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Separations
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Separation Techniques in Drug Analysis
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Separation Techniques in Drug Analysis

A special issue of Separations (ISSN 2297-8739). This special issue belongs to the section "Analysis of Natural Products and Pharmaceuticals".

Deadline for manuscript submissions: closed (20 April 2025) | Viewed by 2329

Special Issue Editors

Dr. Ionel Bogdan Cioroiu

E-Mail Website
Guest Editor
Romanian Academy, Iasi Branch, Iasi, Romania
Interests: liquid chromatography; gas chromatography; mass spectrometry; hyphenated techniques; LC-GC-MS systems; online sample preparation; bidimensional methods
Dr. Marius Niculaua

E-Mail Website
Guest Editor
Research Centre for Oenology Iași, Romanian Academy Iași Branch, 8 Carol I, 700505 Iasi, Romania
Interests: liquid chromatography; gas chromatography; mass spectrometry; hyphenated techniques; LC-GC-MS systems; online sample preparation; bidimensional methods

Special Issue Information

Dear Colleagues,

In current practice, there is an increasing emphasis on the substitution of synthetic active substances with pharmaco-active products of biological nature. This replacement is driven by a growing trend to return to alternative practices for maintaining human health by incorporating bioactive elements in the treatment of pathologies that are considered chronic and advanced, where treatment regimens typically involve synthetic molecules with fully demonstrated efficacy. However, it has been shown that nature plays a significant role in maintaining health, though many of the bioactive principles have not yet been fully elucidated. Recent studies have demonstrated the overwhelming strength of plants, leading to the development of pharmaceutical systems based on plants and the active principles within them. Such systems have proven effective in treating metabolic disorders, psychological disorders, skin conditions, and other ailments with antibiotic properties. Their efficacy has been demonstrated to the extent that official reference monographs have included them in the category of herbal medicines.

It is my pleasure to invite you to contribute through your obtained results to their dissemination in a professional and high-quality publishing environment. This will allow you to gain worldwide recognition and provide a personal development perspective through access to similar studies and projects that support enhanced experimental development.

Dr. Ionel Bogdan Cioroiu
Dr. Marius Niculaua
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

  • LC-MS
  • GC-MS
  • LC-GC-MS
  • sample preparation
  • drug analysis
  • pharmaceuticals
  • bidimensional methods
  • method validation

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Published Papers (2 papers)

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Research

21 pages, 3693 KB  
Article
Electrochemistry–Mass Spectrometry for Generation and Identification of Metabolites of Selected Drugs from Different Therapeutic Groups in Comparison with In Vitro and In Vivo Approaches
by Małgorzata Szultka-Młyńska
Separations 2025, 12(9), 243; https://doi.org/10.3390/separations12090243 - 5 Sep 2025
Viewed by 229
Abstract
The metabolism of antibiotics, antidepressants, and cardiovascular drugs has been investigated widely over the last few decades. The aim of this study was to develop an efficient analytical protocol based on the combination of electrochemistry (EC) and mass spectrometry for the identification of [...] Read more.
The metabolism of antibiotics, antidepressants, and cardiovascular drugs has been investigated widely over the last few decades. The aim of this study was to develop an efficient analytical protocol based on the combination of electrochemistry (EC) and mass spectrometry for the identification of electrochemical products (potential pharmacologically active metabolites) of selected drugs (enalapril, metronidazole, midazolam, propranolol, venlafaxine). The electrochemical mimicry of the oxidative phase I and II metabolism was achieved in a thin-layer cell equipped with different working electrodes (magic diamond (MD), glassy carbon (GC), gold (Au), platinum (Pt)). The structures of the electrochemically generated metabolites were elucidated based on accurate mass ion data and tandem mass spectrometry (MS/MS) experiments. The in silico prediction of the main sites of selected drugs’ metabolism was performed using Biotransformer 3.0, GLORYx, and Xenosite software. Moreover, incubation with liver microsomes (LMs) was performed to examine the proposed metabolic pathways of target compounds. The data from in vitro experiments agreed with the data from electrochemical oxidation, which predicted some potential metabolites found in the real samples from patients. For enzymatic incubation, N-dealkylation, O-demethylation, and hydroxylation were the metabolic pathways involved mainly in their metabolism. Their in vitro phase II metabolites were identified as glucuronic acid conjugates. Finally, different in vivo phase I and II metabolites were identified for the studied drugs, including metabolic pathways for in vivo phase I N-demethylation, N-dealkylation, O-demethylation, and hydroxylation, while the metabolic pathways for in vivo phase II metabolites were identified as glucuronic acid conjugates. Full article
(This article belongs to the Special Issue Separation Techniques in Drug Analysis)
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12 pages, 1622 KB  
Article
Investigation of Metoprolol Concentrations in Plasma Using Automated Sample Preparation and LC-MS/MS Detection
by Ionel-Bogdan Cioroiu, Mona-Elisabeta Dobrin, Marius Niculaua, Constantin-Bogdan Nechita and Valeriu V. Cotea
Separations 2024, 11(11), 306; https://doi.org/10.3390/separations11110306 - 24 Oct 2024
Viewed by 1658
Abstract
Metoprolol (MTP), a selective beta-1 adrenergic blocker, is commonly administered in the form of succinate or tartrate salts, depending on the pharmaceutical formulation. It is typically prescribed in oral forms as either immediate-release or extended-release tablets. This study describes a chromatographic method using [...] Read more.
Metoprolol (MTP), a selective beta-1 adrenergic blocker, is commonly administered in the form of succinate or tartrate salts, depending on the pharmaceutical formulation. It is typically prescribed in oral forms as either immediate-release or extended-release tablets. This study describes a chromatographic method using automated sample clean-up and elution via a reversed-phase mechanism. A TurboFlow approach was applied with a Cyclone P column, and the elution was performed isocratically using a mobile phase of water and acetonitrile (0.1% v/v formic acid) within 4.5 min. Quantification of MTP was achieved using triple quadrupole mass spectrometry, with the transition m/z 268.1 → m/z 130.96 for metoprolol, while bisoprolol fumarate, the internal standard, was detected at m/z 326.3 → m/z 116.2. The method was validated according to bioequivalence guidelines. Selectivity was assessed by checking for potential interferences from blank samples or related compounds formed during sample preparation. Precision and accuracy were evaluated both within and between runs, with a maximum coefficient of variation (CV%) of 10.28 and a maximum relative error (ER%) of 5.38. Linearity was demonstrated over the range of 5 ng/L to 1000 ng/L, with a lower limit of quantification at 0.042 ng/L, made possible by injecting larger sample volumes. A matrix effect of 89% was considered acceptable when compared to standard solutions. Plasma concentrations of MTP were monitored in patients administered either 50 mg or 100 mg doses. For the 50 mg dose, plasma levels reached up to 34 μg/L, while the 100 mg dose produced concentrations ranging from 3.56 to 50.81 μg/L. Although the higher dose generally resulted in elevated plasma levels, significant variability was observed. A strong correlation (r = 0.992) was found between the administered dose and plasma concentration, though variations in absorption rates and patient demographics likely contributed to the observed variability. This method provides a reliable analytical approach suitable for pharmacokinetic and clinical studies involving metoprolol. Full article
(This article belongs to the Special Issue Separation Techniques in Drug Analysis)
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