Analysis of Pharmaceuticals: Sample Preparation and Chromatography/Separation

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

Deadline for manuscript submissions: closed (20 July 2023) | Viewed by 4801

Special Issue Editor

Department of Pharmaceutics, College of Pharmacy, King Saud University, Riyadh 11451, Saudi Arabia
Interests: pharmaceutical analysis; environmental chemistry; separation processes; wastewater treatment; nanoemulsion; drug delivery

Special Issue Information

Dear Colleagues,

The progress in the field of pharmacy and pharmaceutical analysis has reached new heights in last the two decades. The requirement of proper analytical methods is the need of the hour for the identification and estimation of pharmaceutical compounds, keeping in mind their application as well as their presence in various matrices. From a health perspective, active pharmaceutical ingredients and their metabolites and impurities need to be identified in order to achieve maximum efficiency and benefits. Regarding the environment, the presence of these APIs and their metabolites in water bodies has very deleterious effects on the metabolism of living creatures inhabiting these environments. These APIs register their presence in different environmental matrices, such as foods and water, which are supposed to be fit for human consumption. Therefore, analytical methodology for the identification, separation and quantification of APIs/biopharmaceuticals/nutraceuticals/pharmaceutically important phytochemicals and their metabolites is very much required. One of the most important steps of pharmaceutical analysis is sample preparation. If a sample is not prepared properly, it can damage the machine if it contain impurities, or the drug itself will not be identified or quantified exactly, giving erroneous results. Samples from biological matrices (e.g., blood, urine, tissues), environmental matrices (e.g., water bodies such as rivers/ponds/lakes, wastewaters), or foods like animal meats or vegetables need to be prepared in such a manner that the target molecule is free from interference from the matrix itself. There are various sample preparation techniques developed over a period of time, such as direct injection, liquid–liquid extraction and solid-phase extraction (commonly called traditional sample preparation techniques frequently exploited in pharmaceutical industries). In addition to these traditional techniques, some recently developed techniques are also currently employed for the extraction of target compounds from complex matrices, with examples including solid-phase microextraction, accelerated solvent extraction, and microwave extraction. Chemical derivatization is also gaining popularity as a sample preparation tool.

This Special Issue aims to collect recent advances, developments, and analytical innovations in sample preparation and chromatographic/separation techniques for the identification and analysis of active pharmaceutical ingredients in plant, food, and pharmaceutical products; reaction byproducts; animal feed; biological fluids (blood, urine, serum); plant and animal tissues; waste streams; or environmental samples.

Dr. Nazrul Haq
Guest Editor

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Keywords

  • pharmaceutical analysis
  • food composition analysis
  • biological fluids analysis
  • chromatographic techniques
  • liquid–liquid extraction
  • solid-phase extraction
  • solid-phase microextraction
  • accelerated solvent extraction
  • microwave extraction
  • chemical derivatization

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Published Papers (2 papers)

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Research

15 pages, 4002 KiB  
Article
Comparison of Miniaturized Chromatographic Columns and 96-Well Plates for Automated Antibody Purification under Economic and Sustainable Aspects
by Anna Bach, Heidi Fleischer and Kerstin Thurow
Separations 2023, 10(8), 447; https://doi.org/10.3390/separations10080447 - 11 Aug 2023
Viewed by 2093
Abstract
Therapeutic antibodies are an area of major interest in treating infectious diseases, autoimmune diseases, and cancer. Efficient purification strategies are required to discover and produce antibodies, representing a significant cost driver. Miniaturization and automation of the chromatographic purification process may contribute to cost [...] Read more.
Therapeutic antibodies are an area of major interest in treating infectious diseases, autoimmune diseases, and cancer. Efficient purification strategies are required to discover and produce antibodies, representing a significant cost driver. Miniaturization and automation of the chromatographic purification process may contribute to cost reduction. In this article, miniaturized chromatographic columns and 96-well filter plates are used to purify an IgG antibody from cell cultures and are compared in terms of quality, cost, and sustainability. The validation results of the two miniaturized chromatographic antibody purification methods indicate high efficacy and are comparable except for minor differences in yield. The lowest cost per sample can be obtained with the miniaturized chromatographic columns, as annual throughput can be maximized with the miniaturized plates. By evaluating sustainability, significant reductions in laboratory waste produced during antibody purification can be shown, along with an increase in employee safety by using the automation system. Overall, the comparison of results shows that, in the development of new purification strategies, the type of implementation has a decisive influence on the outcomes in terms of recovery, cost-effectiveness, and sustainability. Full article
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16 pages, 2389 KiB  
Article
Green Bio-Analytical Study of Gabapentin in Human Plasma Coupled with Pharmacokinetic and Bioequivalence Assessment Using UPLC-MS/MS
by Rehab Moussa Tony, Mohamed A. El Hamd, Mohammed Gamal, Safaa F. Saleh, Nujud Maslamani, Wejdan T. Alsaggaf and Mohamed B. El-Zeiny
Separations 2023, 10(4), 234; https://doi.org/10.3390/separations10040234 - 2 Apr 2023
Cited by 4 | Viewed by 2172
Abstract
Gabapentin (GAB) is a cyclohexane acetic acid, structurally related to the neurotransmitter gamma-aminobutyric acid (GABA), and considered the principal inhibitory neurotransmitter in the central nervous system (CNS) of mammals. An ultra-performance liquid chromatography–tandem mass spectrophotometry (UPLC-MS/MS) method for assessing pregabalin (PRE) in human [...] Read more.
Gabapentin (GAB) is a cyclohexane acetic acid, structurally related to the neurotransmitter gamma-aminobutyric acid (GABA), and considered the principal inhibitory neurotransmitter in the central nervous system (CNS) of mammals. An ultra-performance liquid chromatography–tandem mass spectrophotometry (UPLC-MS/MS) method for assessing pregabalin (PRE) in human plasma, was developed and validated, via PRE usage as an internal standard. The plasma underwent protein precipitation using methanol, prior to analysis. Chromatographic separation was completed using a mobile phase of methanol: 0.1% formic acid solution, (65:35, v/v), at a flow rate of 0.2 mL/min, with an isocratic approach, on an Agilent Eclipse plus column (50 × 2.1 mm and 1.8 μm), in 1.6 min of running time. An Agilent triple quadrupole was used for mass analysis, to detect the ion transitions for GAB and PER, respectively, at m/z of 172.1 → 154.1 and 160.10 → 142.10. The calibration curve, over the linear range of 0.050–10.0 μg/mL, showed a high correlation coefficient, r = 0.9993. The limits of detection and quantitation were 13.37 ng/mL and 40.52 ng/mL, respectively, based on the standard deviation and slope equation. The results for intra- and inter-day measurement accuracy and precision were in acceptable ranges. The method was extended into the assessment of oral administrations of GAB at different doses, of one 600 mg/tablet and two capsules (each one of them has 300 mg of GAB), to volunteers who were used in pharmacokinetics and bioequivalent studies. The AGREE assessment tool was used to visualize the proposed method’s greenness degree, which revealed a high AGREE rating score, supporting the accepted method’s greenness profile. Full article
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