In vitro degradation and multi-antibacterial mechanisms of β-cyclodextrin@curcumin embodied Mg(OH)2/MAO coating on AZ31 magnesium alloy

doi:10.1016/j.jmst.2022.04.053

Abstract

Abstract:

It is a challenging task to prepare a coating on Mg alloys for desirable corrosion resistance, good antibacterial ability and biocompatibility. In this research work, an in-situ Mg(OH)₂ coating incorporated with sodium alginate (SA) and β-cyclodextrin (β-CD)@curcumin (Cur) was formed on the surface of micro arc oxidation (MAO) coated AZ31 alloy via a low temperature hydrothermal method. Characterization techniques such as X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), Fourier transform infrared spectrometer (FT-IR) and scanning electron microscope (SEM) were employed to characterize the chemical composition and surface morphology of the coatings. The corrosion protection ability of the coatings was monitored via electrochemical polarization, hydrogen evolution and immersion tests. Photothermal antibacterial ability and cytocompatibility of the coatings were evaluated by plate counting method under the irradiation of 808 nm-near infrared light, in vitro cytotoxicity tests (MTT) and live/dead cell staining. The results indicate that a chelation of the organic molecules led to the formation of a MAO/(β-CD@Cur)-SA-Mg(OH)₂ coating with excellent corrosion protection, multi- antibacterial ability and almost no toxicity to the cells. Especially, the coating provided photothermal performance through the light absorption of Cur, which was encapsulated by β-CD to improve its bioavailability. SA enhanced the binding force between the drug and the substrate. This novel coating designated the potential application on bioabsorbable magnesium alloys.

Key words: Magnesium alloys, Photothermal ability, Antibacterial coating, Corrosion, Biomaterials

Kui Xue, Pei-Hong Tan, Ze-Hui Zhao, Lan-Yue Cui, M Bobby Kannan, Shuo-Qi Li, Cheng-Bao Liu, Yu-Hong Zou, Fen Zhang, Zhuo-Yuan Chen, Rong-Chang Zeng. In vitro degradation and multi-antibacterial mechanisms of β-cyclodextrin@curcumin embodied Mg(OH)₂/MAO coating on AZ31 magnesium alloy[J]. J. Mater. Sci. Technol., 2023, 132: 179-192.

Figures/Tables 14

Fig. 1. Schematic of the preparation process of the MAO/(β-CD@Cur)-SA-Mg(OH)2 coating.

Fig. 2. SEM images of (a, b) MAO and (c, d) MAO/(β-CD@Cur)-SA-Mg(OH)2 coatings (insert in a and c are macrographs); (e) elemental contents of the two coatings; cross-sectional image of the (f) MAO, (h) MAO/(β-CD@Cur)-SA-Mg(OH)2 coatings and their C mapping (g, i).

Fig. 3. (a) FT-IR spectra of the MAO, MAO/(β-CD@Cur)-SA-Mg(OH)2 coatings, pure Cur, β-CD, and SA; (b) XRD patterns of the MAO and MAO/(β-CD@Cur)-SA-Mg(OH)2 coatings; (c) XPS overview spectra of the MAO and MAO/(β-CD@Cur)-SA-Mg(OH)2 coatings; detailed regions of Mg 1 s and O 1 s for (e, f) MAO and (g, h) MAO/(β-CD@Cur)-SA-Mg(OH)2 coatings; (i) acoustic signal and frictional force of the MAO/(β-CD@Cur)-SA-Mg(OH)2 coating.

Fig. 4. SEM images of the MAO/(β-CD@Cur)-SA-Mg(OH)2 coating with 0, 20, 40, 60, 120, 180, 240 and 1440 min hydrothermal treatments.

Fig. 5. (a-c) Nyquist plots, (d) bode and bode phase angle plots (e) potentiodynamic polarization curves of AZ31, MAO and MAO/(β-CD@Cur)-SA-Mg(OH)2 coatings; and corresponding EC models for (f) AZ31; (g) MAO and MAO/(β-CD@Cur)-SA-Mg(OH)2 coatings.

Fig. 6. (a) HER curves and (b) XRD patterns of AZ31 alloy, MAO and MAO/(β-CD@Cur)-SA-Mg(OH)2 coatings; microscopic and macroscopic morphology of (c) AZ31 alloy, (d) MAO and (e) MAO/(β-CD@Cur)-SA-Mg(OH)2 coatings; (f) EDS atominc countent of (c, d, e) after an immersion of 468 h in Hank's solution.

Fig. 7. SEM images of MAO/(β-CD@Cur)-SA-Mg(OH)2 coating with the immersion of (a) 0 h, (b) 150 h and (c) 350 h, and the correspongding (d) EDS spectra of (a-c); (e) FT-IR sepectra and (f) XRD patterns of the samples after an immersion of 0 h, 150 h and 350 h.

Fig. 8. (a) Photothermal heating curves of AZ31 Mg alloy, MAO and MAO/(β-CD@Cur)-SA-Mg(OH)2 coatings in atmosphere at room temperature and in Hank's solution, (b) recycling photothermal profiles of MAO/(β-CD@Cur)-SA-Mg(OH)2 coating for six on/off cycles. (c) ultraviolet spectrum of AZ31 substrate, MAO and MAO/(β-CD@Cur)-SA-Mg(OH)2 coatings; Infrared photography of (d) AZ31 substrate, (e) MAO coating, (f) MAO/(β-CD@Cur)-SA-Mg(OH)2 coating in atmosphere and (g) AZ31 substrate, (h) MAO coating, (i) MAO/(β-CD@Cur)-SA-Mg(OH)2 coating in Hank's solution after NIR irradiation. All tests were carried out under irradiation of 808 nm NIR laser (1.0 W cm?2).

Fig. 9. (a) Antibacterial rate of the samples against S. aureus and E. coli in dark and after exposure to 808 nm NIR for 30 min (n = 3, p* <0.05, p?? < 0.01, p??? < 0.001, p???? < 0.0001); (b) pH value of the bacterial solution during the antibacterial test; (c) coresponding photographs of bacterial colonies.

Fig. 10. SEM images of E. coli and S. aureus under dark or NIR irradition after co-cultureed with (a-d) AZ31 substrate, (e-h) MAO and (i-l) MAO/(β-CD@Cur)-SA-Mg(OH)2 coatings.

Fig. 11. (a) Cell viability of MC3T3-E1 cells incubated for 24 and 72 h of negative control, AZ31.

Table 1. Research of antibacterial coating on magnesium alloy surface and some photothermal antibacterial method.

Coating/Particles	Antibacterial factor	Antibacterial rate (%)	Shortcoming	Corrosion resisitance (i_corr)
Mg-Ag [49]	Ag	90%	corrosion	Easily corrosion
Mg-MAO@Cu [50]	Cu	95%	corroison	Increase
MAO/CHI [51]	CHI	weaker	antibacterial ability	Increase (2.48×10⁻⁵ →6.71×10⁻⁶)
MAO@TA [15]	TA	92%	antibacterial ability	Increase (1.47×10⁻⁵→5.22×10⁻⁷)
MAO/CIP-PMTMS [39]	CIP	99%	drug resistance	Increase (1.61×10⁻⁵→7.13×10⁻⁸)
GS/PAH/PAA [52]	GS	99.49%	drug resistance, burst release	Increase (8.01×10⁻⁶→3.67×10⁻⁷)
melanosome [24]	lysozyme	97.90%	/	/
Zn-doped prussian blue [53]	Zinc-doped Prussian blue	98.42%	/	/
graphene oxidemodified porous TiO₂ [55]	Photothermal(graphene)	∼ 90%	/	/
polydopamine nanocoating [54]	Photothermal (polydopamine)	96% (S. aureus), 84% (E. coli), 93% (C. albicans)	/	/
MAO/(β-CD@Cur)-SA-Mg(OH)₂ coating	Photothermal (Curcumin)	99.95% (S.aureus), 98.82% (E.coli)	/	Increase (2.19×10⁻⁵→5.35×10⁻⁹)

Fig. 12. Chart of MAO/(β-CD@Cur)-SA-Mg(OH)2 coating formation mechanism.

Fig. 13. Chart of MAO/(β-CD@Cur)-SA-Mg(OH)2 coating antibacterial mechanism.

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In vitro degradation and multi-antibacterial mechanisms of β-cyclodextrin@curcumin embodied Mg(OH)₂/MAO coating on AZ31 magnesium alloy

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