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. 2022 Aug 4;15(15):5372.
doi: 10.3390/ma15155372.

Impact of Gamma Irradiation on the Properties of Magnesium-Doped Hydroxyapatite in Chitosan Matrix

Daniela Predoi  1 , Carmen Steluta Ciobanu  1 , Simona Liliana Iconaru  1 , Silviu Adrian Predoi  2   3   4 , Mariana Carmen Chifiriuc  4   5   6 , Steinar Raaen  7 , Monica Luminita Badea  1   8 , Krzysztof Rokosz  9
Affiliations

Impact of Gamma Irradiation on the Properties of Magnesium-Doped Hydroxyapatite in Chitosan Matrix

Daniela Predoi et al. Materials (Basel). .

Abstract

This is the first report regarding the effect of gamma irradiation on chitosan-coated magnesium-doped hydroxyapatite (xMg = 0.1; 10 MgHApCh) layers prepared by the spin-coating process. The stability of the resulting 10 MgHApCh gel suspension used to obtain the layers has been shown by ultrasound measurements. The presence of magnesium and the effect of the irradiation process on the studied samples were shown by X-ray photoelectron spectroscopy (XPS). The XPS results obtained for irradiated 10 MgHApCh layers suggested that the magnesium and calcium contained in the surface layer are from tricalcium phosphate (TCP; Ca3(PO4)2) and hydroxyapatite (HAp). The XPS analysis has also highlighted that the amount of TCP in the surface layer increased with the irradiation dose. The energy-dispersive X-ray spectroscopy (EDX) evaluation showed that the calcium decreases with the increase in the irradiation dose. In addition, a decrease in crystallinity and crystallite size was highlighted after irradiation. By atomic force microscopy (AFM) we have obtained images suggesting a good homogeneity of the surface of the non-irradiated and irradiated layers. The AFM results were also sustained by the scanning electron microscopy (SEM) images obtained for the studied samples. The effect of gamma-ray doses on the Fourier transform infrared spectroscopy (ATR-FTIR) spectra of 10 MgHApCh composite layers was also evaluated. The in vitro antifungal assays proved that 10 MgHApCh composite layers presented a strong antifungal effect, correlated with the irradiation dose and incubation time. The study of the stability of the 10 MgHApCh gel allowed us to achieve uniform and homogeneous layers that could be used in different biomedical applications.

Keywords: antifungal activity; chitosan; gamma irradiation; hydroxyapatite; magnesium.

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Conflict of interest statement

The authors declare no conflict of interest. The funders had no role in the design of the study; in the collection, analyses, or interpretation of data; in the writing of the manuscript; or in the decision to publish the results.

Figures

Figure 1
Figure 1
Frequency spectrums for the tested sample (superposing all spectrums) and the reference liquid.
Figure 2
Figure 2
Relative spectral amplitudes of the tested samples.
Figure 3
Figure 3
Time averaged attenuation for the 1000 samples in the selected frequency range.
Figure 4
Figure 4
XRD patterns of 10 MgHApCh-0 (a), 10 MgHApCh-3 (b) and 10 MgHApCh-6 (c) samples.
Figure 5
Figure 5
SEM images obtained on Si (a), 10 MgHApCh-0 (b), 10 MgHApCh-3 (c), and 10 MgHApCh-6 (d) thin films.
Figure 6
Figure 6
SEM images of transversal cross section of 10 MgHApCh-0 (a), 10 MgHApCh-3 (b), and 10 MgHApCh-6 (c) thin films.
Figure 7
Figure 7
Elemental distribution cartographies of constituent chemical elements along with EDX spectra of 10 MgHApCh-0 thin films.
Figure 8
Figure 8
EDX spectra of 10 MgHApCh-3 (a) and 10 MgHApCh-6 (b) thin films.
Figure 9
Figure 9
2D AFM topographies of 10 MgHApCh-0 (a), 10 MgHApCh-3 (c) and 10 MgHApCh-6 (e) composite layers and their 3D representations (b,d,f).
Figure 10
Figure 10
XPS survey results of 10 MgHApCh-0 (a), 10 MgHApCh-3 (b), and 10 MgHApCh-6 (c).
Figure 11
Figure 11
High-resolution XPS spectra for Ca 2p, P2p, and O 1 s spectra of 10 MgHApCh-0 (a), 10 MgHApCh-3 (b), and 10 MgHApCh-6 (c) layers.
Figure 12
Figure 12
XPS high resolution spectra of Mg 1 s and Mg KLL of 10 MgHApCh-0 (a), 10 MgHApCh-3 (b), and 10 MgHApCh-6 (c) layers.
Figure 13
Figure 13
ATR-FTIR spectra of 10 MgHApCh thin films (a) and second-derivative spectra obtained for 10 MgHApCh-0 (b), 10 MgHApCh-3 (c), and 10 MgHApCh-6 (d) thin films.
Figure 14
Figure 14
2D AFM surface topography of Candida albicans ATCC 10231 cell development on Si discs, 10 MgHApCh-0, 10 MgHAp-Ch-3, and 10 MgHAp-Ch-6 composite layers after 24 h, 48 h, and 72 h of incubation collected on an area of 25 × 25 µm2.
Figure 15
Figure 15
3D representation of AFM surface topography of Candida albicans ATCC 10231 cell development on Si discs, 10 MgHApCh-0, 10 MgHAp-Ch-3, and 10 MgHAp-Ch-6 composite layers after 24 h, 48 h, and 72 h of incubation collected on an area of 25 × 25 µm2.
Figure 16
Figure 16
2D CLSM images of Candida albicans ATCC 10231 cell development on Si discs (a,e,i), 10 MgHApCh-0 (b,f,j), 10 MgHApCh-3 (c,g,k), and 10 MgHApCh-6 (d,h,l) coatings after 24, 48, and 72 h of incubation.
Figure 17
Figure 17
The graphical representation of the antimicrobial activity of Si discs, 10 MgHApCh-0, 10 MgHApCh-3, and 10 MgHApCh-6 composite layers against C. albicans (ATCC® 10231) fungal cells after 24, 48, and 72 h of incubation.
See this image and copyright information in PMC

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