Papers (6 papers)

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Research

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16 pages, 2101 KiB  
Article
Simultaneous Determination and Quantification of NineNitrosamine Impurities in Semi-Solid Forms Using a GC–MS/MS Method
by Namjin Lee, Hyejin Go and Young-joon Park
Separations 2025, 12(5), 120; https://doi.org/10.3390/separations12050120 - 11 May 2025
Viewed by 200
Abstract
Many studies are being conducted on the detection of nitrosamine impurities in solid formulations. However, research on semi-solid formulations such as gels, ointments and creams is not common. In particular, excipients used to increase viscosity and add fragrance can significantly impact the sample [...] Read more.
Many studies are being conducted on the detection of nitrosamine impurities in solid formulations. However, research on semi-solid formulations such as gels, ointments and creams is not common. In particular, excipients used to increase viscosity and add fragrance can significantly impact the sample preparation. Volatile compounds derived from natural fragrances are composed of a wide variety of complex components, making them very difficult to handle and completely separate from the analytes. Due to the complex composition of these formulations, an analytical method was developed to accurately separate and analyze nine nitrosamine impurities (NDMA, NDEA, NMEA, NDPA, NDBA, NPIP, NMOR, DIPNA and EIPNA) simultaneously. To overcome challenges in the sample preparation of excipients with physical and chemical properties, the sample was prepared using solvents such as methanol, hexane, water and dichloromethane. The target analytes were extracted with dichloromethane for the final preparation for GC–MS/MS and the optimal conditions were established. While multiple GC columns were tested, peak overlapping interferences were observed, leading to the use of a 60m-long column to overcome peak overlap. The GC–MS/MS condition was set for optimal performance and ionization energy, with parameters adjusted for each analyte. The developed method was validated in accordance with guidelines to ensure its reliability and suitability. As a result, all nine nitrosamine impurities were simultaneously analyzed, confirming excellent performance. The sample preparation method and procedure, column specification and GC–MS/MS conditions have the potential to be adapted not only for semi-solid formulations of pharmaceuticals and cosmetics but also for other formulations such as solid and liquid samples, rendering them suitable for the analysis of nitrosamine impurities. Full article
(This article belongs to the Special Issue Analysis and Bioanalysis of Pharmaceuticals: Sample Preparation and Chromatography)
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17 pages, 2804 KiB  
Article
Quantitation of Copper Tripeptide in Cosmetics via Fabric Phase Sorptive Extraction Combined with Zwitterionic Hydrophilic Interaction Liquid Chromatography and UV/Vis Detection
by Pantelitsa Pingou, Anthi Parla, Abuzar Kabir, Kenneth G. Furton, Victoria Samanidou, Spyridon Papageorgiou, Efthimios Tsirivas, Athanasia Varvaresou and Irene Panderi
Separations 2024, 11(10), 293; https://doi.org/10.3390/separations11100293 - 12 Oct 2024
Cited by 1 | Viewed by 2149
Abstract
The increasing demand for effective cosmetics has driven the development of innovative analytical techniques to ensure product quality. This work presents the development and validation of a zwitterionic hydrophilic interaction liquid chromatography method, coupled with ultraviolet detection, for the quantification of copper tripeptide [...] Read more.
The increasing demand for effective cosmetics has driven the development of innovative analytical techniques to ensure product quality. This work presents the development and validation of a zwitterionic hydrophilic interaction liquid chromatography method, coupled with ultraviolet detection, for the quantification of copper tripeptide in cosmetics. A novel protocol for sample preparation was developed using fabric phase sorptive extraction to extract the targeted analyte from the complex cosmetic cream matrix, followed by chromatographic separation on a ZIC®-pHILIC analytical column. A thorough investigation of the chromatographic behavior of the copper tripeptide on the HILIC column was performed during method development. The mobile phase consisted of 133 mM ammonium formate (pH 9, adjusted with ammonium hydroxide) and acetonitrile at a 40:60 (v/v) ratio, with a flow rate of 0.2 mL/min. A design of experiments (DOE) approach allowed precise adjustments to various factors influencing the extraction process, leading to the optimization of the fabric phase sorptive extraction protocol for copper tripeptide analysis. The method demonstrated excellent linearity over a concentration range of 0.002 to 0.005% w/w for copper tripeptide, with a correlation coefficient exceeding 0.998. The limits of detection and quantitation were 5.3 × 10−4% w/w and 2.0 × 10−3% w/w, respectively. The selectivity of the method was verified through successful separation of copper tripeptide from other cream components within 10 min, establishing its suitability for high-throughput quality control of cosmetic formulations. Full article
(This article belongs to the Special Issue Analysis and Bioanalysis of Pharmaceuticals: Sample Preparation and Chromatography)
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15 pages, 653 KiB  
Article
Development and Validation of an LC-MS/MS Method for the Determination of Plasma and Red Blood Cell Omega Fatty Acids: A Useful Diagnostic Tool
by Lénárd Farczádi, Minodora Dobreanu, Adina Huțanu and Silvia Imre
Separations 2024, 11(5), 140; https://doi.org/10.3390/separations11050140 - 1 May 2024
Cited by 1 | Viewed by 3860
Abstract
Background: LC-MS is an ever-increasingly used methodology for clinical applications. Due to the superior selectivity and sensitivity, in certain situations, it can offer an advantage or be the only option for diagnostics and biomonitoring applications. Methods: A high selectivity sensitive LC-MS/MS method was [...] Read more.
Background: LC-MS is an ever-increasingly used methodology for clinical applications. Due to the superior selectivity and sensitivity, in certain situations, it can offer an advantage or be the only option for diagnostics and biomonitoring applications. Methods: A high selectivity sensitive LC-MS/MS method was developed for direct quantification of free plasma polyunsaturated fatty acids as well as conjugated membrane polyunsaturated fatty acids, using isocratic reverse phase elution. A quick and simple sample purification method was used in order to ensure high-throughput analysis of biological samples. The method was validated with regard to selectivity, sensitivity, linearity, accuracy, precision, carryover, and recovery, as well as other relevant parameters. Results and Conclusions: The method was developed and validated with respect to all relevant parameters and was successfully used in a number of clinical diagnostics and biomonitoring applications. The simple sample purification process allowed for an easy learning curve for analysts and other users, while ensuring a low chance of systematic or random errors and thus reliable results usable in a clinical setting. Full article
(This article belongs to the Special Issue Analysis and Bioanalysis of Pharmaceuticals: Sample Preparation and Chromatography)
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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 - 1 Apr 2024
Cited by 2 | Viewed by 2192
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 - 8 Feb 2024
Viewed by 2180
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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Review

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29 pages, 1668 KiB  
Review
Methods of Analysis of Phytoestrogenic Compounds: An Up-to-Date of the Present State
by Ines Adam-Dima, Andreea Alexandra Olteanu, Octavian Tudorel Olaru, Daniela Elena Popa and Carmen Purdel
Separations 2024, 11(7), 205; https://doi.org/10.3390/separations11070205 - 1 Jul 2024
Cited by 2 | Viewed by 2469
Abstract
Phytoestrogens, natural compounds with structural similarity to 17-β-estradiol, are known to have potential health benefits, including in hormone-dependent malignancies. The therapeutic interest and some safety concerns observed triggered the need to develop accurate methods to assess their level in different matrices. This narrative [...] Read more.
Phytoestrogens, natural compounds with structural similarity to 17-β-estradiol, are known to have potential health benefits, including in hormone-dependent malignancies. The therapeutic interest and some safety concerns observed triggered the need to develop accurate methods to assess their level in different matrices. This narrative review examines the existing analytical methods used to isolate, quantify, and characterize phytoestrogens and their metabolites in plants, foods, and biological samples. Different conventional and modern extraction techniques, such as ultrasonication-assisted extraction, supercritical fluid extraction, or enzyme-assisted extraction, were presented and compared. The advantages and limitations of the existing analytical methods, such as high-performance liquid chromatography using different sensitive detectors, gas chromatography often coupled with mass spectrometry, and immunoassay methods, are highlighted, along with the need for ongoing research to improve the sensitivity and selectivity of the analysis. Full article
(This article belongs to the Special Issue Analysis and Bioanalysis of Pharmaceuticals: Sample Preparation and Chromatography)
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