Solvothermal synthesis of polyvinyl pyrrolidone encapsulated, amine-functionalized copper ferrite and its use as a magnetic resonance imaging contrast agent.

Copper ferrite nanoparticles for use as MRI contrast agents were synthesized using two different methods. A novel microwave-assisted (MW) solvothermal method was developed and compared to a conventional 12-hour synthesis (Reflux) as an eco-friendlier approach. This innovative synthesis method succes...

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Main Authors: Fatemeh Heydari, Ágnes M Ilosvai, Noémi Kovács, Domokos Máthé, Ferenc Kristály, Lajos Daróczi, Zoltán Kaleta, Béla Viskolcz, Miklós Nagy, László Vanyorek, László Forgách, Krisztián Szigeti
Format: Article
Language:English
Published: Public Library of Science (PLoS) 2025-01-01
Series:PLoS ONE
Online Access:https://doi.org/10.1371/journal.pone.0316221
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author Fatemeh Heydari
Ágnes M Ilosvai
Noémi Kovács
Domokos Máthé
Ferenc Kristály
Lajos Daróczi
Zoltán Kaleta
Béla Viskolcz
Miklós Nagy
László Vanyorek
László Forgách
Krisztián Szigeti
author_facet Fatemeh Heydari
Ágnes M Ilosvai
Noémi Kovács
Domokos Máthé
Ferenc Kristály
Lajos Daróczi
Zoltán Kaleta
Béla Viskolcz
Miklós Nagy
László Vanyorek
László Forgách
Krisztián Szigeti
author_sort Fatemeh Heydari
collection DOAJ
description Copper ferrite nanoparticles for use as MRI contrast agents were synthesized using two different methods. A novel microwave-assisted (MW) solvothermal method was developed and compared to a conventional 12-hour synthesis (Reflux) as an eco-friendlier approach. This innovative synthesis method successfully produced nanoparticles with enhanced properties compared to traditional ferrite materials. The nanoparticles' morphological and magnetic properties were evaluated and tested in in-vivo MRI studies. The results revealed both similarities and differences between the amine-functionalized copper ferrite nanoparticles. FTIR, XRD, HRTEM, and VSM analyses indicated improved properties in the CuFe2O4-NH2 MW particles, while AFM confirmed successful polymer encapsulation of the nanoparticles. For the CuFe2O4-NH2 MW sample, 76.8 wt% copper ferrite and 23.2 wt% magnetite were detected, with crystallite sizes of 8 ± 2 nm and 13 ± 2 nm, respectively. In the CuFe2O4-NH2 Refl. sample, in addition to these two magnetic phases, larger copper particles (31.6 wt%) were also formed. DLS analysis demonstrated that the CuFe2O4-NH2 MW sample exhibited excellent colloidal stability, maintaining its size distribution in aqueous media for 3 hours without aggregation, unlike the CuFe2O4-NH2 Refl. sample, which showed slight aggregation. The CuFe2O4-NH2 MW sample displayed superparamagnetic behavior (Ms: 15 emu/g, Mr: 0 emu/g, Hc: 0 Oe), while the CuFe2O4-NH2 Refl. sample exhibited ferromagnetic characteristics (Ms: 40 emu/g, Mr: 1.35 emu/g, Hc: 30 Oe). Both samples produced comparable results during in vitro MRI measurements, showing similar T2* relaxation and signal characteristics. Further in vivo studies demonstrated that both samples induced significant hypointense changes. The study provides valuable insights into the synthesis, properties, and potential applications of these materials, emphasizing the importance of eco-friendly methods and the optimization of ferrite-based MRI contrast agents.
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publisher Public Library of Science (PLoS)
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spelling doaj-art-4e7b7d0187d34b5586e971c2c78b96c82025-02-12T05:30:55ZengPublic Library of Science (PLoS)PLoS ONE1932-62032025-01-01202e031622110.1371/journal.pone.0316221Solvothermal synthesis of polyvinyl pyrrolidone encapsulated, amine-functionalized copper ferrite and its use as a magnetic resonance imaging contrast agent.Fatemeh HeydariÁgnes M IlosvaiNoémi KovácsDomokos MáthéFerenc KristályLajos DarócziZoltán KaletaBéla ViskolczMiklós NagyLászló VanyorekLászló ForgáchKrisztián SzigetiCopper ferrite nanoparticles for use as MRI contrast agents were synthesized using two different methods. A novel microwave-assisted (MW) solvothermal method was developed and compared to a conventional 12-hour synthesis (Reflux) as an eco-friendlier approach. This innovative synthesis method successfully produced nanoparticles with enhanced properties compared to traditional ferrite materials. The nanoparticles' morphological and magnetic properties were evaluated and tested in in-vivo MRI studies. The results revealed both similarities and differences between the amine-functionalized copper ferrite nanoparticles. FTIR, XRD, HRTEM, and VSM analyses indicated improved properties in the CuFe2O4-NH2 MW particles, while AFM confirmed successful polymer encapsulation of the nanoparticles. For the CuFe2O4-NH2 MW sample, 76.8 wt% copper ferrite and 23.2 wt% magnetite were detected, with crystallite sizes of 8 ± 2 nm and 13 ± 2 nm, respectively. In the CuFe2O4-NH2 Refl. sample, in addition to these two magnetic phases, larger copper particles (31.6 wt%) were also formed. DLS analysis demonstrated that the CuFe2O4-NH2 MW sample exhibited excellent colloidal stability, maintaining its size distribution in aqueous media for 3 hours without aggregation, unlike the CuFe2O4-NH2 Refl. sample, which showed slight aggregation. The CuFe2O4-NH2 MW sample displayed superparamagnetic behavior (Ms: 15 emu/g, Mr: 0 emu/g, Hc: 0 Oe), while the CuFe2O4-NH2 Refl. sample exhibited ferromagnetic characteristics (Ms: 40 emu/g, Mr: 1.35 emu/g, Hc: 30 Oe). Both samples produced comparable results during in vitro MRI measurements, showing similar T2* relaxation and signal characteristics. Further in vivo studies demonstrated that both samples induced significant hypointense changes. The study provides valuable insights into the synthesis, properties, and potential applications of these materials, emphasizing the importance of eco-friendly methods and the optimization of ferrite-based MRI contrast agents.https://doi.org/10.1371/journal.pone.0316221
spellingShingle Fatemeh Heydari
Ágnes M Ilosvai
Noémi Kovács
Domokos Máthé
Ferenc Kristály
Lajos Daróczi
Zoltán Kaleta
Béla Viskolcz
Miklós Nagy
László Vanyorek
László Forgách
Krisztián Szigeti
Solvothermal synthesis of polyvinyl pyrrolidone encapsulated, amine-functionalized copper ferrite and its use as a magnetic resonance imaging contrast agent.
PLoS ONE
title Solvothermal synthesis of polyvinyl pyrrolidone encapsulated, amine-functionalized copper ferrite and its use as a magnetic resonance imaging contrast agent.
title_full Solvothermal synthesis of polyvinyl pyrrolidone encapsulated, amine-functionalized copper ferrite and its use as a magnetic resonance imaging contrast agent.
title_fullStr Solvothermal synthesis of polyvinyl pyrrolidone encapsulated, amine-functionalized copper ferrite and its use as a magnetic resonance imaging contrast agent.
title_full_unstemmed Solvothermal synthesis of polyvinyl pyrrolidone encapsulated, amine-functionalized copper ferrite and its use as a magnetic resonance imaging contrast agent.
title_short Solvothermal synthesis of polyvinyl pyrrolidone encapsulated, amine-functionalized copper ferrite and its use as a magnetic resonance imaging contrast agent.
title_sort solvothermal synthesis of polyvinyl pyrrolidone encapsulated amine functionalized copper ferrite and its use as a magnetic resonance imaging contrast agent
url https://doi.org/10.1371/journal.pone.0316221
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