Synthesis and Characterization of Electrospun Sorbent for the Solid-Phase Extraction of Fluoroquinolones in Human Plasma and Their UHPLC-PDA Determination

In this work we investigated the synthesis and the characterization of electrospun polyacrylonitrile (PAN) and polymethyl methacrylate (PMMA) stabilized in air, made in a 5:1 ratio, used as sorbent for the solid-phase extraction of fluoroquinolones in plasma samples and the following quantification...

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Main Authors: Vincenzo Ferrone, Giuseppe Carlucci, Pantaleone Bruni, Lisa Marinelli, Pasquale Avino, Edoardo Milanetti, Serena Pilato, Leonardo Sbrascini, Pietro Di Profio, Stefania Ferrari
Format: Article
Language:English
Published: MDPI AG 2023-02-01
Series:Separations
Subjects:
Online Access:https://www.mdpi.com/2297-8739/10/2/104
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author Vincenzo Ferrone
Giuseppe Carlucci
Pantaleone Bruni
Lisa Marinelli
Pasquale Avino
Edoardo Milanetti
Serena Pilato
Leonardo Sbrascini
Pietro Di Profio
Stefania Ferrari
author_facet Vincenzo Ferrone
Giuseppe Carlucci
Pantaleone Bruni
Lisa Marinelli
Pasquale Avino
Edoardo Milanetti
Serena Pilato
Leonardo Sbrascini
Pietro Di Profio
Stefania Ferrari
author_sort Vincenzo Ferrone
collection DOAJ
description In this work we investigated the synthesis and the characterization of electrospun polyacrylonitrile (PAN) and polymethyl methacrylate (PMMA) stabilized in air, made in a 5:1 ratio, used as sorbent for the solid-phase extraction of fluoroquinolones in plasma samples and the following quantification in UHPLC-PDA. Preliminary analyses of viscosity were carried out on the polymer solution to be sure about the electrospinability. Characterizations were performed on the electrospun membrane to evaluate the morphology (SEM scanning electron microscopy and AFM atomic force microscopy), the thermal degradation behavior (TGA thermogravimetric analysis), the porosity and the surface area (BET, Brunauer Emmett Teller), and the quantitative and qualitative distribution of atomic structures (FTIR infrared analysis in Fourier transform and EDX Energy Dispersive X-ray analysis). A solid-phase extraction method was developed by studying parameters such as the amount of sorbent and the pH of the sample. Finally, a UHPLC-PDA method for the analysis of fluoroquinolones was developed and validated in accordance with the guidelines and successfully applied. The use of the prepared sorbent combined with UHPLC-PDA has allowed the development of a method whose strengths are its speed, accuracy, sensitivity, and high recoveries.
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spelling doaj.art-bd3d57cd92b94d88a88adfa6d347cb3f2023-11-16T23:14:23ZengMDPI AGSeparations2297-87392023-02-0110210410.3390/separations10020104Synthesis and Characterization of Electrospun Sorbent for the Solid-Phase Extraction of Fluoroquinolones in Human Plasma and Their UHPLC-PDA DeterminationVincenzo Ferrone0Giuseppe Carlucci1Pantaleone Bruni2Lisa Marinelli3Pasquale Avino4Edoardo Milanetti5Serena Pilato6Leonardo Sbrascini7Pietro Di Profio8Stefania Ferrari9Department of Pharmacy, University “G. d’Annunzio” of Chieti-Pescara, I-66100 Chieti, ItalyDepartment of Pharmacy, University “G. d’Annunzio” of Chieti-Pescara, I-66100 Chieti, ItalyDepartment of Pharmacy, University “G. d’Annunzio” of Chieti-Pescara, I-66100 Chieti, ItalyDepartment of Pharmacy, University “G. d’Annunzio” of Chieti-Pescara, I-66100 Chieti, ItalyDepartment of Agricoltural Environmental and Food Science (DiAAA), University of Molise, Via De Sanctis, I-86100 Campobasso, ItalyDepartment of Physics, University “La Sapienza”, Ple A. Moro, 5, I-00185 Roma, ItalyDepartment of Pharmacy, University “G. d’Annunzio” of Chieti-Pescara, I-66100 Chieti, ItalyChemistry Division, School of Science and Technologies, University of Camerino, I-62032 Camerino, ItalyDepartment of Pharmacy, University “G. d’Annunzio” of Chieti-Pescara, I-66100 Chieti, ItalyDepartment of Pharmacy, University “G. d’Annunzio” of Chieti-Pescara, I-66100 Chieti, ItalyIn this work we investigated the synthesis and the characterization of electrospun polyacrylonitrile (PAN) and polymethyl methacrylate (PMMA) stabilized in air, made in a 5:1 ratio, used as sorbent for the solid-phase extraction of fluoroquinolones in plasma samples and the following quantification in UHPLC-PDA. Preliminary analyses of viscosity were carried out on the polymer solution to be sure about the electrospinability. Characterizations were performed on the electrospun membrane to evaluate the morphology (SEM scanning electron microscopy and AFM atomic force microscopy), the thermal degradation behavior (TGA thermogravimetric analysis), the porosity and the surface area (BET, Brunauer Emmett Teller), and the quantitative and qualitative distribution of atomic structures (FTIR infrared analysis in Fourier transform and EDX Energy Dispersive X-ray analysis). A solid-phase extraction method was developed by studying parameters such as the amount of sorbent and the pH of the sample. Finally, a UHPLC-PDA method for the analysis of fluoroquinolones was developed and validated in accordance with the guidelines and successfully applied. The use of the prepared sorbent combined with UHPLC-PDA has allowed the development of a method whose strengths are its speed, accuracy, sensitivity, and high recoveries.https://www.mdpi.com/2297-8739/10/2/104electrospun sorbentsolid-phase extractionfluoroquinolonesUHPLC-PDAmethod developmentelectrospinning
spellingShingle Vincenzo Ferrone
Giuseppe Carlucci
Pantaleone Bruni
Lisa Marinelli
Pasquale Avino
Edoardo Milanetti
Serena Pilato
Leonardo Sbrascini
Pietro Di Profio
Stefania Ferrari
Synthesis and Characterization of Electrospun Sorbent for the Solid-Phase Extraction of Fluoroquinolones in Human Plasma and Their UHPLC-PDA Determination
Separations
electrospun sorbent
solid-phase extraction
fluoroquinolones
UHPLC-PDA
method development
electrospinning
title Synthesis and Characterization of Electrospun Sorbent for the Solid-Phase Extraction of Fluoroquinolones in Human Plasma and Their UHPLC-PDA Determination
title_full Synthesis and Characterization of Electrospun Sorbent for the Solid-Phase Extraction of Fluoroquinolones in Human Plasma and Their UHPLC-PDA Determination
title_fullStr Synthesis and Characterization of Electrospun Sorbent for the Solid-Phase Extraction of Fluoroquinolones in Human Plasma and Their UHPLC-PDA Determination
title_full_unstemmed Synthesis and Characterization of Electrospun Sorbent for the Solid-Phase Extraction of Fluoroquinolones in Human Plasma and Their UHPLC-PDA Determination
title_short Synthesis and Characterization of Electrospun Sorbent for the Solid-Phase Extraction of Fluoroquinolones in Human Plasma and Their UHPLC-PDA Determination
title_sort synthesis and characterization of electrospun sorbent for the solid phase extraction of fluoroquinolones in human plasma and their uhplc pda determination
topic electrospun sorbent
solid-phase extraction
fluoroquinolones
UHPLC-PDA
method development
electrospinning
url https://www.mdpi.com/2297-8739/10/2/104
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