Ionic-liquid/Carbowax 20 M functionalized capsule phase microextraction platform for the extraction of phosphodiesterase-5 inhibitors from human serum and urine prior to their determination by LC-MS.

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  • Additional Information
    • Source:
      Publisher: Elsevier Country of Publication: Netherlands NLM ID: 9318488 Publication Model: Print-Electronic Cited Medium: Internet ISSN: 1873-3778 (Electronic) Linking ISSN: 00219673 NLM ISO Abbreviation: J Chromatogr A Subsets: MEDLINE
    • Publication Information:
      Original Publication: Amsterdam ; New York : Elsevier, 1993-
    • Subject Terms:
      Ionic Liquids*/chemistry ; Liquid Phase Microextraction*/methods ; Phosphodiesterase 5 Inhibitors*/blood ; Phosphodiesterase 5 Inhibitors*/urine ; Phosphodiesterase 5 Inhibitors*/chemistry; Humans ; Limit of Detection ; Liquid Chromatography-Mass Spectrometry ; Reproducibility of Results ; Sildenafil Citrate/blood ; Sildenafil Citrate/urine ; Solid Phase Microextraction/methods
    • Abstract:
      Capsule phase microextraction (CPME) is an efficient bioanalytical technique that streamlines the sample preparation by integrating the filtration and stirring mechanism directly into the device. A novel composite sorbent designed to be selective towards the target analytes consisting of mixed-mode sorbent chemistry synthesized by sol-gel technology is found promising and superior to the conventional C 18 sorbents. Herein we describe the encapsulation of an ionic liquid (IL)/Carbowax 20M-functionalized sol-gel sorbent (sol-gel IL/Carbowax 20 M) in the lumen of porous polypropylene tubes for the capsule phase microextraction of three phosphodiesterase-5 inhibitors namely avanafil, sildenafil, and tadalafil in human serum and urine samples. The CPME device was characterized by Scanning Electron Microscopy (SEM) and Fourier-Transform Infrared Spectroscopy (FT-IR). The experimental parameters of CPME procedure (e.g. sample pH and ionic strength, extraction time, stirring rate, elution solvent and volume) were carefully optimized to achieve the highest possible extraction efficiency for the analytes. Method validation was conducted in terms of precision, linearity, accuracy, matrix effect, lower limits of quantification, and limits of detection (LOD). The method linearity was investigated in the range of 50-1000 ng mL -1 for all analytes while the precision was less than 11.8 % in all cases. For all analytes, the LOD values were 17 ng mL -1 . The IL/CW 20M-functionalized microextraction capsules could be reused at least 25 times both for urine and serum samples. The green character and the applicability of the proposed method were evaluated using the ComplexGAPI and BAGI indexes. The optimized CPME protocol exhibited reduced consumption of organic solvent and generation of waste, cost-effectiveness, and simplicity. Finally, the proposed method was successfully applied to the analysis of sildenafil in human urine after administration of drug-containing formulation.
      Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper.
      (Copyright © 2024 Elsevier B.V. All rights reserved.)
    • Contributed Indexing:
      Keywords: Biological samples; Capsule phase microextraction; LC–MS; Mixed-mode sorbent; Phosphodiesterase-5 inhibitors
    • Accession Number:
      0 (Ionic Liquids)
      0 (Phosphodiesterase 5 Inhibitors)
      BW9B0ZE037 (Sildenafil Citrate)
    • Publication Date:
      Date Created: 20240718 Date Completed: 20240727 Latest Revision: 20240802
    • Publication Date:
      20250114
    • Accession Number:
      10.1016/j.chroma.2024.465157
    • Accession Number:
      39025028