Magnetic Resonance-Based Analytical Tools to Study Polyvinylpyrrolidone–Hydroxyapatite Composites

The synthesis of biocompatible and bioresorbable composite materials, such as a “polymer matrix-mineral constituent,” stimulating the natural growth of living tissues and the restoration of damaged parts of the body, is one of the challenging problems in regenerative medicine and materials science....

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Main Authors: Alina Petrova, Georgy Mamin, Oleg Gnezdilov, Inna Fadeeva, Olga Antonova, Anna Forysenkova, Iulian V. Antoniac, Julietta V. Rau, Marat Gafurov
Format: Article
Language:English
Published: MDPI AG 2023-11-01
Series:Polymers
Subjects:
Online Access:https://www.mdpi.com/2073-4360/15/22/4445
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author Alina Petrova
Georgy Mamin
Oleg Gnezdilov
Inna Fadeeva
Olga Antonova
Anna Forysenkova
Iulian V. Antoniac
Julietta V. Rau
Marat Gafurov
author_facet Alina Petrova
Georgy Mamin
Oleg Gnezdilov
Inna Fadeeva
Olga Antonova
Anna Forysenkova
Iulian V. Antoniac
Julietta V. Rau
Marat Gafurov
author_sort Alina Petrova
collection DOAJ
description The synthesis of biocompatible and bioresorbable composite materials, such as a “polymer matrix-mineral constituent,” stimulating the natural growth of living tissues and the restoration of damaged parts of the body, is one of the challenging problems in regenerative medicine and materials science. Composite films of bioresorbable polymer of polyvinylpyrrolidone (PVP) and hydroxyapatite (HA) were obtained. HA was synthesized in situ in the polymer solution. We applied electron paramagnetic resonance (EPR) and nuclear magnetic resonance (NMR) approaches to study the composite films’ properties. The application of EPR in two frequency ranges allowed us to derive spectroscopic parameters of the nitrogen-based light and radiation-induced paramagnetic centers in HA, PVP and PVP-HA with high accuracy. It was shown that PVP did not significantly affect the EPR spectral and relaxation parameters of the radiation-induced paramagnetic centers in HA, while light-induced centers were detected only in PVP. Magic angle spinning (MAS) <sup>1</sup>H NMR showed the presence of two signals at 4.7 ppm and −2.15 ppm, attributed to “free” water and hydroxyl groups, while the single line was attributed to <sup>31</sup>P. NMR relaxation measurements for <sup>1</sup>H and <sup>31</sup>P showed that the relaxation decays were multicomponent processes that can be described by three components of the transverse relaxation times. The obtained results demonstrated that the applied magnetic resonance methods can be used for the quality control of PVP-HA composites and, potentially, for the development of analytical tools to follow the processes of sample treatment, resorption, and degradation.
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spelling doaj.art-68517d05c15a44ec871313328758d1122023-11-24T15:02:39ZengMDPI AGPolymers2073-43602023-11-011522444510.3390/polym15224445Magnetic Resonance-Based Analytical Tools to Study Polyvinylpyrrolidone–Hydroxyapatite CompositesAlina Petrova0Georgy Mamin1Oleg Gnezdilov2Inna Fadeeva3Olga Antonova4Anna Forysenkova5Iulian V. Antoniac6Julietta V. Rau7Marat Gafurov8Institute of Physics, Kazan Federal University, Kremlyovskaya St.18, 420008 Kazan, RussiaInstitute of Physics, Kazan Federal University, Kremlyovskaya St.18, 420008 Kazan, RussiaInstitute of Physics, Kazan Federal University, Kremlyovskaya St.18, 420008 Kazan, RussiaA.A. Baikov Institute of Metallurgy and Material Science, Russian Academy of Sciences, Leninsky Avenue 49, 119334 Moscow, RussiaA.A. Baikov Institute of Metallurgy and Material Science, Russian Academy of Sciences, Leninsky Avenue 49, 119334 Moscow, RussiaA.A. Baikov Institute of Metallurgy and Material Science, Russian Academy of Sciences, Leninsky Avenue 49, 119334 Moscow, RussiaFaculty of Material Science and Engineering, National University of Science and Technology Politehnica Bucharest, 313 Splaiul Independentei Street, District 6, 060042 Bucharest, RomaniaIstituto di Struttura della Materia, Consiglio Nazionale delle Ricerche (ISM-CNR), Via del Fosso del Cavaliere, 100, 00133 Rome, ItalyInstitute of Physics, Kazan Federal University, Kremlyovskaya St.18, 420008 Kazan, RussiaThe synthesis of biocompatible and bioresorbable composite materials, such as a “polymer matrix-mineral constituent,” stimulating the natural growth of living tissues and the restoration of damaged parts of the body, is one of the challenging problems in regenerative medicine and materials science. Composite films of bioresorbable polymer of polyvinylpyrrolidone (PVP) and hydroxyapatite (HA) were obtained. HA was synthesized in situ in the polymer solution. We applied electron paramagnetic resonance (EPR) and nuclear magnetic resonance (NMR) approaches to study the composite films’ properties. The application of EPR in two frequency ranges allowed us to derive spectroscopic parameters of the nitrogen-based light and radiation-induced paramagnetic centers in HA, PVP and PVP-HA with high accuracy. It was shown that PVP did not significantly affect the EPR spectral and relaxation parameters of the radiation-induced paramagnetic centers in HA, while light-induced centers were detected only in PVP. Magic angle spinning (MAS) <sup>1</sup>H NMR showed the presence of two signals at 4.7 ppm and −2.15 ppm, attributed to “free” water and hydroxyl groups, while the single line was attributed to <sup>31</sup>P. NMR relaxation measurements for <sup>1</sup>H and <sup>31</sup>P showed that the relaxation decays were multicomponent processes that can be described by three components of the transverse relaxation times. The obtained results demonstrated that the applied magnetic resonance methods can be used for the quality control of PVP-HA composites and, potentially, for the development of analytical tools to follow the processes of sample treatment, resorption, and degradation.https://www.mdpi.com/2073-4360/15/22/4445polyvinylpyrrolidonehydroxyapatitecompositesNMREPR
spellingShingle Alina Petrova
Georgy Mamin
Oleg Gnezdilov
Inna Fadeeva
Olga Antonova
Anna Forysenkova
Iulian V. Antoniac
Julietta V. Rau
Marat Gafurov
Magnetic Resonance-Based Analytical Tools to Study Polyvinylpyrrolidone–Hydroxyapatite Composites
Polymers
polyvinylpyrrolidone
hydroxyapatite
composites
NMR
EPR
title Magnetic Resonance-Based Analytical Tools to Study Polyvinylpyrrolidone–Hydroxyapatite Composites
title_full Magnetic Resonance-Based Analytical Tools to Study Polyvinylpyrrolidone–Hydroxyapatite Composites
title_fullStr Magnetic Resonance-Based Analytical Tools to Study Polyvinylpyrrolidone–Hydroxyapatite Composites
title_full_unstemmed Magnetic Resonance-Based Analytical Tools to Study Polyvinylpyrrolidone–Hydroxyapatite Composites
title_short Magnetic Resonance-Based Analytical Tools to Study Polyvinylpyrrolidone–Hydroxyapatite Composites
title_sort magnetic resonance based analytical tools to study polyvinylpyrrolidone hydroxyapatite composites
topic polyvinylpyrrolidone
hydroxyapatite
composites
NMR
EPR
url https://www.mdpi.com/2073-4360/15/22/4445
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