Synthesis, Characterization and In Vitro Study of Synthetic and Bovine-Derived Hydroxyapatite Ceramics: A Comparison
Abstract
:1. Introduction
2. Material and Methods
2.1. Sample Preparation
2.2. Sample Characterization
2.2.1. Powder Size Distribution, Chemical Composition and Microstructure of Ceramics
2.2.2. Mechanical Properties
2.2.3. Structural Characteristics
2.3. Biocompatibility Assessment
2.3.1. Simulated Body Fluid (SBF) Immersion
2.3.2. Cell Culture and Exposure
- Cell mitochondrial activity
- Cytotoxicity determination
- Statistical analysis
3. Results and Discussion
3.1. Microstructure
3.2. Structural Analysis
3.2.1. Crystallographic Details (XRD)
3.2.2. Raman Spectroscopy
3.3. In Vitro Assessment in SBF
3.4. In Vitro Assessment in Cell Culture
4. Conclusions
- The in-house developed processing route allowed obtaining highly crystalline HAp from bovine bone. The Na+ and Mg2+ ions intrinsically presented in BHAp seem to influence the sintering behavior evolving to ceramics with lower porosity and coarser microstructure compared to those obtained with synthetic HAp.
- At the structural level, the main differences between the BHAp and CHAp consist in an increase in the orientation degree of a,b-plane and the contraction of a lattice parameter of HAp unit cell. These differences are related to the BHAp source which may have a positive effect in the in vitro performance, quantifiable at longer immersion periods.
- Despite the clear structural differences between BHAp and CHAp at the unit cell level, the hydroxyapatite obtained from bovine bones has comparable in vitro behavior with the commercial one. This result is very significant considering the positive cost/benefit ratio from BHAp and thus can be used with no restrictions for biomedical applications in the same way as CHAp.
Acknowledgments
Author Contributions
Conflicts of Interest
References
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Sample (Sintered at 1200 °C) | Open Porosity (%) | Vickers Hardness (HV) | Grain Size (µm) |
---|---|---|---|
BHAp green sample | 35.04 ± 0.08 | ----- | ----- |
BHAp 2 h | 16.06 ± 0.25 | 227.78 ± 28.80 | 1.18 ± 0.14 |
BHAp 4 h | 12.09 ± 1.12 | 332.30 ± 77.40 | 1.53 ± 0.18 |
CHAp green sample | 35.11 ± 0.23 | ---- | ----- |
CHAp 2 h | 30.40 ± 2.85 | 80.21 ± 10.46 | 0.72 ± 0.06 |
CHAp 4 h | 27.17 ± 0.39 | 109.40 ± 19.70 | 0.89 ± 0.06 |
Source | Sample | a (Å) | c (Å) | Volume (Å3) | Ca/P Rietveld | Ca/P ICP | χ2 |
---|---|---|---|---|---|---|---|
Theoretical | 9.432 | 6.881 | 528.8 | 1.67 | - | - | |
BHAp | Powder | 9.423 | 6.886 | 529.8 | 1.60 | 1.57 | 2.61 |
2h | 9.421 | 6.891 | 529.6 | 1.63 | --- | 1.75 | |
4h | 9.420 | 6.885 | 529.1 | 1.59 | --- | 2.15 | |
CHAp | Powder | 9.426 | 6.893 | 530.4 | 1.66 | 1.63 | 2.25 |
2h | 9.425 | 6.894 | 530.4 | 1.69 | --- | 2.45 | |
4h | 9.425 | 6.892 | 530.2 | 1.65 | --- | 2.36 |
Element | BHAp (ppm) | CHAp (ppm) | Values accepted ISO 13779-1:2008 (ppm) |
---|---|---|---|
As | 0.00 | 0.09 | <3 |
Cd | 0.00 | 0.00 | <5 |
Pb | 0.02 | 0.03 | <30 |
Hg | 0.00 | 0.00 | <5 |
Assignment | Reported [33,34,35,36] | Experimental Values (Powders) | |||||
---|---|---|---|---|---|---|---|
Stoichiometric HAp | CAp Type A | Cap Type B | Bone | CaO | BHAp | CHAp | |
v1PO43− | 964 | 947 | 961 | 961 | 960 | 960 | |
957 | |||||||
v2PO43− | 433 | 440 | 432 | 432 | 429 | 427 | |
448 | 445 | 452 | 444 | 442 | |||
v3PO43− | 1029 | 1018 | 1026 | 1032 | 1026 | 1026 | |
1034 | 1033 | ||||||
1041 | 1038 | ||||||
1048 | 1031 | 1047 | 1044 | 1045 | 1045 | ||
1057 | 1053 | ||||||
1064 | 1064 | ||||||
1077 | 1059 | 1070 | 1071 | 1072 | 1074 | ||
v4PO43−> | 580 | 579 | 579 | 584 | 579 | 577 | |
591 | 589 | 590 | 590 | 589 | 589 | ||
607 | 608 | 609 | 611 | 605 | 604 | ||
614 | 613 | ||||||
Type A v1CO32− | 1107 | 1103 | 1109 | ||||
OH stretch | 3573 | 3576 | NO | 3571 | 3570 | ||
CaO | 1500 | 1500 | |||||
1550 | 1545 | ||||||
1772 | 1771 | ||||||
1935 | 1930 |
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Rincón-López, J.A.; Hermann-Muñoz, J.A.; Giraldo-Betancur, A.L.; De Vizcaya-Ruiz, A.; Alvarado-Orozco, J.M.; Muñoz-Saldaña, J. Synthesis, Characterization and In Vitro Study of Synthetic and Bovine-Derived Hydroxyapatite Ceramics: A Comparison. Materials 2018, 11, 333. https://doi.org/10.3390/ma11030333
Rincón-López JA, Hermann-Muñoz JA, Giraldo-Betancur AL, De Vizcaya-Ruiz A, Alvarado-Orozco JM, Muñoz-Saldaña J. Synthesis, Characterization and In Vitro Study of Synthetic and Bovine-Derived Hydroxyapatite Ceramics: A Comparison. Materials. 2018; 11(3):333. https://doi.org/10.3390/ma11030333
Chicago/Turabian StyleRincón-López, July Andrea, Jennifer Andrea Hermann-Muñoz, Astrid Lorena Giraldo-Betancur, Andrea De Vizcaya-Ruiz, Juan Manuel Alvarado-Orozco, and Juan Muñoz-Saldaña. 2018. "Synthesis, Characterization and In Vitro Study of Synthetic and Bovine-Derived Hydroxyapatite Ceramics: A Comparison" Materials 11, no. 3: 333. https://doi.org/10.3390/ma11030333