Synthesis and Characterization of Synthetic and Natural Nano Hydroxyapatite Composites Containing Poloxamer Coated Demineralized Bone Matrix as Bone Graft Material: A Comparative Study

The present study aimed to developing a bone graft material containing poloxamer (P), demineralized bone matrix (DBM), and nano hydroxyapatite derived from bovine bones (NHA) or prepared via synthetic route (SHA). Thermogravimetric analysis indicates P + DBM + SHA composite to be more stable compared to the P + DBM + NHA composite. XRD results revealed better crystallinity in P + DBM + SHA compared to P + DBM + NHA. The SEM show uniform and homogenous distribution of poloxamer and DBM on the porous nano hydroxyapatite matrix. This shows that the composite P + DBM + SHA can serve as osteoinductive materials.     

羟基磷灰石和含氟羟基磷灰石涂层的制备技术

羟基磷灰石(HA)生物陶瓷涂层被认为是目前最好的用于替代人体硬组织的一种生物医用材料,具有很高的外科应用价值.含氟羟基磷灰石(FHA)涂层由于比羟基磷灰石涂层的溶解度低、热膨胀系数小且生物活性好,有着更为广泛的应用前景.对羟基磷灰石及其涂层的各种制备方法进行了概述,同时介绍了溶胶-凝胶法制备含氟羟基磷灰石涂层的技术特点,并对未来的发展前景进行了分析.     

改性HA纳米粒子在骨组织工程中的应用[ ]

羟基磷灰石(HA)具有优异的生物活性和生物相容性,广泛应用于骨修复、再生和置换等骨组织工程,但HA纳米粒子难分散、强度低、高分子相融性差等缺点限制了其应用。为了克服这些缺点,研究员致力于探索改性或复合HA的方法,以改善其分散性、亲水性、抗菌性以及机械强度等,来满足临床应用的要求。本篇综述总结归纳了当前主流的HA纳米粒子改性方法,包括离子掺杂、表面改性、材料复合等。最后,我们还讨论了当前HA复合材料的研究热点,以期为HA复合材料相关基础研究提供有益的借鉴与启示。     

Preparation and Characterization of Fluorescence Probe from Assembly Hydroxyapatite Nanocomposite

A new nanocomposite fluorescence probe with thioglycolic acid (TA) functional layers embedded inside the hydroxyapatite nanoribbon spherulites has been synthesized. The fluorescence intensity of the novel probe is about 1.5–3.3-fold increase compared with the probe containing no TA. When used to detect cadmium ion, the most of original assembly nanoribbon spherulites structure in the novel probe is found to have been damaged to new flake structures. The mechanism of determining cadmium ion in alcohol solution has been studied. The present systematic study provides significant information on the effect of assembly nanostructure on the metal-enhanced fluorescence phenomenon.     

Behaviour of bone origin hydroxyapatite at elevated temperatures and in O2 and CO2 atmospheres

In the present work the behaviour of HAp extracted from pig bones at elevated temperatures up to 1000 °C in O₂ and CO₂ atmospheres has been studied. It has been found that CO₂ atmosphere arrests HAp decomposition. Chemical analysis and infrared spectroscopy reveal that no free CaO appears and no decrease of CO₃⁻² group concentration occurs in the material calcined in CO₂ atmosphere. In the O₂ atmosphere at elevated temperatures, CaO and CO₂ are emitted from the samples, although the remaining material retains the HAp structure as indicated by the X-ray diffraction.     

Microstructural Development of Natural Hydroxyapatite Originated from Fish-Bone Waste through Heat Treatment

The morphologic and microstructural development of natural fish bone through heat treatment is examined in view of fish-waste management and as a possible route for hydroxyapatite ceramics. Fish bone heated at temperatures ≤1300°C maintains a porous structure, with a sintered wall and a major crystalline phase of hydroxyapatite. Fish-originated ceramics are potentially useful as bioactive media as well as for environmentally compatible materials.     

羟基磷灰石空心纳米球的制备及表征

采用W\O\W复乳法制备羟基磷灰石,内水相为(NH4)2HPO4水溶液,中间油相为易挥发的环己烷,外水相为Ca(NO3)2.4H2O水溶液。分析了反应中传质机理为Ca2+扩散到内水相,在碱性下与内水相的HPO42-反应生成羟基磷灰石。通过XRD、FT-IR、SEM、TEM分析了产物的成分和形貌,证实产物为300nm左右的羟基磷灰石空心球。讨论了反应温度对纳米球形貌的影响,当温度为10℃时发生界面反应,得到空心的纳米球。     

砷羟基磷灰石的水热合成与结构表征

以四水硝酸钙[Ca(NO3)2·4H2O]、磷酸氢二铵[(NH4)2HPO4]、十二水合砷酸钠[Na3AsO4·12H2O]为原料,在200℃下水热反应8h制得掺砷羟基磷灰石[Ca10(PO4)6-x(AsO4)x(OH)2].考察了反应液中不同砷含量对合成砷羟基磷灰石结构的影响.采用X射线衍射分析(XRD)、扫描电镜结合电子能谱分析(SEM/EDS)、傅立叶变换红外光谱分析(FTIR)等测试手段对产物的晶相、化学组成和形貌进行分析.结果表明:As取代部分磷(P)进入羟基磷灰石的晶格中,没有改变其晶体结构,但羟基磷灰石的晶胞参数发生了变化,随着As含量的增加,砷羟基磷灰石的晶体尺寸呈增大的趋势,晶体形状为短棒状.     

生物陶瓷多孔羟基磷灰石的合成及应用

通过对人体活性材料羟基磷灰石的研究,发现它的生物活性和相容性较好,强度适中,并且价格低,是理想的人体骨替代材料。     

Preparation and Characterization of Lanthanum-Incorporated Hydroxyapatite Coatings on Titanium Substrates

Titanium (Ti) has been widely used in clinical applications for its excellent biocompatibility and mechanical properties. However, the bioinertness of the surface of Ti has motivated researchers to improve the physicochemical and biological properties of the implants through various surface modifications, such as coatings. For this purpose, we prepared a novel bioactive material, a lanthanum-incorporated hydroxyapatite (La-HA) coating, using a dip-coating technique with a La-HA sol along with post-heat treatment. The XRD, FTIR and EDX results presented in this paper confirmed that lanthanum was successfully incorporated into the structure of HA. The La-HA coating was composed of rod-like particles which densely compacted together without microcracks. The results of the interfacial shear strength test indicated that the incorporation of lanthanum increased the bonding strength of the HA coating. The mass loss ratios under acidic conditions (pH = 5.5) suggested that the La-HA coatings have better acid resistance. The cytocompatibility of the La-HA coating was also revealed by the relative activity of alkaline phosphatase, cellular morphology and cell proliferation assay in vitro. The present study suggested that La-HA coated on Ti has promising potential for applications in the development of a new type of bioactive coating for metal implants.     

Effect of the calcination temperature on the composition and microstructure of hydroxyapatite derived from human and animal bone

The present work focus the study of cortical bone samples of different origins (human and animal) subjected to different calcination temperatures (600, 900 and 1200 °C) with regard to their chemical and structural properties. For that, not only standard techniques such as thermogravimetric analysis, Fourier transform infrared spectroscopy, X-ray diffraction and scanning electron microscopy were used but also mercury intrusion porosimetry. The latter technique was applied to evaluate the effects of the temperature on the microstructure of the calcined samples regarding porosity and pore size distribution.     

Fabrication and Characterization of Hierarchically Nanostructured Porous Carbonated Hydroxyapatite Coatings

Hierarchically nanostructured porous carbonated hydroxyapatite coatings (HNPCs) on Ti6Al4V substrate were fabricated by a two-stage application route: fabrication of nacre coatings (NCs) on Ti6Al4V substrate by electrophoretic technique, and conversion of NCs to HNPCs in a phosphate buffer solution (PBS) by microwave irradiation method. Their samples were characterized by using XRD, FT-IR, SEM, TEM, and N2 adsorption-desorption isotherms. The results show that the microwave irradiation technique improves obviously the conversion rate of NCs to HNPCs as compared with conventional method. After soaking the NCs in the PBS, calcium ions are released from the nacre particles and react with phosphate ions to form carbonated hydroxyapatite nanoparticles. These nanoparticles aggregate to form the plate-like carbonated apatite. The mesopores with a size of about 3.9 nm and macropores with the diameters of 1~4 mm exist within and among the carbonated apatite plates, respectively. Simulated body fluid immersion tests reveal that the HNPCs have a good in vitro bioactivity.     

Bioactivity and Antibacterial Behaviors of Nanostructured Lithium-Doped Hydroxyapatite for Bone Scaffold Application

The material for bone scaffold replacement should be biocompatible and antibacterial to prevent scaffold-associated infection. We biofunctionalized the hydroxyapatite (HA) properties by doping it with lithium (Li). The HA and 4 Li-doped HA (0.5, 1.0, 2.0, 4.0 wt.%) samples were investigated to find the most suitable Li content for both aspects. The synthesized nanoparticles, by the mechanical alloying method, were cold-pressed uniaxially and then sintered for 2 h at 1250 °C. Characterization using field-emission scanning electron microscopy (FE-SEM) revealed particle sizes in the range of 60 to 120 nm. The XRD analysis proved the formation of HA and Li-doped HA nanoparticles with crystal sizes ranging from 59 to 89 nm. The bioactivity of samples was investigated in simulated body fluid (SBF), and the growth of apatite formed on surfaces was evaluated using SEM and EDS. Cellular behavior was estimated by MG63 osteoblast-like cells. The results of apatite growth and cell analysis showed that 1.0 wt.% Li doping was optimal to maximize the bioactivity of HA. Antibacterial characteristics against Escherichia coli (E. coli) and Staphylococcus aureus (S. aureus) were performed by colony-forming unit (CFU) tests. The results showed that Li in the structure of HA increases its antibacterial properties. HA biofunctionalized by Li doping can be considered a suitable option for the fabrication of bone scaffolds due to its antibacterial and unique bioactivity properties.     

Mechanochemical Synthesis of Hydroxyapatite from Calcium Oxide and Brushite

Fine hydroxyapatite (HA) powders were prepared by mechanically activating a mixture of calcium oxide and brushite powders in a high-energy shaker mill. A defective HA phase was formed when the starting powder mixture was activated for ≤20 h. When the mixture was calcined at 800°C, it was converted to β-tricalcium phosphate. In contrast, a nanocrystalline HA phase was formed when the mechanical activation was extended to 30 h. The material was transformed to a HA compound (Ca₁₀(PO₄)₆(OH)₂) of high crystallinity when it was calcined at 800°C.     

The Properties of Polymethyl Methacrylate (PMMA) Bone Cement Filled with Titania and Hydroxyapatite Fillers

Commercial acrylic bone cement was modified by incorporating different filler loadings of bioactive hydroxyapatite and titania nanopowders. The effects of nanofiller loading on the mechanical and thermal properties were evaluated. The peak temperature during the polymerization of bone cement was observed to decrease with increasing filler loading. In addition, the flexural strength decreased and morphological studies of the fracture surfaces revealed an increase in porosity with the increase in filler loading. Silanation was conducted on the optimum filler loading, and the influence of silanation on the mechanical properties of bone cement was assessed.     

Antibacterial and Cellular Behaviors of Novel Zinc-Doped Hydroxyapatite/Graphene Nanocomposite for Bone Tissue Engineering

Bacteria are one of the significant causes of infection in the body after scaffold implantation. Effective use of nanotechnology to overcome this problem is an exciting and practical solution. Nanoparticles can cause bacterial degradation by the electrostatic interaction with receptors and cell walls. Simultaneously, the incorporation of antibacterial materials such as zinc and graphene in nanoparticles can further enhance bacterial degradation. In the present study, zinc-doped hydroxyapatite/graphene was synthesized and characterized as a nanocomposite material possessing both antibacterial and bioactive properties for bone tissue engineering. After synthesizing the zinc-doped hydroxyapatite nanoparticles using a mechanochemical process, they were composited with reduced graphene oxide. The nanoparticles and nanocomposite samples were extensively investigated by transmission electron microscopy, X-ray diffraction, and Raman spectroscopy. Their antibacterial behaviors against Escherichia coli and Staphylococcus aureus were studied. The antibacterial properties of hydroxyapatite nanoparticles were found to be improved more than 2.7 and 3.4 times after zinc doping and further compositing with graphene, respectively. In vitro cell assessment was investigated by a cell viability test and alkaline phosphatase activity using mesenchymal stem cells, and the results showed that hydroxyapatite nanoparticles in the culture medium, in addition to non-toxicity, led to enhanced proliferation of bone marrow stem cells. Furthermore, zinc doping in combination with graphene significantly increased alkaline phosphatase activity and proliferation of mesenchymal stem cells. The antibacterial activity along with cell biocompatibility/bioactivity of zinc-doped hydroxyapatite/graphene nanocomposite are the highly desirable and suitable biological properties for bone tissue engineering successfully achieved in this work.     

In Vitro Corrosion and Cytocompatibility Properties of Nano-Whisker Hydroxyapatite Coating on Magnesium Alloy for Bone Tissue Engineering Applications

We report here the successful fabrication of nano-whisker hydroxyapatite (nHA) coatings on Mg alloy by using a simple one-step hydrothermal process in aqueous solution. The nHA coating shows uniform structure and high crystallinity. Results indicate that nHA coating is promising for improving the in vitro corrosion and cytocompatibility properties of Mg-based implants and devices for bone tissue engineering. In addition, the simple hydrothermal deposition method used in the current study is also applicable to substrates with complex shapes or surface geometries.     

Surface Characterization and Biocompatibility of Selenium‐Doped Hydroxyapatite Coating on Titanium Alloy

Selenium‐doped hydroxyapatite (HA) was biomimetically coated on Ti6Al4V plates with the aim of combining the anticancer and antibacterial properties of selenium with the biocompatibility and bioactivity of HA. For the coating process, the composition of 1.5 × SBF (solution with ion concentrations at 1.5 times that of simulated body fluid, SBF) was modified to include 0.15 mM selenate (SeO₄^2?) ion. The selenium‐doped HA coating was characterized by several methods, such as scanning electron microscopy, X‐ray diffraction, and Fourier transform infrared spectroscopy. The cytotoxicity of selenium on osteoblast and osteosarcoma cells was determined. The coating was shown to inhibit the growth of Staphylococcus epidermidis.     

Preparation and Characterization of Organically Modified Montmorillonite-Filled High Density Polyethylene/Hydroxyapatite Nanocomposites for Biomedical Applications

The study investigated the introduction of organically modified montmorillonite (MMT) in high density polyethylene/hydroxyapatite (HDPE/HA) composites for biomedical applications. The addition of HA and MMT increased the strength and stiffness of HDPE/HA composites with deterioration in impact strength and elongation at break values. XRD and TEM analysis provided evidence of exfoliated MMT layers in HDPE/HA composites and the MMT layers remained exfoliated even with further addition of HA. Simulated body fluid (SBF) analysis revealed that the size of apatite layer increased with increasing immersion time and the formation of apatite layers on the surface of composites indicates excellent biocompatibility properties.     

Rapid microwave-assisted synthesis of gold loaded hydroxyapatite collagen nano-bio materials for drug delivery and tissue engineering application

A rapid microwave assisted facile synthetic technique was adopted to load gold nanoparticles (Au) on hydroxyapatite (HAp) surface. HAp nanoparticles were primarily synthesized by wet precipitation technique and further used for gold loading and successive collagen coating for biomedical applications. The microwave-assisted controlled synthesis technique with three heating cycles allows the very fast growing of Au seeds over HAp facets. Different sophisticated analytical techniques and spectroscopic characterization were employed to confirm the structural, chemical, and morphological features. The synthesized different concentration “Au” loaded hetero nanostructures coated with collagen (Au–HAp–Col) optimized for drug (Doxorubicin: DOX) loading and releasing purposes for biomedical applications. The maximum drug-loading efficiency of ~58.22% and a pH responsive releasing of ~53% (at pH 4.5) was obtained for 0.1?wt% Au–HAp–Col nanoparticles. To study the cytotoxic effects from the hetero nanostructures, MG-63 osteoblast-like cells were exposed to different concentration ranges on Au–HAp, Au–HAp–Col, and DOX loaded Au–HAp–Col nanoparticles. The non-toxic and bioactive properties of the synthesized nanoparticle-fabricated scaffold promotes cellular attachment, growth, and proliferation. These results indicated that optimized Au–HAp–Col nanoparticles may be promising drug delivery and scaffold materials for multifunctional biomedical applications.