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: 20 April 2025 | Viewed by 707

Special Issue Editors


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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

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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

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Keywords

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

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Published Papers (1 paper)

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Research

12 pages, 1622 KiB  
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 547
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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