Application of Microextraction and Chromatography in Bioanalysis and Pharmaceutical 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 (31 December 2023) | Viewed by 2029

Special Issue Editors


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Guest Editor
Department of Pharmacy, University “G. d’Annunzio” of Chieti-Pescara, I-66100 Chieti, Italy
Interests: HPLC-PDA; GC; LC-MS; sample preparation; SPME; MEPS; DLLME; SPE; method validation

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Guest Editor
Department of Pharmacy, University “G. d’Annunzio” of Chieti-Pescara, I-66100 Chieti, Italy
Interests: HPLC-PDA; sample preparation; MEPS; SPE; electrospinning; polymer; nanomaterials; characterization

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Guest Editor
Department of Pharmacy, University “G. d’Annunzio” of Chieti-Pescara, via dei Vestini 31, 66100 Chieti Scalo, CH, Italy
Interests: supramolecular chemistry; organic chemistry; Raman spectroscopy; graphene technology; host-guest interactions
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Special Issue Information

Dear Colleagues,

Sample preparation is a crucial part of the analytical process and should be part of any analytical chemistry teaching curriculum. Over the last two decades, active research on sample preparation has been fueled by interest in the elimination of organic solvent from environmental analysis and the rapid analysis of biological samples. This new development results in the miniaturization of the extraction process, leading to new micro-configurations and solvent-free approaches. The fundamental understanding of extraction principles has advanced in parallel with the development of new technology. Recently, new sorbents such as silica, carbon-based, polymeric and metal organic frameworks have been introduced, increasing the performance of all sorbent-based sample preparation techniques. Furthermore, technological developments have made it possible to obtain these new nanomaterials (NMs) which immediately showed themselves to be promising in the field of separations. The challenge in this Special Issue is to apply micro-extraction techniques to molecules of bio-pharmaceutical interest from various matrices and their quantification using chromatographic techniques coupled with sensitive detectors.

Dr. Vincenzo Ferrone
Dr. Pantaleone Bruni
Dr. Michele Ciulla
Guest Editors

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Keywords

  • HPLC- UHPLC
  • GC
  • sample preparation
  • nanomaterials
  • micro-extraction
  • DLLME
  • LC-MS
  • sorbent
  • characterization
  • sub-critical and supercritical fluid extraction

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Published Papers (1 paper)

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Research

14 pages, 2178 KiB  
Article
Development of a Fast and Sensitive UPLC–MS/MS Analytical Methodology for Fenebrutinib Estimation in Human Liver Microsomes: In Vitro and In Silico Metabolic Stability Evaluation
by Mohamed W. Attwa, Aishah M. Alsibaee, Haya I. Aljohar, Ali S. Abdelhameed and Adnan A. Kadi
Separations 2023, 10(5), 302; https://doi.org/10.3390/separations10050302 - 9 May 2023
Cited by 8 | Viewed by 1666
Abstract
Fenebrutinib (GDC-0853; FNB) is an oral small molecule that was developed by Roche Pharmaceuticals to slow multiple sclerosis progression. FNB is a reversible bruton tyrosine kinase (BTK) inhibitor, which showed the maximum potency of BTK inhibitors in phase III clinical trials for multiple [...] Read more.
Fenebrutinib (GDC-0853; FNB) is an oral small molecule that was developed by Roche Pharmaceuticals to slow multiple sclerosis progression. FNB is a reversible bruton tyrosine kinase (BTK) inhibitor, which showed the maximum potency of BTK inhibitors in phase III clinical trials for multiple sclerosis. In the current study, a fast, specific, and sensitive UPLC-MS/MS method for FNB quantification in human liver microsomes (HLMs) was established with application to the evaluation of metabolic stability. The UPLC-MS/MS methodology was verified using the stated USFDA validation guidelines for bioanalytical methodologies that involve selectivity, linearity, accuracy and precision, carryover and extraction recovery, stability, and matrix effect. The FNB calibration curve displayed a linearity in the range from 1 ng/mL to 3000 ng/mL (y = 1.731x + 2.013; R2: 0.9954; RSD < 4.37%) in the HLMs matrix. The limit of quantification was 0.88 ng/mL, which verified the UPLC-MS/MS analytical method sensitivity. The intraday and interday precision and accuracy results of the developed UPLC-MS/MS method were −3.99–14.0% and 0.52–3.83%, respectively. FNB and savolitinib (SVB) (internal standard) were chromatographically separated utilizing an isocratic mobile phase system with a ZORBAX Eclipse plus-C18 (50 mm, 2.1 mm, and 1.8 μm) column. The metabolic stability parameters for FNB, involving high intrinsic clearance (58.21 mL/min/kg) and a short in vitro half-life (13.93 min), revealed the high extraction ratio of FNB. Reviewing the literature revealed that the current UPLC-MS/MS method is the first analytical method for FNB quantification in the HLMs matrix with application to the assessment of FNB metabolic stability. Full article
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