Abstract

Calcium phosphate bone cements (CPCs) with antibacterial properties are demanded for clinical applications. In this study, we demonstrated the use of a relatively simple processing route based on preparation of silver-doped CPCs (CPCs-Ag) through the preparation of solid dispersed active powder phase. Real-time monitoring of structural transformations and kinetics of several CPCs-Ag formulations (Ag = 0 wt %, 0.6 wt % and 1.0 wt %) was performed by the Energy Dispersive X-ray Diffraction technique. The partial conversion of β-tricalcium phosphate (TCP) phase into the dicalcium phosphate dihydrate (DCPD) took place in all the investigated cement systems. In the pristine cement powders, Ag in its metallic form was found, whereas for CPC-Ag 0.6 wt % and CPC-Ag 1.0 wt % cements, CaAg(PO3)3 was detected and Ag (met.) was no longer present. The CPC-Ag 0 wt % cement exhibited a compressive strength of 6.5 ± 1.0 MPa, whereas for the doped cements (CPC-Ag 0.6 wt % and CPC-Ag 1.0 wt %) the reduced values of the compressive strength 4.0 ± 1.0 and 1.5 ± 1.0 MPa, respectively, were detected. Silver-ion release from CPC-Ag 0.6 wt % and CPC-Ag 1.0 wt % cements, measured by the Atomic Emission Spectroscopy, corresponds to the average values of 25 µg/L and 43 µg/L, respectively, rising a plateau after 15 days. The results of the antibacterial test proved the inhibitory effect towards pathogenic Escherichia coli for both CPC-Ag 0.6 wt % and CPC-Ag 1.0 wt % cements, better performances being observed for the cement with a higher Ag-content.

Highlights

  • Calcium phosphate bone cements (CPCs) are widely used for bone graft substitution due to their chemical similarity to the bone mineral part

  • We demonstrated the use of a relatively simple processing route based on preparation of silver-doped CPCs (CPCs-Ag) through the preparation of Ag-containing solid dispersed active phase

  • The formation of new phases was followed in situ by the Energy Dispersive X-ray Diffraction technique (EDXRD), allowing one to obtain a 3D map of diffraction patterns, collected as a function of the scattering parameter and of time

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Summary

Introduction

Calcium phosphate bone cements (CPCs) are widely used for bone graft substitution due to their chemical similarity to the bone mineral part. The bone graft associated infections may be prevented by doping of synthetic bone grafting materials with suitable metal ions (e.g., Ag+) at low (non-cytotoxic) concentrations [9,10] This way seems to be more appropriate, because the antimicrobial activity could be provided directly at the implantation site (target delivery). The formation of new phases was followed in situ by the Energy Dispersive X-ray Diffraction technique (EDXRD), allowing one to obtain a 3D map of diffraction patterns, collected as a function of the scattering parameter and of time This technique proved to be suitable to study the real-time monitoring of the CPCs hardening process in situ [13,14,15]. The antibacterial in vitro test, using pathogenic Escherichia coli, was performed to prove the inhibitory effect of the Ag-containing cement formulations

Synthesis of Silver-Doped Tricalcium Phosphate Powders
Hardening Liquid Preparation
Preparation of CPCs-Ag Specimens
Setting Time Measurements
Energy Dispersive X-ray Diffraction
Scanning Electron Microscopy
Compressive Strength Measurements
Silver-Ion Release
2.10. Antibacterial Test
Results and Discussion
Conclusions
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