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J Funct Biomater
2018 Dec 02;94:. doi: 10.3390/jfb9040069.
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Development of Phosphatized Calcium Carbonate Biominerals as Bioactive Bone Graft Substitute Materials, Part I: Incorporation of Magnesium and Strontium Ions.
Sethmann I
,
Luft C
,
Kleebe HJ
.
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Synthetic materials based on calcium phosphate (CaP) are frequently used as bone graft substitutes when natural bone grafts are not available or not suitable. Chemical similarity to bone guarantees the biocompatibility of synthetic CaP materials, whereas macroporosity enables their integration into the natural bone tissue. To restore optimum mechanical performance after the grafting procedure, gradual resorption of CaP implants and simultaneous replacement by natural bone is desirable. Mg and Sr ions released from implants support osteointegration by stimulating bone formation. Furthermore, Sr ions counteract osteoporotic bone loss and reduce the probability of related fractures. The present study aimed at developing porous Ca carbonate biominerals into novel CaP-based, bioactive bone implant materials. Macroporous Ca carbonate biominerals, specifically skeletons of corals (aragonite) and sea urchins (Mg-substituted calcite), were hydrothermally converted into pseudomorphic CaP materials with their natural porosity preserved. Sr ions were introduced to the mineral replacement reactions by temporarily stabilizing them in the hydrothermal phosphate solutions as Sr-EDTA complexes. In this reaction system, Na, Mg, and Sr ions favored the formation of correspondingly substituted β-tricalcium phosphate over hydroxyapatite. Upon dissolution, the incorporated functional ions became released, endowing these CaP materials with bioactive and potentially osteoporotic properties.
Figure 1. Characterization of the starting materials. (a) Porous skeleton of the coral Porites sp. (scanning electron microscopy-backscatter electron (SEM-BSE)); (b) fracture surface of the coral material revealing the internal microstructure (SEM-BSE); (c) chemical composition of the coral skeleton (energy-dispersive X-ray spectroscopy (EDS)); (d) XRD pattern of the coral skeleton corresponding to that of aragonite (PDF 00-041-1475) (XRD raw data S1: C14); (e) porous material of a spine of the sea urchin Heterocentrotus mamillatus (SEM-BSE); (f) fracture surface of the sea urchin material showing a massive internal structure (SEM-BSE); (g) chemical composition of the sea urchin spine (EDS); (h) XRD pattern of the of the sea urchin spine corresponding to that of Mg calcite (PDF 00-043-0697) (XRD raw data S2: SU1).
Figure 2. Hydrothermally phosphatized coral skeleton. (a) Aragonite skeleton partly converted into pseudomorphic hydroxyapatite (HA) (SEM-BSE); (b) a fractured trabecula showing the native, fibrous Ca carbonate microstructure (CC, darker shading), partly converted into microcrystalline HA (lighter shading) (SEM-BSE); (c) chemical composition of the phosphatized material (EDS); (d) mineral phases contained in the partly phosphatized coral material identified by XRD: aragonite (50 wt %, PDF 00-041-1475), hydroxyapatite (45 wt %, PDF 00-009-0432), calcite (5 wt %, PDF 00-047-1743); XRD raw data S4: C3.
Figure 3. Hydrothermally phosphatized sea urchin spine. (a) Mg calcite scaffold partly converted into phosphatic material (SEM-BSE); (b) a fractured trabecula showing the microgranular and microporous structure of the pseudomorphic phosphate material (SEM-BSE); (c) chemical composition of the Na- and Mg-bearing phosphatized material (EDS); (d) mineral phases contained in the partly phosphatized sea urchin material identified by XRD: Mg-calcite (35 wt %, PDF 00-043-0697), merrillite (40 wt %, PDF 01-076-8368), hydroxyapatite (25 wt %, PDF 00-009-0432); XRD raw data S5: SU3.
Figure 4. Phosphatized and Sr-modified coral skeleton. (a) Aragonite skeleton partly converted into pseudomorphic phosphate material (SEM-BSE); (b) a fractured trabecula showing the microcrystalline structure of the phosphate material in the interior (darker shading) and a surface layer of small crystals (see inset) with heavier elements (lighter shading) (SEM-BSE); (c) chemical composition of the surface material (EDS); (d) chemical composition of the phosphatized bulk material (EDS); (e) crystalline phases contained in the partly phosphatized and Sr-modified coral material, identified using XRD (aragonite (PDF 00-041-1475), hydroxyapatite (PDF 00-009-0432), Sr-substituted β-TCP [78]); XRD raw data S6: C32.
Figure 5. Phosphatized and Sr-modified sea urchin spine. (a) Mg calcite scaffold partly converted into pseudomorphic phosphate material (SEM-BSE); (b) a fractured trabecula showing the microcrystalline and microporous structure of the phosphate material in the interior (darker shading) and rose-like aggregates of phosphate crystals containing heavier elements (lighter shading) grown on the surface (see inset) (SEM-BSE); (c) chemical composition of a rose-shaped crystal aggregate on the material surface (EDS); (d) chemical composition of the phosphatized bulk material (EDS); (e) mineral phases contained in the partly phosphatized and Sr-modified sea urchin material, identified by XRD (Mg-calcite (PDF 00-043-0697), merrillite (PDF 01-076-8368), hydroxyapatite (PDF 00-009-0432)); XRD raw data S7: SU24.
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