Suspension thermal spraying of hydroxyapatite: microstructure and in vitro behaviour.

PubMed

Bolelli, Giovanni; Bellucci, Devis; Cannillo, Valeria; Lusvarghi, Luca; Sola, Antonella; Stiegler, Nico; Müller, Philipp; Killinger, Andreas; Gadow, Rainer; Altomare, Lina; De Nardo, Luigi

2014-01-01

In cementless fixation of metallic prostheses, bony ingrowth onto the implant surface is often promoted by osteoconductive plasma-sprayed hydroxyapatite coatings. The present work explores the use of the innovative High Velocity Suspension Flame Spraying (HVSFS) process to coat Ti substrates with thin homogeneous hydroxyapatite coatings. The HVSFS hydroxyapatite coatings studied were dense, 27-37μm thick, with some transverse microcracks. Lamellae were sintered together and nearly unidentifiable, unlike conventional plasma-sprayed hydroxyapatite. Crystallinities of 10%-70% were obtained, depending on the deposition parameters and the use of a TiO2 bond coat. The average hardness of layers with low (<24%) and high (70%) crystallinity was ≈3.5GPa and ≈4.5GPa respectively. The distributions of hardness values, all characterised by Weibull modulus in the 5-7 range, were narrower than that of conventional plasma-sprayed hydroxyapatite, with a Weibull modulus of ≈3.3. During soaking in simulated body fluid, glassy coatings were progressively resorbed and replaced by a new, precipitated hydroxyapatite layer, whereas coatings with 70% crystallinity were stable up to 14days of immersion. The interpretation of the precipitation behaviour was also assisted by surface charge assessments, performed through Z-potential measurements. During in vitro tests, HA coatings showed no cytotoxicity towards the SAOS-2 osteoblast cell line, and surface cell proliferation was comparable with proliferation on reference polystyrene culture plates. © 2013.

Design of Experiment Analysis of the Sulzer Metco DJ High Velocity Oxy-Fuel Coating of Hydroxyapatite for Orthopedic Applications

NASA Astrophysics Data System (ADS)

Hasan, S.; Stokes, J.

2011-01-01

High Velocity Oxy-Fuel (HVOF) has the potential to produce hydroxyapatite (HA; Bio-ceramic) coatings based on its experience with other sprayed ceramic materials. This technique should offer mechanical and biological results comparable to other thermal spraying processes, such as atmospheric plasma thermal spray, currently FDA approved for HA deposition. Deposition of HA via HVOF is a new venture especially using the Sulzer Metco Diamond Jet (DJ) process, and the aim of this article was to establish this technique's potential in providing superior HA coating results compared to the FDA-approved plasma spray technique. In this research, a Design of Experiment (DOE) model was developed to optimize the Sulzer Metco DJ HVOF process for the deposition of HA. In order to select suitable ranges for the production of HA coatings, the parameters were first investigated. Five parameters (factors) were researched over two levels namely: oxygen flow rate, propylene flow rate, air flow rate, spray distance, and powder flow rate. Coating crystallinity and purity were measured at the surface of each sample as the responses to the factors used. The research showed that propylene, air flow rate, spray distance, and powder feed rate had the largest effect on the responses, and the study aimed to find the preferred optimized settings to achieve high crystallinity and purity of percentages of up to 95%. This research found crystallinity and purity values of 93.8 and 99.8%, respectively, for a set of HVOF parameters which showed improvement compared to the crystallinity and purity values of 87.6 and 99.4%, respectively, found using the FDA-approved Sulzer Metco Atmospheric Plasma thermal spray process. Hence, a new technique for HA deposition now exists using the DJ HVOF facility; however, other mechanical and biorelated properties must also be assessed.

Fabrication and characterization of plasma-sprayed HA/SiO(2) coatings for biomedical application.

PubMed

Morks, M F

2008-01-01

Fused silica powder has been mixed with hydroxyapatite (HA) powder and plasma sprayed by using gas tunnel-type plasma jet. The influence of silica content (10 wt% and 20 wt%) on the microstructure and mechanical properties of HA-silica coatings was investigated. For investigating the microstructure and mechanical properties of HA-silica coatings, SUS 304 stainless steel was used as substrate material. The spraying was carried out on roughened substrate in an atmospheric chamber. Scanning electron microscope micrographs of cross-sectioned HA/SiO(2) coatings showed that the sprayed HA coatings with 10 and 20 wt% SiO(2) have dense structure with low porosity compared to the pure HA coatings. On the other hand, as the amount of silica was increased the coatings became denser, harder and exhibited high abrasive wear resistance. The presence of silica significantly improved the adhesive strength of HA/SiO(2) coatings mainly due to the increase in bonding strength of the coating at the interface.

In vitro and in vivo evaluation of the bioactivity of hydroxyapatite-coated polyetheretherketone biocomposites created by cold spray technology.

PubMed

Lee, Jae Hyup; Jang, Hae Lin; Lee, Kyung Mee; Baek, Hae-Ri; Jin, Kyoungsuk; Hong, Kug Sun; Noh, Jun Hong; Lee, Hyun-Kyung

2013-04-01

Polyetheretherketone (PEEK) is a material that is widely used in medicine because its mechanical properties show excellent similarity to those of human bone. However, because it is bioinert, PEEK shows limited ability to bind to natural bone tissue. Here, we applied a cold spray method to make a hydroxyapatite (HA)-coated PEEK hybrid material and evaluated its osteointegration in vitro and in vivo. With the cold spray method, the HA coating formed a homogeneous layer and adhered strongly to the PEEK disk implant. When the material was tested in vitro, early cell adhesion and viability improved. Alkaline phosphatase (ALP) activity and calcium concentration were also higher in cells cultured on HA-coated PEEK disks. In addition, the expression of osteoblast differentiation markers, such as ALP, bone sialoprotein and runt-related transcription factor 2, increased in these cells. For the in vivo test, we designed and implanted HA-coated PEEK cylinders into a rabbit ilium model by the press-fit method. The bone-implant contact ratio, trabecular number and trabecular thickness were determined using either three-dimensional microcomputed tomography or general two-dimensional histomorphometric analysis. This report demonstrates that the HA coating on the PEEK implant added with the cold spray method increased biocompatibility in vitro and promoted osteointegration in vivo, which suggests that the HA coating may improve the biofunctionality of various medical devices used in clinical applications. Copyright © 2012 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Effect of Induced Periimplantitis on Dental Implants With and Without Ultrathin Hydroxyapatite Coating.

PubMed

Madi, Marwa; Zakaria, Osama; Ichinose, Shizuko; Kasugai, Shohei

2016-02-01

The aim of this study was to compare the effect of ligature-induced periimplantitis on dental implants with and without hydroxyapatite (HA) coat. Thirty-two dental implants (3.3 mm wide, 13 mm long) with 4 surface treatments (8 implant/group) (M: machined, SA: sandblasted acid etched, S: sputter HA coat and P: plasma-sprayed HA coat) were inserted into canine mandibles. After 12 weeks, oral hygiene procedures were stopped and silk ligatures were placed around the implant abutments to allow plaque accumulation for the following 16 weeks. Implants with the surrounding tissues were retrieved and prepared for histological examination. Bone-to-implant contact (BIC) and implant surfaces were examined using scanning electron microscopy and energy dispersive x-ray spectroscopy. Histological observation revealed marginal bone loss and large inflammatory cell infiltrates in the periimplant soft tissue. Sputter HA implants showed the largest BIC (98.1%) and machined implant showed the smallest values (70.4%). After 28 weeks, thin sputter HA coat was almost completely dissolved, whereas plasma-sprayed HA coat showed complete thickness preservation. Thin sputter HA-coated implants showed more bone implant contact and less marginal bone loss than thick HA-coated implants under periimplantitis condition.

Cold Spray Coating of Submicronic Ceramic Particles on Poly(vinyl alcohol) in Dry and Hydrogel States

NASA Astrophysics Data System (ADS)

Moreau, David; Borit, François; Corté, Laurent; Guipont, Vincent

2017-06-01

We report an approach using cold spray technology to coat poly(vinyl alcohol) (PVA) in polymer and hydrogel states with hydroxyapatite (HA). Using porous aggregated HA powder, we hypothesized that fragmentation of the powder upon cold spray could lead to formation of a ceramic coating on the surface of the PVA substrate. However, direct spraying of this powder led to complete destruction of the swollen PVA hydrogel substrate. As an alternative, HA coatings were successfully produced by spraying onto dry PVA substrates prior to swelling in water. Dense homogeneous HA coatings composed of submicron particles were obtained using rather low-energy spraying parameters (temperature 200-250 °C, pressure 1-3 MPa). Coated PVA substrates could swell in water without removal of the ceramic layer to form HA-coated hydrogels. Microscopic observations and in situ measurements were used to explain how local heating and impact of sprayed aggregates induced surface roughening and strong binding of HA particles to the molten PVA substrate. Such an approach could lead to design of ceramic coatings whose roughness and crystallinity can be finely adjusted to improve interfacing with biological tissues.

Microstructural inhomogeneity in plasma-sprayed hydroxyapatite coatings and effect of post-heat treatment

NASA Astrophysics Data System (ADS)

Lu, Yu-Peng; Xiao, Gui-Yong; Li, Shi-Tong; Sun, Rui-Xue; Li, Mu-Sen

2006-01-01

The microstructural inhomogeneity in the plasma-sprayed hydroxyapatite (HA) coatings was characterized by using electron probe microanalyser (EPMA). A simple and artful method was developed to detect the interface characteristics. All the samples for observation were ground and polished along the direction parallel to the coating surfaces. The BSE images directly and clearly showed the inhomogeneity in the as-sprayed coatings with the amorphous regions being bright gray and crystalline regions being dark gray. X-ray diffractometer (XRD) patterns indicated that after immersion in deionized water for 20 days, bone-like apatite and α-Ca 2P 2O 7 precipitated on the polished surfaces of the as-sprayed HA coatings. The post-heat treatment could eliminate the microstructural inhomogeneity in the coatings. Only β-Ca 2P 2O 7 precipitated on the surfaces of the heat-treated HA coatings. The immersed samples were re-polished till tiny substrate was bared to investigate the effect of immersion on interface. It was shown that the immersion decreased the cohesive strength of the as-sprayed coatings. There were more and broader cracks in the splats that came into contact with the substrate and amorphous phase increased toward the coating-substrate interface. Post-heat treatment was proved to reduce the peeling off of coating during re-polishing operation. It was proposed that the distributions of amorphous phase and cracks in as-sprayed coatings are detrimental to coating properties and should be modified through improving the plasma spraying processing.

Activity of plasma sprayed yttria stabilized zirconia reinforced hydroxyapatite/Ti-6Al-4V composite coatings in simulated body fluid.

PubMed

Gu, Y W; Khor, K A; Pan, D; Cheang, P

2004-07-01

Hydroxyapatite (HA)/yttria stabilized zirconia/Ti-6Al-4V bio-composite coatings deposited onto Ti-6Al-4V substrate through a plasma spray technique were immersed in simulated body fluid (SBF) to investigate their behavior in vitro. Surface morphologies and structural changes in the coatings were analyzed by scanning electron microscopy, thin-film X-ray diffractometer, and X-ray photoelectron spectroscopy. The tensile bond strength of the coatings after immersion was also conducted through the ASTM C-633 standard for thermal sprayed coatings. Results showed that carbonate-containing hydroxyapatite (CHA) layer formed on the surface of composite coatings after 4 weeks immersion in SBF solution, indicating the composite coating possessed excellent bioactivity. The mechanical properties were found to decrease with immersion duration of maximum 56 days. However, minimal variation in mechanical properties was found subsequent to achieving supersaturation of the calcium ions, which was attained with the precipitation of the calcium phosphate layers. The mechanical properties of the composite coating were found to be significantly higher than those of pure HA coatings even after immersion in the SBF solution, indicating the enhanced mechanical properties of the composite coatings.

Antibacterial Property of Cold-Sprayed HA-Ag/PEEK Coating

NASA Astrophysics Data System (ADS)

Sanpo, Noppakun; Tan, Meng Lu; Cheang, Philip; Khor, K. A.

2009-03-01

The antibacterial behavior of HA-Ag (silver-doped hydroxyapatite) nanopowder and their composite coatings were investigated against Escherichia coli (DH5α). HA-Ag nanopowder and PEEK (poly-ether-ether-ketone)-based HA-Ag composite powders were synthesized using in-house powder processing techniques. Bacteria culture assay of HA-Ag nanopowder and their composite powders displayed excellent bacteriostatic activity against E. coli. The antibacterial activity increased with increasing concentration of HA-Ag nanoparticle in these composite powders. These nanocomposite powders were subsequently used as feedstock to generate antibacterial coatings via cold spray technology. The ratios of HA-Ag to PEEK in their composite powders were 80:20, 60:40, 40:60, and 20:80 (wt.%). Microstructural characterization and phase analysis of feedstock powders and as-deposited coatings were carried out using FESEM/EDX and XRD. Antibacterial nanocomposite HA-Ag/PEEK coatings were successfully deposited using cold spraying parameters of 11-12 bars at preheated air temperature between 150 and 160 °C. These as-sprayed coatings of HA-Ag/PEEK composite powders comprising varying HA-Ag and PEEK ratios retained their inherent antibacterial property as verified from bacterial assay. The results indicated that the antibacterial activity increased with increasing HA-Ag nanopowder concentration in the composite powder feedstock and cold-sprayed coating.

Plasma sprayed hydroxyapatite coatings on titanium substrates. Part 1: Mechanical properties and residual stress levels.

PubMed

Tsui, Y C; Doyle, C; Clyne, T W

1998-11-01

Hydroxyapatite (HA) coatings have been sprayed on to substrates of Ti-6Al-4V, using a range of input power levels and plasma gas mixtures. Coatings have also been produced on substrates of mild steel and tungsten, in order to explore certain aspects of the mechanical behaviour of HA without the complication of yielding or creep in the substrate. Studies have been made of the phase constitution, porosity, degree of crystallinity, OH ion content, microstructure and surface roughness of the HA coatings. The Young's moduli in tension and in compression were evaluated by the cantilever beam bend test using a tungsten/HA composite beam. The flexural Young's modulus was determined using a free-standing deposit under the same test. Adhesion was characterised using the single-edge notch-bend test; this is considered superior to the tensile bond strength test in common use. Measured interfacial fracture energies were of the order 1-10 J m(-2). Stress levels were investigated using specimen curvature measurements in conjunction with a numerical process model. The quenching stress for HA was measured to be about 10-25 MPa and the residual stress level in HA coatings at room temperature are predicted to lie in the approximate range of 20-40 MPa (tensile). These residual stresses could be reduced in magnitude by maintaining the substrate at a low temperature (possibly below room temperature) during spraying and it may be worthwhile to explore this. Ideally, the HA coating should have low porosity, high cohesive strength, good adhesion to the substrate, a high degree of crystallinity and high chemical purity and phase stability. In practice, such combinations are rather difficult to achieve by just varying the spraying parameters.

Recent Developments in Suspension Plasma Sprayed Titanium Oxide and Hydroxyapatite Coatings

NASA Astrophysics Data System (ADS)

Jaworski, R.; Pawlowski, L.; Pierlot, C.; Roudet, F.; Kozerski, S.; Petit, F.

2010-01-01

The paper aims at reviewing of the recent studies related to the development of suspension plasma sprayed TiO2 and Ca5(PO4)3OH (hydroxyapatite, HA) coatings as well as their multilayer composites obtained onto stainless steel, titanium and aluminum substrates. The total thickness of the coatings was in the range 10 to 150 μm. The suspensions on the base of distilled water, ethanol and their mixtures were formulated with the use of fine commercial TiO2 pigment crystallized as rutile and HA milled from commercial spray-dried powder or synthesized from calcium nitrate and ammonium phosphate in an optimized reaction. The powder was crystallized as hydroxyapatite. Pneumatic and peristaltic pump liquid feeders were applied. The injection of suspension to the plasma jet was studied carefully with the use of an atomizer injector or a continuous stream one. The injectors were placed outside or inside of the anode-nozzle of the SG-100 plasma torch. The stream of liquid was tested under angle right or slightly backwards with regard to the torch axis. The sprayed deposits were submitted to the phase analysis by the use of x-ray diffraction. The content of anatase and rutile was calculated in the titanium oxide deposits as well as the content of the decomposition phases in the hydroxyapatite ones. The micro-Raman spectroscopy was used to visualize the area of appearance of some phases. Scratch test enabled to characterize the adhesion of the deposits, their microhardness and friction coefficient. The electric properties including electron emission, impedance spectroscopy, and dielectric properties of some coatings were equally tested.

Mechanical properties of titanium-hydroxyapatite (Ti-HA) composite coating on stainless steel prepared by thermal spraying

NASA Astrophysics Data System (ADS)

Rosmamuhamadani, R.; Azhar, N. H.; Talari, M. K.; Yahaya, Sabrina M.; Sulaiman, S.; Ismail, M. I. S.

2017-09-01

Addition of hydroxyapatite (HA) can enhance the bioactivity of the common metallic implant due to its similarity with natural bones and teeth. In this investigation, high velocity oxy-fuel (HVOFT) technique was used to deposit titanium-hydroxyapatite (Ti-HA) composite on stainless steel substrate plate with different percentage of HA for biomedical applications. The aim of this research is to investigate the mechanical properties of Ti-HA coating such as hardness, adhesion strength and wear behaviour. The hardness and strength was determined by using SHIMADZU-microhardness Vickers tester and PosiTest AT portable adhesion tester respectively. The wear test was performed by using pin-on-disk equipment and field emission scanning electron microscope (FESEM) used to determine the extent of surface damage. From the results obtained, mechanical properties such as hardness and adhesion strength of titanium (Ti) coating decreased with the increased of HA contents. Meanwhile, the coefficient of friction of Ti-10% HA coating shows the highest value compare to others as three-body abrasion had occurred during the test.

Bone-like apatite layer formation on hydroxyapatite prepared by spark plasma sintering (SPS).

PubMed

Gu, Y W; Khor, K A; Cheang, P

2004-08-01

Hydroxyapatite (HA) compacts with high density and superior mechanical properties were fabricated by spark plasma sintering (SPS) using spray-dried HA powders as feedstock. The formation of bone-like apatite layer on SPS consolidated HA compacts were investigated by soaking the HA compacts in simulated body fluid (SBF) for various periods (maximum of 28 days). The structural changes in HA post-SBF were analyzed with scanning electron microscopy, grazing incidence X-ray diffraction and X-ray photoelectron spectroscopy. It was found that a layer consisting microcrystalline carbonate-containing hydroxyapatite was formed on the surface of HA compacts after soaking for 24h. The formation mechanism of apatite on the surface of HA compacts after soaking in SBF was attributed to the ion exchange between HA compacts and the SBF solution. The increase in ionic concentration of calcium and phosphorus as well as the increase in pH after SBF immersion resulted in an increase in ionic activity product of apatite in the solution, and provided a specific surface with a low interface energy that is conducive to the nucleation of apatite on the surface of HA compacts.

Molecular dynamics simulations for the examination of mechanical properties of hydroxyapatite/ poly α-n-butyl cyanoacrylate under additive manufacturing.

PubMed

Wang, Yanen; Wei, Qinghua; Pan, Feilong; Yang, Mingming; Wei, Shengmin

2014-01-01

Molecular dynamics (MD) simulations emerged to be a helpful tool in the field of material science. In rapid prototyping artificial bone scaffolds process, the binder spraying volume and mechanism are very important for bone scaffolds mechanical properties. In this study, we applied MD simulations to investigating the binding energy of α-n-butyl cyanoacrylate (NBCA) on Hydroxyapatite (HA) crystallographic planes (001, 100 and 110), and to calculating and analyzing the mechanical properties and radial distribution function of the HA(110)/NBCA mixed system. The simulation results suggested that HA (110) has the highest binding energy with NBCA owing to the high planar atom density, and the mechanical properties of HA(110)/NBCA mixed system is stronger than pure HA system. Therefore, the multi-grade strength bone scaffold could be fabricated through spraying various volume NBCA binders during 3D printing process. By calculating the radial distribution function of HA(110)/NBCA, the essence of the interface interaction were successfully elucidated. The forming situation parameters can be referred to calculation results. There exists a strong interaction between HA crystallographic plane (110) and NBCA, it is mainly derived from the hydrogen bonds between O atoms which connect with C atoms of NBCA and H atoms in HA crystal. Furthermore, a strong adsorption effect can be demonstrated between HA and NBCA.

Cold-spray coating of hydroxyapatite on a three-dimensional polyetheretherketone implant and its biocompatibility evaluated by in vitro and in vivo minipig model.

PubMed

Lee, Jae Hyup; Jang, Hae Lin; Lee, Kyung Mee; Baek, Hae-Ri; Jin, Kyoungsuk; Noh, Jun Hong

2017-04-01

PEEK is a bioinert material that does not chemically bind to native bone tissue and thus formation of natural bone-like hydroxyapatite (HA) coating layer on PEEK has been an important challenge to improve biocompatibility and to preserve mechanical property of PEEK. Among various coating techniques, cold-spray coating method is suitable to form stable HA coating layer on PEEK while maintaining their chemical properties, because it can be conducted in relatively low-temperature range. Therefore, in this research, we used cold-spray coating method to form a thick layer of HA on the topographically complex PEEK substrates with periodic ridges on the surface and implanted in iliac bone defects of minipigs which is known to be similar with human body system. In addition, PEEK cage for clinical usage was coated with HA and inserted in the lumbar intervertebral disc space of minipig. We observed higher ALP activity, calcium production, and BSP production of human bone marrow mesenchymal stem cells on the HA-coated PEEK implants than the bare PEEK group in in vitro test. In addition, two-dimensional histological analysis and three-dimensional micro CT analysis demonstrated that implantation of complex shape of HA-PEEK hybrid implant in in vivo minipig model resulted sufficient biocompatibility and osseointegration for further clinical applications. Notably, due to the enhanced stability of PEEK cage induced from HA coating layer, osseointegration rate of the small HA blocks loaded inside the PEEK cage was also significantly improved which indicates overall increased fusion rate and adherence of the HA-coated PEEK cage. © 2015 Wiley Periodicals, Inc. J Biomed Mater Res Part B: Appl Biomater, 105B: 647-657, 2017. © 2015 Wiley Periodicals, Inc.

X-ray diffraction analysis of hydroxyapatite-coated in different plasma gas atmosphere on Ti and Ti-6Al-4V

PubMed Central

Kotian, Ravindra; Rao, P. Prasad; Madhyastha, Prashanthi

2017-01-01

Objective: The aim is to study the effect of plasma working gas on composition, crystallinity, and microstructure of hydroxyapatite (HA) coated on Ti and Ti-6Al-4V metal substrates. Materials and Methods: Ti and Ti-6Al-4V metal substrates were coated with HA by plasma spray using four plasma gas atmospheres of argon, argon/hydrogen, nitrogen, and nitrogen/hydrogen. The degree of crystallinity, the phases present, and microstructure of HA coating were characterized using X-ray diffraction and scanning electron microscopy. Results: Variation in crystallinity and the microstructure of HA coating on plasma gas atmosphere was observed. Micro-cracks due to thermal stresses and shift in the 2θ angle of HA compared to feedstock was seen. Conclusion: Plasma gas atmosphere has a significant influence on composition, crystallinity, and micro-cracks of HA-coated dental implants. PMID:29279668

Hydroxyapatite, fluor-hydroxyapatite and fluorapatite produced via the sol-gel method. Optimisation, characterisation and rheology.

PubMed

Tredwin, Christopher J; Young, Anne M; Georgiou, George; Shin, Song-Hee; Kim, Hae-Won; Knowles, Jonathan C

2013-02-01

Currently, most titanium implant coatings are made using hydroxyapatite and a plasma spraying technique. There are however limitations associated with plasma spraying processes including poor adherence, high porosity and cost. An alternative method utilising the sol-gel technique offers many potential advantages but is currently lacking research data for this application. It was the objective of this study to characterise and optimise the production of Hydroxyapatite (HA), fluorhydroxyapatite (FHA) and fluorapatite (FA) using a sol-gel technique and assess the rheological properties of these materials. HA, FHA and FA were synthesised by a sol-gel method. Calcium nitrate and triethylphosphite were used as precursors under an ethanol-water based solution. Different amounts of ammonium fluoride (NH4F) were incorporated for the preparation of the sol-gel derived FHA and FA. Optimisation of the chemistry and subsequent characterisation of the sol-gel derived materials was carried out using X-ray Diffraction (XRD) and Differential Thermal Analysis (DTA). Rheology of the sol-gels was investigated using a viscometer and contact angle measurement. A protocol was established that allowed synthesis of HA, FHA and FA that were at least 99% phase pure. The more fluoride incorporated into the apatite structure; the lower the crystallisation temperature, the smaller the unit cell size (changes in the a-axis), the higher the viscosity and contact angle of the sol-gel derived apatite. A technique has been developed for the production of HA, FHA and FA by the sol-gel technique. Increasing fluoride substitution in the apatite structure alters the potential coating properties. Crown Copyright © 2012. Published by Elsevier Ltd. All rights reserved.

HVOF-Sprayed Nano TiO2-HA Coatings Exhibiting Enhanced Biocompatibility

NASA Astrophysics Data System (ADS)

Lima, R. S.; Dimitrievska, S.; Bureau, M. N.; Marple, B. R.; Petit, A.; Mwale, F.; Antoniou, J.

2010-01-01

Biomedical thermal spray coatings produced via high-velocity oxy-fuel (HVOF) from nanostructured titania (n-TiO2) and 10 wt.% hydroxyapatite (HA) (n-TiO2-10wt.%HA) powders have been engineered as possible future alternatives to HA coatings deposited via air plasma spray (APS). This approach was chosen due to (i) the stability of TiO2 in the human body (i.e., no dissolution) and (ii) bond strength values on Ti-6Al-4V substrates more than two times higher than those of APS HA coatings. To explore the bioperformance of these novel materials and coatings, human mesenchymal stem cells (hMSCs) were cultured from 1 to 21 days on the surface of HVOF-sprayed n-TiO2 and n-TiO2-10 wt.%HA coatings. APS HA coatings and uncoated Ti-6Al-4V substrates were employed as controls. The profiles of the hMSCs were evaluated for (i) cellular proliferation, (ii) biochemical analysis of alkaline phosphatase (ALP) activity, (iii) cytoskeleton organization (fluorescent/confocal microscopy), and (iv) cell/substrate interaction via scanning electron microscopy (SEM). The biochemical analysis indicated that the hMSCs cultured on n-TiO2-10 wt.%HA coatings exhibited superior levels of bioactivity than hMSCs cultured on APS HA and pure n-TiO2 coatings. The cytoskeleton organization demonstrated a higher degree of cellular proliferation on the HVOF-sprayed n-TiO2-10wt.%HA coatings when compared to the control coatings. These results are considered promising for engineering improved performance in the next generation of thermally sprayed biomedical coatings.

A novel jet-based nano-hydroxyapatite patterning technique for osteoblast guidance

PubMed Central

Li, Xiang; Koller, Garrit; Huang, Jie; Di Silvio, Lucy; Renton, Tara; Esat, Minoo; Bonfield, William; Edirisinghe, Mohan

2010-01-01

Surface topography is well known to play a crucial role in influencing cellular responses to an implant material and is therefore important in bone tissue regeneration. A novel jet-based patterning technique, template-assisted electrohydrodynamic atomization spraying, was recently devised to control precisely the surface structure as well as its dimensions. In the present study, a detailed investigation of this patterning process was carried out. A range of nano-hydroxyapatite (nHA) line-shaped patterns <20 µm in width were successfully deposited on a commercially pure Ti surface by controlling the flow of an nHA suspension in an electric field. In vitro studies showed that the nHA patterns generated are capable of regulating the human osteoblast cell attachment and orientation. PMID:19493897

Plasma sprayed hydroxyapatite coatings on titanium substrates. Part 2: optimisation of coating properties.

PubMed

Tsui, Y C; Doyle, C; Clyne, T W

1998-11-01

Heat treatment and the introduction of a Ti bond coat have been applied to hydroxyapatite (HA) coatings sprayed using different plasma powers and gas mixtures. Attempts were made in this way to achieve optimal coating properties for orthopaedic implants. In particular, the effects on the degree of crystallinity, the adhesion, the OH ion content and the purity were evaluated. Heat treatment at 700 C for 1 h in air proved to be effective in increasing the crystallinity, regaining the OH- ion and removing other non-HA compounds, although it caused a significant decrease in the degree of adhesion (interfacial fracture toughness) for those specimens sprayed at high powers. This heat treatment was found to induce significant transformation of amorphous HA to the crystalline form, while not detrimentally changing the properties of the underlying Ti-6Al-4V substrates. Precoating with a 100 microm Ti layer increased the adhesion of the HA coatings on Ti-6Al-4V substrates, primarily by providing a rougher surface and promoting better mechanical interlocking. Changes in coating properties during immersion in biological fluids were also studied and were found to depend critically on the chemical composition of the fluids. Small precipitates formed on the coating surfaces when immersed in Ringers solution. These might account for the apparent drop in the degree of crystallinity when measured using X-ray diffraction. A significant drop in the interfacial adhesion was found for those coatings sprayed at high powers. This could be offset by prior precoating with a titanium bond coat and suitable heat treatment. In summary, the following processing sequence is suggested in order to achieve optimum coating properties: precoating the substrate with a layer of Ti (approximately 100 microm), spraying HA at a sufficiently high-power level (depending on particle size and gas mixture) and heat treatment at 700 degrees C for 1 h in air.

Effect of substrate preheating temperature and coating thickness on residual stress in plasma sprayed hydroxyapatite coating

NASA Astrophysics Data System (ADS)

Tang, Dapei

2015-07-01

A thermal-mechanical coupling model was developed based on thermal-elastic- plastic theory according the special process of plasma spraying Hydroxyapatite (HA) coating upon Ti-6Al-4V substrate. On the one hand, the classical Fourier transient heat conduction equation was modified by introducing the effect item of deformation on temperature, on the other hand, the Johnson-Cook model, suitable for high temperature and high strain rate conditions, was used as constitutive equation after considering temperature softening effect, strain hardening effect and strain rate reinforcement effect. Based on the above coupling model, the residual stress field within the HA coating was simulated by using finite element method (FEM). Meanwhile, the substrate preheating temperature and coating thickness on the influence of residual stress components were calculated, respectively. The failure modes of coating were also preliminary analyzed. In addition, in order to verify the reliability of calculation, the material removal measurement technique was applied to determine the residual stress of HA coating near the interface. Some important conclusions are obtained.

Microstructural design of functionally graded coatings composed of suspension plasma sprayed hydroxyapatite and bioactive glass.

PubMed

Cattini, Andrea; Bellucci, Devis; Sola, Antonella; Pawłowski, Lech; Cannillo, Valeria

2014-04-01

Various bioactive glass/hydroxyapatite (HA) functional coatings were designed by the suspension plasma spraying (SPS) technique. Their microstructure, scratch resistance, and apatite-forming ability in a simulated body fluid (SBF) were compared. The functional coatings design included: (i) composite coating, that is, randomly distributed constituent phases; (ii) duplex coating with glass top layer onto HA layer; and (iii) graded coating with a gradual changing composition starting from pure HA at the interface with the metal substrate up to pure glass on the surface. The SPS was a suitable coating technique to produce all the coating designs. The SBF tests revealed that the presence of a pure glass layer on the working surface significantly improved the reactivity of the duplex and graded coatings, but the duplex coating suffered a relatively low scratch resistance because of residual stresses. The graded coating therefore provided the best compromise between mechanical reliability and apatite-forming ability in SBF. © 2013 Wiley Periodicals, Inc. J Biomed Mater Res Part B: Appl Biomater, 102B: 551-560, 2014. Copyright © 2013 Wiley Periodicals, Inc.

Deposition of Hydroxyapatite Onto Superelastic Nitinol Using an Ambient Temperature Blast Coating Process

NASA Astrophysics Data System (ADS)

Dunne, Conor F.; Roche, Kevin; Ruddy, Mark; Doherty, Kevin A. J.; Twomey, Barry; O'Donoghue, John; Hodgson, Darel; Stanton, Kenneth T.

2018-06-01

This work investigates the deposition of hydroxyapatite (HA) onto superelastic nickel-titanium (NiTi) using an ambient temperature coating process known as CoBlast. The process utilises a stream of abrasive alumina (Al2O3) and a coating medium (HA) sprayed simultaneously at the surface of the substrate. The use of traditional coatings methods, such as plasma spray, is unsuitable due to the high temperatures of the process. This can result in changes to both the crystallinity of the HA and properties of the thermally sensitive NiTi. HA is a biocompatible, biodegradable and osteoconductive ceramic, which when used as a coating can promote bone growth and prevent the release of nickel from NiTi in vivo. Samples were coated using different blast pressures and abrasive particle sizes and were examined using a variety of techniques. The coated samples had a thin adherent coating, which increased in surface roughness and coating thickness with increasing abrasive particle size. X-ray diffraction analysis revealed that the process gave rise to a stress-induced martensite phase in the NiTi which may enhance mechanical properties. The study indicates that the CoBlast process can be used to deposit thin adherent coatings of HA onto the surface of superelastic NiTi.

In vitro performance of Ag-incorporated hydroxyapatite and its adhesive porous coatings deposited by electrostatic spraying.

PubMed

Gokcekaya, Ozkan; Webster, Thomas J; Ueda, Kyosuke; Narushima, Takayuki; Ergun, Celaletdin

2017-08-01

Bacterial infection of implanted materials is a significant complication that might require additional surgical operations for implant retrieval. As an antibacterial biomaterial, Ag-containing hydroxyapatite (HA) may be a solution to reduce the incidences of implant associated infections. In this study, pure, 0.2mol% and 0.3mol% Ag incorporated HA powders were synthesized via a precipitation method. Colloidal precursor dispersions prepared from these powders were used to deposit porous coatings onto titanium and stainless steel substrates via electrostatic spraying. The porous coating layers obtained with various deposition times and heat treatment conditions were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM). Scratch tests were conducted to assess the adhesion strength of the coating. Antibacterial activity of Ag-incorporated HA was tested towards Escherichia coli (E. coli) at various incubation times. Osteoblast adhesion on Ag-incorporated HA was evaluated to assess biocompatibility. Improvement in adhesion strength of the coating layer was observed after the heat treatment process due to mutual ionic diffusion at the interface. The Ag-incorporated HA killed all viable E. coli after 24h of incubation, whereas no antibacterial activity was detected with pure HA. In addition, in vitro cell culture tests demonstrated osteoblast adhesion similar to pure HA, which indicated good cytocompatibility. In summary, results of this study provided significant promise for the future study of Ag-incorporated HA for numerous medical applications. Copyright © 2017 Elsevier B.V. All rights reserved.

Microstructure and mechanical properties of plasma sprayed HA/YSZ/Ti-6Al-4V composite coatings.

PubMed

Khor, K A; Gu, Y W; Pan, D; Cheang, P

2004-08-01

Plasma sprayed hydroxyapatite (HA) coatings on titanium alloy substrate have been used extensively due to their excellent biocompatibility and osteoconductivity. However, the erratic bond strength between HA and Ti alloy has raised concern over the long-term reliability of the implant. In this paper, HA/yttria stabilized zirconia (YSZ)/Ti-6Al-4V composite coatings that possess superior mechanical properties to conventional plasma sprayed HA coatings were developed. Ti-6Al-4V powders coated with fine YSZ and HA particles were prepared through a unique ceramic slurry mixing method. The so-formed composite powder was employed as feedstock for plasma spraying of the HA/YSZ/Ti-6Al-4V coatings. The influence of net plasma energy, plasma spray standoff distance, and post-spray heat treatment on microstructure, phase composition and mechanical properties were investigated. Results showed that coatings prepared with the optimum plasma sprayed condition showed a well-defined splat structure. HA/YSZ/Ti-6Al-4V solid solution was formed during plasma spraying which was beneficial for the improvement of mechanical properties. There was no evidence of Ti oxidation from the successful processing of YSZ and HA coated Ti-6Al-4V composite powders. Small amount of CaO apart from HA, ZrO(2) and Ti was present in the composite coatings. The microhardness, Young's modulus, fracture toughness, and bond strength increased significantly with the addition of YSZ. Post-spray heat treatment at 600 degrees C and 700 degrees C for up to 12h was found to further improve the mechanical properties of coatings. After the post-spray heat treatment, 17.6% increment in Young's modulus (E) and 16.3% increment in Vicker's hardness were achieved. The strengthening mechanisms of HA/YSZ/Ti-6Al-4V composite coatings were related to the dispersion strengthening by homogeneous distribution of YSZ particles in the matrix, the good mechanical properties of Ti-6Al-4V and the formation of solid solution among HA, Ti alloy and YSZ components.

Effect of spark plasma sintering on the microstructure and in vitro behavior of plasma sprayed HA coatings.

PubMed

Yu, L-G; Khor, K A; Li, H; Cheang, P

2003-07-01

The crystalline phases and degree of crystallinity in plasma sprayed calcium phosphate coatings on Ti substrates are crucial factors that influence the biological interactions of the materials in vivo. In this study, plasma sprayed hydroxyapatite (HA) coatings underwent post-spray treatment by the spark plasma sintering (SPS) technique at 500 degrees C, 600 degrees C, and 700 degrees C for duration of 5 and 30 min. The activity of the HA coatings before and after SPS are evaluated in vitro in a simulated body fluid. The surface microstructure, crystallinity, and phase composition of each coating is characterized by scanning electron microscopy and X-ray diffractometry before, and after in vitro incubation. Results show that the plasma sprayed coatings treated for 5 min in SPS demonstrated increased proportion of beta-TCP phase with a preferred-orientation in the (214) plane, and the content of beta-TCP phase corresponded to SPS temperature, up to 700 degrees C. SPS treatment at 700 degrees C for 30 min enhanced the HA content in the plasma spray coating as well. The HA coatings treated in SPS for 5 min revealed rapid surface morphological changes during in vitro incubation (up to 12 days), indicating that the surface activity is enhanced by the SPS treatment. The thickest apatite layer was found in the coating treated by SPS at 700 degrees C for 5 min.

Hydroxyapatite-coated Ti-6Al-4V part 2: the effects of post-deposition heat treatment at low temperatures.

PubMed

Lynn, A K; DuQuesnay, D L

2002-05-01

The present investigation explores the effects of a 90-h post-deposition annealing treatment at 400 degrees C in air on the crystallographic and chemical properties of a plasma-sprayed hydroxyapatite (HA) coating, the thickness and composition of the interfacial oxide layer, and the fatigue behaviour of the underlying Ti-6Al-4V substrate. X-ray diffraction analysis revealed that significant recovery of the crystalline HA structure occurred as a result of the treatment, however, as compared with results obtained through treatment at higher temperatures, recovery obtained through use of the present treatment was incomplete. X-ray photoelectron spectroscopy analysis showed no changes in the constituents of the oxide layer, with the oxide species TiO2, Al2O3, V2O5, V2O3, and VO2 present on both the as-sprayed and the heat-treated substrates. A change in film thickness was observed, however, as evidenced by a change in colour from opaque bronze to dark purple. The fatigue resistance of the substrate was found to be significantly reduced by the heat treatment, with the lives of heat-treated coupons with coatings of all thicknesses closely resembling those of as-sprayed coupons with thick HA coatings and uncoated stress-relieved coupons presented in Part I of this study. Stress relief was identified as the most likely cause of these reductions.

Antibacterial and biological characteristics of plasma sprayed silver and strontium doped hydroxyapatite coatings

PubMed Central

Fielding, Gary A.; Roy, Mangal; Bandyopadhyay, Amit

2012-01-01

Infection in primary total joint prostheses is estimated to occur in up to 3% of all surgeries. As a measure to improve the antimicrobial properties of implant materials, silver (Ag) was incorporated into plasma sprayed hydroxyapatite (HA) coatings. To offset potential cytotoxic effects of Ag in the coatings, strontium (Sr) was also added as a binary dopant. HA powder were doped with 2.0 wt% Ag2O, 1.0 wt% SrO and the powder was then heat treated at 800° C. Titanium substrates were coated using a 30 kW plasma spray system equipped with a supersonic nozzle. X-ray diffraction (XRD) confirmed the phase purity and high crystallinity of the coatings. Samples were evaluated for mechanical stability by adhesive bond strength testing. Results show that the addition of dopants did not affect the overall bond strength of the coatings. The antibacterial efficacies of the coatings were tested against Pseudomonas aeruginosa. Samples that contained the Ag2O dopant were found to be highly effective against the bacterial colonization. In vitro cell-material interactions using human fetal osteoblast (hFOB) cells were characterized by 3-(4,5-Dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide (MTT) assay for cell viability, field emission scanning electron microscopy (FESEM) for cell morphology and confocal imaging for the important differentiation marker alkaline phosphatase (ALP). Our results showed evidence of cytotoxic effects in the Ag-HA coatings, characterized by poor cellular morphology and cell death and nearly complete impediment of functional ALP activity. The addition of SrO to Ag-HA coatings was able to effectively offset these negative effects and improve the performance when compared to pure HA coated samples. PMID:22487928

Influence of deposition temperature on mechanical properties of plasma-sprayed hydroxyapatite coating on titanium alloy with ZrO2 intermediate layer

NASA Astrophysics Data System (ADS)

Chou, Bang-Yen; Chang, Edward

2003-06-01

Hydroxyapatite coatings were plasma sprayed on the Ti6A14V substrate with and without an intermediate ZrO2 layer; meanwhile the temperatures of substrates were varied at 90, 140, and 200 °C. The coatings were subjected to the standard adhesion test per ASTM C633-79. The purpose of the investigation was to study the effects of those processing variables on the bonding strength and failure behavior of the system. It is found that the bonding strengths of HA/ZrO2 and HA coatings generally decrease with increasing substrate temperature, except for the HA/ZrO2 coating deposited at 200 °C. The rationale of the results is attributed to the residual stress reported in the literature. Introducing ZrO2 bond coat is found to significantly promote the bonding strength of HA coating. The possible strengthening mechanism is the rougher surface of ZrO2 bond coat and the higher toughness of ZrO2, which provide the mechanical strengthening effects. The slightly denser HA in 200 °C deposited HA coating cannot explain the high bonding strength of the HA/ZrO2 coating, nor the mechanical strengthening effect of ZrO2 intermediate layer should apply. It is believed that a stronger diffusion bonding is formed at the interface of HA and ZrO2, which increases the bonding between them chemically. The bonding strengths of HA/ZrO2 and HA coatings are correlated with the area fraction of adhesive failure of the coatings. The correlation explains the findings in this study.

Effect of dissolution/precipitation on the residual stress redistribution of plasma-sprayed hydroxyapatite coating on titanium substrate in simulated body fluid (SBF).

PubMed

Rakngarm Nimkerdphol, Achariya; Otsuka, Yuichi; Mutoh, Yoshiharu

2014-08-01

The residual stress distributions in hydroxyapatite (HAp) coating with and without mixed hydroxyapatite/titanium (HAp/Ti) bond coating on commercially pure Titanium substrate (cp-Ti) were evaluated by Raman piezo-spectroscopy analysis. The Raman shifted position 962cm(-1), which is the symmetrical stretching of surrounded oxygen atoms with phosphorous atom ( [Formula: see text] ), was referred to analyses of stress dependency. The piezo-spectroscopic coefficient, which is a Raman shift value per stress (cm(-1)/GPa), was fitted from the result of four-points bending test of rectangular HAp bar and as-sprayed HAp on Zn plate. The calculated values were 3.89cm(-1)/GPa for the former and 7.11cm(-1)/GPa for the latter. By using these calibrations, the compressive residual stress in HAp coating with HAp/Ti bond coating (HA-B) has been found to be distributed in the range of -137MPa to -75MPa. For the heat-treated HAp coating (HA-B-HT) specimen, the compressive residual stresses placed in the range of -40--22MPa. The changes in the values of residual stress of the HAp coating after immersion in SBF were also evaluated. The residual stress in HA-WB specimens tend to change from compressive to tensile after 30 days immersion. The HA-B-HT specimens exhibited similar behavior and reached to zero stress after the immersion. The mechanism of the changes in residual stress would be the effect of stress redistribution around melted calcium phosphate particles to remained HAp splats. Copyright © 2014 Elsevier Ltd. All rights reserved.

Influence of substrate metal alloy type on the properties of hydroxyapatite coatings deposited using a novel ambient temperature deposition technique.

PubMed

Barry, J N; Cowley, A; McNally, P J; Dowling, D P

2014-03-01

Hydroxyapatite (HA) coatings are applied widely to enhance the level of osteointegration onto orthopedic implants. Atmospheric plasma spray (APS) is typically used for the deposition of these coatings; however, HA crystalline changes regularly occur during this high-thermal process. This article reports on the evaluation of a novel low-temperature (<47°C) HA deposition technique, called CoBlast, for the application of crystalline HA coatings. To-date, reports on the CoBlast technique have been limited to titanium alloy substrates. This study addresses the suitability of the CoBlast technique for the deposition of HA coatings on a number of alternative metal alloys utilized in the fabrication of orthopedic devices. In addition to titanium grade 5, both cobalt chromium and stainless steel 316 were investigated. In this study, HA coatings were deposited using both the CoBlast and the plasma sprayed techniques, and the resultant HA coating and substrate properties were evaluated and compared. The CoBlast-deposited HA coatings were found to present similar surface morphologies, interfacial properties, and composition irrespective of the substrate alloy type. Coating thickness however displayed some variation with the substrate alloy, ranging from 2.0 to 3.0 μm. This perhaps is associated with the electronegativity of the metal alloys. The APS-treated samples exhibited evidence of both coating, and significantly, substrate phase alterations for two metal alloys; titanium grade 5 and cobalt chrome. Conversely, the CoBlast-processed samples exhibited no phase changes in the substrates after depositions. The APS alterations were attributed to the brief, but high-intensity temperatures experienced during processing. Copyright © 2013 Wiley Periodicals, Inc.

The Evaluation of Hydroxyapatite (HA) Coated and Uncoated Porous Tantalum for Biomedical Material Applications

NASA Astrophysics Data System (ADS)

Safuan, Nadia; Sukmana, Irza; Kadir, Mohammed Rafiq Abdul; Noviana, Deni

2014-04-01

Porous tantalum has been used as an orthopedic implant for bone defects as it has a good corrosion resistance and fatigue behaviour properties. However, there are some reports on the rejection of porous Ta after the implantation. Those clinical cases refer to the less bioactivity of metallic-based materials. This study aims to evaluate hydroxyapatite coated and uncoated porous Tantalum in order to improve the biocompatibility of porous tantalum implant and osseointegration. Porous tantalum was used as metallic-base substrate and hydroxyapatite coating has been done using plasma-spraying technique. Scanning Electron Microscopy (SEM) and Field Emission Scanning Electron Microscopy (FESEM) techniques were utilizes to investigate the coating characteristics while Confocal Raman Microscopy to investigate the interface and image. The effect of coating to the corrosion behaviour was assessed by employing potentiodynamic polarization tests in simulated body fluid at 37±1 °C. Based on SEM and FESEM results, the morphologies as well the weight element consists in the uncoated and hydroxyapatite coated porous tantalum were revealed. The results indicated that the decrease in corrosion current density for HA coated porous Ta compared to the uncoated porous Ta. This study concluded that by coating porous tantalum with HA supports to decrease the corrosion rate of pure porous.

Induction Plasma Sprayed Nano Hydroxyapatite Coatings on Titanium for Orthopaedic and Dental Implants

PubMed Central

Roy, Mangal; Bandyopadhyay, Amit; Bose, Susmita

2011-01-01

This paper reports preparation of a highly crystalline nano hydroxyapatite (HA) coating on commercially pure titanium (Cp-Ti) using inductively coupled radio frequency (RF) plasma spray and their in vitro and in vivo biological response. HA coatings were prepared on Ti using normal and supersonic plasma nozzles at different plate powers and working distances. X-ray diffraction (XRD) and Fourier transformed infrared spectroscopic (FTIR) analysis show that the normal plasma nozzle lead to increased phase decomposition, high amorphous calcium phosphate (ACP) phase formation, and severe dehydroxylation of HA. In contrast, coatings prepared using supersonic nozzle retained the crystallinity and phase purity of HA due to relatively short exposure time of HA particles in the plasma. In addition, these coatings exhibited a microstructure that varied from porous and glassy structure at the coating-substrate interface to dense HA at the top surface. The microstructural analysis showed that the coating was made of multigrain HA particles of ~200 nm in size, which consisted of recrystallized HA grains in the size range of 15– 20 nm. Apart from the type of nozzle, working distance was also found to have a strong influence on the HA phase decomposition, while plate power had little influence. Depending on the plasma processing conditions, a coating thickness between 300 and 400 μm was achieved where the adhesive bond strengths were found to be between 4.8 MPa to 24 MPa. The cytotoxicity of HA coatings was examined by culturing human fetal osteoblast cells (hFOB) on coated surfaces. In vivo studies, using the cortical defect model in rat femur, evaluated the histological response of the HA coatings prepared with supersonic nozzle. After 2 weeks of implantation, osteoid formation was evident on the HA coated implant surface, which could indicate early implant- tissue integration in vivo. PMID:21552358

Scaffolds for bone regeneration made of hydroxyapatite microspheres in a collagen matrix.

PubMed

Cholas, Rahmatullah; Kunjalukkal Padmanabhan, Sanosh; Gervaso, Francesca; Udayan, Gayatri; Monaco, Graziana; Sannino, Alessandro; Licciulli, Antonio

2016-06-01

Biomimetic scaffolds with a structural and chemical composition similar to native bone tissue may be promising for bone tissue regeneration. In the present work hydroxyapatite mesoporous microspheres (mHA) were incorporated into collagen scaffolds containing an ordered interconnected macroporosity. The mHA were obtained by spray drying of a nano hydroxyapatite slurry prepared by the precipitation technique. X-ray diffraction (XRD) analysis revealed that the microspheres were composed only of hydroxyapatite (HA) phase, and energy-dispersive x-ray spectroscopy (EDS) analysis revealed the Ca/P ratio to be 1.69 which is near the value for pure HA. The obtained microspheres had an average diameter of 6 μm, a specific surface area of 40 m(2)/g as measured by Brunauer-Emmett-Teller (BET) analysis, and Barrett-Joyner-Halenda (BJH) analysis showed a mesoporous structure with an average pore diameter of 16 nm. Collagen/HA-microsphere (Col/mHA) composite scaffolds were prepared by freeze-drying followed by dehydrothermal crosslinking. SEM observations of Col/mHA scaffolds revealed HA microspheres embedded within a porous collagen matrix with a pore size ranging from a few microns up to 200 μm, which was also confirmed by histological staining of sections of paraffin embedded scaffolds. The compressive modulus of the composite scaffold at low and high strain values was 1.7 and 2.8 times, respectively, that of pure collagen scaffolds. Cell proliferation measured by the MTT assay showed more than a 3-fold increase in cell number within the scaffolds after 15 days of culture for both pure collagen scaffolds and Col/mHA composite scaffolds. Attractive properties of this composite scaffold include the potential to load the microspheres for drug delivery and the controllability of the pore structure at various length scales. Copyright © 2016 Elsevier B.V. All rights reserved.

Free form fabricated features on CoCr implants with and without hydroxyapatite coating in vivo: a comparative study of bone contact and bone growth induction.

PubMed

Grandfield, Kathryn; Palmquist, Anders; Gonçalves, Stéphane; Taylor, Andy; Taylor, Mark; Emanuelsson, Lena; Thomsen, Peter; Engqvist, Håkan

2011-04-01

The current study evaluates the in vivo response to free form fabricated cobalt chromium (CoCr) implants with and without hydroxyapatite (HA) plasma sprayed coatings. The free form fabrication method allowed for integration of complicated pyramidal surface structures on the cylindrical implant. Implants were press fit into the tibial metaphysis of nine New Zealand white rabbits. Animals were sacrificed and implants were removed and embedded. Histological analysis, histomorphometry and electron microscopy studies were performed. Focused ion beam was used to prepare thin sections for high-resolution transmission electron microscopy examination. The fabricated features allowed for effective bone in-growth and firm fixation after 6 weeks. Transmission electron microscopy investigations revealed intimate bone-implant integration at the nanometre scale for the HA coated samples. In addition, histomorphometry revealed a significantly higher bone contact on HA coated implants compared to native CoCr implants. It is concluded that free form fabrication in combination with HA coating improves the early fixation in bone under experimental conditions.

Acute and Subacute Toxicity In Vivo of Thermal-Sprayed Silver Containing Hydroxyapatite Coating in Rat Tibia

PubMed Central

Tsukamoto, Masatsugu; Miyamoto, Hiroshi; Ando, Yoshiki; Eto, Shuichi; Akiyama, Takayuki; Yonekura, Yutaka; Mawatari, Masaaki

2014-01-01

To reduce the incidence of implant-associated infection, we previously developed a novel coating technology using hydroxyapatite (HA) containing silver (Ag). This study examined in vivo acute and subacute toxicity associated with the Ag-HA coating in rat tibiae. Ten-week-old rats received implantation of HA-, 2% Ag-HA-, or 50% Ag-HA-coated titanium rods. Concentrations of silver in serum, brain, liver, kidneys, and spleen were measured in the acute phase (2–4 days after treatment) and subacute phase (4–12 weeks after treatment). Biochemical and histological examinations of those organs were also performed. Mean serum silver concentration peaked in the acute phase and then gradually decreased. Mean silver concentrations in all examined organs from the 2% Ag-HA coating groups showed no significant differences compared with the HA coating group. No significant differences in mean levels of glutamic-oxaloacetic transaminase, glutamic-pyruvic transaminase, lactate dehydrogenase, creatinine, or blood urea nitrogen were seen between the three groups and controls. Histological examinations of all organs revealed no abnormal pathologic findings. No acute or subacute toxicity was seen in vivo for 2% Ag-HA coating or HA coating. Ag-HA coatings on implants may represent biologically safe antibacterial biomaterials and may be of value for reducing surgical-site infections related to implantation. PMID:24779019

Alternate Spray-coating for the Direct Fabrication of Hydroxyapatite Films without Crystal Growth Step in Solution.

PubMed

Watanabe, Satoshi; Kashiwagi, Rei; Matsumoto, Mutsuyoshi

2017-03-01

We discuss an alternate spray-coating technique for the direct fabrication of hydroxyapatite films using metal masks, suction-type spray nozzles and two calcification solutions of calcium hydroxide and phosphoric acid aqueous solutions. Hydroxyapatite films were formed only on the hydrophobic surface of the substrates. Scanning electron microscopy and energy dispersive X-ray spectroscopy showed that the spray-coated films consisted of hydroxyapatite nanoparticles. The Ca/P ratio was estimated to be about 1.26. X-ray diffraction patterns of the spray-coated films almost coincided with those of the hydroxyapatite powders, showing that the spray-coated films consisted of hydroxyapatite nanoparticles. Dot arrays of hydroxyapatite films at a diameter of 100 μm were formed by tuning the concentrations of calcium hydroxide and phosphoric acid aqueous solutions. This technique allows for the direct fabrication of the hydroxyapatite films without crystal growth process in hydroxyapatite precursors, the scaffolds of crystal growth such as biocompatibility SiO 2 -CaO glasses, or electrophoresis processes. By using this technique, large-area ceramic films with biocompatibility will be micropatterned with minimized material consumption, short fabrication time, and reduced equipment investments.

Hydroxyapatite, fluor-hydroxyapatite and fluorapatite produced via the sol-gel method: bonding to titanium and scanning electron microscopy.

PubMed

Tredwin, Christopher J; Georgiou, George; Kim, Hae-Won; Knowles, Jonathan C

2013-05-01

Hydroxyapatite (HA), fluor-hydroxyapatite (FHA) with varying levels of fluoride ion substitution and fluorapatite (FA) production has been characterised and optimised by the sol-gel method and the dissolution and biological properties of these materials were investigated. It was the objective of this study to investigate the potential bond strength and interaction of these materials with titanium. HA, FHA and FA were synthesised by a sol-gel method. Calcium nitrate and triethyl phosphite were used as precursors under an ethanol-water based solution. Different amounts of ammonium fluoride (NH4F) were incorporated for the preparation of the FHA and FA sol-gels. Using a spin coating technique the sol-gels were coated onto commercially pure titanium disks and crystallised at various temperatures. Using scanning electron microscopy (SEM) and elemental analysis, the surface characteristics, coating thickness and interaction of the Ti substrate and coating were investigated. The bond strengths of the coating to the Ti were investigated using an Instron Universal Load Testing Machine. Statistical analysis was performed with a two-way analysis of variance and post hoc testing with a Bonferroni correction. (1) Coating speed inversely influenced the coating thickness. (2) Increasing fluoride ion substitution and heating temperature significantly increased bond strength and (3) increasing fluoride ion substitution increased the coating thickness. FHA and FA synthesised using the sol-gel technique may offer a superior alternative to coating titanium implants with HA and plasma spraying. HA, FHA and FA materials synthesised by the sol-gel method may also have a use as bone grafting materials. Copyright © 2013 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Nanophase hydroxyapatite coatings for dental and orthopedic applications

NASA Astrophysics Data System (ADS)

Sato, Michiko

In order to improve dental and orthopedic implant performance, the objective of this study was to synthesize nanocrystalline hydroxyapatite (HA) powders to coat metals (specifically, titanium and tantalum). Precipitated HA powders were either sintered in order to produce UltraCaP HA (or microcrystalline size HA) or were treated hydrothermally to produce nanocrystalline HA. Some of the UltraCaP and nanocrystalline HA powders were doped with yttrium (Y) since previous in vitro studies demonstrated that Y-doped HA in bulk improved osteoblast (or bone-forming cell) function over undoped HA. The nanocrystalline HA powders were also mixed with nanophase titania powders because previous studies demonstrated that titania/HA composite coatings increased coating adhesive strength and HA nucleation. These powders were then deposited onto titanium by a novel room-temperature process, called IonTiteT(TM). The results demonstrated that the chemical properties and crystallite size of the original HA powders were maintained in the coatings. More importantly, in vitro studies showed increased osteoblast (bone-forming cell) adhesion on the single phase nanocrystalline HA and nano-titania/HA coatings compared to traditionally used plasma-sprayed HA coatings and uncoated metals. Results further demonstrated greater amounts of calcium deposition by osteoblasts cultured on nanocrystalline HA coatings compared to UltraCaP coatings and conventionally used plasma-sprayed HA coatings. To elucidate mechanisms that influenced osteoblast functions on the HA coatings, the amount of proteins (fibronectin and vitronectin) onto the HA powders and the adsorbed fibronectin conformation were investigated. Exposure of cell integrin binding domains (in fibronectin III10 segments) was greater in fibronectin adsorbed onto 1.2 mole% Y-doped UltraCaP HA coatings compared to nanocrystalline HA coatings tested. However, 1.2 mole% Y-doped UltraCaP HA coatings did not increase mineralization by osteoblasts compared to the nanocrystalline HA coatings. These results suggested that the availability of integrin binding domains in fibronectin did not correlate to enhanced mineralization by osteoblasts on nanocrystalline HA coatings. Lastly, undoped nanocrystalline HA coatings were studied using a well-established rat calvaria in vivo. Histological analysis showed that nanocrystalline HA coated on tantalum scaffolds increased bone and fibrous tissue infiltration into the scaffolds while uncoated and UltraCaP HA coated scaffolds did not after as early as 6 weeks. In summary, these results encourage further studies on nanocrystalline IonTiteTM HA coatings on various metals for orthopedic and dental applications.

The effects of hydroxyapatite coating and bone allograft on fixation of loaded experimental primary and revision implants.

PubMed

Søballe, Kjeld; Mouzin, Olivier R G; Kidder, Louis A; Overgaard, Søren; Bechtold, Joan E

2003-06-01

We used our established experimental model of revision joint replacement to examine the roles of hydroxyapatite coating and bone graft in improving the fixation of revision implants. The revision protocol uses the Søballe micromotion device in a preliminary 8-week period of implant instability for the presence of particulate polyethylene. During this procedure, a sclerotic endosteal bone rim forms, and a dense fibrous membrane is engendered, having macrophages with ingested polyethylene and high levels of inflammatory cytokines. At the time of revision after 8 weeks, the cavity is revised with either a titanium alloy (Ti) or a hydroxyapatite (HA) 6.0 mm plasma-sprayed implant, in the presence or absence of allograft packed into the initial 0.75 mm peri-implant gap. The contralateral limb is subjected to primary surgery with the same implant configuration, and serves as control. 8 implants were included in each of the 8 treatment groups (total 64 implants in 32 dogs). The observation period was 4 weeks after revision. Outcome measures are based on histomorphometry and mechanical pushout properties. The revision setting was always inferior to its primary counterpart. Bone graft improved the revision fixation in all treatment groups, as also did the HA coating. The sole exception was revision-grafted HA implants, which reached the same fixation as primary Ti and HA grafted implants. The revision, which was less active in general, seems to need the dual stimulation of bone graft and HA implant surface, to obtain the same level of fixation associated with primary implants. Our findings suggest that the combination of HA implant and bone graft may be of benefit in the clinical revision implant setting.

The effects of hydroxyapatite coating and bone allograft on fixation of loaded experimental primary and revision implants

PubMed Central

Søballe, Kjeld; Mouzin, Olivier R G; Kidder, Louis A; Overgaard, Søren; Bechtold, Joan E

2015-01-01

We used our established experimental model of revision joint replacement to examine the roles of hydroxyapatite coating and bone graft in improving the fixation of revision implants. The revision protocol uses the Søballe micromotion device in a preliminary 8-week period of implant instability for the presence of particulate polyethylene. During this procedure, a sclerotic endosteal bone rim forms, and a dense fibrous membrane is engendered, having macrophages with ingested polyethylene and high levels of inflammatory cytokines. At the time of revision after 8 weeks, the cavity is revised with either a titanium alloy (Ti) or a hydroxyapatite (HA) 6.0 mm plasma-sprayed implant, in the presence or absence of allograft packed into the initial 0.75 mm peri-implant gap. The contralateral limb is subjected to primary surgery with the same implant configuration, and serves as control. 8 implants were included in each of the 8 treatment groups (total 64 implants in 32 dogs). The observation period was 4 weeks after revision. Outcome measures are based on histomorphometry and mechanical pushout properties. The revision setting was always inferior to its primary counterpart. Bone graft improved the revision fixation in all treatment groups, as also did the HA coating. The sole exception was revision-grafted HA implants, which reached the same fixation as primary Ti and HA grafted implants. The revision, which was less active in general, seems to need the dual stimulation of bone graft and HA implant surface, to obtain the same level of fixation associated with primary implants. Our findings suggest that the combination of HA implant and bone graft may be of benefit in the clinical revision implant setting. PMID:12899541

Hydroxyapatite coatings deposited by liquid precursor plasma spraying: controlled dense and porous microstructures and osteoblastic cell responses.

PubMed

Huang, Yi; Song, Lei; Liu, Xiaoguang; Xiao, Yanfeng; Wu, Yao; Chen, Jiyong; Wu, Fang; Gu, Zhongwei

2010-12-01

Hydroxyapatite coatings were deposited on Ti-6Al-4V substrates by a novel plasma spraying process, the liquid precursor plasma spraying (LPPS) process. X-ray diffraction results showed that the coatings obtained by the LPPS process were mainly composed of hydroxyapatite. The LPPS process also showed excellent control on the coating microstructure, and both nearly fully dense and highly porous hydroxyapatite coatings were obtained by simply adjusting the solid content of the hydroxyapatite liquid precursor. Scanning electron microscope observations indicated that the porous hydroxyapatite coatings had pore size in the range of 10-200 µm and an average porosity of 48.26 ± 0.10%. The osteoblastic cell responses to the dense and porous hydroxyapatite coatings were evaluated with human osteoblastic cell MG-63, in respect of the cell morphology, proliferation and differentiation, with the hydroxyapatite coatings deposited by the atmospheric plasma spraying (APS) process as control. The cell experiment results indicated that the heat-treated LPPS coatings with a porous structure showed the best cell proliferation and differentiation among all the hydroxyapatite coatings. Our results suggest that the LPPS process is a promising plasma spraying technique for fabricating hydroxyapatite coatings with a controllable microstructure, which has great potential in bone repair and replacement applications.

Characteristics of hydroxyapatite coated titanium porous coatings on Ti-6Al-4V substrates by plasma sprayed method.

PubMed

Yang, C Y; Chen, C R; Chang, E; Lee, T M

2007-08-01

A porous metal coating applied to solid substrate implants has been shown, in vivo, to anchor implants by bone ingrowth. Calcium phosphate ceramics, in particular hydroxyapatite [Ca(10)(PO(4))(6)(OH)(2), HA], are bioactive ceramics, which are known to be biocompatible and osteoconductive, and these ceramics deposited on to porous-coated devices may enhance bone ingrowth and implant fixation. In this study, bi-feedstock of the titanium powder and composite (Na(2)CO(3)/HA) powder were simultaneously deposited on a Ti-6Al-4V substrate by a plasma sprayed method. At high temperature of plasma torch, the solid state of Na(2)CO(3) would decompose to release CO(2) gas and then eject the molten Ti powder to induce the interconnected pores in the coatings. After cleaning and soaking in deionized water, the residual Na(2)CO(3) in the coating would dissolve to form the open pores, and the HA would exist at the surface of pores in the inner coatings. By varying the particle size of the composite powder, the porosity of porous coating could be varied from 25.0 to 34.0%, and the average pore size of the porous coating could be varied to range between 158.5 and 202.0 microm. Using a standard adhesive test (ASTM C-633), the bonding strength of the coating is between 27.3 and 38.2 MPa. By SEM, the HA was observed at the surface of inner pore in the porous coating. These results suggest that the method exhibits the potential to manufacture the bioactive ceramics on to porous-coated specimen to achieve bone ingrowth fixation for biomedical applications.

[Study on the antibacterial activity of four kinds of nano-hydroxyapatite composites against Enterococcus faecalis].

PubMed

Liu, Yi; Zhou, Rongjing; Wu, Hongkun

2015-06-01

This study aims to compare and determine a kind of nano-hydroxyapatite composite material with good antibacterial efficacy on Enterococcusfaecalis (E. faecalis) in vitro. We investigated the antimicrobial activity of four kinds of nano-hydroxyapatite composites, namely, silver/hydroxyapatite composite nanoparticles (Ag/nHA), yttrium/hydroxyapatite composite nanoparticles (Yi/nHA), cerium/hydroxyapatite composite nanoparticles (Ce/nHA), and hydroxyapatite nanoparticles (nHA), against E. faecalis in vitro using the agar diffusion and broth dilution method by measuring the growth inhibition zone and the minimum inhibitory concentration (MIC), respectively. The agar diffusion test results showed that Ag/nHA displayed an obvious growth inhibition zone, whereas Yi/nHA, Ce/nHA, and nHA showed no influence on E. faecalis. The MIC value of Ag/nHA was 1.0 g.L-1, and the three other materials had no effect on E.faecalis even at the high concentration of 32.0 g.L-1. Ag/nHA display a potential antimicrobial efficacy to planktonic E.faecalis. Whereas, the three other kinds of nano-hydroxyapatite composites (Yi/nHA, Ce/nHA, nHA) show no influence.

Coupling of HDPE/hydroxyapatite composites by silane-based methodologies.

PubMed

Sousa, R A; Reis, R L; Cunha, A M; Bevis, M J

2003-06-01

Several coupling treatments based on silane chemicals were investigated for the development of high density (HDPE)/hydroxyapatite (HA) composites. Two HA powders, sintered HA (HAs) and non sintered HA (HAns), were studied in combination with five silanes, namely y-methacryloxy propyltrimethoxy silane (MEMO), 3-(2-aminoethyl)aminopropyltrimethoxy silane (DAMO), vinyltrimethoxy silane (VTMO), 3-aminopropyltriethoxy silane (AMEO) and trimethoxypropyl silane (PTMO). The HA particles were treated by a dipping in method or by spraying with silane solutions. After drying, the treated powders were compounded with HDPE or HDPE with acrylic acid and/or organic peroxide and subsequently compression molded. The tensile test specimens obtained from the molded plates were tensile tested and their fracture surfaces were observed by scanning electron microscopy (SEM). For the sintered HA (HAs) composites, the most effective coupling treatments concerning stiffness are those based on MEMO and AMEO. The low influence of these coupling procedures on strength is believed to be associated to the low volume fraction and the relatively smooth surface of the used HA particles. For the non-sintered HA (HAns) composites, it was possible to improve significantly both the stiffness and the strength. Amino silanes demonstrated to be highly efficient concerning strength enhancement. The higher effectiveness of the coupling treatments for HAns filled composites is attributed to their higher particle surface area, smaller particle size distribution and expected higher chemical reactivity. For both cases, the improvement in mechanical performance after the coupling treatment is consistent with the enhancement in interfacial adhesion observed by SEM.

Bone integration capability of nanopolymorphic crystalline hydroxyapatite coated on titanium implants

PubMed Central

Yamada, Masahiro; Ueno, Takeshi; Tsukimura, Naoki; Ikeda, Takayuki; Nakagawa, Kaori; Hori, Norio; Suzuki, Takeo; Ogawa, Takahiro

2012-01-01

The mechanism by which hydroxyapatite (HA)-coated titanium promotes bone–implant integration is largely unknown. Furthermore, refining the fabrication of nano-structured HA to the level applicable to the mass production process for titanium implants is challenging. This study reports successful creation of nanopolymorphic crystalline HA on microroughened titanium surfaces using a combination of flame spray and low-temperature calcination and tests its biological capability to enhance bone–implant integration. Sandblasted microroughened titanium implants and sandblasted + HA-coated titanium implants were subjected to biomechanical and histomorphometric analyses in a rat model. The HA was 55% crystallized and consisted of nanoscale needle-like architectures developed in various diameters, lengths, and orientations, which resulted in a 70% increase in surface area compared to noncoated microroughened surfaces. The HA was free from impurity contaminants, with a calcium/phosphorus ratio of 1.66 being equivalent to that of stoichiometric HA. As compared to microroughened implants, HA-coated implants increased the strength of bone–implant integration consistently at both early and late stages of healing. HA-coated implants showed an increased percentage of bone–implant contact and bone volume within 50 μm proximity of the implant surface, as well as a remarkably reduced percentage of soft tissue intervention between bone and the implant surface. In contrast, bone volume outside the 50 μm border was lower around HA-coated implants. Thus, this study demonstrated that the addition of pure nanopolymorphic crystalline HA to microroughened titanium not only accelerates but also enhances the level of bone–implant integration and identified the specific tissue morphogenesis parameters modulated by HA coating. In particular, the nanocrystalline HA was proven to be drastic in increasing osteoconductivity and inhibiting soft tissue infiltration, but the effect was limited to the immediate microenvironment surrounding the implant. PMID:22359461

Preparation of bone-implants by coating hydroxyapatite nanoparticles on self-formed titanium dioxide thin-layers on titanium metal surfaces.

PubMed

Wijesinghe, W P S L; Mantilaka, M M M G P G; Chathuranga Senarathna, K G; Herath, H M T U; Premachandra, T N; Ranasinghe, C S K; Rajapakse, R P V J; Rajapakse, R M G; Edirisinghe, Mohan; Mahalingam, S; Bandara, I M C C D; Singh, Sanjleena

2016-06-01

Preparation of hydroxyapatite coated custom-made metallic bone-implants is very important for the replacement of injured bones of the body. Furthermore, these bone-implants are more stable under the corrosive environment of the body and biocompatible than bone-implants made up of pure metals and metal alloys. Herein, we describe a novel, simple and low-cost technique to prepare biocompatible hydroxyapatite coated titanium metal (TiM) implants through growth of self-formed TiO2 thin-layer (SFTL) on TiM via a heat treatment process. SFTL acts as a surface binder of HA nanoparticles in order to produce HA coated implants. Colloidal HA nanorods prepared by a novel surfactant-assisted synthesis method, have been coated on SFTL via atomized spray pyrolysis (ASP) technique. The corrosion behavior of the bare and surface-modified TiM (SMTiM) in a simulated body fluid (SBF) medium is also studied. The highest corrosion rate is found to be for the bare TiM plate, but the corrosion rate has been reduced with the heat-treatment of TiM due to the formation of SFTL. The lowest corrosion rate is recorded for the implant prepared by heat treatment of TiM at 700 °C. The HA-coating further assists in the passivation of the TiM in the SBF medium. Both SMTiM and HA coated SMTiM are noncytotoxic against osteoblast-like (HOS) cells and are in high-bioactivity. The overall production process of bone-implant described in this paper is in high economic value. Copyright © 2016 Elsevier B.V. All rights reserved.

Methods of synthesizing hydroxyapatite powders and bulk materials

DOEpatents

Luo, Ping

1999-01-12

Methods are provided for producing non-porous controlled morphology hydroxyapatite granules of less than 8 .mu.m by a spray-drying process. Solid or hollow spheres or doughnuts can be formed by controlling the volume fraction and viscosity of the slurry as well as the spray-drying conditions. Methods of providing for homogenous cellular structure hydroxyapatite granules are also provided. Pores or channels or varying size and number can be formed by varying the temperature at which a hydroxyapatite slurry formed in basic, saturated ammonium hydroxide is spray-dried. Methods of providing non-porous controlled morphology hydroxyapatite granules in ammonium hydroxide are also provided. The hydroxyapatite granules and bulk materials formed by these methods are also provided.

Methods of synthesizing hydroxyapatite powders and bulk materials

DOEpatents

Luo, P.

1999-01-12

Methods are provided for producing non-porous controlled morphology hydroxyapatite granules of less than 8 {micro}m by a spray-drying process. Solid or hollow spheres or doughnuts can be formed by controlling the volume fraction and viscosity of the slurry as well as the spray-drying conditions. Methods of providing for homogeneous cellular structure hydroxyapatite granules are also provided. Pores or channels or varying size and number can be formed by varying the temperature at which a hydroxyapatite slurry formed in basic, saturated ammonium hydroxide is spray-dried. Methods of providing non-porous controlled morphology hydroxyapatite granules in ammonium hydroxide are also provided. The hydroxyapatite granules and bulk materials formed by these methods are also provided. 26 figs.

Development of HA/Ag-NPs Composite Coating from Green Process for Hip Applications.

PubMed

Lozoya-Rodríguez, Denisse A; de Lima, Renata; Fraceto, Leonardo F; Ledezma Pérez, Antonio; Bazaldua Domínguez, Mercedes; Gómez Batres, Roberto; Reyes Rojas, Armando; Orozco Carmona, Víctor

2017-08-08

In the present study, biological hydroxyapatite (HA) was obtained from bovine bones through a thermal process. A total of 0% and 1% of silver nanoparticles (Ag-NPs) synthesized from Opuntia ficus (nopal) were added to the biological hydroxyapatite coatings using an atmospheric plasma spray (APS) on a Ti6Al4V substrate. Following this, its antimicrobial efficiency was evaluated against the following bacterial strains: Escherichia coli , Staphylococcus aureus , and Pseudomonas aeruginosa . This was conducted according to the Japanese Industrial Standard (JIS) Z2801:2000 "Antimicrobial Product-Test for Antimicrobial Activity and Efficacy". Scanning electron microscopy (SEM) showed that the silver nanoparticles (Ag-NPs) were evenly distributed on the coating surface. Energy dispersive X-ray spectroscopy (EDX) shows that apatite deposition occurs on a daily basis, maintaining a Ca/P rate between 2.12 and 1.45. Biocompatibility properties were evaluated with osteoblast-like cells (MC3T3-E1) by single-cell gel electrophoresis assay and Tali image cytometry.

Structure of Biocompatible Coatings Produced from Hydroxyapatite Nanoparticles by Detonation Spraying

NASA Astrophysics Data System (ADS)

Nosenko, Valentyna; Strutynska, Nataliia; Vorona, Igor; Zatovsky, Igor; Dzhagan, Volodymyr; Lemishko, Sergiy; Epple, Matthias; Prymak, Oleg; Baran, Nikolai; Ishchenko, Stanislav; Slobodyanik, Nikolai; Prylutskyy, Yuriy; Klyui, Nickolai; Temchenko, Volodymyr

2015-12-01

Detonation-produced hydroxyapatite coatings were studied by scanning electron microscopy (SEM), X-ray powder diffraction (XRD), Raman spectroscopy, and electron paramagnetic resonance (EPR) spectroscopy. The source material for detonation spraying was a B-type carbonated hydroxyapatite powder. The coatings consisted of tetracalcium phosphate and apatite. The ratio depended slightly on the degree of crystallinity of the initial powder and processing parameters of the coating preparation. The tetracalcium phosphate phase was homogeneous; the apatite phase contained defects localized on the sixfold axis and consisted of hydroxyapatite and oxyapatite. Technological factors contributing to the transformation of hydroxyapatite powder structure during coating formation by detonation spraying are discussed.

Structure of Biocompatible Coatings Produced from Hydroxyapatite Nanoparticles by Detonation Spraying.

PubMed

Nosenko, Valentyna; Strutynska, Nataliia; Vorona, Igor; Zatovsky, Igor; Dzhagan, Volodymyr; Lemishko, Sergiy; Epple, Matthias; Prymak, Oleg; Baran, Nikolai; Ishchenko, Stanislav; Slobodyanik, Nikolai; Prylutskyy, Yuriy; Klyui, Nickolai; Temchenko, Volodymyr

2015-12-01

Detonation-produced hydroxyapatite coatings were studied by scanning electron microscopy (SEM), X-ray powder diffraction (XRD), Raman spectroscopy, and electron paramagnetic resonance (EPR) spectroscopy. The source material for detonation spraying was a B-type carbonated hydroxyapatite powder. The coatings consisted of tetracalcium phosphate and apatite. The ratio depended slightly on the degree of crystallinity of the initial powder and processing parameters of the coating preparation. The tetracalcium phosphate phase was homogeneous; the apatite phase contained defects localized on the sixfold axis and consisted of hydroxyapatite and oxyapatite. Technological factors contributing to the transformation of hydroxyapatite powder structure during coating formation by detonation spraying are discussed.

Hydroxyapatite-nanotube composites and coatings for orthopedic applications

NASA Astrophysics Data System (ADS)

Lahiri, Debrupa

Hydroxyapatite (HA) has received wide attention in orthopedics, due to its biocompatibility and osseointegration ability. Despite these advantages, the brittle nature and low fracture toughness of HA often results in rapid wear and premature fracture of implant. Hence, there is a need to improve the fracture toughness and wear resistance of HA without compromising its biocompatibility. The aim of the current research is to explore the potential of nanotubes as reinforcement to HA for orthopedic implants. HA- 4 wt.% carbon nanotube (CNT) composites and coatings are synthesized by spark plasma sintering and plasma spraying respectively, and investigated for their mechanical, tribological and biological behavior. CNT reinforcement improves the fracture toughness (>90%) and wear resistance (>66%) of HA for coating and free standing composites. CNTs have demonstrated a positive influence on the proliferation, differentiation and matrix mineralization activities of osteoblasts, during in-vitro biocompatibility studies. In-vivo exposure of HA-CNT coated titanium implant in animal model (rat) shows excellent histocompatibility and neobone integration on the implant surface. The improved osseointegration due to presence of CNTs in HA is quantified by the adhesion strength measurement of single osteoblast using nano-scratch technique. Considering the ongoing debate about cytotoxicity of CNTs in the literature, the present study also suggests boron nitride nanotube (BNNT) as an alternative reinforcement. BNNT with the similar elastic modulus and strength as CNT, were added to HA. The resulting composite having 4 wt.% BNNTs improved the fracture toughness (˜85%) and wear resistance (˜75%) of HA in the similar range as HA-CNT composites. BNNTs were found to be non-cytotoxic for osteoblasts and macrophages. In-vitro evaluation shows positive role of BNNT in osteoblast proliferation and viability. Apatite formability of BNNT surface in ˜4 days establishes its osseointegration ability.

Optimization of implant/bone attachment: The effects of implant surface porosity, bioactive ceramic coatings, and delivery of adsorbed growth factors

NASA Astrophysics Data System (ADS)

Melican, Mora Carolynne

Various surface treatments and coating materials have been tested for use on metal alloy orthopaedic implants. Their purpose has been to enhance the bioactivity of the implant surfaces, and thus to increase the rate and degree of bony attachment in vivo in an attempt to hasten recovery time, increase implant service lifetime, and lessen pain associated with loosened orthopaedic implants. A series of in vivo and in vitro studies were performed to determine the influence of different implant surfaces including porous metal surfaces with varied porosity with depth, resorbable and non-resorbable plasma-sprayed hydroxyapatite (HA) coatings, and finally HA coatings with an adsorbed layer of human recombinant bone morphogenetic protein (rhBMP-2), an osteoinductive protein. Textured as-cast metal surfaces produced by investment casting in three dimensionally printed ceramic molds have exhibited superior bony ingrowth and attachment. Plasma-sprayed HA coatings have been shown to be appropriate substrates for osteoblast proliferation (particularly on highly crystalline HA) and stem cell proliferation (particularly on less crystalline HA). Less crystalline HA coatings have shown promise as delivery systems for different levels of rhBMP-2. The osteoinductive protein has been shown to remain active after delivery to the system, and was most effective when delivered in concentrations ranging from 30 to 50 ng/ml. Combinations of these surface treatments for metal implant surfaces warrant further investigation.

HA and double-layer HA-P2O5/CaO glass coatings: influence of chemical composition on human bone marrow cells osteoblastic behavior.

PubMed

Ferraz, M P; Fernandes, M H; Santos, J D; Monteiro, F J

2001-07-01

Human osteoblastic bone marrow derived cells were cultured for 28 days onto the surface of a glass reinforced hydroxyapatite (HA) composite and a commercial type HA plasma sprayed coatings, both in the "as-received" condition and after an immersion treatment with culture medium during 21 days. Cell proliferation and differentiation were analyzed as a function of the chemical composition of the coatings and the immersion treatment. Cell attachment, growth and differentiation of osteoblastic bone marrow cells seeded onto "as-received" plasma sprayed coatings were strongly affected by the time-dependent variation of the surface structure occurring during the first hours of culture. Initial interactions leading to higher amounts of adsorbed protein and zeta potential shifts towards negative charges appeared to result in surface structures with better biological performance. Cultures grown onto the pretreated coatings showed higher rate of cell proliferation and increased functional activity, as compared to those grown onto the corresponding "as-received" materials. However, the cell behavior was similar in the glass composite and HA coatings. The results showed that the glass composites present better characteristics for bone cell growth and function than HA. In addition, this work also provide evidence that the biological performance of the glass composites can be modulated and improved by manipulations in the chemical composition, namely in the content of glass added to HA. Copyright 2001 Kluwer Academic Publishers

Decreased Staphylococcus aureus and increased osteoblast density on nanostructured electrophoretic-deposited hydroxyapatite on titanium without the use of pharmaceuticals.

PubMed

Mathew, Dennis; Bhardwaj, Garima; Wang, Qi; Sun, Linlin; Ercan, Batur; Geetha, Manisavagam; Webster, Thomas J

2014-01-01

Plasma-spray deposition of hydroxyapatite on titanium (Ti) has proven to be a suboptimal solution to improve orthopedic-implant success rates, as demonstrated by the increasing number of orthopedic revision surgeries due to infection, implant loosening, and a myriad of other reasons. This could be in part due to the high heat involved during plasma-spray deposition, which significantly increases hydroxyapatite crystal growth into the nonbiologically inspired micron regime. There has been a push to create nanotopographies on implant surfaces to mimic the physiological nanostructure of native bone and, thus, improve osteoblast (bone-forming cell) functions and inhibit bacteria functions. Among the several techniques that have been adopted to develop nanocoatings, electrophoretic deposition (EPD) is an attractive, versatile, and effective material-processing technique. The in vitro study reported here aimed to determine for the first time bacteria responses to hydroxyapatite coated on Ti via EPD. There were six and three times more osteoblasts on the electrophoretic-deposited hydroxyapatite on Ti compared with Ti (control) and plasma-spray-deposited hydroxyapatite on Ti after 5 days of culture, respectively. Impressively, there were 2.9 and 31.7 times less Staphylococcus aureus on electrophoretic-deposited hydroxyapatite on Ti compared with Ti (control) and plasma-spray-deposited hydroxyapatite on Ti after 18 hours of culture, respectively. Compared with uncoated Ti and plasma-sprayed hydroxyapatite coated on Ti, the results provided significant promise for the use of EPD to improve bone-cell density and be used as an antibacterial coating without resorting to the use of antibiotics.

X-ray and neutron diffraction studies of crystallinity in hydroxyapatite coatings.

PubMed

Girardin, E; Millet, P; Lodini, A

2000-02-01

To standardize industrial implant production and make comparisons between different experimental results, we have to be able to quantify the crystallinity of hydroxyapatite. Methods of measuring crystallinity ratio were developed for various HA samples before and after plasma spraying. The first series of methods uses X-ray diffraction. The advantage of these methods is that X-ray diffraction equipment is used widely in science and industry. In the second series, a neutron diffraction method is developed and the results recorded are similar to those obtained by the modified X-ray diffraction methods. The advantage of neutron diffraction is the ability to obtain measurements deep inside a component. It is a nondestructive method, owing to the very low absorption of neutrons in most materials. Copyright 2000 John Wiley & Sons, Inc.

[Cytocompatibility of nanophase hydroxyapatite ceramics].

PubMed

Wen, Bo; Chen, Zhi-qing; Jiang, Yin-shan; Yang, Zheng-wen; Xu, Yong-zhong

2004-12-01

To evaluate the cytocompatibility of nanophase hydroxyapatite ceramics in vitro. Hydroxyapatite (HA) was prepared via wet method. The grain size of the hydroxyapatite in the study was determined by scanning electron microscope and atomic force microscope with image analysis software. Primary osteoblast culture was established from rat calvaria. Cell adherence and proliferation on nanophase hydroxyapatite ceramics and conventional hydroxyapatite ceramics were examined at 1, 3, 5, 7 days. Morphology of the cells was observed by microscope. The average grain size of the nanophase and conventional HA was 55 nm and 780 nm, respectively. Throughout 7 days period, osteoblast proliferation on the HA was similar to that on tissue culture borosilicate glass controls, osteoblasts could attach, spread and proliferate on HA. However, compared to conventional ceramics, osteoblast proliferation on nanophase HA was significantly better after 1, 3, 5 and 7 days. Cytocompatibility of nanophase HA was significantly better than conventional ceramics.

Calcium phosphate coating on titanium using laser and plasma spray

NASA Astrophysics Data System (ADS)

Roy, Mangal

Though calcium phosphate (CaP) coated implants are commercially available, its acceptance is still not wide spread due to challenges related to weaker interfacial bonding between metal and ceramic, and low crystallinity of hydroxyapatite (HA). The objectives of this research are to improve interfacial strength, crystallinity, phase purity and bioactivity of CaP coated metallic implants for orthopaedic applications. The rationale is that forming a diffuse and gradient metal-ceramic interface will improve the interfacial strength. Moreover, reducing CaP particles exposure to high temperature during coating preparation, can lead to improvement in both crystallinity and phase purity of CaP. In this study, laser engineered net shaping (LENS(TM)) was used to coat Ti metal with CaP. LENS(TM) processing enabled generation of Ti+TCP (tricalcium phosphate) composite coating with diffused interface, that also increased the coating hardness to 1049+/-112 Hv compared to a substrate hardness of 200+/-15 Hv. In vitro bone cell-material interaction studies confirmed the bioactivity of TCP coatings. Antimicrobial properties of the TCP coatings were improved by silver (Ag) electrodeposition. Along with LENS(TM), radio frequency induction plasma spray, equipped with supersonic plasma nozzle, was used to prepare HA coatings on Ti with improved crystallinity and phase purity. The coating was made of multigrain HA particles of ˜200 nm in size, which consisted of 15--20 nm HA grains. In vitro bone cell-material interaction and in vivo rat model studies confirmed the HA coatings to be bioactive. Furthermore, incorporation of Sr2+ improved bone cell of HA coatings interaction. A combination of LENS(TM) and plasma spray was used to fabricate a compositionally graded HA coatings on Ti where the microstructure varied from pure HA at the surface to pure Ti substrate with a diffused Ti+TCP composite region in between. The plasma spray system was used to synthesize spherical HA nano powder from HA sol, where the production rate was 20 g/h, which is only 16% of the total powder produced. The effects of Sr2+ and Mg2+ doping on bone cell-CaP interaction was further studied with osteoclast cells. Mg2+ doing was found to be an effective way of controlling osteoclast differentiation.

The macroscopic, microscopic and spectrometric effects of various chemotherapeutic agents on the plasma-sprayed hydroxyapatite-coated implant surface.

PubMed

Zablotsky, M; Meffert, R; Mills, O; Burgess, A; Lancaster, D

1992-12-01

The purpose of this research was to determine the nature of the residual hydroxyapatite (HA)-coated implant surface after treatment with various chemotherapeutic modalities, including: citric acid, chlorhexidine gluconate, hydrogen peroxide, tetracycline HCl, stannous fluoride, polymyxin B and a prototype plastic Cavitron tip. Implant surfaces were evaluated macroscopically, microscopically (scanning electron microscopy (SEM)) and spectrometrically (energy-dispersive spectrometry and X-ray diffraction). HA-substrate bond strength and dissolution testing was also performed for surfaces treated with a supersaturated citric acid solution. All treatments left either microscopic residues or a loss of surface roughness when viewed on SEM. A 30- to 60-s application of citric acid left a significantly greater coating thickness than all other treatments, whereas a 3-min application of citric acid removed significantly more HA than untreated controls. Significant changes in Ca/P ratios were seen with most treatments. The clinical significance of this phenomenon is not known. No treatments altered the crystallinity of the residual HA coating. A 1-min application of citric acid did not significantly alter the tensile bond strength of the coating to the substrate. The clinical significance of these findings is not known at present. However, when taken with results from previous studies, it appears that in treating the infected HA-coated implant surface, a 30- to 60-s application of citric acid (pH 1) may be beneficial in detoxifying the HA coating prior to regenerative procedures. Further in vitro and in vivo studies are necessary to evaluate the biological response to citric acid when used to detoxify the infected implant surface.

Effect of precursor concentration and spray pyrolysis temperature upon hydroxyapatite particle size and density.

PubMed

Cho, Jung Sang; Lee, Jeong-Cheol; Rhee, Sang-Hoon

2016-02-01

In the synthesis of hydroxyapatite powders by spray pyrolysis, control of the particle size was investigated by varying the initial concentration of the precursor solution and the pyrolysis temperature. Calcium phosphate solutions (Ca/P ratio of 1.67) with a range of concentrations from 0.1 to 2.0 mol/L were prepared by dissolving calcium nitrate tetrahydrate and diammonium hydrogen phosphate in deionized water and subsequently adding nitric acid. Hydroxyapatite powders were then synthesized by spray pyrolysis at 900°C and at 1500°C, using these calcium phosphate precursor solutions, under the fixed carrier gas flow rate of 10 L/min. The particle size decreased as the precursor concentration decreased and the spray pyrolysis temperature increased. Sinterability tests conducted at 1100°C for 1 h showed that the smaller and denser the particles were, the higher the relative densities were of sintered hydroxyapatite disks formed from these particles. The practical implication of these results is that highly sinterable small and dense hydroxyapatite particles can be synthesized by means of spray pyrolysis using a low-concentration precursor solution and a high pyrolysis temperature under a fixed carrier gas flow rate. © 2015 Wiley Periodicals, Inc.

Nano-crystalline hydroxyapatite bio-mineral for the treatment of strontium from aqueous solutions.

PubMed

Handley-Sidhu, Stephanie; Renshaw, Joanna C; Yong, Ping; Kerley, Robert; Macaskie, Lynne E

2011-01-01

Hydroxyapatites were analysed using electron microscopy, X-ray diffraction (XRD) and X-ray fluorescence (XRF) analysis. Examination of a bacterially produced hydroxyapatite (Bio-HA) by scanning electron microscopy showed agglomerated nano-sized particles; XRD analysis confirmed that the Bio-HA was hydroxyapatite, with an organic matter content of 7.6%; XRF analysis gave a Ca/P ratio of 1.55, also indicative of HA. The size of the Bio-HA crystals was calculated as ~25 nm from XRD data using the Scherrer equation, whereas Comm-HA powder size was measured as ≤ 50 μm. The nano-crystalline Bio-HA was ~7 times more efficient in removing Sr(2+) from synthetic groundwater than Comm-HA. Dissolution of HA as indicated by the release of phosphate into the solution phase was higher in the Comm-HA than the Bio-HA, indicating a more stable biomaterial which has a potential for the remediation of contaminated sites.

Ultrafine-grained commercially pure titanium and microstructure response to hydroxyapatite coating methods

NASA Astrophysics Data System (ADS)

Calvert, Kayla L.

Commercially pure titanium (cp-Ti) is an ideal biomaterial as it does not evoke an inflammatory foreign body response in the body. However, the low strength of cp-Ti prevents the use in most orthopaedic load bearing applications. Therefore, many metal orthopaedic implants are commonly made of higher strength metal alloys that are less biocompatible. Nanostructured materials exhibit superior mechanical properties compared to their conventional grain sized counterparts. Severe plastic deformation (SPD) of metals has been shown to produce nanostructured materials. SPD by machining is a single-step deformation route that refines the grain microstructure, to develop an ultrafine grained (UFG) microstructure. UFG cp-Ti strips were developed with induced shear strains of up to 4.0 using a machining-based process. Both Vickers microhardness evaluation and microstructural analysis were used to characterize the as-received (annealed) and machined states. For induced shear strains between 1.9 and 4.0 in grade 2 cp-Ti the hardness was increased from 188 +/- 7 kg/mm2 in the as-received state to between 244 +/- 6 and 264 +/- 12 kg/mm 2 in the as-machined state, corresponding to an increase in hardness between 31 and 41%. The microstructural analysis revealed a grain size reduction from 34 +/- 11 mum in the as-received state to ˜ 100 nm for machined grade 2-Ti. A complete annealing study suggested that recovery/recrystallization occurs between 300 and 400°C, with a significant hardness drop between 400 and 600°C, while grain growth is continuous, starting at the lowest annealing temperature of 300°C. Hydroxyapatite (HA) is commonly applied to orthopaedic devices to promote bone growth. Machined Ti strips were coated with HA using conventional plasma spray as well as two alternative low-temperature application routes (sol-gel with calcination and anodization with hydrothermal treatment) to evaluate the thermal influence on the UFG-Ti substrate. Plasma spray produced a thick (20 to 70 mum) HA crystalline coating, sol-gel followed by calcination did not produce crystalline HA, while anodization with the proper hydrothermal treatment yielded a homogenous crystalline HA coating 5 to 15 mum thick based on the anodization condition. Mechanical and microstructural evaluation of the UFG-Ti substrates revealed that both the plasma spray and anodization followed by hydrothermal treatment (220 -- 225°C) did not affect the substrate grain size or hardness, while the thermal processing and calcination treatment at 313 -- 446°C for the sol-gel method caused recovery and grain growth, as well as a significant decrease in the hardness of the Ti-substrates.

Fabrication and Microstructure of Hydroxyapatite Coatings on Zirconia by Room Temperature Spray Process.

PubMed

Seo, Dong Seok; Chae, Hak Cheol; Lee, Jong Kook

2015-08-01

Hydroxyapatite coatings were fabricated on zirconia substrates by a room temperature spray process and were investigated with regards to their microstructure, composition and dissolution in water. An initial hydroxyapatite powder was prepared by heat treatment of bovine-bone derived powder at 1100 °C for 2 h, while dense zirconia substrates were fabricated by pressing 3Y-TZP powder and sintering it at 1350 °C for 2 h. Room temperature spray coating was performed using a slit nozzle in a low pressure-chamber with a controlled coating time. The phase composition of the resultant hydroxyapatite coatings was similar to that of the starting powder, however, the grain size of the hydroxyapatite particles was reduced to about 100 nm due to their formation by particle impaction and fracture. All areas of the coating had a similar morphology, consisting of reticulated structure with a high surface roughness. The hydroxyapatite coating layer exhibited biostability in a stimulated body fluid, with no severe dissolution being observed during in vitro experimentation.

Biocomposite Plasma-Sprayed Coatings Based on Zinc-Substituted Hydroxyapatite: Structure, Properties, and Prospects of Application

NASA Astrophysics Data System (ADS)

Lyasnikova, A. V.; Markelova, O. A.; Lyasnikov, V. N.; Dudareva, O. A.

2016-01-01

The method of synthesis of a zinc-substituted hydroxyapatite powder is presented, and the technology of creating coatings by its spraying is described. The results of studies on the morphological, physical, and chemical parameters of a zinc-substituted hydroxyapatite coating by using X-ray analysis, infrared spectroscopy, transmission electron microscopy, optical microscopy, SEM, and other methods are given.

Three-dimensional printed bone scaffolds: The role of nano/micro-hydroxyapatite particles on the adhesion and differentiation of human mesenchymal stem cells.

PubMed

Domingos, Marco; Gloria, Antonio; Coelho, Jorge; Bartolo, Paulo; Ciurana, Joaquim

2017-06-01

Bone tissue engineering is strongly dependent on the use of three-dimensional scaffolds that can act as templates to accommodate cells and support tissue ingrowth. Despite its wide application in tissue engineering research, polycaprolactone presents a very limited ability to induce adhesion, proliferation and osteogenic cell differentiation. To overcome some of these limitations, different calcium phosphates, such as hydroxyapatite and tricalcium phosphate, have been employed with relative success. This work investigates the influence of nano-hydroxyapatite and micro-hydroxyapatite (nHA and mHA, respectively) particles on the in vitro biomechanical performance of polycaprolactone/hydroxyapatite scaffolds. Morphological analysis performed with scanning electron microscopy allowed us to confirm the production of polycaprolactone/hydroxyapatite constructs with square interconnected pores of approximately 350 µm and to assess the distribution of hydroxyapatite particles within the polymer matrix. Compression mechanical tests showed an increase in polycaprolactone compressive modulus ( E) from 105.5 ± 11.2 to 138.8 ± 12.9 MPa (PCL_nHA) and 217.2 ± 21.8 MPa (PCL_mHA). In comparison to PCL_mHA scaffolds, the addition of nano-hydroxyapatite enhanced the adhesion and viability of human mesenchymal stem cells as confirmed by Alamar Blue assay. In addition, after 14 days of incubation, PCL_nHA scaffolds showed higher levels of alkaline phosphatase activity compared to polycaprolactone or PCL_mHA structures.

The pathway to intelligent implants: osteoblast response to nano silicon-doped hydroxyapatite patterning

PubMed Central

Munir, G.; Koller, G.; Di Silvio, L.; Edirisinghe, M. J.; Bonfield, W.; Huang, J.

2011-01-01

Bioactive hydroxyapatite (HA) with addition of silicon (Si) in the crystal structure (silicon-doped hydroxyapatite (SiHA)) has become a highly attractive alternative to conventional HA in bone replacement owing to the significant improvement in the in vivo bioactivity and osteoconductivity. Nanometre-scaled SiHA (nanoSiHA), which closely resembles the size of bone mineral, has been synthesized in this study. Thus, the silicon addition provides an extra chemical cue to stimulate and enhance bone formation for new generation coatings, and the next stage in metallic implantation design is to further improve cellular adhesion and proliferation by control of cell alignment. Topography has been found to provide a powerful set of signals for cells and form contact guidance. Using the recently developed novel technique of template-assisted electrohydrodynamic atomization (TAEA), patterns of pillars and tracks of various dimensions of nanoSiHA were achieved. Modifying the parameters of TAEA, the resolution of pattern structures was controlled, enabling the topography of a substrate to be modified accordingly. Spray time, flow rate and distance between the needle and substrate were varied to improve the pattern formation of pillars and tracks. The 15 min deposition time provided the most consistent patterned topography with a distance of 50 mm and flow rate of 4 µl min−1. A titanium substrate was patterned with pillars and tracks of varying widths, line lengths and distances under the optimized TAEA processing condition. A fast bone-like apatite formation rate was found on nanoSiHA after immersion in simulated body fluid, thus demonstrating its high in vitro bioactivity. Primary human osteoblast (HOB) cells responded to SiHA patterns by stretching of the filopodia between track and pillar, attaching to the apex of the pillar pattern and stretching between two. HOB cells responded to the track pattern by elongating along and between the track, and the length of HOB cells was proportional to the gaps between track patterns, but this relationship was not observed on the pillar patterns. The study has therefore provided an insight for future design of next generation implant surfaces to control and guide cellular responses, while TAEA patterning provides a controllable technique to provide topography to medical implants. PMID:21208969

Advanced Microstructural Study of Suspension Plasma Sprayed Hydroxyapatite Coatings

NASA Astrophysics Data System (ADS)

Podlesak, Harry; Pawlowski, Lech; D'Haese, Romain; Laureyns, Jacky; Lampke, Thomas; Bellayer, Severine

2010-03-01

Fine, home-synthesized, hydroxyapatite powder was formulated with water and alcohol to obtain a suspension used to plasma spray coatings onto a titanium substrate. The deposition process was optimized using statistical design of 2 n experiments with two variables: spray distance and electric power input to plasma. X-ray diffraction (XRD) was used to determine quantitatively the phase composition of obtained deposits. Raman microscopy and electron probe microanalysis (EPMA) enabled localization of the phases in different positions of the coating cross sections. Transmission electron microscopic (TEM) study associated with energy-dispersive x-ray spectroscopy (EDS) enabled visualization and analysis of a two-zone microstructure. One zone contained crystals of hydroxyapatite, tetracalcium phosphate, and a phase rich in calcium oxide. This zone included lamellas, usually observed in thermally sprayed coatings. The other zone contained fine hydroxyapatite grains that correspond to nanometric and submicrometric solids from the suspension that were agglomerated and sintered in the cold regions of plasma jet and on the substrate.

Synthesis, structural properties and thermal stability of Mn-doped hydroxyapatite

NASA Astrophysics Data System (ADS)

Paluszkiewicz, Czesława; Ślósarczyk, Anna; Pijocha, Dawid; Sitarz, Maciej; Bućko, Mirosław; Zima, Aneta; Chróścicka, Anna; Lewandowska-Szumieł, Małgorzata

2010-07-01

Hydroxyapatite (HA) - Ca 10(PO 4) 6(OH) 2 is a basic inorganic model component of hard biological tissues, such as bones and teeth. The significant property of HA is its ability to exchange Ca 2+ ions, which influences crystallinity, physico-chemical and biological properties of modified hydroxyapatite materials. In this work, FTIR, Raman spectroscopy, XRD, SEM and EDS techniques were used to determine thermal stability, chemical and phase composition of Mn containing hydroxyapatite (MnHA). Described methods confirmed thermal decomposition and phase transformation of MnHA to αTCP, βTCP and formation of Mn 3O 4 depending on sintering temperature and manganese content. In vitro biological evaluation of Mn-modified HA ceramics was also performed using human osteoblast cells.

Nanocrystalline hydroxyapatite enriched in selenite and manganese ions: physicochemical and antibacterial properties

NASA Astrophysics Data System (ADS)

Kolmas, Joanna; Groszyk, Ewa; Piotrowska, Urszula

2015-07-01

In this work, we used the co-precipitation method to synthesize hydroxyapatite (Mn-SeO3-HA) containing both selenium IV (approximately 3.60 wt.%) and manganese II (approximately 0.29 wt.%). Pure hydroxyapatite (HA), hydroxyapatite-containing manganese (II) ions (Mn-HA), and hydroxyapatite-containing selenite ions alone (SeO3-HA), prepared with the same method, were used as reference materials. The structures and physicochemical properties of all the obtained samples were investigated. PXRD studies showed that the obtained materials were homogeneous and consisted of apatite phase. Introducing selenites into the hydroxyapatite crystals considerably affects the size and degree of ordering. Experiments with transmission electron microscopy (TEM) showed that Mn-SeO3-HA crystals are very small, needle-like, and tend to form agglomerates. Fourier transform infrared spectroscopy (FT-IR) and solid-state nuclear magnetic resonance (ssNMR) were used to analyze the structure of the obtained material. Preliminary microbiological tests showed that the material demonstrated antibacterial activity against Staphylococcus aureus, yet such properties were not confirmed regarding Escherichia coli. PACS codes: 61, 76, 81

Nutrient-substituted hydroxyapatites: synthesis and characterization

NASA Technical Reports Server (NTRS)

Golden, D. C.; Ming, D. W.

1999-01-01

Incorporation of Mg, S, and plant-essential micronutrients into the structure of synthetic hydroxyapatite (HA) may be advantageous for closed-loop systems, such as will be required on Lunar and Martian outposts, because these apatites can be used as slow-release fertilizers. Our objective was to synthesize HA with Ca, P, Mg, S, Fe, Cu, Mn, Zn, Mo, B, and Cl incorporated into the structure, i.e., nutrient-substituted apatites. Hydroxyapatite, carbonate hydroxyapatite (CHA), nutrient-substituted hydroxyapatite (NHA), and nutrient-substituted carbonate hydroxyapatite (NCHA) were synthesized by precipitating from solution. Chemical and mineralogical analysis of precipitated samples indicated a considerable fraction of the added cations were incorporated into HA, without mineral impurities. Particle size of the HA was in the 1 to 40 nm range, and decreased with increased substitution of nutrient elements. The particle shape of HA was elongated in the c-direction in unsubstituted HA and NHA but more spherical in CHA and NCHA. The substitution of cations and anions in the HA structure was confirmed by the decrease of the d[002] spacing of HA with substitution of ions with an ionic radius less than that of Ca or P. The DTPA-extractable Cu ranged from 8 to 8429 mg kg-1, Zn ranged from 57 to 1279 mg kg-1, Fe from 211 to 2573 mg kg-1, and Mn from 190 to 1719 mg kg-1, depending on the substitution level of each element in HA. Nutrient-substituted HA has the potential to be used as a slow-release fertilizer to supply micronutrients, S, and Mg in addition to Ca and P.

Direct morphological comparison of vacuum plasma sprayed and detonation gun sprayed hydroxyapatite coatings for orthopaedic applications.

PubMed

Gledhill, H C; Turner, I G; Doyle, C

1999-02-01

Hydroxyapatite coatings on titanium substrates were produced using two thermal spray techniques vacuum plasma spraying and detonation gun spraying. X-ray diffraction was used to compare crystallinity and residual stresses in the coatings. Porosity was measured using optical microscopy in conjunction with an image analysis system. Scanning electron microscopy and surface roughness measurements were used to characterise the surface morphologies of the coatings. The vacuum plasma sprayed coatings were found to have a lower residual stress, a higher crystallinity and a higher level of porosity than the detonation gun coatings. It is concluded that consideration needs to be given to the significance of such variations within the clinical context.

Preparation and characterization of hydroxyapatite/sodium alginate biocomposites for bone implant application

NASA Astrophysics Data System (ADS)

Kanasan, Nanthini; Adzila, Sharifah; Suid, Mohd Syafiq; Gurubaran, P.

2016-07-01

In biomedical fields, synthetic scaffolds are being improved by using the ceramics, polymers and composites materials to avoid the limitations of allograft. Ceramic-polymer composites are appearing to be the most successful bone graft substitute in human body. The natural bones itself are well-known as composite of collagen and hydroxyapatite. In this research, precipitation method was used to synthesis hydroxyapatite (HA)/sodium alginate (SA) in various parameters. This paper describes the hydroxyapatite/sodium alginate biocomposite which suitable for use in bone defects or regeneration of bone through the characterizations which include FTIR, FESEM, EDS and DTA. In FTIR, the characteristi peaks of PO4-3 and OH- groups which corresponding to hydroxyapatite are existed in the mixing powders. The needle-size particle of hydroxyapatite/ alginate (HA/SA) are observed in FESEM in the range of 15.8nm-38.2nm.EDS confirmed the existence of HA/SA composition in the mixing powders. There is an endothermic peak which corresponds to the dehydration and the loss of physically adsorbed water molecules of the hydroxyapatite (HA)/sodium alginate (SA) powder which are described in DTA.

Determination of Microstructural Parameters of Nanocrystalline Hydroxyapatite Prepared by Mechanical Alloying Method

NASA Astrophysics Data System (ADS)

Joughehdoust, Sedigheh; Manafi, Sahebali

2011-12-01

Hydroxyapatite [HA, Ca10(PO4)6(OH)2] is chemically similar to the mineral component of bones and hard tissues. HA can support bone ingrowth and osseointegration when used in orthopaedic, dental and maxillofacial applications. In this research, HA nanostructure was synthesized by mechanical alloying method. Phase development, particle size and morphology of HA were investigated by X-ray diffraction (XRD) pattern, zetasizer instrument, scanning electron microscopy (SEM), respectively. XRD pattern has been used to determination of the microstructural parameters (crystallite size, lattice parameters and crystallinity percent) by Williamson-Hall equation, Nelson-Riley method and calculating the areas under the peaks, respectively. The crystallite size and particle size of HA powders were in nanometric scales. SEM images showed that some parts of HA particles have agglomerates. The ratio of lattice parameters of synthetic hydroxyapatite (c/a = 0.73) was determined in this study is the same as natural hydroxyapatite structure.

Electrophoretic co-deposition of PEEK-hydroxyapatite composite coatings for biomedical applications.

PubMed

Baştan, Fatih E; Atiq Ur Rehman, Muhammad; Avcu, Yasemin Yıldıran; Avcu, Egemen; Üstel, Fatih; Boccaccini, Aldo R

2018-05-03

This study focuses on the optimization of electrophoretic deposition (EPD) and suspension parameters for producing PEEK-hydroxyapatite (HA) coatings with feasible microstructure, adhesion strength, and in-vitro bioactivity. Nanostructured hydroxyapatite (HA) micro-granules were incorporated with PEEK to form PEEK-hydroxyapatite composite coatings via EPD. After EPD, a heat-treatment at 375 °C was applied for densification of the coatings and for enhancing the adhesion between the coatings and the substrates. It was found that both adhesion strength and in-vitro bioactivity of the coatings were dependent on the PEEK and HA relative contents. Thus, increasing the amount of HA improved the bioactivity while decreased the adhesion strength of the coatings. Apatite-like layer formation was observed on coatings with high HA content after incubation for three days in simulated body fluid (SBF). Finally, a deposition mechanism was proposed for the EPD of the PEEK-hydroxyapatite composite system. Copyright © 2018 Elsevier B.V. All rights reserved.

Preparation and characterization of hydroxyapatite-coated iron oxide particles by spray-drying technique.

PubMed

Donadel, Karina; Felisberto, Marcos D V; Laranjeira, Mauro C M

2009-06-01

Magnetic particles of iron oxide have been increasingly used in medical diagnosis by magnetic resonance imaging and in cancer therapies involving targeted drug delivery and magnetic hyperthermia. In this study we report the preparation and characterization of iron oxide particles coated with bioceramic hydroxyapatite by spray-drying. The iron oxide magnetic particles (IOMP) were coated with hydroxyapatite (HAp) by spray-drying using two IOMP/HAp ratios (0.7 and 3.2). The magnetic particles were characterized by way of scanning electronic microscopy, energy dispersive X-ray, X-ray diffraction, Fourier transformed infrared spectroscopy, flame atomic absorption spectrometry,vibrating sample magnetometry and particle size distribution (laser diffraction). The surface morphology of the coated samples is different from that of the iron oxide due to formation of hydroxyapatite coating. From an EDX analysis, it was verified that the surface of the coated magnetic particles is composed only of HAp, while the interior containsiron oxide and a few layers of HAp as expected. The results showed that spray-drying technique is an efficient and relatively inexpensive method for forming spherical particles with a core/shell structure.

Zinc-Containing Hydroxyapatite Enhances Cold-Light-Activated Tooth Bleaching Treatment In Vitro

PubMed Central

Shi, Xinchang

2017-01-01

Cold-light bleaching treatment has grown to be a popular tooth whitening procedure in recent years, but its side effect of dental enamel demineralization is a widespread problem. The aim of this study was to synthesize zinc-substituted hydroxyapatite as an effective biomaterial to inhibit demineralization or increase remineralization. We synthesized zinc-substituted hydroxyapatite containing different zinc concentrations and analysed the product using X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, and energy dispersive spectrometer (EDS). The biological assessment of Zn-HA was conducted by CCK-8 assay and bacterial inhibition tests. pH cycling was performed to estimate the effect of Zn-HA on the enamel surface after cold-light bleaching treatment. The XRD, FTIR, and EDS results illustrated that zinc ions and hydroxyapatite combined in two forms: (1) Zn2+ absorbed on the surface of HA crystal and (2) Zn2+ incorporated into the lattice of HA. The results indicated that 2% Zn-HA, 4% Zn-HA, and 8% Zn-HA effectively inhibited the growth of bacteria yet showed poor biocompatibility, whereas 1% Zn-HA positively affected osteoblast proliferation. The XRD and scanning electron microscopy (SEM) results showed that the use of Zn-HA in pH cycling is obviously beneficial for enamel remineralization. Zinc-substituted hydroxyapatite could be a promising biomaterial for use in cold-light bleaching to prevent enamel demineralization. PMID:29159178

Intercalated chitosan/hydroxyapatite nanocomposites: Promising materials for bone tissue engineering applications.

PubMed

Nazeer, Muhammad Anwaar; Yilgör, Emel; Yilgör, Iskender

2017-11-01

Preparation and characterization of chitosan/hydroxyapatite (CS/HA) nanocomposites displaying an intercalated structure is reported. Hydroxyapatite was synthesized through sol-gel process. Formic acid was introduced as a new solvent to obtain stable dispersions of nano-sized HA particles in polymer solution. CS/HA dispersions with HA contents of 5, 10 and 20% by weight were prepared. Self-assembling of HA nanoparticles during the drying of the solvent cast films led to the formation of homogeneous CS/HA nanocomposites. Composite films were analyzed by scanning electron microscopy (SEM), atomic force microscopy (AFM), energy dispersive X-rays (EDX) analysis, Fourier transform infrared (FTIR) spectroscopy, X-rays diffraction (XRD) analysis and thermogravimetric analysis (TGA). SEM and AFM confirmed the presence of uniformly distributed HA nanoparticles on the chitosan matrix surface. XRD patterns and cross-sectional SEM images showed the formation of layered nanocomposites. Complete degradation of chitosan matrix in TGA experiments, led to the formation of nanoporous 3D scaffolds containing hydroxyapatite, β-tricalcium phosphate and calcium pyrophosphate. CS/HA composites can be considered as promising materials for bone tissue engineering applications. Copyright © 2017 Elsevier Ltd. All rights reserved.

Composition of chitosan-hydroxyapatite-collagen composite scaffold evaluation after simulated body fluid immersion as reconstruction material

NASA Astrophysics Data System (ADS)

Verisqa, F.; Triaminingsih, S.; Corputty, J. E. M.

2017-08-01

Hydroxyapatite (HA) formation is one of the most important aspects of bone regeneration. Because domestically made chitosan-hydroxyapatite-collagen composite scaffolding from crab shell and bovine bone and tendon has potential as a maxillofacial reconstruction material, the material’s HA-forming ability requires evaluation. The aim of this research is to investigate chitosan-hydroxyapatite-collagen composite scaffold’s potential as a maxillofacial reconstruction material by observing the scaffold’s compositional changes. Scaffold specimens were immersed in 37°C simulated body fluid (SBF) for periods of 2, 4, 6, and 8 days. Scaffold composition was then evaluated by using energy dispersive spectroscopy (EDS). The calcium (Ca) and phosphorus (P) percentages of the scaffold were found to increase following SBF immersion. The high Ca/P ratio (3.82) on the scaffold indicated HA formation. Ion exchange played a significant role in the increased percentages of Ca and P, which led to new HA layer formation. The scaffold’s HA acted as a nucleation site of Ca and P from the SBF, with collagen and chitosan as the scaffold’s matrix. Chitosan-hydroxyapatite-collagen composite scaffold shows potential as a maxillofacial reconstruction material, since its composition favors HA formation.

Influence of Starting Powders on Hydroxyapatite Coatings Fabricated by Room Temperature Spraying Method.

PubMed

Seo, Dong Seok; Lee, Jong Kook; Hwang, Kyu Hong; Hahn, Byung Dong; Yoon, Seog Young

2015-08-01

Three types of raw materials were used for the fabrication of hydroxyapatite coatings by using the room temperature spraying method and their influence on the microstructure and in vitro characteristics were investigated. Starting hydroxyapatite powders for coatings on titanium substrate were prepared by a heat treatment at 1100 °C for 2 h of bovine bone, bone ash, and commercial hydroxyapatite powders. The phase compositions and Ca/P ratios of the three hydroxyapatite coatings were similar to those of the raw materials without decomposition or formation of a new phase. All hydroxyapatite coatings showed a honeycomb structure, but their surface microstructures revealed different features in regards to surface morphology and roughness, based on the staring materials. All coatings consisted of nano-sized grains and had dense microstructure. Inferred from in vitro experiments in pure water, all coatings have a good dissolution-resistance and biostability in water.

A Solid-State NMR Study of Selenium Substitution into Nanocrystalline Hydroxyapatite

PubMed Central

Kolmas, Joanna; Kuras, Marzena; Oledzka, Ewa; Sobczak, Marcin

2015-01-01

The substitution of selenium oxyanions in the hydroxyapatite structure was examined using multinuclear solid-state resonance spectroscopy (ssNMR). The study was supported by powder X-ray diffractometry (PXRD) and wavelength dispersion X-ray fluorescence (WD-XRF). Samples of pure hydroxyapatite (HA300) and selenate (HA300-1.2SeO4) or selenite (HA300-1.2SeO3) substituted hydroxyapatites were synthesized using the standard wet method and heated at 300 °C to remove loosely bonded water. PXRD data showed that all samples are single-phase, nanocrystalline hydroxyapatite. The incorporation of selenite and selenate ions affected the lattice constants. In selenium-containing samples the concentration of Se was very similar and amounted to 9.55% and 9.64%, for HA300-1.2SeO4 and HA300-1.2SeO3, respectively. PXRD and ssNMR data showed that the selenite doping significantly decreases the crystallite size and crystallinity degree. 31P and 1H NMR experiments demonstrated the developed surface hydrated layer in all samples, especially in HA300-1.2SeO3. 1H NMR studies showed the dehydroxylation of HA during the selenium oxyanions substitution and the existence of hydrogen bonding in structural hydroxyl group channels. 1H→77Se cross polarization NMR experiments indicated that selenites and selenates are located in the crystal lattice and on the crystal surface. PMID:25997001

Incorporation of cerium oxide into hydroxyapatite coating regulates osteogenic activity of mesenchymal stem cell and macrophage polarization.

PubMed

Li, Kai; Shen, Qingyi; Xie, Youtao; You, Mingyu; Huang, Liping; Zheng, Xuebin

2017-02-01

Biomedical coatings for orthopedic implants should facilitate osseointegration and mitigate implant-induced inflammatory reactions. Cerium oxide (CeO 2 ) ceramics possess anti-oxidative properties and can be used to decrease mediators of inflammation, which makes them attractive for biomedical applications. In our work, two kinds of CeO 2 incorporated hydroxyapatite coatings (HA-10Ce and HA-30Ce) were prepared via plasma spraying technique and the effects of CeO 2 addition on the responses of bone mesenchymal stem cells (BMSCs) and RAW264.7 macrophages were investigated. An increase in CeO 2 content in the HA coatings resulted in better osteogenic behaviors of BMSCs in terms of cell proliferation, alkaline phosphatase (ALP) activity and mineralized nodule formation. RT-PCR and western blot analysis suggested that the incorporation of CeO 2 may promote the osteogenic differentiation of BMSCs through the Smad-dependent BMP signaling pathway, which activated Runx2 expression and subsequently enhanced the expression of ALP and OCN. The expression profiles of macrophages cultured on the CeO 2 modified coating revealed a tendency toward a M2 phenotype, because of an upregulation of M2 surface markers (CD163 and CD206), anti-inflammatory cytokines (TNF-α and IL-6) and osteoblastogenesis-related genes (BMP2 and TGF-β1) as well as a downregulation of M1 surface markers (CCR7 and CD11c), proinflammatory cytokines (IL-10 and IL-1ra) and reactive oxygen species production. The results suggested the regulation of BMSCs behaviors and macrophage-mediated responses at the coating's surface were associated with CeO 2 incorporation. The incorporation of CeO 2 in HA coatings can be a valuable strategy to promote osteogenic responses and reduce inflammatory reactions.

In vitro fatigue behaviour of vacuum plasma and detonation gun sprayed hydroxyapatite coatings.

PubMed

Gledhill, H C; Turner, I G; Doyle, C

2001-06-01

The fatigue behaviour of vacuum plasma sprayed (VPS) and detonation gun sprayed (DGUN) hydroxyapatite coatings on titanium substrates has been compared in air and in buffered Ringer's solution. There was an increase in the surface microcracking and bulk porosity of both types of coating tested in air. After 1 million cycles in Ringer's solution the VPS coatings had completely delaminated from their substrates. In contrast the DGUN coatings retained their integrity when tested up to 10 million cycles but were beginning to show signs of delamination at the interface.

Surface modification of hydroxyapatite nanoparticles by poly( L-phenylalanine) via ROP of L-phenylalanine N-carboxyanhydride (Pha-NCA)

NASA Astrophysics Data System (ADS)

Dai, Yanfeng; Xu, Min; Wei, Junchao; Zhang, Haobin; Chen, Yiwang

2012-01-01

The surface of hydroxyapatite nanoparticles was modified by poly(L-phenylalanine) via the ring opening polymerization (ROP) of L-phenylalanine N-carboxyanhydride. The preparation procedure was monitored by Fourier transform infrared spectroscopy (FTIR), and the modified hydroxyapatite was characterized by thermal gravimetric analysis (TGA) and X-ray diffraction (XRD). The results showed that the surface grafting amounts of poly(L-phenylalanine) on HA ranging from 20.26% to 38.92% can be achieved by tuning the reaction condition. The XRD patterns demonstrated that the crystalline structure of the modified hydroxyapatite was nearly the same with that of HA, implying that the ROP was an efficient surface modification method. The MTT assay proved that the biocompatibility of modified HA was very good, which showed the potential application of modified HA in bone tissue engineering.

Synthesis and characterization of TEP-EDTA-regulated bioactive hydroxyapatite

NASA Astrophysics Data System (ADS)

Haders, Daniel Joseph, II

Hydroxyapatite (HA), Ca10(PO4)6(OH) 2, the stoichiometric equivalent of the ceramic phase of bone, is the preferred material for hard tissue replacement due to its bioactivity. However, bioinert metals are utilized in load-bearing orthopedic applications due to the poor mechanical properties of HA. Consequently, attention has been given to HA coatings for metallic orthopedic implants to take advantage of the bioactivity of HA and the mechanical properties of metals. Commercially, the plasma spray process (PS-HA) is the method most often used to deposit HA films on metallic implants. Since its introduction in the 1980's, however, concerns have been raised about the consequences of PS-HA's low crystallinity, lack of phase purity, lack of film-substrate chemical adhesion, passivation properties, and difficulty in coating complex geometries. Thus, there is a need to develop inexpensive reproducible next-generation HA film deposition techniques, which deposit high crystallinity, phase pure, adhesive, passivating, conformal HA films on clinical metallic substrates. The aim of this dissertation was to intelligently synthesize and characterize the material and biological properties of HA films on metallic substrates synthesized by hydrothermal crystallization, using thermodynamic phase diagrams as the starting point. In three overlapping interdisciplinary studies the potential of using ethylenediamine-tetraacetic acid/triethyl phosphate (EDTA/TEP) doubly regulated hydrothermal crystallization to deposit HA films, the TEP-regulated, time-and-temperature-dependent process by which films were deposited, and the bioactivity of crystallographically engineered films were investigated. Films were crystallized in a 0.232 molal Ca(NO3)2-0.232 molal EDTA-0.187 molal TEP-1.852 molal KOH-H2O chemical system at 200°C. Thermodynamic phase diagrams demonstrated that the chosen conditions were expected to produce Ca-P phase pure HA, which was experimentally confirmed. EDTA regulation of Ca2+ concentration enabled the HA crystallization process to be growth dominated, producing films composed of high crystallinity, hexagonal grains on multiple metallic substrates. TEP regulation of HA crystallization enabled the deposition of an adhesive CaTiO3 intermediate layer, and then HA in a continuous, phase sequenced process on Ti6Al4V substrates, the first such process reported in the hydrothermal HA literature. The HA film was found to be deposited by a passivating competitive growth mechanism that enabled the [0001] crystallographic orientation of hexagonal single crystals to be engineered with synthesis time. Bioactivity analysis demonstrated that films were bioactive and bone bonding. Together, these results suggest that these HA films are candidates for use on metallic orthopedic implants, namely Ti6Al4V.

Cell death induced by hydroxyapatite on L929 fibroblast cells.

PubMed

Inayat-Hussain, S H; Rajab, N F; Roslie, H; Hussin, A A; Ali, A M; Annuar, B O

2004-05-01

Biomaterials intended for end-use application as bone-graft substitutes have to undergo safety evaluation. In this study, we investigated the in vitro cytotoxic effects especially to determine the mode of death of two hydroxyapatite compounds (HA2, HA3) which were synthesized locally. The methods used for cytotoxicity was the standard MTT assay whereas AO/PI staining was performed to determine the mode of cell death in HA treated L929 fibroblasts. Our results demonstrated that both HA2 and HA3 were not significantly cytotoxic as more than 75% cells after 72 hours treatment were viable. Furthermore, we found that the major mode of cell death in HA treated cells was apoptosis. In conclusion, our results demonstrated that these hydroxyapatite compounds are not cytotoxic where the mode of death was primarily via apoptosis.

Surface and biological evaluation of hydroxyapatite-based coatings on titanium deposited by different techniques.

PubMed

Massaro, C; Baker, M A; Cosentino, F; Ramires, P A; Klose, S; Milella, E

2001-01-01

Hydroxyapatite coatings have been deposited on titanium cp by plasma spray, sol-gel, and sputtering techniques for dental implant applications. The latter two techniques are of current interest, as they allow coatings of micrometer dimensions to be deposited. Coating morphology, composition, and structure have been investigated by scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS) and X-ray diffraction (XRD). All coatings were homogeneous and exhibited a rough morphology suitable for implant applications. The sputtered (after annealing), plasma spray, and sol-gel coatings all showed diffraction peaks corresponding to hydroxyapatite. The surface contaminants were observed to be different for the different coating types. The sputtered coatings were found to have a composition most similar to hydroxyapatite; the sol-gel deposits also showed a high concentration of hydroxyl ions. A discrepancy in the Ca/P ratio was observed for the plasma spray coatings, and a small concentration of carbonate ions was found in the sputter-deposited coatings. The in vitro cell-culture studies using MG63 osteoblast-like cells demonstrated the ability of cells to proliferate on the materials tested. The sol-gel coating promotes higher cell growth, greater alkaline phosphatase activity, and greater osteocalcin production compared to the sputtered and plasma-sprayed coatings. Copyright 2001 John Wiley & Sons, Inc.

Biological response of Sr-containing coating with various surface treatments on titanium substrate for medical applications

NASA Astrophysics Data System (ADS)

Yang, Shih-Ping; Lee, Tzer-Min; Lui, Truan-Sheng

2015-08-01

An implant requires a suitable surface to trigger osteointegration. The surface characteristics and chemical composition are important factors in this process. Plasma spraying and micro-arc oxidation can be used to fabricate rough and porous structures for medical applications. Strontium (Sr) has been shown to prevent osteoporosis in vitro and in vivo. However, few scientists have evaluated the biological response of Sr-containing coatings on different surface treatments. In this study, a sand-blasted (SB) surface (as the control), plasma-sprayed hydroxyapatite (HA) and Sr-substituted HA coatings (HAPS and SrHAPS, respectively), calcium phosphate and Sr-containing calcium phosphate micro-arc oxidation surface (CPM and SrCPM, respectively) were analyzed in terms of human osteoblastic cell (MG63) response. Sr was confirmed to be incorporated into the surface. SrHAPS and SrCPM specimens had higher cell responses than those of the HAPS and CPM groups, respectively. The cells cultured on SrCPM and SrHAPS specimens exhibited high proliferation and differentiation. However, CPM and SrCPM specimens stimulated more ECM-like structures than other specimens. The results show that Sr-containing coatings have good characteristics that enhance cell response. The SrCPM coating is a suitable implant surface treatment for clinical applications.

Studies on corrosion resistance and bio-activity of plasma spray deposited hydroxylapatite (HA) based TiO2 and ZrO2 dispersed composite coatings on titanium alloy (Ti-6Al-4V) and the same after post spray heat treatment

NASA Astrophysics Data System (ADS)

Kumari, Renu; Majumdar, Jyotsna Dutta

2017-10-01

In the present study, the effect of plasma spray deposited hydroxylapatite (HA) based TiO2 dispersed (HA + 50 wt.% TiO2), coating and post spray heat treatment to be referred as HA-TiO2 (heat treated at 650 °C for 2 h) and ZrO2 dispersed (HA + 10 wt.% ZrO2), to be referred as HA-ZrO2 coating (heat treated at 750 °C for 2 h) on corrosion resistance and bioactivity of Ti-6Al-4V substrate has been undertaken. There is partial decomposition of HA to tri-calcium-phosphate (Ca3(PO4)2) and formation of CaTiO3 phase in HA-TiO2 coating and CaZrO3 phase in the HA-ZrO2 coating. Corrosion study in Hank's solution shows that there is shifting of corrosion potential (Ecorr) towards active potential (-1.1 V(SCE) for as-sprayed and post spray heat treated HA-TiO2 coating, -1.1 V(SCE) for as-sprayed HA-ZrO2 coating and -1 V(SCE) for HA-ZO2 coating after post spray heat treatment), and deterioration in pitting corrosion (Epit) resistance in as-sprayed coatings and the same after heat treatment (-0.7 V(SCE) for both HA-TiO2 and HA-ZrO2 coating as compared to as received substrate (-0.3 V(SCE)). The corrosion rate was increased for both the coatings with a maximum increase in HA-ZrO2 coating. Bioactivity test shows a higher degree of apatite deposition in as-sprayed coating and the same after heat treatment as compared to as received Ti-6Al-4V though the as-sprayed one showed a superior behavior.

Preparation and characterization of selenite substituted hydroxyapatite.

PubMed

Ma, Jun; Wang, Yanhua; Zhou, Lei; Zhang, Shengmin

2013-01-01

Selenite-substituted hydroxyapatite (Se-HA) with different Se/P ratios was synthesized by a co-precipitation method, using sodium selenite (Na2SeO3) as a Se source. Selenium has been incorporated into the hydroxyapatite lattice by partially replacing phosphate (PO4(3-)) groups with selenite (SeO3(2-)) groups. X-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FTIR), and transmission electron microscopy (TEM) techniques reveal that substitutions of phosphate groups by selenite groups cause lower carbonate groups occupying at phosphate sites and change the lattice parameters of hydroxyapatite. The powders obtained are nano-crystalline hydroxyapatite when the Se/P ratios are not more than 0.1. The particle shape of Se-HA has not been altered compared with selenite-free hydroxyapatite but Se-incorporation reduces the crystallite size. The crystallinity was reduced as the Se/P ratios increased until amorphous phase (Se/P=0.3) appeared in the Se-HA powder obtained, and then another crystal phase presented as calcium selenite hydrate (Se/P=10). In addition, the sintering tests show that the Se-HA powders with the Se/P ratio of 0.1 have thermal stability at 900 °C for 2 h; hence they have great potential in the fabrication of bone repair scaffolds. Copyright © 2012 Elsevier B.V. All rights reserved.

Rapid hydrothermal flow synthesis and characterisation of carbonate- and silicate-substituted calcium phosphates

PubMed Central

Knowles, Jonathan C; Rehman, Ihtesham; Darr, Jawwad A

2013-01-01

A range of crystalline and nano-sized carbonate- and silicate-substituted hydroxyapatite has been successfully produced by using continuous hydrothermal flow synthesis technology. Ion-substituted calcium phosphates are better candidates for bone replacement applications (due to improved bioactivity) as compared to phase-pure hydroxyapatite. Urea was used as a carbonate source for synthesising phase pure carbonated hydroxyapatite (CO3-HA) with ≈5 wt% substituted carbonate content (sample 7.5CO3-HA) and it was found that a further increase in urea concentration in solution resulted in biphasic mixtures of carbonate-substituted hydroxyapatite and calcium carbonate. Transmission electron microscopy images revealed that the particle size of hydroxyapatite decreased with increasing urea concentration. Energy-dispersive X-ray spectroscopy result revealed a calcium deficient apatite with Ca:P molar ratio of 1.45 (±0.04) in sample 7.5CO3-HA. For silicate-substituted hydroxyapatite (SiO4-HA) silicon acetate was used as a silicate ion source. It was observed that a substitution threshold of ∼1.1 wt% exists for synthesis of SiO4-HA in the continuous hydrothermal flow synthesis system, which could be due to the decreasing yields with progressive increase in silicon acetate concentration. All the as-precipitated powders (without any additional heat treatments) were analysed using techniques including Transmission electron microscopy, X-ray powder diffraction, Differential scanning calorimetry, Thermogravimetric analysis, Raman spectroscopy and Fourier transform infrared spectroscopy. PMID:22983020

Microstructural disintegration in dense hydroxyapatite and hydroxyapatite-coated metal implants

NASA Astrophysics Data System (ADS)

Seo, Dong Seok; Lee, Jong Kook

2007-08-01

Hydroxyapatite (HA) has been widely used as a coating for orthopedic metal implants. An important concern regarding HA coating is its degradation of the biological milieu. In this study, the microstructure of a retrieved HA-coated acetabular cup implanted for four years after total hip arthroplasty (THA) was investigated by field emission scanning electron microscopy. In order to understand the underlying mechanism, of degradation and exfoliation of the HA coating, degradation of phase-pure and dense HA ceramics was also observed by in vitro and in vivo testing. The surface morphology and fracture surfaces of HA ceramics revealed that the dissolution starting at the surface extended inwards resulting in particle loosening and microstructural-level degradation. The dissolution features of HA ceramics were similar to the case of HA coating. It was found that extensive dissolution of the coating occurred and most of the coating disappeared. The majority of the remaining graints were fractured by the intergranular mode, suggesting that grain boundaries should be predominantly dissolved. These observations may explain the mechanism through which the biological stability of the HA coated layer becomes unexpectedly poor.

Influence of sodium fluoride on the synthesis of hydroxyapatite by gel method

NASA Astrophysics Data System (ADS)

Kanchana, P.; Sekar, C.

2010-03-01

Hydroxyapatite (HA) is a good candidate for bone substitutes due to its chemical and structural similarity to bone mineral. Hydroxyapatite has been grown by the gel method using sodium fluoride (NaF) as additive. The growth was carried out at room temperature under the physiological pH of 7.4. The addition of NaF has significantly reduced growth rate and the yield was much less when compared to pure system. The samples of pure and fluoride doped HA were sintered at 600, 900 and 1200 °C in ambient atmosphere. Scanning electron microscopy (SEM), powder X-ray diffraction (XRD), thermogravimetric analysis (TG) and Fourier transform infrared spectroscopy (FTIR) were adopted to investigate the influence of NaF on the morphology, crystallinity, stability and phase purity of HA. EDAX and FTIR studies confirm that the fluoride is doped into the hydroxyapatite. Powder XRD and TGA results suggested that the incorporation of fluorine into the HA matrix improves the phase formation and crystallinity. SEM studies show that the microstructural morphology of HA changes from the fibers for pure to granular structure for the fluoride doped.

Spherical porous hydroxyapatite granules containing composites of magnetic and hydroxyapatite nanoparticles for the hyperthermia treatment of bone tumor.

PubMed

Kamitakahara, Masanobu; Ohtoshi, Naohiro; Kawashita, Masakazu; Ioku, Koji

2016-05-01

Spherical porous granules of hydroxyapatite (HA) containing magnetic nanoparticles would be suitable for the hyperthermia treatment of bone tumor, because porous HA granules act as a scaffold for bone regeneration, and magnetic nanoparticles generate sufficient heat to kill tumor cells under an alternating magnetic field. Although magnetic nanoparticles are promising heat generators, their small size makes them difficult to support in porous HA ceramics. We prepared micrometer-sized composites of magnetic and HA nanoparticles, and then supported them in porous HA granules composed of rod-like particles. The spherical porous HA granules containing the composites of magnetic and HA nanoparticle were successfully prepared using a hydrothermal process without changing the crystalline phase and heat generation properties of the magnetic nanoparticles. The obtained granules generated sufficient heat for killing tumor cells under an alternating magnetic field (300 Oe at 100 kHz). The obtained granules are expected to be useful for the hyperthermia treatment of bone tumors.

Antimicrobial and osteogenic properties of a hydrophilic-modified nanoscale hydroxyapatite coating on titanium.

PubMed

Murakami, Asuka; Arimoto, Takafumi; Suzuki, Dai; Iwai-Yoshida, Misato; Otsuka, Fukunaga; Shibata, Yo; Igarashi, Takeshi; Kamijo, Ryutaro; Miyazaki, Takashi

2012-04-01

Hydroxyapatite (HA)-coated titanium (Ti) is commonly used for implantable medical devices. This study examined in vitro osteoblast gene expression and antimicrobial activity against early and late colonizers of supra-gingival plaque on nanoscale HA-coated Ti prepared by discharge in a physiological buffered solution. The HA-coated Ti surface showed super-hydrophilicity, whereas the densely sintered HA and Ti surfaces alone showed lower hydrophilicity. The sintered HA and HA-coated Ti surfaces enhanced osteoblast phenotypes in comparison with the bare Ti surface. The HA-coated Ti enabled antimicrobial activity against early colonizers of supra-gingival plaques, namely Streptococcus mitis and Streptococcus gordonii. Such antimicrobial activity may be caused by the surface hydrophilicity, thereby leading to a repulsion force between the HA-coated Ti surface and the bacterial cell membranes. On the contrary, the sintered HA sample was susceptible to infection of microorganisms. Thus, hydrophilic-modified HA-coated Ti may have potential for use in implantable medical devices. From the Clinical Editor: This study establishes that Hydroxyapatite (HA)-coated titanium (Ti) surface of implanted devices may result in an optimal microenvironment to control and prevent infections and may have potential future clinical applications. Copyright © 2012 Elsevier Inc. All rights reserved.

Improved bonding strength of bioactive cermet Cold Gas Spray coatings.

PubMed

Gardon, M; Concustell, A; Dosta, S; Cinca, N; Cano, I G; Guilemany, J M

2014-12-01

The fabrication of cermet biocompatible coatings by means Cold Gas Spray (CGS) provides prosthesis with outstanding mechanical properties and the required composition for enhancing the bioactivity of prosthetic materials. In this study, hydroxyapatite/Titanium coatings were deposited by means of CGS technology onto titanium alloy substrates with the aim of building-up well-bonded homogeneous coatings. Powders were blended in different percentages and sprayed; as long as the amount of hydroxyapatite in the feedstock increased, the quality of the coating was reduced. Besides, the relation between the particle size distribution of ceramic and metallic particles is of significant consideration. Plastic deformation of titanium particles at the impact eased the anchoring of hard hydroxyapatite particles present at the top surface of the coating, which assures the looked-for interaction with the cells. Coatings were immersed in Hank's solution for 1, 4 and 7 days; bonding strength value was above 60 MPa even after 7 days, which enhances common results of HAp coatings obtained by conventional thermal spray technologies. Copyright © 2014 Elsevier B.V. All rights reserved.

Bone response adjacent to calcium phosphate electrostatic spray deposition coated implants: an experimental study in goats.

PubMed

Manders, Peter J D; Wolke, Joop G C; Jansen, John A

2006-10-01

A new technique to deposit calcium phosphate (CaP) coatings onto titanium substrates has been developed recently. This electrostatic spray deposition (ESD) technique seems to be very promising. It appears to have clinical advantages such as an inexpensive and simple set-up, high deposition efficiency and the possibility to synthesize layers with a defined surface morphology. The aim of this study was to examine biological properties and osteoconductivity of ESD CaP coatings when inserted into the femoral condyle of a goat. Twenty-four implants with two gaps, i.e. 1 or 2 mm, were inserted into the femoral condyles of six goats. The implants were coated on one side with either a commercially available plasma-sprayed hydroxyapatite (HAPS) coating or an ESD carbonate apatite (CAESD) coating. The other side of the implant was always left uncoated (Ti). Twelve weeks after implantation the animals were sacrificed and the characteristics of bone ingrowth and bone contact were evaluated. At 3 months, histological and quantitative histomorphometrical measurements demonstrated more bone ingrowth and bone contact for coated sites as compared with uncoated sites. Statistical testing revealed that for both the 1 and 2 mm gaps HAPS (plasma-sprayed hydroxyapatite) as well as CAESD (ESD carbonate apatite) -coated surfaces always had a significantly higher (P<0.05) amount of bone contact than uncoated Ti surfaces. On HAPS surfaces always significantly more bone was present than on CAESD surfaces. Further statistical testing revealed a significant difference in bone ingrowth between the HAPS as well as CAESD and Ti 1+2 mm gap specimens (P<0.05). Further, HAPS 1 mm gaps showed more bone ingrowth than CAESD 1 mm gaps. No significant difference existed between HAPS and CAESD 2 mm gaps. On the basis of our observations, we conclude that the used ESD technique is a promising new method to deposit CaP coatings onto titanium substrates. On the other hand, plasma-spray HA-coated implants have a still more favourable effect on the bone response.

Co-blasting of titanium surfaces with an abrasive and hydroxyapatite to produce bioactive coatings: substrate and coating characterisation.

PubMed

Dunne, Conor F; Twomey, Barry; O'Neill, Liam; Stanton, Kenneth T

2014-01-01

The aim of this work is to assess the influence of two blast media on the deposition of hydroxyapatite onto a titanium substrate using a novel ambient temperature coating technique named CoBlast. CoBlast was developed to address the problems with high temperature coating techniques. The blasting media used in this study were Al2O3 and a sintered apatite powder. The prepared and coated surfaces were compared to plasma sprayed hydroxyapatite on the same substrates using the same hydroxyapatite feedstock powder. X-ray diffraction analysis revealed the coating crystallinity was the same as the original hydroxyapatite feedstock powder for the CoBlast samples while evidence of amorphous hydroxyapatite phases and β-TCP was observed in the plasma sprayed samples. The blast media type significantly influences the adhesive strength of the coating, surface roughness of both the substrate and coating and the microstructure of the substrate. The coating adhesion increased for the CoBlasted samples from 50 MPa to 60 MPa for sintered apatite powder and alumina, respectively, while plasma spray samples were significantly lower (5 MPa) when tested using a modified pull-test. In conclusion, the choice of blast medium is shown to be a key parameter in the CoBlast process. This study indicates that sintered apatite powder is the most suitable candidate for use as a blast medium in the coating of medical devices.

Osteoconductive composite graft based on bacterial synthesized hydroxyapatite nanoparticles doped with different ions: From synthesis to in vivo studies.

PubMed

Ahmadzadeh, Elham; Talebnia, Farid; Tabatabaei, Meisam; Ahmadzadeh, Hossein; Mostaghaci, Babak

2016-07-01

To repair damaged bone tissues, osteoconductive bone graft substitutes are required for enhancement of the regenerative potential of osteoblast cells. Nanostructured hydroxyapatite is a bioactive ceramic used for bone tissue engineering purposes. In this study, carbonate hydroxyapatite (cHA) and zinc-magnesium substituted hydroxyapatite (Zn-Mg-HA) nanoparticles were synthesized via biomineralization method using Enterobacter aerogenes. The structural phase composition and the morphology of the samples were analyzed using appropriate powder characterization methods. Next, a composite graft was fabricated by using polyvinyl alcohol and both cHA and Zn-Mg-HA samples. In vivo osteogenic potential of the graft was then investigated in a rabbit tibial osteotomy model. Histological, radiological and morphological studies showed that the graft was mineralized by the newly formed bone tissue without signs of inflammation or infection after 4 weeks of implantation. These histomorphometric results suggest that the fabricated graft can function as a potent osteoconductive bone tissue substitute. Copyright © 2016 Elsevier Inc. All rights reserved.

Microstructures of plasma-sprayed hydroxyapatite-coated Ti-6Al-4V dental implants.

PubMed

Tufekci, E; Brantley, W A; Mitchell, J C; McGlumphy, E A

1997-01-01

The purpose of this study was to investigate the microstructure of plasma-sprayed hydroxyapatite coatings and the elemental composition near the coating-substrate interface for two commercial implants, using the scanning electron microscope. Both coating surfaces and cross-sectioned specimens were examined. The results indicated that while the surface microstructures of both implants were consistent with the plasma-spraying process, the scale of the constituents was much finer for one product. In cross-section, both coatings exhibited minimal porosity and intimate contact with the titanium alloy substrate. It was found that limited interdiffusion of titanium and calcium occurred near the interface.

Effect of surface roughness of hydroxyapatite-coated titanium on the bone-implant interface shear strength.

PubMed

Hayashi, K; Inadome, T; Tsumura, H; Nakashima, Y; Sugioka, Y

1994-11-01

We have investigated the bone-implant interface shear strength of hydroxyapatite (HA)-coated Ti-6Al-4V (HA-coating A) (roughness average, Ra = 3.4 +/- 0.5 microns) and HA-coated Ti-6Al-4V with a rougher surface (HA-coating B) (Ra = 8.4 +/- 1.8 microns). There was no significant difference between HA-coating A and HA-coating B implants with respect to the bone-implant interface shear strength as determined in push-out tests using the transcortical model in adult dogs. The bone-implant interface shear strength of bead-coated porous Ti-6Al-4V was significantly greater than that of both HA-coating A and HA-coating B implants. The failure site, as determined by scanning electron microscopy, was the coating-substrate interface, not the coating-bone interface. This indicates a need to protect the HA coating from the direct shear forces. HA coating enhances early bone growth into the porous surface of the implant. Long-term fixation should depend on bone anchoring to this porous surface. Hydroxyapatite coatings must be developed which do not obstruct the pores of the surface of the implant.

Micro- and nano-hydroxyapatite as active reinforcement for soft biocomposites.

PubMed

Munarin, F; Petrini, P; Gentilini, R; Pillai, R S; Dirè, S; Tanzi, M C; Sglavo, V M

2015-01-01

Pectin-based biocomposite hydrogels were produced by internal gelation, using different hydroxyapatite (HA) powders from commercial source or synthesized by the wet chemical method. HA possesses the double functionality of cross-linking agent and inorganic reinforcement. The mineralogical composition, grain size, specific surface area and microstructure of the hydroxyapatite powders are shown to strongly influence the properties of the biocomposites. Specifically, the grain size and specific surface area of the HA powders are strictly correlated to the gelling time and rheological properties of the hydrogels at room temperature. Pectin pH is also significant for the formation of ionic cross-links and therefore for the hydrogels stability at higher temperatures. The obtained results point out that micrometric-size hydroxyapatite can be proposed for applications which require rapid gelling kinetics and improved mechanical properties; conversely the nanometric hydroxyapatite synthesized in the present work seems the best choice to obtain homogeneous hydrogels with more easily controlled gelling kinetics. Copyright © 2014 Elsevier B.V. All rights reserved.

Hydroxyapatite Fibers: A Review of Synthesis Methods

NASA Astrophysics Data System (ADS)

Qi, Mei-Li; He, Kun; Huang, Zhen-Nan; Shahbazian-Yassar, Reza; Xiao, Gui-Yong; Lu, Yu-Peng; Shokuhfar, Tolou

2017-08-01

Hydroxyapatite (HA) exhibits excellent biocompatibility, bioactivity, osteoconductivity, non-toxicity and so on, making it a perfect candidate for biomedical applications. However, HA is not qualified to be used in load-bearing sites due to its poor flexural strength and fracture toughness. Design, synthesis and application of fibrous HA is a promising strategy to overcome the inherent brittleness. This review provides a brief description of HA and hydroxyapatite fiber (HAF), then introduces different synthesis methods of HAF and highlights the inherent merits and drawbacks involved in each method. Finally, the future perspectives in this active research area are given. The purpose of this review is to acquaint the reader with this promising new field of biomaterials research and with emphasis on recent techniques to obtain continuous, uniform and long HAF.

Microfluidic vascularized bone tissue model with hydroxyapatite-incorporated extracellular matrix.

PubMed

Jusoh, Norhana; Oh, Soojung; Kim, Sudong; Kim, Jangho; Jeon, Noo Li

2015-10-21

Current in vitro systems mimicking bone tissues fail to fully integrate the three-dimensional (3D) microvasculature and bone tissue microenvironments, decreasing their similarity to in vivo conditions. Here, we propose 3D microvascular networks in a hydroxyapatite (HA)-incorporated extracellular matrix (ECM) for designing and manipulating a vascularized bone tissue model in a microfluidic device. Incorporation of HA of various concentrations resulted in ECM with varying mechanical properties. Sprouting angiogenesis was affected by mechanically modulated HA-extracellular matrix interactions, generating a model of vascularized bone microenvironment. Using this platform, we observed that hydroxyapatite enhanced angiogenic properties such as sprout length, sprouting speed, sprout number, and lumen diameter. This new platform integrates fibrin ECM with the synthetic bone mineral HA to provide in vivo-like microenvironments for bone vessel sprouting.

Functionalized coatings by cold spray: An in vitro study of micro- and nanocrystalline hydroxyapatite compared to porous titanium.

PubMed

Vilardell, A M; Cinca, N; Garcia-Giralt, N; Dosta, S; Cano, I G; Nogués, X; Guilemany, J M

2018-06-01

Three different surface treatments on a Ti6Al4V alloy have been in vitro tested for possible application in cementless joint prosthesis. All of them involve the novelty of using the Cold Spray technology for their deposition: (i) an as-sprayed highly rough titanium and, followed by the deposition of a thin hydroxyapatite layer with (ii) microcrystalline or (iii) nanocrystalline structure. Primary human osteoblasts were extracted from knee and seeded onto the three different surfaces. Cell viability was tested by MTS and LIVE/DEAD assays, cell differentiation by alkaline phosphatase (ALP) quantification and cell morphology by Phalloidin staining. All tests were carried out at 1, 7 and 14 days of cell culture. Different cell morphologies between titanium and hydroxyapatite surfaces were exhibited. At 1 day of cell culture, cells on the titanium coating were spread and flattened, expanding the filopodia actin filaments in all directions, while cells on the hydroxyapatite coatings showed round like-shape morphology due to slower attachment. Higher cell viability was detected at all times of cell culture on titanium coating due to a better attachment at 1 day. However, from 7 days of cell culture, cells on hydroxyapatite showed good attachment onto surfaces and highly increased their proliferation, mostly on nanocrystalline, achieving similar cell viability levels than titanium coatings. ALP levels were significantly higher in titanium, in part, because of greatest cell number. Overall, the best cell functional results were obtained on titanium coatings whereas microcrystalline hydroxyapatite presented the worst cellular parameters. However, results indicate that nanocrystalline hydroxyapatite coatings may achieve promising results for the faster cell proliferation once cells are attached on the surface. Copyright © 2018 Elsevier B.V. All rights reserved.

[Remediation Pb, Cd contaminated soil in lead-zinc mining areas by hydroxyapatite and potassium chloride composites].

PubMed

Wang, Li; Li, Yong-Hua; Ji, Yan-Fang; Yang, Lin-Sheng; Li, Hai-Rong; Zhang, Xiu-Wu; Yu, Jiang-Ping

2011-07-01

The composite agents containing potassium chloride (KCl) and Hydroxyapatite (HA) were used to remediate the lead and cadmium contaminated soil in Fenghuang lead-zinc mining-smelting areas, Hunan province. The objective of this study was to identify and evaluate the influence of Cl- to the fixing efficiency of Pb and Cd by HA. Two types of contaminated soil (HF-1, HF-2) were chosen and forty treatments were set by five different Hydroxyapatite (HA) dosages and four different Cl- dosages. The toxicity characteristic leaching procedure (TCLP) was used to evaluate the results. It showed that HA could efficiently fix the Pb and Cd from TCLP form. The maximum Pb-fixing efficiency and Cd-fixing efficiency of two types of soil were 83.3%, 97.27% and 35.96%, 57.82% when the HA: Pb: KCl molar ratio was 8: 1: 2. Compared to the fixing efficiency without KCl, KCl at the KCl: Pb molar ratio of 2 improved Pb-fixing efficiency and Cd-fixing efficiency by 6.26%, 0.33% and 7.74%, 0.83% respectively when the HA: Pb molar ratio was 8. Generally, Cl- can improve the Pb/Cd-fixing efficiency in heavy metal contaminated soil by Hydroxyapatite.

Fabrication of nano-structured HA/CNT coatings on Ti6Al4V by electrophoretic deposition for biomedical applications.

PubMed

Zhang, Bokai; Kwok, Chi Tat; Cheng, Fai Tsun; Man, Hau Chung

2011-12-01

In order to improve the bone bioactivity and osteointegration of metallic implants, hydroxyapatite (HA) is often coated on their surface so that a real bond with the surrounding bone tissue can be formed. In the present study, cathodic electrophoretic deposition (EPD) has been attempted for depositing nanostructured HA coatings on titanium alloy Ti6Al4V followed by sintering at 800 degrees C. Nano-sized HA powder was used in the EPD process to produce dense coatings. Moreover, multiwalled carbon nanotubes (CNTs) were also used to reinforce the HA coating for enhancing its mechanical strength. The surface morphology, compositions and microstructure of the monolithic coating of HA and nanocomposite coatings of HA with different CNT contents (4 to 25%) on Ti6Al4V were investigated by scanning-electron microscopy, energy-dispersive X-ray spectroscopy and Xray diffractometry, respectively. Electrochemical corrosion behavior of the various coatings in Hanks' solution at 37 degrees C was investigated by means of open-circuit potential measurement and cyclic potentiodynamic polarization tests. Surface hardness, adhesion strength and bone bioactivity of the coatings were also studied. The HA and HA/CNT coatings had a thickness of about 10 microm, with corrosion resistance higher than that of the substrate and adhesion strength higher than that of plasma sprayed HA coating. The properties of the composite coatings were optimized by varying the CNT contents. The enhanced properties could be attributed to the use of nano-sized HA particles and CNTs. Compared with the monolithic HA coating, the CNT-reinforced HA coating markedly increased the coating hardness without deteriorating the corrosion resistance or adhesion strength.

Preparation and properties of in-situ growth of carbon nanotubes reinforced hydroxyapatite coating for carbon/carbon composites.

PubMed

Liu, Shoujie; Li, Hejun; Su, Yangyang; Guo, Qian; Zhang, Leilei

2017-01-01

Carbon nanotubes (CNTs) possess excellent mechanical properties for their role playing in reinforcement as imparting strength to brittle hydroxyapatite (HA) bioceramic coating. However, there are few reports relating to the in-situ grown carbon nanotubes reinforced hydroxyapatite (CNTs-HA) coating. Here we demonstrate the potential application in reinforcing biomaterials by an attempt to use in-situ grown of CNTs strengthen HA coating, using a combined method composited of injection chemical vapor deposition (ICVD) and pulsed electrodeposition. The microstructure, phases and chemical compositions of CNTs-HA coatings were characterized by various advanced methods. The scanning electron microscopy (SEM) images indicated that CNTs-HA coatings avoided the inhomogeneous dispersion of CNTs inside HA coating. The result show that the interfacial shear strength between CNTs-HA coating and the C/C composite matrix reaches to 12.86±1.43MPa. Potenitodynamic polarization and electrochemical impedance spectroscopy (EIS) studies show that the content of CNTs affects the corrosion resistance of CNTs-HA coating. Cell culturing and simulated body fluid test elicit the biocompatibility with living cells and bioactivity of CNTs-HA coatings, respectively. Copyright © 2016 Elsevier B.V. All rights reserved.

Preparation of nano-hydroxyapatite particles with different morphology and their response to highly malignant melanoma cells in vitro

NASA Astrophysics Data System (ADS)

Li, Bo; Guo, Bo; Fan, Hongsong; Zhang, Xingdong

2008-11-01

To investigate the effects of nano-hydroxyapatite (HA) particles with different morphology on highly malignant melanoma cells, three kinds of HA particles with different morphology were synthesized and co-cultured with highly malignant melanoma cells using phosphate-buffered saline (PBS) as control. A precipitation method with or without citric acid addition as surfactant was used to produce rod-like hydroxyapatite (HA) particles with nano- and micron size, respectively, and a novel oil-in-water emulsion method was employed to prepare ellipse-like nano-HA particles. Particle morphology and size distribution of the as prepared HA powders were characterized by transmission electron microscope (TEM) and dynamic light scattering technique. The nano- and micron HA particles with different morphology were co-cultured with highly malignant melanoma cells. Immunofluorescence analysis and MTT assay were employed to evaluate morphological change of nucleolus and proliferation of tumour cells, respectively. To compare the effects of HA particles on cell response, the PBS without HA particles was used as control. The experiment results indicated that particle nanoscale effect rather than particle morphology of HA was more effective for the inhibition on highly malignant melanoma cells proliferation.

Bioactivity evaluation of titanium/hydroxyapatite composite coating on stainless steel prepared by thermal spraying

NASA Astrophysics Data System (ADS)

Azhar, Nurul Humaira; Talari, Mahesh Kumar; Koong, Chue Keen

2015-08-01

In this study, titanium powder mixed with different wt % of HA was coated on stainless steel (SS) substrate using high velocity oxy-fuel (HVOF) technique to produce composite coating for biomedical applications. As the addition of HA is expected to influence the bioactivity of the coatings, these coatings were investigated for bioactivity by immersing the samples in a simulated body fluid (SBF) solution for 14 days. The apatite growth rate was evaluated by measuring Ca and P concentration in the SBF using Inductively Coupled Plasma-Optical Emission Spectrometry (ICP-OES). The concentrations of Ca and P have decreased over time in the SBF, suggesting a bone like apatite precipitation on the sample surface. It was observed that pH value increased with the increase of immersion time during initial three days and a subsequent drop after 7 days. Microstructure analysis done using FESEM technique showed nucleation and growth of bone-like apatite on the surface of the coating.

Hydroxyapatite grafted carbon nanotubes and graphene nanosheets: Promising bone implant materials

NASA Astrophysics Data System (ADS)

Oyefusi, Adebola; Olanipekun, Opeyemi; Neelgund, Gururaj M.; Peterson, Deforest; Stone, Julia M.; Williams, Ebonee; Carson, Laura; Regisford, Gloria; Oki, Aderemi

2014-11-01

In the present study, hydroxyapatite (HA) was successfully grafted to carboxylated carbon nanotubes (CNTs) and graphene nanosheets. The HA grafted CNTs and HA-graphene nanosheets were characterized using FT-IR, TGA, SEM and X-ray diffraction. The HA grafted CNTs and graphene nanosheets (CNTs-HA and Gr-HA) were further used to examine the proliferation and differentiation rate of temperature-sensitive human fetal osteoblastic cell line (hFOB 1.19). Total protein assays and western blot analysis of osteocalcin expression were used as indicators of cell proliferation and differentiation. Results indicated that hFOB 1.19 cells proliferate and differentiate well in treatment media containing CNTs-HA and graphene-HA. Both CNTs-HA and graphene-HA could be promising nanomaterials for use as scaffolds in bone tissue engineering.

Silicon-hydroxyapatite bioactive coatings (Si-HA) from diatomaceous earth and silica. Study of adhesion and proliferation of osteoblast-like cells.

PubMed

López-Alvarez, M; Solla, E L; González, P; Serra, J; León, B; Marques, A P; Reis, R L

2009-05-01

The aim of this study consisted on investigating the influence of silicon substituted hydroxyapatite (Si-HA) coatings over the human osteoblast-like cell line (SaOS-2) behaviour. Diatomaceous earth and silica, together with commercial hydroxyapatite were respectively the silicon and HA sources used to produce the Si-HA coatings. HA coatings with 0 wt% of silicon were used as control of the experiment. Pulsed laser deposition (PLD) was the selected technique to deposit the coatings. The Si-HA thin films were characterized by Fourier Transformed Infrared Spectroscopy (FTIR) demonstrating the efficient transfer of Si to the HA structure. The in vitro cell culture was established to assess the cell attachment, proliferation and osteoblastic activity respectively by, Scanning Electron Microscopy (SEM), DNA and alkaline phosphatase (ALP) quantification. The SEM analysis demonstrated a similar adhesion behaviour of the cells on the tested materials and the maintenance of the typical osteoblastic morphology along the time of culture. The Si-HA coatings did not evidence any type of cytotoxic behaviour when compared with HA coatings. Moreover, both the proliferation rate and osteoblastic activity results showed a slightly better performance on the Si-HA coatings from diatoms than on the Si-HA from silica.

Carbon-centered radicals in γ-irradiated bone substituting biomaterials based on hydroxyapatite.

PubMed

Sadlo, Jaroslaw; Strzelczak, Grazyna; Lewandowska-Szumiel, Malgorzata; Sterniczuk, Marcin; Pajchel, Lukasz; Michalik, Jacek

2012-09-01

Gamma irradiated synthetic hydroxyapatite, bone substituting materials NanoBone(®) and HA Biocer were examined using EPR spectroscopy and compared with powdered human compact bone. In every case, radiation-induced carbon centered radicals were recorded, but their molecular structures and concentrations differed. In compact bone and synthetic hydroxyapatite the main signal assigned to the CO(2) (-) anion radical was stable, whereas the signal due to the CO(3) (3-) radical dominated in NanoBone(®) and HA Biocer just after irradiation. However, after a few days of storage of these samples, also a CO(2) (-) signal was recorded. The EPR study of irradiated compact bone and the synthetic graft materials suggest that their microscopic structures are different. In FT-IR spectra of NanoBone(®), HA Biocer and synthetic hydroxyapatite the HPO(4) (2-) and CO(3) (2-) in B-site groups are detected, whereas in compact bone signals due to collagen dominate.

Ready to Use Tissue Construct for Military Bone & Cartilage Trauma

DTIC Science & Technology

2013-10-01

scaffolds composed of 90% poly-caprolactone (PCL) and 10% hydroxyapatite (HA) by weight (PCL+HA) without any seeding with either canine MSC or biologic...ligaments of the 5 knee. The implant consisted of a two layer Polycarprolacton (PCL) mixed with 10% hydroxyapatite (HA) scaffold with a 500 μm top...denoted by arrows, are apparent on both tibiae. Ratios of the biomechanical test parameters (experimental/control) in terms of percentage for

Biological activity of lactoferrin-functionalized biomimetic hydroxyapatite nanocrystals

PubMed Central

Nocerino, Nunzia; Fulgione, Andrea; Iannaccone, Marco; Tomasetta, Laura; Ianniello, Flora; Martora, Francesca; Lelli, Marco; Roveri, Norberto; Capuano, Federico; Capparelli, Rosanna

2014-01-01

The emergence of bacterial strains resistant to antibiotics is a general public health problem. Progress in developing new molecules with antimicrobial properties has been made. In this study, we evaluated the biological activity of a hybrid nanocomposite composed of synthetic biomimetic hydroxyapatite surface-functionalized by lactoferrin (LF-HA). We evaluated the antimicrobial, anti-inflammatory, and antioxidant properties of LF-HA and found that the composite was active against both Gram-positive and Gram-negative bacteria, and that it modulated proinflammatory and anti-inflammatory responses and enhanced antioxidant properties as compared with LF alone. These results indicate the possibility of using LF-HA as an antimicrobial system and biomimetic hydroxyapatite as a candidate for innovative biomedical applications. PMID:24623976

Zinc and Carbonate Co-Substituted Nano-Hydroxyapatite

NASA Astrophysics Data System (ADS)

Girija, E. K.; Kumar, G. Suresh; Thamizhavel, A.

2011-07-01

Synthesis of Zn or CO32- substituted nano-hydroxyapatite (HA) and its physico-chemical properties have been well documented. However, the effects of the simultaneous substitution of Zn and CO32- in nano-HA have not been reported. In the present study, Zn and CO32- substitutions in nano HA independently and concurrently have been done by wet precipitation method and characterized by XRD and FT-IR for its phase purity and chemical homogeneity. Further modulations of the bioactivity and thermal stability of HA due to the substitutions have been studied.

In vitro performance of ceramic coatings obtained by high velocity oxy-fuel spray.

PubMed

Melero, H; Garcia-Giralt, N; Fernández, J; Díez-Pérez, A; Guilemany, J M

2014-01-01

Hydroxyapatite coatings obtained by plasma-spraying have been used for many years to improve biological performance of bone implants, but several studies have drawn attention to the problems arising from high temperatures and the lack of mechanical properties. In this study, plasma-spraying is substituted by high velocity oxy-fuel (HVOF) spray, with lower temperatures reached, and TiO2 is added in low amounts to hydroxyapatite in order to improve the mechanical properties. Four conditions have been tested to evaluate which are those with better biological properties. Viability and proliferation tests, as well as differentiation assays and morphology observation, are performed with human osteoblast cultures onto the studied coatings. The hydroxyapatite-TiO2 coatings maintain good cell viability and proliferation, especially the cases with higher amorphous phase amount and specific surface, and promote excellent differentiation, with a higher ALP amount for these cases than for polystyrene controls. Observation by SEM corroborates this excellent behaviour. In conclusion, these coatings are a good alternative to those used industrially, and an interesting issue would be improving biological behaviour of the worst cases, which in turn show the better mechanical properties.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Boskey, Adele L., E-mail: boskeya@hss.edu; Christensen, Brian, E-mail: bc@mb.au.dk; Taleb, Hayat, E-mail: Talebh@hss.edu

Highlights: Black-Right-Pointing-Pointer Thrombin-cleaved fragments of milk-osteopontin effect hydroxyapatite formation differently. Black-Right-Pointing-Pointer N- and C-terminal fragments promoted hydroxyapatite formation and growth. Black-Right-Pointing-Pointer A central fragment inhibited hydroxyapatite formation and growth. Black-Right-Pointing-Pointer Binding to collagen or hydroxyapatite seed crystals modified these effects. -- Abstract: The manuscript tests the hypothesis that posttranslational modification of the SIBLING family of proteins in general and osteopontin in particular modify the abilities of these proteins to regulate in vitro hydroxyapatite (HA) formation. Osteopontin has diverse effects on hydroxyapatite (HA) mineral crystallite formation and growth depending on the extent of phosphorylation. We hypothesized that different regions of full-lengthmore » OPN would also have distinct effects on the mineralization process. Thrombin fragmentation of milk OPN (mOPN) was used to test this hypothesis. Three fragments were tested in a de novo HA formation assay; an N-terminal fragment (aa 1-147), a central fragment (aa 148-204) denoted SKK-fragment and a C-terminal fragment (aa 205-262). Compared to intact mOPN the C- and N-terminal fragments behaved comparably, promoting HA formation and growth, but the central SKK-fragment acted as a mineralization inhibitor. In a seeded growth experiment all fragments inhibited mineral proliferation, but the SKK-fragment was the most effective inhibitor. These effects, seen in HA-formation and seeded growth assays in a gelatin gel system and in a pH-stat experiment were lost when the protein or fragments were dephosphorylated. Effects of the fully phosphorylated protein and fragments were also altered in the presence of fibrillar collagen. The diverse effects can be explained in terms of the intrinsically disordered nature of OPN and its fragments which enable them to interact with their multiple partners.« less

Hydroxyapatite grafted carbon nanotubes and graphene nanosheets: promising bone implant materials.

PubMed

Oyefusi, Adebola; Olanipekun, Opeyemi; Neelgund, Gururaj M; Peterson, Deforest; Stone, Julia M; Williams, Ebonee; Carson, Laura; Regisford, Gloria; Oki, Aderemi

2014-11-11

In the present study, hydroxyapatite (HA) was successfully grafted to carboxylated carbon nanotubes (CNTs) and graphene nanosheets. The HA grafted CNTs and HA-graphene nanosheets were characterized using FT-IR, TGA, SEM and X-ray diffraction. The HA grafted CNTs and graphene nanosheets (CNTs-HA and Gr-HA) were further used to examine the proliferation and differentiation rate of temperature-sensitive human fetal osteoblastic cell line (hFOB 1.19). Total protein assays and western blot analysis of osteocalcin expression were used as indicators of cell proliferation and differentiation. Results indicated that hFOB 1.19 cells proliferate and differentiate well in treatment media containing CNTs-HA and graphene-HA. Both CNTs-HA and graphene-HA could be promising nanomaterials for use as scaffolds in bone tissue engineering. Copyright © 2014 Elsevier B.V. All rights reserved.

Bone Regeneration of Hydroxyapatite with Granular Form or Porous Scaffold in Canine Alveolar Sockets

PubMed Central

JANG, SEOK JIN; KIM, SE EUN; HAN, TAE SUNG; SON, JUN SIK; KANG, SEONG SOO; CHOI, SEOK HWA

2017-01-01

This study was undertaken to assess bone regeneration using hydroxyapatite (HA). The primary focus was comparison of bone regeneration between granular HA (gHA) forms and porous HA (pHA) scaffold. The extracted canine alveolar sockets were divided with three groups: control, gHA and pHA. Osteogenic effect in the gHA and pHA groups showed bone-specific surface and bone mineral density to be significantly higher than that of the control group (p<0.01). Bone volume fraction, bone mineral density, and amount of connective tissue related to disturbing osseointegration of the gHA group was higher than in the pHA group. Quantity of new bone formation of the pHA group was higher than that of the gHA group. This study demonstrated that gHA and pHA are potentially good bone substitutes for alveolar socket healing. For new bone formation during 8 weeks' post-implantation, HA with porous scaffold was superior to the granular form of HA. PMID:28438860

Inflammatory cell response to ultra-thin amorphous and crystalline hydroxyapatite surfaces.

PubMed

Rydén, Louise; Omar, Omar; Johansson, Anna; Jimbo, Ryo; Palmquist, Anders; Thomsen, Peter

2017-01-01

It has been suggested that surface modification with a thin hydroxyapatite (HA) coating enhances the osseointegration of titanium implants. However, there is insufficient information about the biological processes involved in the HA-induced response. This study aimed to investigate the inflammatory cell response to titanium implants with either amorphous or crystalline thin HA. Human mononuclear cells were cultured on titanium discs with a machined surface or with a thin, 0.1 μm, amorphous or crystalline HA coating. Cells were cultured for 24 and 96 h, with and without lipopolysaccharide (LPS) stimulation. The surfaces were characterized with respect to chemistry, phase composition, wettability and topography. Biological analyses included the percentage of implant-adherent cells and the secretion of pro-inflammatory cytokine (TNF-α) and growth factors (BMP-2 and TGF-β1). Crystalline HA revealed a smooth surface, whereas the amorphous HA displayed a porous structure, at nano-scale, and a hydrophobic surface. Higher TNF-α secretion and a higher ratio of adherent cells were demonstrated for the amorphous HA compared with the crystalline HA. TGF-β1 secretion was detected in all groups, but without any difference. No BMP-2 secretion was detected in any of the groups. The addition of LPS resulted in a significant increase in TNF-α in all groups, whereas TGF-β1 was not affected. Taken together, the results show that thin HA coatings with similar micro-roughness but a different phase composition, nano-scale roughness and wettability are associated with different monocyte responses. In the absence of strong inflammatory stimuli, crystalline hydroxyapatite elicits a lower inflammatory response compared with amorphous hydroxyapatite.

Hydroxyapatite-magnetite-MWCNT nanocomposite as a biocompatible multifunctional drug delivery system for bone tissue engineering.

PubMed

Pistone, Alessandro; Iannazzo, Daniela; Panseri, Silvia; Montesi, Monica; Tampieri, Anna; Galvagno, Signorino

2014-10-24

New magnetic hydroxyapatite-based nanomaterials as bone-specific systems for controlled drug delivery have been synthesized. The synthesized hydroxyapatite, HA, decorated with magnetite nanoparticles by a deposition method (HA/Fe3O4) and the nanocomposite system obtained using magnetic multi-walled carbon nanotubes (HA/MWCNT/Fe3O4) as a filler for HA have been characterized by chemical and morphological analyses, and their biological behavior was investigated. The systems have also been doped with clodronate in order to combine the effect of bone biomineralization induced by hydroxyapatite-based composites with the decrease of osteoclast formation induced by the drug. An analysis of the preosteoclastic RAW264.7 cell proliferation by MTT assay confirmed the high biocompatibility of the three systems. TRAP staining of RAW 264.7 conditioned with sRAKL to induce osteoclastogenesis, cultured in the presence of the systems doped and undoped with clodronate, showed the inhibitory effect of clodronate after we counted the MNC TRAP(+)cells but only in the osteoclast formation; in particular, the system HA/Fe3O4-Clo exerted a high inhibitory effect compared to the drug alone. These results demonstrate that the synthesized nanocomposites are a biocompatible magnetic drug delivery system and can represent a useful multimodal platform for applications in bone tissue engineering.

Adsorption of Amorphous Silica Nanoparticles onto Hydroxyapatite Surfaces Differentially Alters Surfaces Properties and Adhesion of Human Osteoblast Cells

PubMed Central

Kalia, Priya; Brooks, Roger A.; Kinrade, Stephen D.; Morgan, David J.; Brown, Andrew P.; Rushton, Neil; Jugdaohsingh, Ravin

2016-01-01

Silicon (Si) is suggested to be an important/essential nutrient for bone and connective tissue health. Silicon-substituted hydroxyapatite (Si-HA) has silicate ions incorporated into its lattice structure and was developed to improve attachment to bone and increase new bone formation. Here we investigated the direct adsorption of silicate species onto an HA coated surface as a cost effective method of incorporating silicon on to HA surfaces for improved implant osseointegration, and determined changes in surface characteristics and osteoblast cell adhesion. Plasma-sprayed HA-coated stainless steel discs were incubated in silica dispersions of different concentrations (0–42 mM Si), at neutral pH for 12 h. Adsorbed Si was confirmed by XPS analysis and quantified by ICP-OES analysis following release from the HA surface. Changes in surface characteristics were determined by AFM and measurement of surface wettability. Osteoblast cell adhesion was determined by vinculin plaque staining. Maximum Si adsorption to the HA coated disc occurred after incubation in the 6 mM silica dispersion and decreased progressively with higher silica concentrations, while no adsorption was observed with dispersions below 6 mM Si. Comparison of the Si dispersions that produced the highest and lowest Si adsorption to the HA surface, by TEM-based analysis, revealed an abundance of small amorphous nanosilica species (NSP) of ~1.5 nm in diameter in the 6 mM Si dispersion, with much fewer and larger NSP in the 42 mM Si dispersions. 29Si-NMR confirmed that the NSPs in the 6 mM silica dispersion were polymeric and similar in composition to the larger NSPs in the 42 mM Si dispersion, suggesting that the latter were aggregates of the former. Amorphous NSP adsorbed from the 6 mM dispersion on to a HA-coated disc surface increased the surface’s water contact angle by 53°, whereas that adsorbed from the 42 mM dispersion decreased the contact angle by 18°, indicating increased and decreased hydrophobicity, respectively. AFM showed an increase in surface roughness of the 6 mM Si treated surface, which correlated well with an increase in number of vinculin plaques. These findings suggest that NSP of the right size (relative to charge) adsorb readily to the HA surface, changing the surface characteristics and, thus, improving osteoblast cell adhesion. This treatment provides a simple way to modify plasma-coated HA surfaces that may enable improved osseointegration of bone implants. PMID:26863624

Development of osteoblast colonies on new bioactive coatings

NASA Astrophysics Data System (ADS)

Legoux, J. G.; Chellat, F.; Lima, R. S.; Marple, B. R.; Bureau, M. N.; Shen, H.; Candeliere, G. A.

2006-12-01

The aging baby boomer population coupled with an increase in life expectancy is leading to a rising number of active elderly persons in occidental countries. As a result, the orthopedic implant industry is facing numerous challenges such as the need to extend implant life, reduce the incidence of revision surgery, and improve implant performance. This paper reports results of an investigation on the bioperformance of newly developed coating-substrate systems. Hydroxyapatite (HA) and nano-titania (nano-TiO2) coatings were produced on Ti-6Al-4V and fiber reinforced polymer composite substrates. In vitro studies were conducted to determine the capacity of bioactive coatings developed to sustain osteoblast cells (fetal rat calvaria) adherence, growth, and differentiation. As revealed by scanning electron microscopy (SEM) observations and alkaline phosphatase activity, cell adhesion and proliferation demonstrated that HA coatings over a polymer composite are at least as good as HA coatings made over Ti-6Al-4V substrate in terms of osteoblast cell activity. Nano-TiO2 coatings produced by high-velocity oxyfuel (HVOF) spraying led to different results. For short-term cell culture (4.5 and 24 h), the osteoblasts appeared more flattened when grown on nano-TiO2 than on HA. The surface cell coverage after seven days of incubation was also more complete on nano-TiO2 than HA. Preliminary results indicate that osteoblast activity after 15 days of incubation on nano-TiO2 is equivalent to or greater than that observed on HA.

Comparative study of hydroxyapatite from eggshells and synthetic hydroxyapatite for bone regeneration.

PubMed

Lee, Sang-Woon; Kim, Seong-Gon; Balázsi, Csaba; Chae, Weon-Sik; Lee, Hee-Ok

2012-03-01

The objective of this study was to evaluate the physical properties of synthetic hydroxyapatite (sHA) and hydroxyapatite from eggshells (eHA) by Fourier-transform infrared (FT-IR) and x-ray diffraction (XRD) and to compare the regenerative ability of the bone using sHA and eHA in a rabbit calvarial defect model. FT-IR and XRD were used to compare the physical properties of sHA and eHA. sHA was purchased from Sigma, and eHA was kindly donated from the Hungarian academy of science. Sixteen New Zealand white rabbits were used for the animal study. After the formation of a bilateral parietal bony defect (diameter 8.0 mm), either sHA or eHA was grafted into the defect. The defect in the control was left unfilled. Bone regeneration was evaluated by histomorphometry at 4 and 8 weeks after the operation. The peak broadening of the XRD experiments were in agreement with scanning electron microscope observation; the sHA had a smaller granule size than the eHA. The eHA had impurities phases of CaO (International Center for Diffraction Data (ICDD) 075-0264) and Ca(OH)(2) (ICDD 072-0156). Total new bone was 17.11 ± 10.24% in the control group, 28.81 ± 12.63% in sHA group, and 25.68 ± 10.89% in eHA group at 4 weeks after the operation. The difference was not statistically significant (P > .05). Total new bone at 8 weeks after the operation was 27.50 ± 10.89% in the control group, 38.62 ± 17.42% in sHA group, and 41.99 ± 8.44% in the eHA group. When comparing the sHA group to the control group, the difference was not statistically significant (P > .05). However, the eHA group was significantly different from the control group (P = .038). When comparing the eHA group to the sHA group, the difference was not statistically significant (P > .05). Both types of HA showed higher bone formation than the unfilled control. However, eHA had significantly higher bone formation than the unfilled control at 8 weeks after operation. Copyright © 2012 Elsevier Inc. All rights reserved.

Monolithic Pellets, Composites and Thick Films of Hydroxyapatite: Correlation of Mechanical Properties with Microstructure.

NASA Astrophysics Data System (ADS)

Wang, Pauchiu Either

Hydroxyapatite Ca_{10}(PO _4)_6(OH)_2 (abbreviated as HA) has great biocompatibility. Poor mechanical properties of HA implants and decomposition of HA during processing are the major obstacles for widespread uses of HA. In the present thesis we have attempted to understand the sintering behavior of monolithic HA and metal-reinforced HA-matrix composites, and the mechanism of formation of HA coating in the solutions at the normal temperature. The powders of two calcium phosphates, namely hydroxyapatite and dicalcium phosphate (DCP: chemical formula Ca_2P_2O_7), were sintered at various temperatures and in various environments. The density, flexural strength and knoop hardness of both phosphates sintered in air for 4 h initially increased with the sintering temperature, reaching maxima at around 1000-1150 ^circC, and then decreased due to decomposition. To reduce dehydroxylation, HA powder was sintered in moisture at various temperatures up to 1350^circ C and X-ray diffraction study did not indicate any decomposition at the highest sintering temperature. It is seen that dehydroxylation did not hinder sintering, but decomposition obstructed sintering of both HA and DCP. Ductile-phase reinforcement of hydroxyapatite was achieved by addition of silver particulates (5-30 vol.%) in HA powder compacts. A composite made by sintering 10 vol.% Ag and balance HA at 1200^circ C for 1 h in air had flexural strength of 75 +/- 7 MPa, which was almost double that of pure HA sintered under an identical condition. Silver in the composite melted during sintering, but due to poor wetting, did not spread in between HA particles. The increase in the flexural strength of the composites was thought to be due to crack-bridging and crack-arrest by silver inclusions. Thick films (several μm) of hydroxyapatite were deposited on silicon single crystal placed in close proximity to a plate of apatite- and wollastonite -containing glass and dipped into a simulated body fluid (SBF) at 36^circC. Amorphous calcium phosphate phase present in the glass leached into the SBF, causing supersaturation of Ca^ {2+} and (PO_4)^ {3-} ions. HA films grown on Si(111) showed strong (102) texture. As a contrast hardly any HA film could be grown on Si(100) surface. Our results suggest that the driving force for formation of apatite films arises from lowering of free energy of the supersatured solution by deposition of ions in certain crystallographic arrangements on suitable substrates with low interface energies.

Comparison of new bone formation, implant integration, and biocompatibility between RGD-hydroxyapatite and pure hydroxyapatite coating for cementless joint prostheses--an experimental study in rabbits.

PubMed

Bitschnau, Achim; Alt, Volker; Böhner, Felicitas; Heerich, Katharina Elisabeth; Margesin, Erika; Hartmann, Sonja; Sewing, Andreas; Meyer, Christof; Wenisch, Sabine; Schnettler, Reinhard

2009-01-01

This is the first work to report on additional Arginin-Glycin-Aspartat (RGD) coating on precoated hydroxyapatite (HA) surfaces regarding new bone formation, implant bone contact, and biocompatibility compared to pure HA coating and uncoated stainless K-wires. There were 39 rabbits in total with 6 animals for the RGD-HA and HA group for the 4 week time period and 9 animals for each of the 3 implant groups for the 12 week observation. A 2.0 K-wire either with RGD-HA or with pure HA coating or uncoated was placed into the intramedullary canal of the tibia. After 4 and 12 weeks, the tibiae were harvested and three different areas of the tibia were assessed for quantitative and qualitative histology for new bone formation, direct implant bone contact, and formation of multinucleated giant cells. Both RGD-HA and pure HA coating showed statistically higher new bone formation and implant bone contact after 12 weeks than the uncoated K-wire. There were no significant differences between the RGD-HA and the pure HA coating in new bone formation and direct implant bone contact after 4 and 12 weeks. The number of multinucleated giant did not differ significantly between the RGD-HA and HA group after both time points. Overall, no significant effects of an additional RGD coating on HA surfaces were detected in this model after 12 weeks. (c) 2008 Wiley Periodicals, Inc.

[Enforcing osseointegration of dental implantates spray-coated by bioceramics with the help of hyaluronic acid and hydroxyapatite gel in experimental conditions].

PubMed

Kulakov, A A; Volozhin, A I; Tkachenko, V M; Doktorov, A A; Salim, Ibrakhim Samir

2007-01-01

Influence of HAP-gel (2 g of 2% solution of hyaluronic acid mixed with 0,5 g of hydroxyapatite and 0,1 ml of colloidal silver) upon osseointegration in case of delayed introduction of titanium implantates in dog jaw. By scanning electron microscopy it was shown that solely use either of HAP-gel or of ceramic spraying increased direct contact area between bone and implantates in the 6 and 9 months time period. Combination of spray-coated ceramic with HAP-gel was effective in 3 months after implantation, when solely the HAP-gel or the ceramic spraying were little effective. In the following terms of experiment (6 and 9 months) significant differences between groups 3 and 4 (implantate with ceramic spraying but without HAP-gel in the alveolus and implantate with ceramic spraying and with HAP-gel in the alveolus) were not found. The area of implantate integration with jaw bone (cortical part of it was excluded) was equal to 80% and was maximal for the given conditions of the experiment.

Biodegradable composites with aligned hydroxyapatite nanoneedles.

PubMed

Sun, Shih-Po; Wei, Mei; Olson, James R; Shaw, Montgomery T

2012-10-01

We prepared an anisotropic bone graft composite to mimic the hierarchical structure of the natural bone in which aligned hydroxyapatite (HA) nanocrystals deposit along collagen fibers. To approach the modulus and strength of the bone, we incorporated synthesized HA nanoneedles and melt drawn poly(L-lactic acid) fibers in our composite as reinforcing components. Their preferred orientation was induced via a modified pultrusion process. The HA orientation distribution was examined using wide angle X-ray diffraction. Micromechanical Halpin-Tsai model predictions considering the amount, shape, and orientation distribution of HA were compared, favorably, with the experimental observations. Copyright © 2012 Wiley Periodicals, Inc.

Biomedical properties of laser prepared silver-doped hydroxyapatite

NASA Astrophysics Data System (ADS)

Jelínek, M.; Weiserová, M.; Kocourek, T.; Zezulová, M.; Strnad, J.

2011-07-01

Thin films of hydroxyapatite (HA) and silver-doped HA were synthesized using KrF excimer laser deposition. Material was ablated from one target composed from silver and HA segments. Layers properties as silver content, structure, color, FTIR spectra and antibacterial properties (Gram-positive Bacillus subtilis) were measured. Silver concentration in HA layers of 0.06, 0.3, 1.2, 4.4, 8.3, and 13.7 at % was detected. The antibacterial efficacy changed with silver dopation from 71.0 to 99.9%. The focus is on investigation of minimum Ag concentration needed to reach a high antibacterial efficacy.

Compressive and swelling behavior of cuttlebone derived hydroxyapatite loaded PVA hydrogel implants for articular cartilage

NASA Astrophysics Data System (ADS)

Kumar, B. Y. Santosh; Kumar, G. C. Mohan; Isloor, Arun M.

2018-04-01

Developing a novel antibacterial, nontoxic and biocompatible hydrogel with superior physio mechanical properties is still becoming a challenge. Herein, we synthesize hydroxyapatite (HA) powder from cuttlefish bone and prepare a series of stiff, tough, high strength, biocompatible hydrogel reinforced with HA by integrating glutaraldehyde into PVA/HA. Powder was characterized by SEM and XRD. Compressive strength and swelling properties are studied and compare the results with the properties of healthy natural articular cartilage.

Synthesis of Hydroxyapatite through Ultrasound and Calcination Techniques

NASA Astrophysics Data System (ADS)

Akindoyo, John O.; Beg, M. D. H.; Ghazali, Suriati; Akindoyo, Edward O.; Jeyaratnam, Nitthiyah

2017-05-01

There is a growing demand for hydroxyapatite (HA) especially in medical applications, production of HA which is totally green is however a challenge. In this research, HA was produced from biowaste through ultrasound followed by calcination techniques. Pre-treatment of the biowaste was effectively achieved through the help of ultrasound. After calcination at 950°C, the obtained HA was characterized through Thermogravimetric (TGA) analysis, X-ray diffraction analysis (XRD) and Fourier transform infrared spectroscopy (FTIR). Spectrum of the produced HA was compared with standard HA index. The spectrum is in agreement with the standard HA as confirmed through FTIR, XRD and TGA result. Furthermore, morphological study of the HA through Field emission scanning electron microscope (FESEM) shows almost uniform spherical shape for the HA as expected. Based on the results obtained herein, combining ultrasound with calcination can help to produce pure HA with potential medical applications without the use of any organic solvent.

Effect of Hydroxyapatite on Bone Integration in a Rabbit Tibial Defect Model

PubMed Central

Sohn, Sung-Keun; Kim, Kyung-Taek; Kim, Chul-Hong; Ahn, Hee-Bae; Rho, Mee-Sook; Jeong, Min-Ho; Sun, Sang-Kyu

2010-01-01

Background The aim of the present study was to prepare hydroxyapatite (HA) and then characterize its effect on bone integration in a rabbit tibial defect model. The bone formation with different designs of HA was compared and the bony integration of several graft materials was investigated qualitatively by radiologic and histologic study. Methods Ten rabbits were included in this study; two holes were drilled bilaterally across the near cortex and the four holes in each rabbit were divided into four treatment groups (HAP, hydroxyapatite powder; HAC, hydroxyapatite cylinder; HA/TCP, hydroxyapatite/tri-calcium phosphate cylinder, and titanium cylinder). The volume of bone ingrowth and the change of bone mineral density were statistically calculated by computed tomography five times for each treatment group at 0, 2, 4, 6, and 8 weeks after grafting. Histologic analysis was performed at 8 weeks after grafting. Results The HAP group showed the most pronounced effect on the bone ingrowth surface area, which seen at 4, 6, and 8 weeks after graft (p < 0.05). On comparing the change of bone mineral density the bone ingrowth surface area among the 4 groups, there were no statistically significant differences among the groups found for any period (p > 0.05). On histological examination, the HAP group revealed well-recovered cortical bone, but the bone was irregularly thickened and haphazardly admixed with powder. The HAC group showed similar histological features to those of the HA/TCP group; the cortical surface of the newly developed bone was smooth and the bone matrix on the surface of the cylinder was regularly arranged. Conclusions We concluded that both the hydroxyapatite powder and cylinder models investigated in our study may be suitable as a bone substitute in the rabbit tibial defect model, but their characteristic properties are quite different. In contrast to hydroxyapatite powder, which showed better results for the bone ingrowth surface, the hydroxyapatite cylinder showed better results for the sustained morphology. PMID:20514266

Thermal spraying of functionally graded calcium phosphate coatings for biomedical implants

NASA Astrophysics Data System (ADS)

Wang, Y.; Khor, K. A.; Cheang, P.

1998-03-01

Biomedical requirements in a prosthesis are often complex and diverse in nature. Biomaterials for implants have to display a wide range of adaptability to suit the various stages of the bio-integration process of any foreign material into the human body. Often, a combination of materials is needed. The preparation of a functionally graded bioceramic coating composed of essentially calcium phosphate compounds is explored. The coating is graded in accordance to adhesive strength, bioactivity, and bioresorbability. The bond coat on the Ti-6Al-4V stub is deposited with a particle range of the hydroxyapatite (HA) that will provide a high adhesive strength and bioactivity but have poor bioresorption properties. The top coat, however, is composed of predominantly α-tricalcium phosphate (α-TCP) that is highly bioresorbable. This arrangement has the propensity of allowing accelerated bio-integration of the coating by the body tissues as the top layer is rapidly resorbed, leaving the more bioactive intermediate layer to facilitate the much needed bioactive properties for proper osteoconduction. The processing steps and problems are highlighted, as well as the results of post-spray heat treatment.

Hydroxyapatite/MCM-41 and SBA-15 Nano-Composites: Preparation, Characterization and Applications

PubMed Central

Anunziata, Oscar A.; Martínez, Maria L.; Beltramone, Andrea R.

2009-01-01

Composites of hydroxyapatite (HaP) and highly ordered large pore mesoporous silica molecular sieves such as, Al-SBA-15 and Al-MCM-41 (denoted as SBA-15 and MCM-41, respectively) were developed, characterized by XRD, BET, FTIR, HRTEM and NMR-MAS, and applied to fluoride retention from contaminated water. The proposed procedure by a new route to prepare the HaP/SBA-15 and HaP/MCM-41, composites generates materials with aluminum only in tetrahedral coordination, according to the 27Al NMR-MAS results. Free OH- groups of HaP nanocrystals, within the hosts, allowed high capacity fluoride retention. The activity of fluoride retention using HaP/MCM-41 or HaP/SBA-15 was 1-2 orders of magnitude greater, respectively, than with pure HaP.

Dissolution-resistance of glass-added hydroxyapatite composites

NASA Astrophysics Data System (ADS)

Seo, Dong Seok; Lee, Jong Kook

2009-04-01

Hydroxyapatite (HA) has generated a great deal of interest as a promising implant material. However, its poor mechanical properties induced by severe dissolution in biological milieu limit medical applications and lead to clinical failure. In this study, HA ceramics with 30P2O5-30CaO-40Na2O glass (1.0 wt.% and 2.5 wt.%) were prepared to improve the resistance of monophase HA. The monophase HA sintered body showed microstructural degradation due to grain boundary dissolution in buffered water. However, the dissolution-resistance of HA/glass composites was significantly improved and showed no apparent evidence of dissolution. This suggests that a less soluble glass phase should be placed at grain boundaries to protect HA from dissolution.

Antibacterial properties of Ag-doped hydroxyapatite layers prepared by PLD method

NASA Astrophysics Data System (ADS)

Jelínek, Miroslav; Kocourek, Tomáš; Jurek, Karel; Remsa, Jan; Mikšovský, Jan; Weiserová, Marie; Strnad, Jakub; Luxbacher, Thomas

2010-12-01

Thin hydroxyapatite (HA), silver-doped HA and silver layers were prepared using a pulsed laser deposition method. Doped layers were ablated from silver/HA targets. Amorphous and crystalline films of silver concentrations of 0.06 at.%, 1.2 at.%, 4.4 at.%, 8.3 at.% and 13.7 at.% were synthesized. Topology was studied using scanning electron microscopy and atomic force microscopy. Contact angle and zeta potential measurements were conducted to determine the wettability, surface free energy and electric surface properties. In vivo measurement (using Escherichia coli cells) of antibacterial properties of the HA, silver-doped HA and silver layers was carried out. The best antibacterial results were achieved for silver-doped HA layers of silver concentration higher than 1.2 at.%.

High strength yttria-reinforced HA scaffolds fabricated via honeycomb ceramic extrusion.

PubMed

Elbadawi, M; Shbeh, M

2018-01-01

The present study investigated the effects of hydroxyapatite (HA) reinforced with yttria on porous scaffolds fabricated via honeycomb ceramic extrusion. Yttria was selected as it has been demonstrated to toughen other ceramics. Moreover, yttria has been surmised to suppress dehydroxylation in HA, a characteristic that prefigures decomposition thereof during sintering into mechanically weaker phases. However, the compressive strength of yttria-reinforced hydroxyapatite (Y-HA) porous scaffolds has hitherto not been reported. Y-HA was synthesised by calcining a commercially available HA with 10wt% yttria at 1000°C. Y-HA was then fabricated into porous scaffolds using an in-house honeycomb extruder, and subsequently sintered at 1200 and 1250°C. The results were compared to the uncalcined as-received commercial powder (AR-HA) and calcined pure HA powder at 1000°C (C-HA). It was discovered that calcination alone caused marked improvements to the stoichiometry, thermal stability, porosity and compressive strength of scaffolds. The improvements were ascribed to the calcined powders with less susceptibility to both agglomeration and enhanced densification. Still, differences were observed between C-HA and Y-HA at 1250°C. The compressive strength increased from 105.9 to 127.3MPa, a larger microporosity was descried and the HA matrix in Y-HA was more stoichiometric. The latter was confirmed by XRD and EDS analyses. Therefore, it was concluded that the reinforcing of hydroxyapatite with yttria improved the compressive strength and suppressed dehydroxylation of porous HA scaffolds. In addition, the compressive strength achieved demonstrated great potential for load-bearing application. Copyright © 2017 Elsevier Ltd. All rights reserved.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mohd Zaheruddin, K., E-mail: zaheruddin@unimap.edu.my; Rahmat, A., E-mail: azmirahmat@unimap.edu.my; Shamsul, J. B., E-mail: sbaharin@unimap.edu.my

Cobalt-hydroxyapatite (Co-HA) composites was successfully prepared by simple electroless deposition process of Co on the surface of hydroxyapatite (HA) particles. Co deposition was carried out in an alkaline bath with sodium hypophosphite as a reducing agent. The electroless process was carried out without sensitization and activation steps. The deposition of Co onto HA was characterized by scanning electron microscopy (SEM) and energy-dispersive X-ray spectroscopy (EDX). The Co-HA composite powder was compacted and sintered at 1250°C. The Co particles were homogeneously dispersed in the HA matrix after sintering and the mechanical properties of composites was enhanced to 100 % with 3more » % wt Co and gradually decreased at higher Co content.« less

Biomimetic Bone-like Hydroxyapatite by Mineralization on Supramolecular Porous Fiber Networks.

PubMed

Li, Bo; Kan, Lei; Zhang, Xinyue; Li, Jie; Li, Ruiting; Gui, Qinyuan; Qiu, Dengli; He, Fei; Ma, Ning; Wang, Yapei; Wei, Hao

2017-08-29

Hydroxyapatite (HA), the main inorganic component of bone tissue, is mineralized with collagen fibril scaffolds during bone formation. Inspired by the process, a self-assembled porous network architecture was designed and synthesized by using the 2-ureido-4[1H]-pyrimidone (UPy) modified glycerol molecule UPy-Gly, which was further utilized as a template for biomimetic mineralization. When incubated in simulated body fluid (SBF), the HA nucleus first formed in the holes of the template by the induction of hydroxyls on the surface, grew along the nanofibers, and fused with the template to fabricate hydroxyapatite composites (UPy-Gly/HA). Transmission electron microscopic observation demonstrates that the mineral clusters are accumulated by lamella-like nano hydroxyapatite and the elasticity modulus measured by atomic force microscopy is about 5.5 GPa, which is quite close to the natural cancellous bone tissue of human both in structure and in mechanical properties. The Cell Counting Kit 8 (CCK-8) assay of UPy-Gly and UPy-Gly/HA shows noncytotoxicity to mouse fibroblast L-929 cells. This bioinspired composite will be a promising material for potential use in bone tissue implantation and regeneration engineering.

Controlled release of NELL-1 protein from chitosan/hydroxyapatite-modified TCP particles.

PubMed

Zhang, Yulong; Dong, Rui; Park, Yujin; Bohner, Marc; Zhang, Xinli; Ting, Kang; Soo, Chia; Wu, Benjamin M

2016-09-10

NEL-like molecule-1 (NELL-1) is a novel osteogenic protein that showing high specificity to osteochondral cells. It was widely used in bone regeneration research by loading onto carriers such as tricalcium phosphate (TCP) particles. However, there has been little research on protein controlled release from this material and its potential application. In this study, TCP was first modified with a hydroxyapatite coating followed by a chitosan coating to prepare chitosan/hydroxyapatite-coated TCP particles (Chi/HA-TCP). The preparation was characterized by SEM, EDX, FTIR, XRD, FM and Zeta potential measurements. The NELL-1 loaded Chi/HA-TCP particles and the release kinetics were investigated in vitro. It was observed that the Chi/HA-TCP particles prepared with the 0.3% (wt/wt) chitosan solution were able to successfully control the release of NELL-1 and maintain a slow, steady release for up to 28 days. Furthermore, more than 78% of the loaded protein's bioactivity was preserved in Chi/HA-TCP particles over the period of the investigation, which was significantly higher than that of the protein released from hydroxyapatite coated TCP (HA-TCP) particles. Collectively, this study suggests that the osteogenic protein NELL-1 showed a sustained release pattern after being encapsulated into the modified Chi/HA-TCP particles, and the NELL-1 integrated composite of Chi/HA-TCP showed a potential to function as a protein delivery carrier and as an improved bone matrix for use in bone regeneration research. Copyright © 2016 Elsevier B.V. All rights reserved.

The effect of adhesive strength of hydroxyapatite coating on the stability of hydroxyapatite-coated prostheses in vivo at the early stage of implantation

PubMed Central

Duan, Yonghong; Zhu, Shu; Guo, Fei; Zhu, Jinyu; Li, Mao; Ma, Jie

2012-01-01

Introduction With the increase in joint revision surgery after arthroplasty, defects of hydroxyapatite (HA)-coated prostheses have been observed increasingly often. These defects adversely affect the prosthetic stability in vivo. This study has analyzed the potential effect of the adhesive strength of HA coating on the stability of HA-coated prostheses in vivo after its implantation. Material and methods Sixty experimental rabbits were divided into HA- and Ti-coated groups. HA-coated prostheses were implanted into the bilateral epicondyle of rabbits femurs. Ti-coated prostheses were implanted as control. At different time points(4, 9, and 15 weeks) after implantation, bone tissue samples were fetched out respectively for histomorphometric analysis. Push-out testing was used to detect the ultimate shear strength at the bone-prosthesis interface. Scanning electron microscope (SEM) observation and energy-dispersive X-ray spectroscopy (EDX) analysis were used to observe the changes in surface composition of the prostheses after the ultimate shear strength testing. The coating adhesive strength of two kinds of coatings were also examined by scratch testing. Results Hydroxyapatite coating has an obvious advantage in facilitating osteogenesis and its plays a critical role in the stability of prostheses. However, the ultimate shear strength of HA-coated prostheses is much lower than that of Ti-coated implants (p < 0.01). Further study has demonstrated that the stability of HA-coated prostheses in vivo is affected by the relatively low adhesive strength between coating and substrate. Conclusions Obvious advantage in facilitating osteogenesis around HA-coated prostheses is not the only factor that determines the stability of prostheses in vivo. PMID:22661990

Support for the initial attachment, growth and differentiation of MG-63 cells: a comparison between nano-size hydroxyapatite and micro-size hydroxyapatite in composites

PubMed Central

Filová, Elena; Suchý, Tomáš; Sucharda, Zbyněk; Šupová, Monika; Žaloudková, Margit; Balík, Karel; Lisá, Věra; Šlouf, Miroslav; Bačáková, Lucie

2014-01-01

Hydroxyapatite (HA) is considered to be a bioactive material that favorably influences the adhesion, growth, and osteogenic differentiation of osteoblasts. To optimize the cell response on the hydroxyapatite composite, it is desirable to assess the optimum concentration and also the optimum particle size. The aim of our study was to prepare composite materials made of polydimethylsiloxane, polyamide, and nano-sized (N) or micro-sized (M) HA, with an HA content of 0%, 2%, 5%, 10%, 15%, 20%, 25% (v/v) (referred to as N0–N25 or M0–M25), and to evaluate them in vitro in cultures with human osteoblast-like MG-63 cells. For clinical applications, fast osseointegration of the implant into the bone is essential. We observed the greatest initial cell adhesion on composites M10 and N5. Nano-sized HA supported cell growth, especially during the first 3 days of culture. On composites with micro-size HA (2%–15%), MG-63 cells reached the highest densities on day 7. Samples M20 and M25, however, were toxic for MG-63 cells, although these composites supported the production of osteocalcin in these cells. On N2, a higher concentration of osteopontin was found in MG-63 cells. For biomedical applications, the concentration range of 5%–15% (v/v) nano-size or micro-size HA seems to be optimum. PMID:25125978

Mimix hydroxyapatite cement use in the reconstruction of the craniofacial skeleton.

PubMed

Mann, Robert J; Blount, Andrew L; Neaman, Keith C; Korepta, Lindsey

2011-11-01

Reconstruction of the craniofacial skeleton has undergone a significant evolution during the past century. Initially, the use of autogenous bone grafts from various sites was the criterion standard. However, owing to donor site morbidity and lack of sufficient bone for large defects, surgeons have relied on various bone substitutes. Hydroxyapatite (HA) has served as an alternative to autogenous grafts, but questions regarding biocompatibility, risk of infection, and slow set times have hampered its acceptance. This article serves as a review of a single surgeon's experience using HA in the craniofacial skeleton. Eighteen patients receiving HA between March 2000 and November 2006 were observed. Sixteen underwent recontouring of skull-based bone defects, and 2 underwent recontouring for nasal and alveolar defects. The mean amount of HA used in each patient was 30.2 g. For large contour irregularities, the maximum thickness of HA used was 8 mm. The size of bone defects ameliorated averaged 4.8 cm(2). Complications occurred in 3 (16.7%) of 18 patients and included scalp hematoma and superficial cellulitis. In addition, 1 patient developed a facial abscess after placement along the alveolar floor, which necessitated removal. Hydroxyapatite represents a viable alternative to autogenous bone grafts when used in the correct manner. Hydroxyapatite should be used only for smaller defects or used in conjunction with absorbable plates when attempting to fill larger defects. Use of HA for nasal piriform augmentation or alveolar bone grafting should not be considered owing to problems with late infections.

Inhibition of hydroxyapatite growth by casein, a potential salivary phosphoprotein homologue.

PubMed

Romero, Maria J R H; Nakashima, Syozi; Nikaido, Toru; Ichinose, Shizuko; Sadr, Alireza; Tagami, Junji

2015-08-01

Salivary phosphoproteins are essential in tooth mineral regulation but are often overlooked in vitro. This study aimed to evaluate the effect of casein, as a salivary phosphoprotein homologue, on the deposition and growth of hydroxyapatite (HA) on tooth surfaces. Hydroxyapatite growth was quantified using seeded crystal systems. Artificial saliva (AS) containing HA powder and 0, 10, 20, 50, or 100 μg ml(-1) of casein, or 100 μg ml(-1) of dephosphorylated casein (Dcasein), was incubated for 0-8 h at 37°C, pH 7.2. Calcium concentrations were measured using atomic absorption spectroscopy (AAS). Surface precipitation of HA on bovine enamel and dentine blocks, incubated in similar conditions for 7 d, was examined using field emission scanning electron microscopy (FE-SEM) and transmission electron microscopy (TEM) with selected area electron diffraction (SAED). Casein adsorption was assessed using modified Lowry assays and zeta-potential measurements. The AAS results revealed a concentration-dependent inhibition of calcium consumption. Hydroxyapatite precipitation occurred when no casein was present, whereas precipitation of HA was apparently completely inhibited in casein-containing groups. Adsorption data demonstrated increasingly negative zeta-potential with increased casein concentration and an affinity constant similar to proline-rich proteins with Langmuir modelling. Casein inhibited the deposition and growth of HA primarily through the binding of esterized phosphate to HA active sites, indicating its potential as a mineral-regulating salivary phosphoprotein homologue in vitro. © 2015 Eur J Oral Sci.

Influence of hydroxyapatite on the corrosion resistance of the Ti-13Nb-13Zr alloy.

PubMed

Duarte, Laís T; Biaggio, Sonia R; Rocha-Filho, Romeu C; Bocchi, Nerilso

2009-05-01

Electrochemical analyses on the biocompatible alloy Ti-13Nb-13Zr wt% in an electrolyte simulating physiological medium (PBS solution) are reported. Hydroxyapatite (HA) films were obtained on the alloy by electrodeposition at constant cathodic current. Samples of the alloy covered with an anodic-oxide film or an anodic-oxide/HA film were analyzed by open circuit potential and electrochemical impedance spectroscopy measurements during 180 days in the PBS electrolyte. Analyses of the open-circuit potential (E (oc)) values indicated that the oxide/HA film presents better protection characteristics than the oxide only. This behavior was corroborated by the higher film resistances obtained from impedance data, indicating that, besides improving the alloy osteointegration, the hydroxyapatite film may also increase the corrosion protection of the biomaterial.

Hydroxyapatite-anatase-carbon nanotube nanocomposite coatings fabricated by electrophoretic codeposition for biomedical applications.

PubMed

Zhang, Bokai; Kwok, Chi Tat

2011-10-01

In order to eliminate micro-cracks in the monolithic hydroxyapatite (HA) and composite hydroxyapatite/carbon nanotube (HA/CNT) coatings, novel HA/TiO(2)/CNT nanocomposite coatings on Ti6Al4V were attempted to fabricate by a single-step electrophoretic codeposition process for biomedical applications. The electrophoretically deposited layers with difference contents of HA, TiO(2) (anatase) and CNT nanoparticles were sintered at 800°C for densification with thickness of about 7-10 μm. A dense and crack-free coating was achieved with constituents of 85 wt% HA, 10 wt% TiO(2) and 5 wt% CNT. Open-circuit potential measurements and cyclic potentiodynamic polarization tests were used to investigate the electrochemical corrosion behavior of the coatings in vitro conditions (Hanks' solution at 37°C). The HA/TiO(2)/CNT coatings possess higher corrosion resistance than that of the Ti6Al4V substrate as reflected by nobler open circuit potential and lower corrosion current density. In addition, the surface hardness and adhesion strength of the HA/TiO(2)/CNT coatings are higher than that of the monolithic HA and HA/CNT coatings without compromising their apatite forming ability. The enhanced properties were attributed to the nanostructure of the coatings with the appropriate TiO(2) and CNT contents for eliminating micro-cracks and micro-pores.

Comparison on mechanical properties of single layered and bilayered chitosan-gelatin coated porous hydroxyapatite scaffold prepared through freeze drying method

NASA Astrophysics Data System (ADS)

Effendi, M. D.; Gustiono, D.; Lukmana; Ayu, D.; Kurniawati, F.

2017-02-01

Biopolymer coated porous hydroxyapatite (HA) scaffolds were prepared for tissue engineering trough freeze drying method and impregnation. in this study, to mimic the mineral and organic component of natural bone, synthetic hydroxapatite (HA) scaffolds coated by polymer were prepared. Highly porous Hap scaffolds, fabricated by synthetic HA impregnation method on polyurethane foam, were coated with polymer coating solution, consisting of chitosan, Gelatin, and bilayered chitosan-gelatin prepared by aging and impregnating technique. For the purpose of comparison, The bare scaffolds without polymer coating layer were investigated. The Bare scaffolds were highly porous and interconnected with a pore size of around 150 µm-714 µm, has porosity at around 67,7% -85,7%, and has mechanical strength at around 0.06 Mpa - 0.071 Mpa, which is suitable for osteoblast cell Proliferation. Chitosan coated porous HA scaffold and gelatin coated porous HA scaffold had mechanical strength at around 0.81-0.85 Mpa, and 1.32-1.34 Mpa, respectively, with weight ratio of biopolymer and Hap was around 18%-22%. To compare these results, the coating on the bare scaffold with gelatin and chitosan had been conducted. Based on the result of FTIR, it could be concluded that coating procedure applied on porous hydroxy apatite (HA) coated by gelatin, chitosan coated HA scaffold, and bilayered Gelatin-chitosan coated porous HA scaffold, confirming that for allsampleshad no significant chemical effect on the coating structure. The compressive strength of bilayered Gelatin-chitosan coated HA scaffold had middle values between the rest, at around 1,06-1.2 Mpa for the samples at the same weight ratio of biopolymer: HA (around 18% - 22%). These results also confirming that coating by gelatin on porous hydroxyapatite was highest compresive strength and can be applied to improve mechanical properties of porous hydroxyapatite bare scaffold

Laser engineered multilayer coating of biphasic calcium phosphate/titanium nanocomposite on metal substrates.

PubMed

Zhang, Martin Yi; Ye, Chang; Erasquin, Uriel Joseph; Huynh, Toan; Cai, Chengzhi; Cheng, Gary J

2011-02-01

In this work, laser coating of biphasic calcium phosphate/titanium (BCP/Ti) nanocomposite on Ti-6Al-4 V substrates was developed. A continuous wave neodymium-doped yttrium aluminium garnet (Nd:YAG) laser was used to form a robust multilayer of BCP/Ti nanocomposite starting from hydroxyapatite and titanium nanoparticles. In this process, low power coating is realized because of the strong laser-nanoparticle interaction and good sinterability of nanosized titanium. To guide the optimization of laser processing conditions for the coating process, a multiphysics model coupling electromagnetic module with heat transfer module was developed. This model was validated by laser coating experiments. Important features of the coated samples, including microstructures, chemical compositions, and interfacial bonding strength, were characterized. We found that a multilayer of BCP, consisting of 72% hydroxyapatite (HA) and 28% beta-tricalcium phosphate (β-TCP), and titanium nanocomposite was formed on Ti-6Al-4 V substrates. Significantly, the coating/substrate interfacial bonding strength was found to be two times higher than that of the commercial plasma sprayed coatings. Preliminary cell culture studies showed that the resultant BCP/Ti nanocomposite coating supported the adhesion and proliferation of osteoblast-like UMR-106 cells.

Effect of modification substrate on the microstructure of hydroxyapatite coating

NASA Astrophysics Data System (ADS)

Realpe-Jaramillo, J.; Morales-Morales, J. A.; González-Sánchez, J. A.; Cabanzo, R.; Mejía-Ospino, E.; Rodríguez-Pereira, J.

2017-01-01

Bioactive hydroxyapatite (HA) coatings were fabricated by a precipitation, sol-gel and dip-coating method. The effects of the aging time and the base used to adjust pH and substrate materials on the phases and microstructures of HA coatings were studied by field emission scanning electron microscopy FESEM, energy dispersive spectroscopy EDS, X-ray photoelectron spectroscopy XPS, and the vibrations of the phosphate groups were determined by Raman spectroscopy. The results showed that all the films were composed of the phases of TiO2 and HA. With coated titanium substrate with TiO2, the crystallinity of the HA coating increases, the structure became more compact and the Ca/P ratio increased because of the loss of P in the films. The addition of sodium hydroxide (adjusting the pH level to about 10) can increase the HA content in the coating. XPS and EDS results for steel substrate and titanium showed poor calcium content as obtained with a Ca/P ratio of 1.38 and 1.58, respectively, composition is similar to that of natural apatite. However, spectroscopic results suggest the presence of a mixture of hydroxyapatite and octacalcium phosphate. The different substrate materials have a high influence on the microstructure of the separated double films. However, hydroxyapatite nanopowders coatings were obtained using a simple method, with potential biomedical applications.

Do Bone Graft and Cracking of the Sclerotic Cavity Improve Fixation of Titanium and Hydroxyapatite-coated Revision Implants in an Animal Model?

PubMed

Elmengaard, Brian; Baas, Joergen; Jakobsen, Thomas; Kold, Soren; Jensen, Thomas B; Bechtold, Joan E; Soballe, Kjeld

2017-02-01

We previously introduced a manual surgical technique that makes small perforations (cracks) through the sclerotic bone shell that typically forms during the process of aseptic loosening ("crack" revision technique). Perforating just the shell (without violating the proximal cortex) can maintain overall bone continuity while allowing marrow and vascular elements to access the implant surface. Because many revisions require bone graft to fill defects, we wanted to determine if bone graft could further increase implant fixation beyond what we have experimentally shown with the crack technique alone. Also, because both titanium (Ti6Al4V) and hydroxyapatite (HA) implant surfaces are used in revisions, we also wanted to determine their relative effectiveness in this model. We hypothesized that both (1) allografted plasma-sprayed Ti6Al4V; and (2) allografted plasma-sprayed HA-coated implants inserted with a crack revision technique have better fixation compared with a noncrack revision technique in each case. Under approval from our Institutional Animal Care and Use Committee, a female canine animal model was used to evaluate the uncemented revision technique (crack, noncrack) using paired contralateral implants while implant surface (Ti6Al4V, HA) was qualitatively compared between the two (unpaired) series. All groups received bone allograft tightly packed around the implant. This revision model includes a cylindrical implant pistoning 500 μm in a 0.75-mm gap, with polyethylene particles, for 8 weeks. This engenders a bone and tissue response representative of the metaphyseal cancellous region of an aseptically loosened component. At 8 weeks, the original implants were revised and followed for an additional 4 weeks. Mechanical fixation was assessed by load, stiffness, and energy to failure when loaded in axial pushout. Histomorphometry was used to determine the amount and location of bone and fibrous tissue in the grafted gap. The grafted crack revision improved mechanical shear strength, stiffness, and energy to failure (for Ti6Al4V 27- to 69-fold increase and HA twofold increases). The histomorphometric analysis demonstrated primarily fibrous membrane ongrowth and in the gap for the allografted Ti6Al4V noncrack revisions. For allografted HA noncrack revisions, bone ongrowth at the implant surface was observed, but fibrous tissue also was present in the inner gap. Although both Ti6Al4V and HA surfaces showed improved fixation with grafted crack revision, and Ti6Al4V achieved the highest percent gain, HA demonstrated the strongest overall fixation. The results of this study suggest that novel osteoconductive or osteoinductive coatings and bone graft substitutes or tissue-engineered constructs may further improve bone-implant fixation with the crack revision technique but require evaluation in a rigorous model such as presented here. This experimental study provides data on which to base clinical trials aimed to improve fixation of revision implants. Given the multifactorial nature of complex human revisions, such a protocoled clinical study is required to determine the clinical applicability of this approach.

[Study on biocompatibility of hydroxyapatite/high density polyethylene (HA/HDPE) nano-composites artificial ossicle].

PubMed

Wang, Guohui; Zhu, Shaihong; Tan, Guolin; Zhou, Kechao; Huang, Suping; Zhao, Yanzhong; Li, Zhiyou; Huang, Boyun

2008-06-01

This study was aimed to evaluate the biocompatibility of Hydroxyapatite/High density polyethylene (HA/ HDPE) nano-composites artificial ossicle. The percentage of S-period cells were detected by flow cytometry after L929 cells being incubated with extraction of the HA/HDPE nano-composites; the titanium materials for clinical application served as the contrast. In addition, both materials were implanted in animals and the histopathological evaluations were conducted. There were no statistically significant differences between the two groups (P >0.05). The results demonstrated that the HA/HDPE nano-composite artificial ossicle made by our laboratory is of a good biocompatibility and clinical application outlook.

Evaluation of a setting reaction pathway in the novel composite TiHA-CSD bone cement by FT-Raman and FT-IR spectroscopy

NASA Astrophysics Data System (ADS)

Paluszkiewicz, Czesława; Czechowska, Joanna; Ślósarczyk, Anna; Paszkiewicz, Zofia

2013-02-01

The aim of this study was to determine a setting reaction pathway in a novel, surgically handy implant material, based on calcium sulfate hemihydrate (CSH) and titanium doped hydroxyapatite (TiHA). The previous studies confirmed superior biological properties of TiHA in comparison to the undoped hydroxyapatite (HA) what makes it highly attractive for future medical applications. In this study the three types of titanium modified HA powders: untreated, calcined at 800 °C, sintered at 1250 °C and CSH were used to produce bone cements. The Fourier Transform-InfraRed (FT-IR) spectroscopy and Raman spectroscopy were applied to evaluate processes taking place during the setting of the studied materials. Our results undoubtedly confirmed that the reaction pathways and the phase compositions differed significantly for set cements and were dependent on the initial heat treatment of TiHA powder. Final materials were multiphase composites consisting of calcium sulfate dihydrate, bassanite, tricalcium phosphate, hydroxyapatite and calcium titanate (perovskite). The FT-IR and Scanning Electron Microscopy (SEM) measurements performed after the incubation of the cement samples in the simulated body fluid (SBF), indicate on high bioactive potential of the obtained bone cements.

Monodisperse selenium-substituted hydroxyapatite: Controllable synthesis and biocompatibility.

PubMed

Sun, Jianpeng; Zheng, Xiaoyan; Li, Hui; Fan, Daidi; Song, Zhanping; Ma, Haixia; Hua, Xiufu; Hui, Junfeng

2017-04-01

Hydroxyapatite (HA) is the major inorganic component of natural bone tissue. As an essential trace element, selenium involves in antioxidation and anticancer of human body. So far, ion-doped hydroxyapatites (HAs) are widely investigated owing to their great applications in field of biomaterial, biological labeling. In this paper, series of monodisperse HA doped with SeO 3 2- (SeHA) was successfully synthesized based on the liquid-solid-solution (LSS) strategy. The obtained samples were characterized by transmission electron microscopy (TEM), X-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FTIR) and energy-dispersive spectrometer (EDS). The results indicated that the SeO 3 2- doping level of the Se/(P+Se) molar ratio of 0-0.4 can be requisitely controlled, and the morphology of SeHA nanoparticles varied from nanorods to nanoneedles with increasing Se/(P+Se) molar ratio. Significantly, the as-synthesized SeHA nanocrystals exhibit a low cytotoxicity for osteoblastic cells, showing exciting potentials for application in artificial scaffold materials inhibiting of tumor growth in bone. Copyright © 2016 Elsevier B.V. All rights reserved.

Hydroxyapatite-chitosan based bioactive hybrid biomaterials with improved mechanical strength

NASA Astrophysics Data System (ADS)

Zima, A.

2018-03-01

Composites consisting of hydroxyapatite (HA) and chitosan (CTS) have recently been intensively studied. In this work, a novel inorganic-organic (I/O) HA/CTS materials in the form of granules were prepared through a simple solution-based chemical method. During the synthesis of these hybrids, the electrostatic complexes between positively charged, protonated amine groups of chitosan and the negative phosphate species (HPO42 - and H2PO4-) were formed. Our biocomposites belong to the class I of hybrids, which was confirmed by FTIR studies. XRD analysis revealed that the obtained materials consisted of hydroxyapatite as the only crystalline phase. Homogeneous dispersion of the components in HA/CTS composites was confirmed. The use of 17 wt% and 23 wt% of chitosan resulted in approximately 12-fold and 16-fold increase in the compressive strength of HA/CTS as compared to the non-modified HA material. During incubation of the studied materials in SBF, pH of the solution remained close to the physiological one. Formation of apatite layer on their surfaces indicated bioactive nature of the developed biomaterials.

Biocompatibility of MG-63 cells on collagen, poly-L-lactic acid, hydroxyapatite scaffolds with different parameters.

PubMed

Cecen, Berivan; Kozaci, Didem; Yuksel, Mithat; Erdemli, Diler; Bagriyanik, Alper; Havitcioglu, Hasan

2015-03-18

In this study, osteoblast-like MG-63 cells were cultured on 3 different scaffold types composed of (a) collagen + poly-L-lactic acid (PLLA), (b) collagen + hydroxyapatite (HA; 30ºC) or (c) collagen + hydroxyapatite (HA; 37ºC) and produced with different porosities. Biomechanical properties of the scaffolds were characterized by tensile strength measurements. Properties of the cell-seeded scaffolds were evaluated with scanning electron microscopy (SEM). Cell adhesion and proliferation capacities were evaluated. Alkaline phosphatase (ALP) levels in media were measured. Transmission electron microscopy (TEM) and histological analyses were used to assess morphological characteristics. Our results showed that collagen-based PLLA and HA scaffolds have good cell biocompatibility. MTT test showed that the scaffolds exhibited no cytotoxicity. According to the force and displacement data, collagen + HA at 37ºC showed the highest mechanical strength and displacement. The results suggest that collagen-based PLLA and HA scaffolds might improve osteoblastic growth in vitro and have biomaterial integration potential in possible therapeutic approaches for future clinical studies.

Synthesis and characterization of new composite materials based on poly(methacrylic acid) and hydroxyapatite with applications in dentistry.

PubMed

Cucuruz, Andrei Tiberiu; Andronescu, Ecaterina; Ficai, Anton; Ilie, Andreia; Iordache, Florin

2016-08-30

The use of methacrylic acid (MAA) in medicine was poorly investigated in the past but can be of great importance because the incorporation of hydroxyapatite (HA) can lead to new composite materials with good properties due to the strong electrostatic interactions between carboxylate groups of polymer and Ca(2+) ions from HA. The scope of this study was to determine the potential of using composite materials based on poly(methacrylic acid) (PMAA) and hydroxyapatite in dentistry. Two routes of synthesis were taken into account: i) HA was synthesised in situ and ii) commercial HA was used. Fourier transform infrared spectroscopy and X-ray diffraction were used for compositional assessments. Scanning electron microscopy was performed to determine the morphology and differential thermal analysis (DTA) coupled with thermogravimetric analysis (TG) was used to study the thermal behaviour and to observe quantitative changes. In-vitro tests were also performed in order to evaluate the biocompatibility of both PMAA/HA composites by monitoring the development potential of human endothelial cells using MTT assay and fluorescent microscopy. Copyright © 2016 Elsevier B.V. All rights reserved.

Biomimetic composite microspheres of collagen/chitosan/nano-hydroxyapatite: In-situ synthesis and characterization.

PubMed

Teng, Shu-Hua; Liang, Mian-Hui; Wang, Peng; Luo, Yong

2016-01-01

The collagen/chitosan/hydroxyapatite (COL/CS/HA) composite microspheres with a good spherical form and a high dispersity were successfully obtained using an in-situ synthesis method. The FT-IR and XRD results revealed that the inorganic phase in the microspheres was crystalline HA containing carbonate ions. The morphology of the composite microspheres was dependent on the HA content, and a more desirable morphology was achieved when 20 wt.% HA was contained. The composite microspheres exhibited a narrow particle distribution, most of which ranged from 5 to 10 μm. In addition, the needle-like HA nano-particles were uniformly distributed in the composite microspheres, and their crystallinity and crystal size decreased with the HA content. Copyright © 2015 Elsevier B.V. All rights reserved.

The Production of Porous Hydroxyapatite Scaffolds with Graded Porosity by Sequential Freeze-Casting.

PubMed

Lee, Hyun; Jang, Tae-Sik; Song, Juha; Kim, Hyoun-Ee; Jung, Hyun-Do

2017-03-31

Porous hydroxyapatite (HA) scaffolds with porosity-graded structures were fabricated by sequential freeze-casting. The pore structures, compressive strengths, and biocompatibilities of the fabricated porous HA scaffolds were evaluated. The porosities of the inner and outer layers of the graded HA scaffolds were controlled by adjusting the initial HA contents of the casting slurries. The interface between the dense and porous parts was compact and tightly adherent. The porosity and compressive strengths of the scaffold were controlled by the relative thicknesses of the dense/porous parts. In addition, the porous HA scaffolds showed good biocompatibility in terms of preosteoblast cell attachment and proliferation. The results suggest that porous HA scaffolds with load-bearing parts have potential as bone grafts in hard-tissue engineering.

The Production of Porous Hydroxyapatite Scaffolds with Graded Porosity by Sequential Freeze-Casting

PubMed Central

Lee, Hyun; Jang, Tae-Sik; Song, Juha; Kim, Hyoun-Ee; Jung, Hyun-Do

2017-01-01

Porous hydroxyapatite (HA) scaffolds with porosity-graded structures were fabricated by sequential freeze-casting. The pore structures, compressive strengths, and biocompatibilities of the fabricated porous HA scaffolds were evaluated. The porosities of the inner and outer layers of the graded HA scaffolds were controlled by adjusting the initial HA contents of the casting slurries. The interface between the dense and porous parts was compact and tightly adherent. The porosity and compressive strengths of the scaffold were controlled by the relative thicknesses of the dense/porous parts. In addition, the porous HA scaffolds showed good biocompatibility in terms of preosteoblast cell attachment and proliferation. The results suggest that porous HA scaffolds with load-bearing parts have potential as bone grafts in hard-tissue engineering. PMID:28772735

Surface characterization of colloidal-sol gel derived biphasic HA/FA coatings.

PubMed

Cheng, Kui; Zhang, Sam; Weng, Wenjian

2007-10-01

Hydroxyapatite (HA) powders are ultrasonically dispersed in the precursor of fluoridated hydroxyapatite (FHA) or fluorapatite (FA) to form a "colloidal sol". HA/FA biphasic coatings are prepared on Ti6Al4V substrate via dip coating, 150 degrees C drying and 600 degrees C firing. The coatings show homogenous distribution of HA particles in the FA matrix. The relative phase proportion can be tailored by the amount of HA in the colloidal sol. The surfaces of the coatings consist of two kinds of distinct domains: HA and FA, resulting in a compositionally heterogeneous surface. The biphasic coating surface becomes increasingly rougher with HA powders, from around 200 nm of pure FA to 400-600 nm in Ra of biphasic coatings. The rougher biphasic HA/FA surfaces with chemically controllable domains will favor cell attachment, apatite layer deposition and necessary dissolution in clinical applications.

Direct and ultrasonic measurements of macroscopic piezoelectricity in sintered hydroxyapatite

NASA Astrophysics Data System (ADS)

Tofail, S. A. M.; Haverty, D.; Cox, F.; Erhart, J.; Hána, P.; Ryzhenko, V.

2009-03-01

Macroscopic piezoelectricity in hydroxyapatite (HA) ceramic was measured by a direct quasistatic method and an ultrasonic interference technique. The effective symmetry of polycrystalline aggregate was established and a detailed theoretical analysis was carried out to determine by these two methods the shear piezoelectric coefficient, d14, of HA. Piezoelectric nature of HA was proved qualitatively although a specific quantitative value for the d14 coefficient could not be established. Ultrasound method was also employed to anisotropic elastic constants, which agreed well with those measured from the first principles.

Collagen hydrolysate based collagen/hydroxyapatite composite materials

NASA Astrophysics Data System (ADS)

Ficai, Anton; Albu, Madalina Georgiana; Birsan, Mihaela; Sonmez, Maria; Ficai, Denisa; Trandafir, Viorica; Andronescu, Ecaterina

2013-04-01

The aim of this study was to study the influence of collagen hydrolysate (HAS) on the formation of ternary collagen-hydrolysate/hydroxyapatite composite materials (COLL-HAS/HA). During the precipitation process of HA, a large amount of brushite is resulted at pH = 7 but, practically pure HA is obtained at pH ⩾ 8. The FTIR data reveal the duplication of the most important collagen absorption bands due to the presence of the collagen hydrolysate. The presence of collagen hydrolysate is beneficial for the management of bone and joint disorders such as osteoarthritis and osteoporosis.

Hydroxyapatite substituted by transition metals: experiment and theory.

PubMed

Zilm, M E; Chen, L; Sharma, V; McDannald, A; Jain, M; Ramprasad, R; Wei, M

2016-06-28

Bioceramics are versatile materials for hard tissue engineering. Hydroxyapatite (HA) is a widely studied biomaterial for bone grafting and tissue engineering applications. The crystal structure of HA allows for a wide range of substitutions, which allows for tailoring materials properties. Transition metals and lanthanides are of interest since substitution in HA can result in magnetic properties. In this study, experimental results were compared to theoretical calculations of HA substituted with a transition metal. Calculation of a 10 atomic percent substitution of a transition metal ion Mn(2+), Fe(2+), and Co(2+) substituted HA samples lead to magnetic moments of 5, 4, and 3 Bohr magnetons, respectively. Hydroxyapatite substituted by transition metals (MHA) was fabricated through an ion exchange procedure and characterized with X-ray diffraction, Fourier transform infra-red spectroscopy (FTIR), X-ray photoelectron spectroscopy, and vibrating sample magnetometer, and results were compared to theoretical calculations. All the substitutions resulted in phase-pure M(2+)HA with lattice parameters and FTIR spectra in good agreement with calculations. Magnetic measurements revealed that the substitution of Mn(2+) has the greatest effect on the magnetic properties of HA followed by the substitution of Fe(2+) and then Co(2+). The present work underlines the power of synergistic theoretical-experimental work in guiding the rational design of materials.

Novel selenium-doped hydroxyapatite coatings for biomedical applications.

PubMed

Rodríguez-Valencia, C; López-Álvarez, M; Cochón-Cores, B; Pereiro, I; Serra, J; González, P

2013-03-01

Nowadays there is a short-term need of investigating in orthopedic implants with a greater functionality, including an improved osseointegration and also antibacterial properties. The coating of metallic implants with hydroxyapatite (HA) remains to be the main proposal, but superior quality HA coatings with compositions closer to natural bone apatites, including carbonates, trace elements are required. Selenium is an essential nutrient in biological tissues and, at the same time, it also presents antibacterial properties. A pioneering study on the fabrication of selenium-doped carbonated hydroxyapatite (iHA:Se) coatings by Pulsed Laser Deposition (PLD) is presented. Different proportions of selenium were incorporated to obtain the iHA:Se coatings. Their physicochemical characterization, performed by SEM/EDS, FTIR, FT-Raman, Interferometric Profilometry and XPS, revealed typical columnar growth of HA in globular aggregates and the efficient incorporation of selenium into the HA coatings by the, most probably, substitution of SeO(3)(2-) groups in the CO(3)(2-) sites. Biological evaluation illustrated the absence of cytotoxicity when an amount of 0.6 at.% of Se was added to the iHA:Se coatings and excellent proliferation of the MC3T3-E1 preosteoblasts. Antibacterial properties were also proved with the inhibition of P. aeruginosa and S. aureus from establishing bacterial biofilms. Copyright © 2012 Wiley Periodicals, Inc.

Chemo-spectroscopic sensor for carboxyl terminus overexpressed in carcinoma cell membrane.

PubMed

Stanca, Sarmiza E; Matthäus, Christian; Neugebauer, Ute; Nietzsche, Sandor; Fritzsche, Wolfgang; Dellith, Jan; Heintzmann, Rainer; Weber, Karina; Deckert, Volker; Krafft, Christoph; Popp, Jürgen

2015-10-01

Certain carboxyl groups of the plasma membrane are involved in tumorgenesis processes. A gold core-hydroxyapatite shell (AuHA) nanocomposite is introduced as chemo-spectroscopic sensor to monitor these carboxyl groups of the cell membrane. Hydroxyapatite (HA) plays the role both of a chemical detector and of a biocompatible Raman marker. The principle of detection is based on chemical interaction between the hydroxyl groups of the HA and the carboxyl terminus of the proteins. The AuHA exhibits a surface enhanced Raman scattering (SERS) signal at 954 cm(-1) which can be used for its localization. The bio-sensing capacity of AuHA towards human skin epidermoid carcinoma (A431) and Chinese hamster ovary (CHO) cell lines is investigated using Raman microspectroscopic imaging. The localization of AuHA on cells is correlated with scanning electron microscopy, transmission electron microscopy and structured illumination fluorescence microscopy. This qualitative approach is a step towards a quantitative study of the proteins terminus. This method would enable further studies on the molecular profiling of the plasma membrane, in an attempt to provide accurate cell identification. Using a gold core-hydroxyapatite shell (AuHA) nanocomposite, the authors in this paper showed the feasibility of detecting and differentiating cell surface molecules by surface enhanced Raman scattering. Copyright © 2015 Elsevier Inc. All rights reserved.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gao, Shan, E-mail: coralgao@hotmail.com; Engineering Ceramics Key Laboratory of Shandong Province, Shandong University, Jinan 250061; Sun, Kangning, E-mail: sunkangning@sdu.edu.cn

Highlights: ► We succeeded in synthesizing hydroxyapatite nano fibers by a chemical method. ► The reaction temperature is only 90 °C. ► The synthetic hydroxyapatite nano fiber is single crystal. - Abstract: We report a novel chemical precipitation route for the synthesis of hydroxyapatite (Ca{sub 10}(PO{sub 4}){sub 6}(OH){sub 2}, HA) fibers using surfactants as templates. Fourier transform infrared spectroscopy (FTIR) and powder X-ray diffraction (PXRD) reveal the characteristic peaks of HA. Transmission electron microscope (TEM) and high-resolution TEM revealed the nano structure, crystallinity and morphology of the HA fibers. The morphology of the HA fibers after calcinations were characterized bymore » scanning electron microscope (SEM). Br{sup −} ions were quickly replaced by the excess PO{sub 4}{sup 3−} ions in the solution after the addition of cetyltrime-thylammonium bromide (CTAB). Meanwhile, CTAB formed a rod-like micelles. Precursors reacted with PO{sub 4}{sup 3−} at the surface of CTAB micelles and finally formed the nanofiber structure.« less

A bioactive triphasic ceramic-coated hydroxyapatite promotes proliferation and osteogenic differentiation of human bone marrow stromal cells.

PubMed

Nair, Manitha B; Bernhardt, Anne; Lode, Anja; Heinemann, Christiane; Thieme, Sebastian; Hanke, Thomas; Varma, Harikrishna; Gelinsky, Michael; John, Annie

2009-08-01

Hydroxyapatite (HA) ceramics are widely used as bone graft substitutes because of their biocompatibility and osteoconductivity. However, to enhance the success of therapeutic application, many efforts are undertaken to improve the bioactivity of HA. We have developed a triphasic, silica-containing ceramic-coated hydroxyapatite (HASi) and evaluated its performance as a scaffold for cell-based tissue engineering applications. Human bone marrow stromal cells (hBMSCs) were seeded on both HASi and HA scaffolds and cultured with and without osteogenic supplements for a period of 4 weeks. Cellular responses were determined in vitro in terms of cell adhesion, viability, proliferation, and osteogenic differentiation, where both materials exhibited excellent cytocompatibility. Nevertheless, an enhanced rate of cell proliferation and higher levels of both alkaline phosphatase expression and activity were observed for cells cultured on HASi with osteogenic supplements. These findings indicate that the bioactivity of HA endowed with a silica-containing coating has definitely influenced the cellular activity, projecting HASi as a suitable candidate material for bone regenerative therapy.

Influence of a TiN interlayer on the microstructure and mechanical properties of hydroxyapatite films grown by pulsed laser deposition

NASA Astrophysics Data System (ADS)

Nelea, Valentin D.; Ristoscu, Carmen; Colis, Silviu; Arens, Simona; Pelletier, Herve; Mihailescu, Ion N.; Mille, Pierre

2001-04-01

Crystalline hydroxyapatite (HA) thin films grown on metallic substrates is the best choice for bone restoration. This is due to the good biological compatibility of the hydroxyapatite material combined with the good mechanical characteristics of the substrates. We deposit HA thin films by Pulsed Laser Deposition (PLD) in vacuum at room temperature using a KrF* excimer laser ((lambda) equals 248 nm, (tau) FWHM >= 20 ns). The depositions were performed directly on Ti-5Al-2.5Fe or on substrates previously coated with a TiN buffer layer. The HA deposited structures were characterized by complementary techniques: GIXRD, SEM, TEM, SAED, EDS and nanoindentation. Properties of the HA films grown with and without the TiN buffer were discussed in term of microstructure and mechanical behavior. The films with interlayer preserve the stoichiometry, are completely recrystallized and present better mechanical characteristics as compared with those without buffer.

In vitro and in vivo mechanical evaluations of plasma-sprayed hydroxyapatite coatings on titanium implants: the effect of coating characteristics.

PubMed

Yang, C Y; Lin, R M; Wang, B C; Lee, T M; Chang, E; Hang, Y S; Chen, P Q

1997-12-05

This study was undertaken to evaluate the effect of coating characteristics on the mechanical strengths of the plasma-sprayed HA-coated Ti-6Al-4V implant system both in vitro and in vivo. Two types of HA coatings (HACs) with quite different microstructures, concentrations of impurity-phases, and indices-of-crystallinity were used. In vitro testings were done by measuring the bonding-strength at the Ti-6Al-4V-HAC interface, with HACs that had and had not been immersed in a pH-buffered, serum-added simulated body fluid (SBF). The shear-strength at the HAC-bone interface was investigated in a canine transcortical femoral model after 12 and 24 weeks of implantation. The results showed a bonding degradation of approximately 32% or higher of the original strength after 4 weeks of immersion in SBF, and this predominantly depended on the constructed microstructure of the HACs. After the push-out measurements, it was demonstrated that the HACs with higher bonding-strength in vitro would correspondingly result in significantly higher shear-strength at each implant period in vivo. Nevertheless, there were no substantial histological variations between the two types of HACs evaluated. The most important point elucidated in this study was that, among coating characteristics, the microstructure was the key factor in influencing the mechanical stability of the HACs both in vitro and in vivo. As a consequence, a denser HAC was needed to ensure mechanical stability at both interfaces.

Characterization of mechanical properties of hydroxyapatite-silicon-multi walled carbon nano tubes composite coatings synthesized by EPD on NiTi alloys for biomedical application.

PubMed

Khalili, Vida; Khalil-Allafi, Jafar; Sengstock, Christina; Motemani, Yahya; Paulsen, Alexander; Frenzel, Jan; Eggeler, Gunther; Köller, Manfred

2016-06-01

Release of Ni(1+) ions from NiTi alloy into tissue environment, biological response on the surface of NiTi and the allergic reaction of atopic people towards Ni are challengeable issues for biomedical application. In this study, composite coatings of hydroxyapatite-silicon multi walled carbon nano-tubes with 20wt% Silicon and 1wt% multi walled carbon nano-tubes of HA were deposited on a NiTi substrate using electrophoretic methods. The SEM images of coated samples exhibit a continuous and compact morphology for hydroxyapatite-silicon and hydroxyapatite-silicon-multi walled carbon nano-tubes coatings. Nano-indentation analysis on different locations of coatings represents the highest elastic modulus (45.8GPa) for HA-Si-MWCNTs which is between the elastic modulus of NiTi substrate (66.5GPa) and bone tissue (≈30GPa). This results in decrease of stress gradient on coating-substrate-bone interfaces during performance. The results of nano-scratch analysis show the highest critical distance of delamination (2.5mm) and normal load before failure (837mN) as well as highest critical contact pressure for hydroxyapatite-silicon-multi walled carbon nano-tubes coating. The cell culture results show that human mesenchymal stem cells are able to adhere and proliferate on the pure hydroxyapatite and composite coatings. The presence of both silicon and multi walled carbon nano-tubes (CS3) in the hydroxyapatite coating induce more adherence of viable human mesenchymal stem cells in contrast to the HA coated samples with only silicon (CS2). These results make hydroxyapatite-silicon-multi walled carbon nano-tubes a promising composite coating for future bone implant application. Copyright © 2016 Elsevier Ltd. All rights reserved.

Nanocrystallinity effects on osteoblast and osteoclast response to silicon substituted hydroxyapatite.

PubMed

Casarrubios, Laura; Matesanz, María Concepción; Sánchez-Salcedo, Sandra; Arcos, Daniel; Vallet-Regí, María; Portolés, María Teresa

2016-11-15

Silicon substituted hydroxyapatites (SiHA) are highly crystalline bioceramics treated at high temperatures (about 1200°C) which have been approved for clinical use with spinal, orthopedic, periodontal, oral and craniomaxillofacial applications. The preparation of SiHA with lower temperature methods (about 700°C) provides nanocrystalline SiHA (nano-SiHA) with enhanced bioreactivity due to higher surface area and smaller crystal size. The aim of this study has been to know the nanocrystallinity effects on the response of both osteoblasts and osteoclasts (the two main cell types involved in bone remodelling) to silicon substituted hydroxyapatite. Saos-2 osteoblasts and osteoclast-like cells (differentiated from RAW-264.7 macrophages) have been cultured on the surface of nano-SiHA and SiHA disks and different cell parameters have been evaluated: cell adhesion, proliferation, viability, intracellular content of reactive oxygen species, cell cycle phases, apoptosis, cell morphology, osteoclast-like cell differentiation and resorptive activity. This comparative in vitro study evidences that nanocrystallinity of SiHA affects the cell/biomaterial interface inducing bone cell apoptosis by loss of cell anchorage (anoikis), delaying osteoclast-like cell differentiation and decreasing the resorptive activity of this cell type. These results suggest the potential use of nano-SiHA biomaterial for preventing bone resorption in treatment of osteoporotic bone. Copyright © 2016 Elsevier Inc. All rights reserved.

Electrophoretic Deposition of Hydroxyapatite Film Containing Re-Doped MoS₂ Nanoparticles.

PubMed

Shalom, Hila; Feldman, Yishay; Rosentsveig, Rita; Pinkas, Iddo; Kaplan-Ashiri, Ifat; Moshkovich, Alexey; Perfilyev, Vladislav; Rapoport, Lev; Tenne, Reshef

2018-02-26

Films combining hydroxyapatite (HA) with minute amounts (ca. 1 weight %) of (rhenium doped) fullerene-like MoS₂ (IF) nanoparticles were deposited onto porous titanium substrate through electrophoretic process (EPD). The films were analyzed by scanning electron microscopy (SEM), X-ray diffraction and Raman spectroscopy. The SEM analysis showed relatively uniform coatings of the HA + IF on the titanium substrate. Chemical composition analysis using energy dispersive X-ray spectroscopy (EDS) of the coatings revealed the presence of calcium phosphate minerals like hydroxyapatite, as a majority phase. Tribological tests were undertaken showing that the IF nanoparticles endow the HA film very low friction and wear characteristics. Such films could be of interest for various medical technologies. Means for improving the adhesion of the film to the underlying substrate and its fracture toughness, without compromising its biocompatibility are discussed at the end.

On the fate of particles liberated from hydroxyapatite coatings in vivo.

PubMed

Dunne, C F; Gibbons, J; FitzPatrick, D P; Mulhall, K J; Stanton, K T

2015-03-01

Hydroxyapatite (HA) has been used as a coating for orthopaedic implants for over 30 years to help promote the fixation of orthopaedic implants into the surrounding bone. However, concerns exist about the fate of the hydroxyapatite coating and hydroxyapatite particles in vivo, especially in the wake of recent concerns about particulates from metal-on-metal bearings. Here, we assess the mechanisms of particle detachment from coated orthopaedic devices as well as the safety and performance concerns and biomedical implications arising from the liberation of the particles by review of the literature. The mechanisms that can result in the detachment of the HA coating from the implant can be mechanical or biochemical, or both. Mechanical mechanisms include implant insertion, abrasion, fatigue and micro-motion. Biochemical mechanisms that contribute to the liberation of HA particles include dissolution into extra-cellular fluid, cell-mediated processes and crystallisation of amorphous phases. The form the particles take once liberated is influenced by a number of factors such as coating method, the raw powder morphology, processing parameters, coating thickness and coating structure. This review summarises and discusses each of these factors and concludes that HA is a safe biomimetic material to use as a coating and does not cause any problems in particulate form if liberated as debris from an orthopaedic implant.

Boron nitride nanotube reinforced hydroxyapatite composite: mechanical and tribological performance and in-vitro biocompatibility to osteoblasts.

PubMed

Lahiri, Debrupa; Singh, Virendra; Benaduce, Ana Paula; Seal, Sudipta; Kos, Lidia; Agarwal, Arvind

2011-01-01

This study proposes boron nitride nanotube (BNNT) reinforced hydroxyapatite (HA) as a novel composite material for orthopedic implant applications. The spark plasma sintered (SPS) composite structure shows higher density compared to HA. Minimal lattice mismatch between HA and BNNT leads to coherent bonding and strong interface. HA-4 wt% BNNT composite offers excellent mechanical properties-120% increment in elastic modulus, 129% higher hardness and 86% more fracture toughness, as compared to HA. Improvements in the hardness and fracture toughness are related to grain refinement and crack bridging by BNNTs. HA-BNNT composite also shows 75% improvement in the wear resistance. The wear morphology suggests localized plastic deformation supported by the sliding of outer walls of BNNT. Osteoblast proliferation and cell viability show no adverse effect of BNNT addition. HA-BNNT composite is, thus, envisioned as a potential material for stronger orthopedic implants. Copyright © 2010 Elsevier Ltd. All rights reserved.

Preparation and characterization of bio-composite PEEK/nHA

NASA Astrophysics Data System (ADS)

Jin, Y. S.; Bian, C. C.; Zhang, Z. Q.; Zhao, Y.; Yang, L.

2017-01-01

PEEK/nHA composite material, with excellent mechanical property as polyetheretherketone (PEEK) and biological activity as hydroxyapatite (HA), has attracted wide attention of medical experts and materials science experts. The addition of hydroxyapatite was the decisive factor for biological activity in PEEK/nHA composite. In this paper, acicular nanohydroxyapatite was prepared by chemical precipitation method with Ca(NO3)2, (NH4)2HPO4 as raw material; PEEK/nHA composite was prepared by solution blending and vacuum sintering method. The composite was characterized with FT-IR, XRD, DSC, TG and mechanical property test. Results showed that the composite has good thermal stability and compressive property when the mass ratio of PEEK to nHA is 10:3; and high nHA content can improve the biological activity of the composite, which can meet the basic requirements for bone tissue engineering scaffold.

MC3T3-E1 osteoblast attachment and proliferation on porous hydroxyapatite scaffolds fabricated with nanophase powder

PubMed Central

Smith, Ian O; McCabe, Laura R; Baumann, Melissa J

2006-01-01

Porous bone tissue engineering scaffolds were fabricated using both nano hydroxyapatite (nano HA) powder (20 nm average particle size) and micro HA powder (10 μm average particle size), resulting in sintered scaffolds of 59 vol% porosity and 8.6±1.9 μm average grain size and 72 vol% porosity and 588±55 nm average grain size, respectively. Scanning electron microscopy was used to measure both the grain size and pore size. MC3T3-E1 osteoblast (OB) attachment and proliferation on both nano HA and micro HA porous scaffolds were quantified. As expected, OB cell number was greater on nano HA scaffolds compared with similarly processed micro HA scaffolds 5 days after seeding, while OB attachment did not appear greater on the nano HA scaffolds (p<0.05). PMID:17722535

[Construction of porous hydroxyapatite (HA) block loaded with cultured chondrocytes].

PubMed

Yan, M; Dang, G

1999-07-01

To construct a kind of bone healing enhancing implant with cultured chondrocytes bound to hydroxyapatite (HA). Chondrocytes were obtained from the costicartilage of rat and were cultured on the porous HA blocks, 3 mm x 3 mm x 4 mm size, for three and seven days. Scanning electron micrograph was taken to show whether the cells grew outside and inside the pore of HA block. The cells cultured on tiny glass sheet for 2 days were used to prove where the cells come from by in situ hybridization technique with alpha1 (II) cDNA probe. Scanning electron micrographs showed that the pores of the HA surface and inside of the blocks are filled with cultured cells, especially the longer cultured block. The cells were chondrocytes confirmed by in situ hybridization. The porous HA can be used as cell cultured substrate and chondrocyte can adhere and proliferate inside the porous HA block.

Activation of Osteoblastic Function on Titanium Surface with Titanium-Doped Hydroxyapatite Nanoparticle Coating: An In Vitro Study.

PubMed

Nakazawa, Masahiro; Yamada, Masahiro; Wakamura, Masato; Egusa, Hiroshi; Sakurai, Kaoru

Titanium-doped hydroxyapatite (TiHA) nanoparticles contain titanium atoms in the hydroxyapatite lattice, which can physicochemically functionalize the titanium surface without modification of the surface topography. This study aimed to evaluate the physicochemical properties of machined or microroughened titanium surfaces coated with TiHA nanoparticles and the functions of osteoblasts cultured on them. Titanium disks with commercially available surface topography, such as machined or sandblasted, large-grit, and acid-etched (SLA) surfaces, were coated with TiHA. The disks with original or TiHA-coated surfaces were evaluated in topography, wettability, and chemical composition. Osteoblastic cells from rat femurs were cultured on the disks and evaluated in proliferation and differentiation. TiHA coating changed from hydrophobicity to hydrophilicity on both machined and SLA surfaces. Calcium and phosphate atoms were detected all over the surface with TiHA coating regardless of the surface topography. However, the considerable change in the inherent surface topographies was not observed on both types of surfaces after TiHA coating. Osteoblastic proliferative activity at day 4 was increased by TiHA coating on both types of surfaces. TiHA coating did not enhance expressions of bone matrix-related genes such as osteocalcin, osteopontin, bone sialoprotein, alkaline phosphatase, and collagen I. However, depositions of collagen, osteocalcin, and calcium in the culture at days 7 and 20 were increased on both types of surface topographies with TiHA coating. TiHA coating enhanced extracellular matrix formation on smooth and microroughened titanium surfaces by increasing osteoblastic proliferative activity without the deterioration of differentiation through hydrophilic and chemical functionalization.

The Influence of Chitosan Concentration on Synthesis of Hydroxyapatite Scaffold on Crystallinity and Surface Morphology

NASA Astrophysics Data System (ADS)

Yudyanto; Hartatiek; Prasasti, R. W.; Hariyanto, Y. A.; Hidayat, N.

2018-05-01

Hydroxyapatite (HA) is a bioceramic material having a chemical formula (Ca10(PO4)6(OH)2) similar to the chemical structure of bone and hard tissue in humans. Recently, HA-scaffold has been intensively developed by many researchers due to its potential application in dealing with tissue injured. The implantation of HA-scaffold into bone defect aims to help and stimulate the growth of new bone tissue. Crystallinity and microstructure are properties that need to be considered to synthesis HA scaffold. Although, HA is biocompatible and osteoconductive but low biodegradable, to solve these problems added chitosan. Chitosan is a biopolymeric material with specific properties, in terms of biocompatible, non-toxic, osteoconductive, biodegradable, and not carcinogenc. In addition, a natural polymeric chitosan has similarities with the extracellular matrix, in terms of good biological performance and inherent cellular interactions. In this study, HA-scaffold was synthesized using Ca(OH)2 as the raw material of natural calcite mineral, H3PO4, and a solid polyurethane polymer (sponge) as forming of pores by sol-gel method. The addition of chitosan concentration of 0 %, 2 % and 3 % in hydroxyapatite scaffold evaluated its influences on crystallinity and surface morphology. The phase, crystallinity and crystal size are evaluated by XRD. Functional groups in HA scaffold and HA compounds were evaluated with FTIR. The results showed that HA has Ca/P ratio of 1.64. The addition of chitosan concentration caused the decrease of crystallinity and increased the pore size. Meanwhile the crystal sizes were obtained: 49.99 nm (HA), 54.37 nm (HA-scaffold without chitosan), 54.98 nm (HA-scaffold with 2% chitosan), and 40.44 nm (HA-scaffold with 3 % chitosan).

Invitro Evaluation of Fluoride Release from Hydroxyapatite Reinforced Glass Ionomer with or without Protective Coating.

PubMed

Tiwari, Shilpi; Nandlal, Bhojraj

2016-04-01

Glass Ionomer Cement (GIC) is well known for its fluoride releasing property but has its own drawbacks of poor mechanical properties, sensitivity to initial desiccation and moisture contamination. To overcome these, search led to the reinforcement of hydroxyapatite and application of surface coating agent but their effect on fluoride release is still not clear. To evaluate and compare the release of fluoride from Hydroxyapatite Reinforced Glass Ionomer (HA-GIC) with and without protective coating. Specimens were prepared as follows- Eight percent by weight conventional glass ionomer was replaced by hydroxyapatite powder (HA) and an indigenous product was prepared (HA-GIC). This powder was mixed with liquid of conventional GIC and allowed to set, then G coat plus coating agent was applied in surface coated group and light cured. Fluoride release of the sample was measured every 24 hrs for seven days and weekly from 7(th) to 21(st) day using combination ion selective electrode. Mean values clearly reveal a significant decrease in the fluoride release from day 1 to day 21 for both the groups. Results of repeated measure ANOVA revealed statistically significant difference between two groups (p <0.001). Coating the hydroxyapatite reinforced glass ionomer will allow for slow and steady release of fluoride for a long period of time into oral environment.

Sol-gel-derived hydroxyapatite-carbon nanotube/titania coatings on titanium substrates.

PubMed

Ji, Xiaoli; Lou, Weiwei; Wang, Qi; Ma, Jianfeng; Xu, Haihong; Bai, Qing; Liu, Chuantong; Liu, Jinsong

2012-01-01

In this paper, hydroxyapatite-carbon nanotube/titania (HA-CNT/TiO(2)) double layer coatings were successfully developed on titanium (Ti) substrates intended for biomedical applications. A TiO(2) coating was firstly developed by anodization to improve bonding between HA and Ti, and then the layer of HA and CNTs was coated on the surface by the sol-gel process to improve the biocompatibility and mechanical properties of Ti. The surfaces of double layer coatings were uniform and crack-free with a thickness of about 7 μm. The bonding strength of the HA-CNT/TiO(2) coating was higher than that of the pure HA and HA-CNT coatings. Additionally, in vitro cell experiments showed that CNTs promoted the adhesion of preosteoblasts on the HA-CNT/TiO(2) double layer coatings. These unique surfaces combined with the osteoconductive properties of HA exhibited the excellent mechanical properties of CNTs. Therefore, the developed HA-CNT/TiO(2) coatings on Ti substrates might be a promising material for bone replacement.

Strength and fatigue properties of three-step sintered dense nanocrystal hydroxyapatite bioceramics

NASA Astrophysics Data System (ADS)

Guo, Wen-Guang; Qiu, Zhi-Ye; Cui, Han; Wang, Chang-Ming; Zhang, Xiao-Jun; Lee, In-Seop; Dong, Yu-Qi; Cui, Fu-Zhai

2013-06-01

Dense hydroxyapatite (HA) ceramic is a promising material for hard tissue repair due to its unique physical properties and biologic properties. However, the brittleness and low compressive strength of traditional HA ceramics limited their applications, because previous sintering methods produced HA ceramics with crystal sizes greater than nanometer range. In this study, nano-sized HA powder was employed to fabricate dense nanocrystal HA ceramic by high pressure molding, and followed by a three-step sintering process. The phase composition, microstructure, crystal dimension and crystal shape of the sintered ceramic were examined by X-ray diffraction (XRD) and scanning electron microscopy (SEM). Mechanical properties of the HA ceramic were tested, and cytocompatibility was evaluated. The phase of the sintered ceramic was pure HA, and the crystal size was about 200 nm. The compressive strength and elastic modulus of the HA ceramic were comparable to human cortical bone, especially the good fatigue strength overcame brittleness of traditional sintered HA ceramics. Cell attachment experiment also demonstrated that the ceramics had a good cytocompatibility.

Cytotoxicity and genotoxicity property of hydroxyapatite-mullite eluates.

PubMed

Kalmodia, Sushma; Sharma, Vyom; Pandey, Alok K; Dhawan, Alok; Basu, Bikramjit

2011-02-01

Long-term biomedical applications of implant materials may cause osteolysis, aseptic losing and toxicity. Therefore, we investigated the cytotoxic and genotoxic potential of hydroxyapatite (HA) mullite eluates in L929 mouse fibroblast cells. The spark plasma sintered HA-20% mullite biocomposite (HA20M) were ground using mortar and pestle as well as ball milling. The cells were exposed for 6 h to varying concentrations (10, 25, 50, 75 and 100%) of the eluates of HA-20% mullite (87 nm), HA (171 nm) and mullite (154 nm). The scanning electron microscopy and MTT assay revealed the concentration dependent toxicity of H20M eluate at and above 50%. The analysis of the DNA damaging potential of HA, mullite and HA20M eluates using Comet assay demonstrated a significant DNA damage by HA20M which was largely related to the presence of mullite. The results collectively demonstrate the cytotoxic and genotoxic potential of HA20M eluate in L929 cells is dependent on particle size, concentration and composition.

Influence of Magnesium Ion Substitution on Structural and Thermal Behavior of Nanodimensional Hydroxyapatite

NASA Astrophysics Data System (ADS)

Batra, Uma; Kapoor, Seema; Sharma, Sonia

2013-06-01

Hydroxyapatite (HA), incorporating small amount of magnesium, shows attractive biological performance in terms of improved bone metabolism, osteoblast and osteoclast activity, and bone in-growth. This article reports a systematic investigation on the influence of magnesium (Mg) substitution on structural and thermal behavior of nanodimensional HA. HA and Mg-substituted HA nanopowders were synthesized through sol-gel route. The morphology and size of nanopowders were characterized by transmission electron microscopy. The BET surface area was evaluated from N2 adsorption isotherms. Structural analysis and thermal behavior were investigated by means of Fourier transform infrared spectroscopy, x-ray diffraction, thermogravimetry, and differential thermal analysis. As-synthesized powders consisted of flake-like agglomerates of HA and calcium-deficient HA. The incorporation of magnesium in HA resulted in decrease of crystallite size, crystallinity, and lattice parameters a and c and increase in BET surface area. β-tricalcium phosphate formation occured at lower calcination temperature in Mg-substituted HA than HA.

Observations on the microvasculature of bone defects filled with biodegradable nanoparticulate hydroxyapatite.

PubMed

Kilian, Olaf; Wenisch, Sabine; Karnati, Srikanth; Baumgart-Vogt, Eveline; Hild, Anne; Fuhrmann, Rosemarie; Jonuleit, Tarja; Dingeldein, Elvira; Schnettler, Reinhard; Franke, Ralf-Peter

2008-01-01

The microvascularization of metaphyseal bone defects filled with nanoparticulate, biodegradable hydroxyapatite biomaterial with and without platelet factors enrichment was investigated in a minipig model. Results from morphological analysis and PECAM-1 immunohistochemistry showed the formation of new blood vessels into the bone defects by sprouting and intussusception of pre-existing ones. However, no significant differences were observed in the microvascularization of the different biomaterials applied (pure versus platelet factors-enriched hydroxyapatite), concerning the number of vessels and their morphological structure at day 20 after operation. The appearance of VEGFR-2 positive endothelial progenitor cells in the connective tissue between hydroxyapatite particles was also found to be independent from platelet factors enrichment of the hydroxyapatite bone substitute. In both groups formation of lymphatic vessels was detected with a podoplanin antibody. No differences were noted between HA/PLF- and HA/PLF+ implants with respect to the podoplanin expression level, the staining pattern or number of lymphatic vessels. In conclusion, the present study demonstrates different mechanisms of blood and lymphatic vessel formation in hydroxyapatite implants in minipigs.

Does hydroxyapatite coating enhance ingrowth and improve longevity of a Zweymuller type stem? A double-blinded randomised RSA trial.

PubMed

Hoornenborg, Daniel; Sierevelt, Inger N; Spuijbroek, Joost A; Cheung, John; van der Vis, Harm M; Beimers, Lijkele; Haverkamp, Daniel

2017-09-11

An ongoing discussion is whether using a hydroxyapatite coating enhances the ingrowth and longevity of a femoral stem in total hip arthroplasty. The best way to predict speed of ingrowth and long-term outcome is by evaluating micromotion by radiostereometric analysis. To study the effect of hydroxyapatite (HA) coating on the migration of the SL-PLUS hip stem, we performed a prospective double blind randomised controlled trial comparing the early migration of the hydroxyapatite (HA)-coated SL-PLUS stem compared to the Standard (non-coated) SL-PLUS stem. 51 patients were randomly assigned to receive either an uncoated or a HA-coated femoral component during total hip replacement. RSA images were obtained direct postoperatively and at 6 weeks, 12 weeks, 6 months, 12 months and 24 months. HOOS scores were obtained preoperative and at final follow-up. RSA evaluation demonstrated significant migration up to 3 months postoperatively in both groups. After initial setting no significant migration was observed. There was no significant difference in migration between the HA-coated group and the uncoated group.Both Harris Hip Score (HHS) and HOOS domain scores (pain and ADL) significantly improved compared to baseline at 24 months after surgery in both treatment groups (p<0.001 for all comparisons). Improvement did not differ significantly between the 2 groups. At 2 years follow-up, the HA-coated and uncoated Zweymuller type, distal fitting stem do not show different migration patterns.

Hydroxyapatite-binding peptides for bone growth and inhibition

DOEpatents

Bertozzi, Carolyn R [Berkeley, CA; Song, Jie [Shrewsbury, MA; Lee, Seung-Wuk [Walnut Creek, CA

2011-09-20

Hydroxyapatite (HA)-binding peptides are selected using combinatorial phage library display. Pseudo-repetitive consensus amino acid sequences possessing periodic hydroxyl side chains in every two or three amino acid sequences are obtained. These sequences resemble the (Gly-Pro-Hyp).sub.x repeat of human type I collagen, a major component of extracellular matrices of natural bone. A consistent presence of basic amino acid residues is also observed. The peptides are synthesized by the solid-phase synthetic method and then used for template-driven HA-mineralization. Microscopy reveal that the peptides template the growth of polycrystalline HA crystals .about.40 nm in size.

In vitro corrosion and cytocompatibility properties of nano-whisker hydroxyapatite coating on magnesium alloy for bone tissue engineering applications.

PubMed

Yang, Huawei; Yan, Xueyu; Ling, Min; Xiong, Zuquan; Ou, Caiwen; Lu, Wei

2015-03-17

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.

[Preparation of elastic porous cell scaffold fabricated with combined polydimethylsiloxane (PDMS) and hydroxyapatite (HA)].

PubMed

Yang, Yang; Lan, Ding; Huang, Yan; Li, Yanming; Wang, Yuren; Sun, Lianwen; Fan, Yubo

2014-06-01

Polydimethylsiloxane (PDMS) and hydroxyapatite (HA) were combined in our laboratory to fabricate an elastic porous cell scaffold with pore-forming agent, and then the scaffold was used as culture media for rat bone marrow derived mesenchymal stem cells (rBMSCs). Different porous materials (square and circular in shape) were prepared by different pore-forming agents (NaCl or paraffin spheres) with adjustable porosity (62%-76%). The HA crystals grew on the wall of hole when the material was exposed to SBF solutions, showing its biocompatibility and ability to support the cells to attach on the materials.

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

PubMed Central

Yang, Huawei; Yan, Xueyu; Ling, Min; Xiong, Zuquan; Ou, Caiwen; Lu, Wei

2015-01-01

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. PMID:25789500

Study of BSA protein adsorption/release on hydroxyapatite nanoparticles

NASA Astrophysics Data System (ADS)

Swain, Sanjaya Kumar; Sarkar, Debasish

2013-12-01

Three different spherical, rod and fibrous morphologies of hydroxyapatite (HA) nanoparticles have been prepared through control over the processing parameters like temperature, pH and Ca:P ratio. Protein adsorption/release with respect to HA nanoparticle morphologies are investigated using model protein bovine serum albumin (BSA). BSA adsorption on HA nanoparticles follows Langmuir adsorption isotherm. Thermal analysis and FT-IR spectrum confirms the BSA adhesion and retention of their secondary structure. High surface area with high Ca:P ratio nanorod adsorbs relatively more amount (28 mg BSA/gm of nanorod HA) of BSA within 48 h in comparison with counterpart fibroid and spherical morphologies. Slow and steady BSA release (75 wt% of adsorbed BSA in 96 h) from nanorod HA is found as futuristic drug delivery media.

Limitation of biocompatibility of hydrated nanocrystalline hydroxyapatite

NASA Astrophysics Data System (ADS)

Minaychev, V. V.; Teleshev, A. T.; Gorshenev, V. N.; Yakovleva, M. A.; Fomichev, V. A.; Pankratov, A. S.; Menshikh, K. A.; Fadeev, R. S.; Fadeeva, I. S.; Senotov, A. S.; Kobyakova, M. I.; Yurasova, Yu B.; Akatov, V. S.

2018-04-01

Nanostructured hydroxyapatite (HA) in the form of hydrated paste is considered to be a promising material for a minor-invasive surgical curing of bone tissue injure. However questions about adhesion of cells on this material and its biocompatibility still remain. In this study biocompatibility of paste-formed nanosized HA (nano-HA) by in vitro methods is investigated. Nano-HA (particles sized about 20 nm) was synthesized under conditions of mechano-acoustic activation of an aqueous reaction mixture of ammonium hydrophosphate and calcium nitrate. It was ascertained that nanocrystalline paste was not cytotoxic although limitation of adhesion, spreading and growth of the cells on its surface was revealed. The results obtained point on the need of modification of hydrated nano-HA in the aims of increasing its biocompatibility and osteoplastic potential.

Development of strontium and magnesium substituted porous hydroxyapatite/poly(3,4-ethylenedioxythiophene) coating on surgical grade stainless steel and its bioactivity on osteoblast cells.

PubMed

Gopi, D; Ramya, S; Rajeswari, D; Surendiran, M; Kavitha, L

2014-02-01

The present study deals with the successful development of bilayer coatings by electropolymerisation of poly(3,4-ethylenedioxythiophene) (PEDOT) on surgical grade stainless steel (316L SS) followed by the electrodeposition of strontium (Sr) and magnesium (Mg) substituted porous hydroxyapatite (Sr, Mg-HA). The bilayer coatings were characterised by Fourier transform infrared spectroscopy (FT-IR) and high resolution scanning electron microscopy (HRSEM). Corrosion resistance of the obtained coatings was investigated in Ringer's solution by electrochemical techniques and the results were in good agreement with those obtained from chemical analysis, namely inductively coupled plasma atomic emission spectrometry (ICP-AES). Also, the mechanical and biological properties of the bilayer coatings were analyzed. From the obtained results it was evident that the PEDOT/Sr, Mg-HA bilayer exhibited greater adhesion strength than the Sr, Mg-HA coated 316L SS. In vitro cell adhesion test of the Sr, Mg-HA coating on PEDOT coated specimen is found to be more bioactive compared to that of the single substituted hydroxyapatite (Sr or Mg-HA) on the PEDOT coated 316L SS. Thus, the PEDOT/Sr, Mg-HA bilayer coated 316L SS can serve as a prospective implant material for biomedical applications. Copyright © 2013 Elsevier B.V. All rights reserved.

Hydroxyapatite-alginate nanocomposite as drug delivery matrix for sustained release of ciprofloxacin.

PubMed

Venkatasubbu, G Devanand; Ramasamy, S; Ramakrishnan, V; Kumar, J

2011-12-01

Hydroxyapatite is a bioceramic which has a wide range of medical application for bone diseases. To enhance its usage, we have prepared ciprofloxacin loaded nano hydroxyapatite (HA) composite with a natural polymer, alginate, using wet chemical method at low temperature. The prepared composites were analyzed by various physicochemical methods. The results show that the nano HA crystallites are well intact with the alginate macromolecules. For the composite system FT-IR and micro Raman results are reported in this paper. Studies on the drug loading and drug release have been done. The drug is pre-adsorbed onto the ceramic particle before the formation of composite. The thermal behavior of composite has been studied using thermo gravimetric analysis (TGA). This work, reports that the nanocomposite prepared under optimum condition could prolong the release of ciprofloxacin compared with the ciprofloxacin loaded hydroxyapatite.

[Experimental research on the effect of nanophase ceramics on osteoblasts functions].

PubMed

Wen, Bo; Chen, Zhiqing; Jiang, Yinshan; Yang, Zhengwen; Xu, Yongzhong

2005-06-01

In order to study the cytocompatibility of nanophase hydroxyapatite ceramic in vitro, we prepared hydroxyapatite by use of the wet chemistry techniques. The grain size of hydroxyapatite of interest to the present study was determined by scanning electron microscopy and atomic force microscopy with image analysis software. Primary culture of osteoblast from rat calvaria was established. Protein content, synthesis of alkaline phosphatase and deposition of calcium-containing mineral by osteoblasts cultured on nanophase hydroxyapatite ceramics and on conventional hydroxyapatite ceramics for 7, 14, 21 and 28 days were examined. The results showed that the average surface grain size of the nanophase and that of the conventional HA compact formulations was 55 (nanophase) and 780 (conventional) nm, respectively. More importantly, compared to the synthesis of alkaline phosphatase and deposition of calcium-containing mineral by osteoblasts cultured on nanophase was significantly greater than that on conventional ceramics after 21 and 28 days. The cytocompatibility was significantly greater on nanophase HA than on conventional formulations of the same ceramic.

DNA damage evaluation of hydroxyapatite on fibroblast cell L929 using the single cell gel electrophoresis assay.

PubMed

Rajab, N F; Yaakob, T A; Ong, B Y; Hamid, M; Ali, A M; Annuar, B O; Inayat-Hussain, S H

2004-05-01

Hydroxyapatite is the main component of the bone which is a potential biomaterial substance that can be applied in orthopaedics. In this study, the biocompatibility of this biomaterial was assessed using an in vitro technique. The cytotoxicity and genotoxicity effect of HA2 and HA3 against L929 fibroblast cell was evaluated using the MTT Assay and Alkaline Comet Assay respectively. Both HA2 and HA3 compound showed low cytotoxicity effect as determined using MTT Assay. Cells viability following 72 hours incubation at maximum concentration of both HA2 and HA3 (200 mg/ml) were 75.3 +/- 8.8% and 86.7 +/- 13.1% respectively. However, the cytotoxicity effect of ZnSO4.7H2O as a positive control showed an IC50 values of 46 mg/ml (160 microM). On the other hand, both HA2 and HA3 compound showed a slight genotoxicity effect as determined using the Alkaline Comet Assay following incubation at the concentration 200 mg/ml for 72 hours. This assay has been widely used in genetic toxicology to detect DNA strand breaks and alkali-labile site. The percentage of the cells with DNA damage for both substance was 27.7 +/- 1.3% and 15.6 +/- 1.0% for HA2 and HA3 respectively. Incubation of the cells for 24 hours with 38 microg/ml (IC25) of positive control showed an increase in percentage of cells with DNA damage (67.5 +/- 0.7%). In conclusion, our study indicated that both hydroxyapatite compounds showed a good biocompatibility in fibroblast cells.

Promotion of osteogenesis by a piezoelectric biological ceramic.

PubMed

Feng, J; Yuan, H; Zhang, X

1997-12-01

Hydroxyapatite (HA) ceramic and piezoelectric biological ceramic, hydroxyapatite and barium titanate (HABT), were implanted in the jawbones of dogs. Histological observation showed that, compared with HA ceramics, HABT promoted the growth and repair of the bone significantly, the tissue growth around the HABT ceramic was direction-dependent, the collagen arranged orderly and the bone grew orderly. The order growth of the bone increased the efficiency of osteogenesis on the surface of the implanted HABT ceramics.

Cementless Hydroxyapatite Coated Hip Prostheses

PubMed Central

Herrera, Antonio; Mateo, Jesús; Gil-Albarova, Jorge; Lobo-Escolar, Antonio; Ibarz, Elena; Gabarre, Sergio; Más, Yolanda

2015-01-01

More than twenty years ago, hydroxyapatite (HA), calcium phosphate ceramics, was introduced as a coating for cementless hip prostheses. The choice of this ceramic is due to its composition being similar to organic apatite bone crystals. This ceramic is biocompatible, bioactive, and osteoconductive. These qualities facilitate the primary stability and osseointegration of implants. Our surgical experience includes the implantation of more than 4,000 cementless hydroxyapatite coated hip prostheses since 1990. The models implanted are coated with HA in the acetabulum and in the metaphyseal area of the stem. The results corresponding to survival and stability of implants were very satisfactory in the long-term. From our experience, HA-coated hip implants are a reliable alternative which can achieve long term survival, provided that certain requirements are met: good design selection, sound choice of bearing surfaces based on patient life expectancy, meticulous surgical technique, and indications based on adequate bone quality. PMID:25802848

Electrophoretic Deposition of Hydroxyapatite Film Containing Re-Doped MoS2 Nanoparticles

PubMed Central

Shalom, Hila; Feldman, Yishay; Rosentsveig, Rita; Pinkas, Iddo; Kaplan-Ashiri, Ifat; Moshkovich, Alexey; Perfilyev, Vladislav; Rapoport, Lev

2018-01-01

Films combining hydroxyapatite (HA) with minute amounts (ca. 1 weight %) of (rhenium doped) fullerene-like MoS2 (IF) nanoparticles were deposited onto porous titanium substrate through electrophoretic process (EPD). The films were analyzed by scanning electron microscopy (SEM), X-ray diffraction and Raman spectroscopy. The SEM analysis showed relatively uniform coatings of the HA + IF on the titanium substrate. Chemical composition analysis using energy dispersive X-ray spectroscopy (EDS) of the coatings revealed the presence of calcium phosphate minerals like hydroxyapatite, as a majority phase. Tribological tests were undertaken showing that the IF nanoparticles endow the HA film very low friction and wear characteristics. Such films could be of interest for various medical technologies. Means for improving the adhesion of the film to the underlying substrate and its fracture toughness, without compromising its biocompatibility are discussed at the end. PMID:29495394

Mechanical properties of natural chitosan/hydroxyapatite/magnetite nanocomposites for tissue engineering applications.

PubMed

Heidari, Fatemeh; Razavi, Mehdi; E Bahrololoom, Mohammad; Bazargan-Lari, Reza; Vashaee, Daryoosh; Kotturi, Hari; Tayebi, Lobat

2016-08-01

Chitosan (CS), hydroxyapatite (HA), and magnetite (Fe3O4) have been broadly employed for bone treatment applications. Having a hybrid biomaterial composed of the aforementioned constituents not only accumulates the useful characteristics of each component, but also provides outstanding composite properties. In the present research, mechanical properties of pure CS, CS/HA, CS/HA/magnetite, and CS/magnetite were evaluated by the measurements of bending strength, elastic modulus, compressive strength and hardness values. Moreover, the morphology of the bending fracture surfaces were characterized using a scanning electron microscope (SEM) and an image analyzer. Studies were also conducted to examine the biological response of the human Mesenchymal Stem Cells (hMSCs) on different composites. We conclude that, although all of these composites possess in-vitro biocompatibility, adding hydroxyapatite and magnetite to the chitosan matrix can noticeably enhance the mechanical properties of the pure chitosan. Copyright © 2016 Elsevier B.V. All rights reserved.

Preparation and corrosion resistance of magnesium phytic acid/hydroxyapatite composite coatings on biodegradable AZ31 magnesium alloy.

PubMed

Zhang, Min; Cai, Shu; Zhang, Feiyang; Xu, Guohua; Wang, Fengwu; Yu, Nian; Wu, Xiaodong

2017-06-01

In this work, a magnesium phytic acid/hydroxyapatite composite coating was successfully prepared on AZ31 magnesium alloy substrate by chemical conversion deposition technology with the aim of improving its corrosion resistance and bioactivity. The influence of hydroxyapatite (HA) content on the microstructure and corrosion resistance of the coatings was investigated. The results showed that with the increase of HA content in phytic acid solution, the cracks on the surface of the coatings gradually reduced, which subsequently improved the corrosion resistance of these coated magnesium alloy. Electrochemical measurements in simulated body fluid (SBF) revealed that the composite coating with 45 wt.% HA addition exhibited superior surface integrity and significantly improved corrosion resistance compared with the single phytic acid conversion coating. The results of the immersion test in SBF showed that the composite coating could provide more effective protection for magnesium alloy substrate than that of the single phytic acid coating and showed good bioactivity. Magnesium phytic acid/hydroxyapatite composite, with the desired bioactivity, can be synthesized through chemical conversion deposition technology as protective coatings for surface modification of the biodegradable magnesium alloy implants. The design idea of the new type of biomaterial is belong to the concept of "third generation biomaterial". Corrosion behavior and bioactivity of coated magnesium alloy are the key issues during implantation. In this study, preparation and corrosion behavior of magnesium phytic acid/hydroxyapatite composite coatings on magnesium alloy were studied. The basic findings and significance of this paper are as follows: 1. A novel environmentally friendly, homogenous and crack-free magnesium phytic acid/hydroxyapatite composite coating was fabricated on AZ31 magnesium alloy via chemical conversion deposition technology with the aim of enhancing its corrosion resistance and bioactivity. The chemical conversion coatings, which are formed through the reaction between the substrate and the environment, have attracted increasing attention owing to the relative low treatment temperature, favorable bonding to substrate and simple implementation process. 2. With the increasing of hydroxyapatite (HA) content, the crack width in the composite coatings and the thickness of the coatings exhibit obviously decreased. The reason is probably that when adding HA into the phytic acid solution, the amount of active hydroxyl groups in the phytic acid are reduced via forming the coordination bond between P-OH groups from phytic acid and P-OH groups from the surface of HA, thus decreasing the coating thickness and hydrogen formation, as well as avoiding coating cracking. 3. By adjusting the HA content to 45 wt.%, a dense and relatively smooth composite coating with ~1.4 μm thickness is obtained on magnesium alloy, and exhibits high corrosion resistance and good bioactivity when compared with the single phytic acid conversion coating.

Growth of hydroxyapatite in a biocompatible mesoporous ordered silica.

PubMed

Díaz, A; López, T; Manjarrez, J; Basaldella, E; Martínez-Blanes, J M; Odriozola, J A

2006-03-01

A novel biomaterial (HA-SBA-15) has been developed based on the growth of calcium phosphate hydroxyapatite (HA) nanoparticles within an organized silica structure (SBA-15). Characterization of the material was carried out using a combination of X-ray diffraction, X-ray fluorescence, transmission electron microscopy, N2 adsorption-desorption isotherms and nuclear magnetic resonance. Transmission electron microscopy observations and N2 porosimetry revealed the crystallization of hydroxyapatite nanoparticles inside the mesopore cavities of the silica structure. Specific surface areas of 760 m2 g(-1) and 260 m2 g(-1) were measured for the SBA-15 and the HA-SBA-15 material, respectively. The hydroxyl groups present in the silica nanostructure surface have brought about cationic defects in the silicium sites, mainly with those of tetrahedral symmetry, and promoted the formation of siloxanes. 29Si MAS-NMR analysis shows a significant reduction of the silanol groups concentration with HA growing within the base (SBA-15) material. Studies and brain tissue biocompatibility tests were carried out. Histopathological studies on the SBA-15 implant material showed no changes to the tissue nearby. The results confirmed the synthesis of a silica-based composite containing HA nanoparticles with the potential for biomedical applications.

Improving the degradation behavior and in vitro biological property of nano-hydroxyapatite surface- grafted with the assist of citric acid.

PubMed

Jiang, Liuyun; Jiang, Lixin; Xiong, Chengdong; Su, Shengpei

2016-10-01

To obtain ideal nano-hydroxyapatite(n-HA) filler for poly(lactide-co-glycolide) (PLGA), a new surface-grafting with the assist of citric acid for nano-hydroxyapatite (n-HA) was designed, and the effect of n-HA surface-grafted with or without citric acid on in vitro degradation behavior and cells viability was studied by the experiments of soaking in simulated body fluid (SBF) and incubating with human osteoblast-like cells (MG-63). The change of pH value, tensile strength reduction, the surface deposits, cells attachment and proliferation of samples during the soaking and incubation were investigated by means of pH meter, electromechanical universal tester, scanning electron microscope (SEM) coupled with energy-dispersive spectro-scopy (EDS), fluorescence microscope and MTT method. The results showed that the introduction of citric acid not only delayed the strength reduction during the degradation by inhibiting the detachment of n-HA from PLGA, but also endowed it better cell attachment and proliferation, suggesting that the n-HA surface-grafted with the assist of citric acid was an important bioactive ceramic fillers for PLGA used as bone materials. Copyright © 2016 Elsevier B.V. All rights reserved.

Properties of natural and synthetic hydroxyapatite and their surface free energy determined by the thin-layer wicking method

NASA Astrophysics Data System (ADS)

Szcześ, Aleksandra; Yan, Yingdi; Chibowski, Emil; Hołysz, Lucyna; Banach, Marcin

2018-03-01

Surface free energy is one of the parameters accompanying interfacial phenomena, occurring also in the biological systems. In this study the thin layer wicking method was used to determine surface free energy and its components for synthetic hydroxyapatite (HA) and natural one obtained from pig bones. The Raman, FTIR and X-Ray photoelectron spectroscopy, X-ray diffraction techniques and thermal analysis showed that both samples consist of carbonated hydroxyapatite without any organic components. Surface free energy and its apolar and polar components were found to be similar for both investigated samples and equalled γSTOT = 52.4 mJ/m2, γSLW = 40.2 mJ/m2 and γSAB = 12.3 mJ/m2 for the synthetic HA and γSTOT = 54.6 mJ/m2, γSLW = 40.3 mJ/m2 and γSAB = 14.3 mJ/m2 for the natural one. Both HA samples had different electron acceptor (γs+) and electron donor (γs-) parameters. The higher value of the electron acceptor was found for the natural HA whereas the electron donor one was higher for the synthetic HA

Preparation and characterization of carbon nanofibrous/hydroxyapatite sheets for bone tissue engineering.

PubMed

Abd El-Aziz, A M; El Backly, Rania M; Taha, Nahla A; El-Maghraby, Azza; Kandil, Sherif H

2017-07-01

Critical size bone defects are orthopedic defects that will not heal without intervention or that will not completely heal over the natural life time of the animal. Although bone generally has the ability to regenerate completely however, critical defects require some sort of scaffold to do so. In the current study we proposed a method to obtain a carbon nanofibrous/Hydroxyapatite (HA) bioactive scaffold. The carbon nanofibrous (CNF) nonwoven fabrics were obtained by the use of the electrospinning process of the polymeric solution of poly acrylonitrile "PAN" and subsequent stabilization and carbonization processes. The CNFs sheets were functionalized by both hydroxyapatite (HA) and bovine serum albumin (BSA). The HA was added to the electrospun solution, but in case of (BSA), it was adsorbed after the carbonization process. The changes in the properties taking place in the precursor sheets were investigated using the characterization methods (SEM, FT-IR, TGA and EDX). The prepared materials were tested for biocompatibility via subcutaneous implantation in New Zealand white rabbits. We successfully prepared biocompatible functionalized sheets, which have been modified with HA or HA and BSA. The sheets that were functionalized by both HA and BSA are more biocompatible with fewer inflammatory cells of (neutrophils and lymphocytes) than ones with only HA over the period of 3weeks. Copyright © 2017 Elsevier B.V. All rights reserved.

Experimental studies on a new bioactive material: HAIonomer cements.

PubMed

Yap, A U J; Pek, Y S; Kumar, R A; Cheang, P; Khor, K A

2002-02-01

The lack of exotherm during setting, absence of monomer and improved release of incorporated therapeutic agents has resulted in the development of glass ionomer cements (GICs) for biomedical applications. In order to improve biocompatibility and biomechanically match GICs to bone, hydroxyapatite-ionomer (HAIonomer) hybrid cements were developed. Ultra-fine hydroxyapatite (HA) powders were produced using a new induction spraying technique that utilizes a radio-frequency source to spheriodize an atomized suspension containing HA crystallites. The spheriodized particulates were then held at 800 degrees C for 4 h in a carbolite furnace using a heating and cooling rate of 25 degrees C/min to obtain almost fully crystalline HA powders. The heat-treated particles were characterized and introduced into a commercial glass ionomer cement. 4 (H4), 12 (H12) and 28 (H28) vol% of fluoroalumino silicate were substituted by crystalline HA particles that were dispersed using a high-speed dispersion technique. The HAIonomer cements were subjected to hardness, compressive and diametral tensile strength testing based upon BS6039:1981. The storage time were extended to one week to investigate the effects of cement maturation on mechanical properties. Commercially available capsulated GIC (GC) and GIC at maximum powder:liquid ratio (GM) served as comparisons. Results were analyzed using factorial ANOVA/Scheffe's post-hoc tests and independent samples t-test at significance level 0.05. The effect of time on hardness was material dependent. With the exception of H12, a significant increase in hardness was observed for all materials at one week. A significant increase in compressive strength was, however, observed for H12 over time. At 1 day and 1 week, the hardness of H28 was significantly lower than for GM, H4, and H12. No significant difference in compression and diametral tensile strengths were observed between materials at both time intervals. Results show that HAIonomers is a promising material, which possess good mechanical properties. Potential uses of this new material include bone cements and performed implants for hard tissue replacement in the field of otological, oral-maxillofacial and orthopedic surgery.

Investigation of chronic toxicity of hydroxyapatite nanoparticles administered orally for one year in wistar rats.

PubMed

Remya, N S; Syama, S; Sabareeswaran, A; Mohanan, P V

2017-07-01

Although the toxicity/biocompatibility of hydroxyapatite nanoparticles (nano HA), a prospective nano biomaterial is extensively studied, its interaction on biological systems following chronic exposure is less exploited. In the present study, Wistar rats were given various concentrations of nano HA in the diet to determine the chronic toxicity and potential carcinogenicity. Altogether 140 rats were used for the study under various administration dosages along with control. The animals were sacrificed after 12months of controlled continuous dosing. All in-life parameters, including body weight, food consumption, clinical observations, survival, biochemical and hematology, were unaffected by the chronic exposure of nano HA orally. Similarly, gross and histopathological evaluation was also unchanged following exposure to nano HA. No evidence of nano HA-related lesions or Nano HA-induced neoplasia was suggested in this rodent bioassay study. Copyright © 2017 Elsevier B.V. All rights reserved.

Preparation and Characterisation of Hydroxyapatite Coatings on Nanotubular TiO2 Surface Obtained by Sol-Gel Process.

PubMed

Shin, Jin-Ho; Kim, Jung-Hwa; Koh, Jeong-Tae; Lim, Hyun-Pil; Oh, Gye-Jeong; Lee, Seok-Woo; Lee, Kwang-Min; Yun, Kwi-Dug; Park, Sang-Won

2015-08-01

Hydroxyapatite (HA) coating on titanium dioxide (TiO2) nanotubular surface has been developed to complement the defects of both TiO2 and HA. A sol-gel processing technique was used to coat HA on TiO2 nanotubular surface. All the titanium discs were blasted with resorbable blast media (RBM). RBM-blasted Ti surface, anodized Ti surface, and sol-gel HA coating on the anodized Ti surface were prepared. The characteristics of samples were observed using scanning electron microscopy and X-ray photoemission spectroscopy. Biologic responses were evaluated with human osteosarcoma MG63 cells in vitro. The top of the TiO2 nanotubes was not completely covered by HA particles when the coating time was less than 60 sec. It was demonstrated the sol-gel derived HA film was well-crystallized and this enhanced biologic responses in early stage cell response.

Removal of heavy metal ions by biogenic hydroxyapatite: Morphology influence and mechanism study

NASA Astrophysics Data System (ADS)

Wang, Dandan; Guan, Xiaomei; Huang, Fangzhi; Li, Shikuo; Shen, Yuhua; Chen, Jun; Long, Haibo

2016-08-01

Based on the synthesis of hydroxyapatite (HA) with different morphologies, such as nanorod-like, flower-like and sphere-like assembled HA nanorods, a new strategy has been developed for the removal of heavy metal ions such as Pb2+, Cu2+, Mn2+, Zn2+. The dependence of removal efficiency on the morphology and the suspended concentration of trapping agent, the removal time and selectivity were evaluated and discussed. The experimental results proved that the removal capacity of flower-like assembled HA nanorods (NAFL-HA) was the best, and the maximum removal ratio for Pb2+ ion was 99.97%. The mechanism of Pb2+ removal was studied in detail, noting that some metal ions were completely incorporated into hydroxyapatitie to produce Pb-HA. It reveals that the metal ions capture by HA is mainly controlled by sample surface adsorption and co-precipitation, which are directly controlled by sample morphology.

Facile and controllable synthesis of hydroxyapatite/graphene hybrid materials with enhanced sensing performance towards ammonia.

PubMed

Zhang, Qing; Liu, Yong; Zhang, Ying; Li, Huixia; Tan, Yanni; Luo, Lanlan; Duan, Junhao; Li, Kaiyang; Banks, Craig E

2015-08-07

In this work, needle-like and micro-spherical agglomerates of nanocrystalline hydroxyapatite (HA) were successfully assembled on the surface of graphene sheets with the aid of dopamine having two roles, as a template and a reductant for graphite oxide during the process of self-polymerization. The crystalline structure and micromorphology of HA can be conveniently regulated by controlling the mineralization route either with a precipitation (cHA/GR) or biomimetic methodology (bHA/GR). Both the composites exhibit improvements of ∼150% and ∼250% in sensitivity towards the sensing of ammonia at room temperature, compared with that of bare graphene. The combination of the multi-adsorption capability of HA and the electric conductivity of graphene is proposed to be the major reason for the observed enhancements. Gas sensing tests demonstrated that the HA/GR composites exhibit excellent selectivity, high sensitivity and repeatable stability towards the analytical sensing of ammonia.

Efficacy of a mouthrinse based on hydroxyapatite to reduce initial bacterial colonisation in situ.

PubMed

Kensche, A; Holder, C; Basche, S; Tahan, N; Hannig, C; Hannig, M

2017-08-01

The present in situ - investigation aimed to specify the impact of pure hydroxyapatite microclusters on initial bioadhesion and bacterial colonization at the tooth surface. Pellicle formation was carried out in situ on bovine enamel slabs (9 subjects). After 1min of pellicle formation rinses with 8ml of hydroxyapatite (HA) microclusters (5%) in bidestilled water or chlorhexidine 0.2% were performed. As negative control no rinse was adopted. In situ biofilm formation was promoted by the intraoral slab exposure for 8h overnight. Afterwards initial bacterial adhesion was quantified by DAPI staining and bacterial viability was determined in vivo/in vitro by live/dead-staining (BacLight). SEM analysis evaluated the efficacy of the mouthrinse to accumulate hydroxyapatite microclusters at the specimens' surface and spit-out samples of the testsolution were investigated by TEM. Compared to the control (2.36×10 6 ±2.01×10 6 bacteria/cm 2 ), significantly reduced amounts of adherent bacteria were detected on specimens rinsed with chlorhexidine 0.2% (8.73×10 4 ±1.37×10 5 bacteria/cm 2 ) and likewise after rinses with the hydroxyapatite testsolution (2.08×10 5 ±2.85×10 5 bacteria/cm 2 , p<0.001). No demonstrable effect of HA-particles on Streptococcus mutans viability could be shown. SEM analysis confirmed the temporary adsorption of hydroxyapatite microclusters at the tooth surface. Adhesive interactions of HA-particles with oral bacteria were shown by TEM. Hydroxyapatite microclusters reduced initial bacterial adhesion to enamel in situ considerably and could therefore sensibly supplement current approaches in dental prophylaxis. Copyright © 2017 Elsevier Ltd. All rights reserved.

Experimental and numerical measurements of adhesion energies between PHEMA and PGLYMA with hydroxyapatite crystal.

PubMed

Youssefian, Sina; Liu, Pingsheng; Askarinejad, Sina; Shalchy, Faezeh; Song, Jie; Rahbar, Nima

2015-07-16

Synthetic orthopaedic materials consisting of a single bioinert polymeric material do not meet the complex biological and physical requirements of scaffold-guided bone tissue repair and regeneration. Of particular interest is the design of biocompatible hydrogel-hydroxyapatite composite bone substitutes with outstanding interfacial adhesion that would warranty the ability for the composite to withstand functional loadings without exhibiting brittle fractures during the dynamic guided tissue regeneration. For this purpose, the hydroxylated side chain of chemically cross-linked poly (2-hydroxyethyl methacrylate) (pHEMA) is substitute with a carboxylated side chain to make poly (glycerol methacrylate) (pGLYMA). Here, we carry out atomistic simulations and atomic force microscopy to predict and experimentally determine the interfacial adhesion energies of pHEMA and pGLYMA with the surface of single-crystalline hydroxyapatite (HA) whiskers. Both experimental and numerical results showed that pGLYMA has stronger adhesion forces with HA and may be used for preparing a high-affinity polymer-HA composite. The high adhesive interactions between pGLYMA and HA were found to be due to strong electrostatic energies.

A novel thermo-sensitive hydrogel based on thiolated chitosan/hydroxyapatite/beta-glycerophosphate.

PubMed

Liu, Xujie; Chen, Yan; Huang, Qianli; He, Wei; Feng, Qingling; Yu, Bo

2014-09-22

In order to get a water-soluble in situ gel-forming system, a thiolated chitosan, chitosan-4-thio-butylamidine (CS-TBA) conjugate was synthesized and used to replace the unmodified chitosan in the application of the in situ gel-forming system. A novel thermo-sensitive hydrogel was prepared based on CS-TBA/hydroxyapatite (HA)/beta-glycerophosphate disodium (β-GP). The gel formation, rheological properties, morphology, degradation, cytotoxicity, as well as protein release process of the novel gel system were investigated in this study. The CS-TBA/HA/β-GP gel showed a higher storage modulus (G') and loss modulus (G″) and a decreased bovine serum albumin (BSA) release rate which was maintained the protein release for a longer time compared with the unmodified chitosan (CS)/HA/β-GP gel, due to the existence of thiol groups and/or disulfide bonds. The CS-TBA/HA/β-GP gel has a porous structure with a uniform distribution of nano-hydroxyapatite, an appropriate degradation rate and low cytotoxicity, showing potential applications in drug delivery and tissue engineering. Copyright © 2014 Elsevier Ltd. All rights reserved.

Biocompatibility of nano-hydroxyapatite/polyetheretherketone composite materials with osteoblasts cultured in vitro

NASA Astrophysics Data System (ADS)

Wang, Lin; Huang, Feijuan; Wu, Zhengzhi; Ma, Rui

2017-04-01

The biocompatibility of the Sprague Dawley (SD) rat osteoblasts, which were cultured on the surfaces of nano-hydroxyapatite/polyetheretherketone (n-HA/PEEK) composites were investigated in this work. The osteoblasts of 24- hour old SD rats were cultured and identified by modified enzymatic digestion in vitro. The morphology and proliferation of cells were observed in CCK-8 regent staining, inverted microscopes, and by scanning electron microscopy (SEM) respectively. The results show that n-HA/PEEK composites have good biocompatibility with SD osteoblasts and that they can promote the growth of the cells that were cultured on the surfaces of the composites. The content of HA in n- HA/PEEK composites plays an important role in cell proliferation.

The influence of micropore size on the mechanical properties of bulk hydroxyapatite and hydroxyapatite scaffolds.

PubMed

Cordell, Jacqueline M; Vogl, Michelle L; Wagoner Johnson, Amy J

2009-10-01

While recognized as a promising bone substitute material, hydroxyapatite (HA) has had limited use in clinical settings because of its inherent brittle behavior. It is well established that macropores ( approximately 100 microm) in a HA implant, or scaffold, are required for bone ingrowth, but recent research has shown that ingrowth is enhanced when scaffolds also contain microporosity. HA is sensitive to synthesis and processing parameters and therefore characterization for specific applications is necessary for transition to the clinic. To that end, the mechanical behavior of bulk microporous HA and HA scaffolds with multi-scale porosity (macropores between rods in the range of 250-350 microm and micropores within the rods with average size of either 5.96 microm or 16.2 microm) was investigated in order to determine how strength and reliability were affected by micropore size (5.96 microm versus 16.2 microm). For the bulk microporous HA, strength increased with decreasing micropore size in both bending (19 MPa to 22 MPa) and compression (71 MPa to 110 MPa). To determine strength reliability, the Weibull moduli for the bulk microporous HA were determined. The Weibull moduli for bending increased (became more reliable) with decreasing pore size (7 to 10) while the Weibull moduli for compression decreased (became less reliable) with decreasing pore size (9 to 6). Furthermore, the elastic properties of the bulk microporous HA (elastic modulus of 30 GPa) and the compressive strengths of the HA scaffolds with multi-scale porosity (8 MPa) did not vary with pore size. The mechanisms responsible for the trends observed were discussed.

Bone integration capability of a series of strontium-containing hydroxyapatite coatings formed by micro-arc oxidation.

PubMed

Yan, Jun; Sun, Ji-Feng; Chu, Paul K; Han, Yong; Zhang, Yu-Mei

2013-09-01

Strontium-containing hydroxyapatites (Sr-HA) combine the desirable bone regenerative properties of hydroxyapatites (HA) with anabolic and anti-catabolic effects of strontium cations. In the present work, a series of Sr(y)HA [Sr(y)Ca(10-y)(PO4)6(OH)2; y = 0, 0.5, 1, 2] coatings on titanium are produced by micro-arc oxidation (MAO), and the effects of the in vivo osseointegration ability of the coatings are investigated by using a rabbit model. All samples are subjected to biomechanical, surface elemental, micro-CT and histological analysis after 4 and 12 weeks of healing. The obtained results show that the MAO-formed coatings exhibit a microporous network structure composed of Sr(y)HA/Sr(y)HA-Sr(x)Ca(1-x)TiO3/Sr(x)Ca(1-x)TiO3-TiO2 multilayers, in which the outer Sr(y)HA and intermediate Sr(y)HA-Sr(x)Ca(1-x)TiO3 layers have a nanocrystalline structure. All Sr-HA coated implants induce marked improvements in the behavior of bone formation, quantity and quality of bone tissue around the implants than the control HA implant and in particular, the 20%Sr-HA coating promotes early bone formation as identified by polyfluorochrome sequential labeling. The bone-to-implant contact is increased by 46% (p < 0.05) and the pull-out strength is increased by 103% over the HA group (p < 0.01). Extensive areas of mineralized tissue densely deposit on the 20%Sr-HA coating after biomechanical testing, and the greatest improvement of bone microarchitecture are observed around the 20%Sr-HA implant. The identified biological parameters successfully demonstrate the osteoconductivity of 20%Sr-HA surfaces, which results not only in an acceleration but also an improvement of bone-implant integration. The study demonstrates the immense potential of 20%Sr-HA coatings in dental and orthopedic applications. Copyright © 2012 Wiley Periodicals, Inc.

Mechanical and biological properties of the micro-/nano-grain functionally graded hydroxyapatite bioceramics for bone tissue engineering.

PubMed

Zhou, Changchun; Deng, Congying; Chen, Xuening; Zhao, Xiufen; Chen, Ying; Fan, Yujiang; Zhang, Xingdong

2015-08-01

Functionally graded materials (FGM) open the promising approach for bone tissue repair. In this study, a novel functionally graded hydroxyapatite (HA) bioceramic with micrograin and nanograin structure was fabricated. Its mechanical properties were tailored by composition of micrograin and nanograin. The dynamic mechanical analysis (DMA) indicated that the graded HA ceramics had similar mechanical property compared to natural bones. Their cytocompatibility was evaluated via fluorescent microscopy and MTT colorimetric assay. The viability and proliferation of rabbit bone marrow mesenchymal stem cells (BMSCs) on ceramics indicated that this functionally graded HA ceramic had better cytocompatibility than conventional HA ceramic. This study demonstrated that functionally graded HA ceramics create suitable structures to satisfy both the mechanical and biological requirements of bone tissues. Copyright © 2015 Elsevier Ltd. All rights reserved.

Invitro Evaluation of Fluoride Release from Hydroxyapatite Reinforced Glass Ionomer with or without Protective Coating

PubMed Central

Nandlal, Bhojraj

2016-01-01

Introduction Glass Ionomer Cement (GIC) is well known for its fluoride releasing property but has its own drawbacks of poor mechanical properties, sensitivity to initial desiccation and moisture contamination. To overcome these, search led to the reinforcement of hydroxyapatite and application of surface coating agent but their effect on fluoride release is still not clear. Aim To evaluate and compare the release of fluoride from Hydroxyapatite Reinforced Glass Ionomer (HA-GIC) with and without protective coating. Materials and Methods Specimens were prepared as follows- Eight percent by weight conventional glass ionomer was replaced by hydroxyapatite powder (HA) and an indigenous product was prepared (HA-GIC). This powder was mixed with liquid of conventional GIC and allowed to set, then G coat plus coating agent was applied in surface coated group and light cured. Fluoride release of the sample was measured every 24 hrs for seven days and weekly from 7th to 21st day using combination ion selective electrode. Results Mean values clearly reveal a significant decrease in the fluoride release from day 1 to day 21 for both the groups. Results of repeated measure ANOVA revealed statistically significant difference between two groups (p <0.001). Conclusion Coating the hydroxyapatite reinforced glass ionomer will allow for slow and steady release of fluoride for a long period of time into oral environment. PMID:27190957

Longevity of ultra-low-volume sprays of fipronil and malathion on cotton in Mexico

Treesearch

Joseph E. Mulrooney; K.A. Holmes; R.A. Shaw; D. Goli

2003-01-01

In 1996, fipronil and malathion residues were evaluated after four ultra-low-volume (ULV) spray applications in northeastern Tarnaulipas, Mexico. Sprays were applied at 0.88 L/ha. Fipronil was applied at 28 and 56 g A.I./ha and malathion at 840 g A.I./ha. Four applications were made beginning 23 May at four, five and six day intervals. Leaf surface residues of...

The effects of hydroxyapatite coatings on stress distribution near the dental implant bone interface

NASA Astrophysics Data System (ADS)

Jiang, W.; Wang, W. D.; Shi, X. H.; Chen, H. Z.; Zou, W.; Guo, Z.; Luo, J. M.; Gu, Z. W.; Zhang, X. D.

2008-11-01

The effects of different thickness of hydroxyapatite (HA) coatings on bone stress distribution near the dental implant-bone interface are very important factors for the HA-coated dental implant design and clinical application. By means of finite element analysis (FEA), the bone stress distributions near the dental implant coated with different thicknesses from 0 to 200 μm were calculated and analyzed under the 200 N chewing load. In all cases, the maximal von Mises stresses in the bone are at the positions near the neck of dental implant on the lingual side, and decrease with the increase of the HA coatings thickness. The HA coatings weaken the stress concentration and improve the biomechanical property in the bone, however, in HA coatings thickness range of 60-120 μm, the distinctions of that benefit are not obvious. In addition, considering the technical reason of HA coatings, we conclude that thickness of HA coatings range from 60 to 120 μm would be the better choice for clinical application.

Fabrication of hydroxyapatite-poly(epsilon-caprolactone) scaffolds by a combination of the extrusion and bi-axial lamination processes.

PubMed

Sun, Jong-Jae; Bae, Chang-Jun; Koh, Young-Hag; Kim, Hyoun-Ee; Kim, Hae-Won

2007-06-01

Hydroxyapatite (HA)/poly(epsilon-caprolactone) (PCL) composite scaffolds were fabricated using a combination of the extrusion and bi-axial lamination processes. Firstly, HA/PCL composites with various HA contents (0, 50, 60, 70 wt%) were prepared by mixing the HA powders and the molten PCL at 100 degrees C and then extruded through an orifice with dimensions of 600 x 600 microm to produce HA/PCL composite fibers. Isobutyl methacrylate (IBMA) polymer fiber was also prepared in a similar manner for use as a fugitive material. The 3-D scaffold was then produced by the bi-axial lamination of the HA/PCL and IBMA fibers, followed by solvent leaching to remove the IBMA. It was observed that the HA/PCL composites had a superior elastic modulus and biological properties, as compared to the pure PCL. The fabricated HA/PCL scaffold showed a controlled pore structure (porosity of approximately 49% and pore size of approximately 512 microm) and excellent welding between the HA/PCL fibers, as well as a high compressive strength of approximately 7.8 MPa.

Chondroitin sulfate template-mediated biomimetic synthesis of nano-flake hydroxyapatite

NASA Astrophysics Data System (ADS)

He, Dan; Xiao, Xiufeng; Liu, Fang; Liu, Rongfang

2008-11-01

By Ca(NO 3) 2·4H 2O and (NH 4) 3PO 4·3H 2O as reagents and chondroitin sulfate (ChS) as a template, nano-flake hydroxyapatite (HA) is synthesized using a biomimetic method according to the biomineralization theory. HA crystals obtained are characterized in crystalline phase, microstructure, chemical composition and morphology by X-ray diffraction (XRD), Fourier transform infrared spectroscope (FTIR), transmission electron microscopy (TEM) and elemental analysis respectively. UV-vis spectrum is adopted to investigate interactions between functional groups ChS and HA. The results show that HA crystal nucleation and growth take place in chemical interactions between HA crystals and ChS as a template. And elemental analysis indicates that obtained HA contains a small amount of ChS. Furthermore, ChS concentration significantly affects the morphology of HA crystals. Staple-fiber-like HA crystals can be obtained at a low concentration in ChS, and flake-like HA crystals synthesized at a high concentration (≥0.5 wt.%) of ChS as a template.

Surface-enrichment with hydroxyapatite nanoparticles in stereolithography-fabricated composite polymer scaffolds promotes bone repair.

PubMed

Guillaume, O; Geven, M A; Sprecher, C M; Stadelmann, V A; Grijpma, D W; Tang, T T; Qin, L; Lai, Y; Alini, M; de Bruijn, J D; Yuan, H; Richards, R G; Eglin, D

2017-05-01

Fabrication of composite scaffolds using stereolithography (SLA) for bone tissue engineering has shown great promises. However, in order to trigger effective bone formation and implant integration, exogenous growth factors are commonly combined to scaffold materials. In this study, we fabricated biodegradable composite scaffolds using SLA and endowed them with osteopromotive properties in the absence of biologics. First we prepared photo-crosslinkable poly(trimethylene carbonate) (PTMC) resins containing 20 and 40wt% of hydroxyapatite (HA) nanoparticles and fabricated scaffolds with controlled macro-architecture. Then, we conducted experiments to investigate how the incorporation of HA in photo-crosslinked PTMC matrices improved human bone marrow stem cells osteogenic differentiation in vitro and kinetic of bone healing in vivo. We observed that bone regeneration was significantly improved using composite scaffolds containing as low as 20wt% of HA, along with difference in terms of osteogenesis and degree of implant osseointegration. Further investigations revealed that SLA process was responsible for the formation of a rich microscale layer of HA corralling scaffolds. To summarize, this work is of substantial importance as it shows how the fabrication of hierarchical biomaterials via surface-enrichment of functional HA nanoparticles in composite polymer stereolithographic structures could impact in vitro and in vivo osteogenesis. This study reports for the first time the enhance osteopromotion of composite biomaterials, with controlled macro-architecture and microscale distribution of hydroxyapatite particles, manufactured by stereolithography. In this process, the hydroxyapatite particles are not only embedded into an erodible polymer matrix, as reported so far in the literature, but concentrated at the surface of the structures. This leads to robust in vivo bone formation at low concentration of hydroxyapatite. The reported 3D self-corralling composite architecture provides significant opportunities to develop functional biomaterials for bone repair and tissue engineering. Copyright © 2017. Published by Elsevier Ltd.

Synthesis of hydroxyapatite/multi-walled carbon nanotubes for the removal of fluoride ions from solution

NASA Astrophysics Data System (ADS)

Ruan, Zhongyuan; Tian, Yaxi; Ruan, Jifu; Cui, Guijia; Iqbal, Kanwal; Iqbal, Anam; Ye, Herui; Yang, Zhangzhong; Yan, Shiqiang

2017-08-01

A novel composite material, hydroxyapatite (HA)-multi-walled carbon nanotubes (MWCNTs), was prepared using a simple in-situ sol-gel method, and was used for the first time to remove fluoride from water. The novel HA-MWCNTs were characterized using TEM, FT-IR, BET and XRD analysis. The TEM and SAED results revealed that the MWCNTs were uniformly encapsulated by hydroxyapatite nanoparticles. The synthesized HA-MWCNTs had a high specific surface area (180.504 m2 g-1), with an average pore width (14.607 nm) and pore volume (0.774 cm3 g-1), which produced a defluoridation capacity (DC) of 30.22 mgF- g-1. This value was greater than unmodified hydroxyapatite (HA), which exhibited a larger specific surface area (172.233 m2 g-1) and an excellent DC of 17.80 mgF- g-1. A number of pertinent parameters that could affect the defluoridation performance of the HA/MWCNTs including weight ratios of the two key materials, solution pH and competing anions were carefully and comprehensively examined. It was found that the adsorption results followed the Langmuir and Freundlich isotherm model, and the sorption kinetics of the F- appeared to exhibit a pseudo second order. Moreover, the adsorption reaction was spontaneous and endothermic and appeared to exhibit a higher initial adsorption rate. This reaction appeared to occur result from both anion exchange and electrostatic interactions. When the HA-MWCNTs (MH6) were at an adsorbent dose of 2.0 g L-1, they were able to decrease the fluoride concentration of actual nuclear industry wastewater from 8.79 mg L-1 to about 0.25 mg L-1 (97.15% removal efficiency). The experimental results of this study showed that the HA-MWCNTs composites have application potential for the removal of fluoride ions from wastewater.

Response of Human Osteoblast to n-HA/PEEK—Quantitative Proteomic Study of Bio-effects of Nano-Hydroxyapatite Composite

NASA Astrophysics Data System (ADS)

Zhao, Minzhi; Li, Haiyun; Liu, Xiaochen; Wei, Jie; Ji, Jianguo; Yang, Shu; Hu, Zhiyuan; Wei, Shicheng

2016-03-01

Nano-sized hydroxyapatite (n-HA) is considered as a bio-active material, which is often mixed into bone implant material, polyetheretherketone (PEEK). To reveal the global protein expression modulations of osteoblast in response to direct contact with the PEEK composite containing high level (40%) nano-sized hydroxyapatite (n-HA/PEEK) and explain its comprehensive bio-effects, quantitative proteomic analysis was conducted on human osteoblast-like cells MG-63 cultured on n-HA/PEEK in comparison with pure PEEK. Results from quantitative proteomic analysis showed that the most enriched categories in the up-regulated proteins were related to calcium ion processes and associated functions while the most enriched categories in the down-regulated proteins were related to RNA process. This enhanced our understanding to the molecular mechanism of the promotion of the cell adhesion and differentiation with the inhibition of the cell proliferation on n-HA/PEEK composite. It also exhibited that although the calcium ion level of incubate environment hadn’t increased, merely the calcium fixed on the surface of material had influence to intracellular calcium related processes, which was also reflect by the higher intracellular Ca2+ concentration of n-HA/PEEK. This study could lead to more comprehensive cognition to the versatile biocompatibility of composite materials. It further proves that proteomics is useful in new bio-effect discovery.

Nano-hydroxyapatite-coated metal-ceramic composite of iron-tricalcium phosphate: Improving the surface wettability, adhesion and proliferation of mesenchymal stem cells in vitro.

PubMed

Surmeneva, Maria A; Kleinhans, Claudia; Vacun, Gabriele; Kluger, Petra Juliane; Schönhaar, Veronika; Müller, Michaela; Hein, Sebastian Boris; Wittmar, Alexandra; Ulbricht, Mathias; Prymak, Oleg; Oehr, Christian; Surmenev, Roman A

2015-11-01

Thin radio-frequency magnetron sputter deposited nano-hydroxyapatite (HA) films were prepared on the surface of a Fe-tricalcium phosphate (Fe-TCP) bioceramic composite, which was obtained using a conventional powder injection moulding technique. The obtained nano-hydroxyapatite coated Fe-TCP biocomposites (nano-HA-Fe-TCP) were studied with respect to their chemical and phase composition, surface morphology, water contact angle, surface free energy and hysteresis. The deposition process resulted in a homogeneous, single-phase HA coating. The ability of the surface to support adhesion and the proliferation of human mesenchymal stem cells (hMSCs) was studied using biological short-term tests in vitro. The surface of the uncoated Fe-TCP bioceramic composite showed an initial cell attachment after 24h of seeding, but adhesion, proliferation and growth did not persist during 14 days of culture. However, the HA-Fe-TCP surfaces allowed cell adhesion, and proliferation during 14 days. The deposition of the nano-HA films on the Fe-TCP surface resulted in higher surface energy, improved hydrophilicity and biocompatibility compared with the surface of the uncoated Fe-TCP. Furthermore, it is suggested that an increase in the polar component of the surface energy was responsible for the enhanced cell adhesion and proliferation in the case of the nano-HA-Fe-TCP biocomposites. Copyright © 2015 Elsevier B.V. All rights reserved.

Response of Human Osteoblast to n-HA/PEEK--Quantitative Proteomic Study of Bio-effects of Nano-Hydroxyapatite Composite.

PubMed

Zhao, Minzhi; Li, Haiyun; Liu, Xiaochen; Wei, Jie; Ji, Jianguo; Yang, Shu; Hu, Zhiyuan; Wei, Shicheng

2016-03-09

Nano-sized hydroxyapatite (n-HA) is considered as a bio-active material, which is often mixed into bone implant material, polyetheretherketone (PEEK). To reveal the global protein expression modulations of osteoblast in response to direct contact with the PEEK composite containing high level (40%) nano-sized hydroxyapatite (n-HA/PEEK) and explain its comprehensive bio-effects, quantitative proteomic analysis was conducted on human osteoblast-like cells MG-63 cultured on n-HA/PEEK in comparison with pure PEEK. Results from quantitative proteomic analysis showed that the most enriched categories in the up-regulated proteins were related to calcium ion processes and associated functions while the most enriched categories in the down-regulated proteins were related to RNA process. This enhanced our understanding to the molecular mechanism of the promotion of the cell adhesion and differentiation with the inhibition of the cell proliferation on n-HA/PEEK composite. It also exhibited that although the calcium ion level of incubate environment hadn't increased, merely the calcium fixed on the surface of material had influence to intracellular calcium related processes, which was also reflect by the higher intracellular Ca(2+) concentration of n-HA/PEEK. This study could lead to more comprehensive cognition to the versatile biocompatibility of composite materials. It further proves that proteomics is useful in new bio-effect discovery.

Synergistic anticancer efficacy of Bendamustine Hydrochloride loaded bioactive Hydroxyapatite nanoparticles: In-vitro, ex-vivo and in-vivo evaluation.

PubMed

Thomas, Shindu C; Sharma, Harshita; Rawat, Purnima; Verma, Anita K; Leekha, Ankita; Kumar, Vijay; Tyagi, Aakriti; Gurjar, Bahadur S; Iqbal, Zeenat; Talegaonkar, Sushama

2016-10-01

The present work evaluates the synergistic anticancer efficacy of bioactive Hydroxyapatite (HA) nanoparticles (HA NPs) loaded with Bendamustine HCl. Hydroxyapatite is a material with an excellent biological compatibility, a well-known fact which was also supported by the results of the Hemolytic studies and a high IC50 value observed in the MTT assay. HA NPs were prepared by the chemical precipitation method and loaded with the drug via physical adsorption. In-vitro release study was performed, which confirmed the sustained release of the drug from the drug loaded HA NPs. MTT assay, Cell Uptake and FACS studies on JURKAT E6.1 cell line and in-vivo pharmacokinetic studies in Wistar rats revealed that the drug loaded HA NPs could be easily internalized by the cells and release drug in a sustained manner. The drug loaded HA NPs showed cytotoxicity similar to the drug solution at 1/10th of the drug content, which indicates a possible synergism between the activity of the anticancer drug and calcium ions derived from the carrier. An increase in intracellular Ca(2+) ions is reported to induce apoptosis in cells. Tumor regression study in Balb/c mice Ehrlich's ascites model presented a similar synergistic efficacy. The drug solution was able to decrease the tumor volume by half, while the drug loaded HA NPs reduced the tumor size by 6 times. Copyright © 2016 Elsevier B.V. All rights reserved.

Porous bodies of hydroxyapatite produced by a combination of the gel-casting and polymer sponge methods

PubMed Central

González Ocampo, Jazmín I.; Escobar Sierra, Diana M.; Ossa Orozco, Claudia P.

2015-01-01

A combination of gel-casting and polymeric foam infiltration methods is used in this study to prepare porous bodies of hydroxyapatite (HA), to provide a better control over the microstructures of samples. These scaffolds were prepared by impregnating a body of porous polyurethane foam with slurry containing HA powder, and using a percentage of solids between 40% and 50% w/v, and three different types of monomers to provide a better performance. X-Ray Diffraction (XRD), and Fourier Transformed Infrared (FTIR) and Scanning Electron Microscopy (SEM) were employed to evaluate both the powder hydroxyapatite and the scaffolds obtained. In addition, porosity and interconnectivity measurements were taken in accordance with the international norm. Bioactivity was checked using immersion tests in Simulated Body Fluids (SBF). After the sintering process of the porous bodies, the XRD results showed peaks characteristic of a pure and crystalline HA (JCPDS 9-432) as a single phase. SEM images indicate open and interconnected pores inside the material, with pore sizes between 50 and 600 μm. Also, SEM images demonstrate the relatively good bioactivity of the HA scaffolds after immersion in SBF. All results for the porous HA bodies suggest that these materials have great potential for use in tissue engineering. PMID:26966570

The effects of ageing time on the microstructure and properties of mesoporous silica-hydroxyapatite nanocomposite

NASA Astrophysics Data System (ADS)

Yousefpour, Mardali; Taherian, Zahra

2013-02-01

In this study, a mesoporous silica-hydroxyapatite nanocomposite (MCM-41/HA) was synthesized via sol-gel technique as a drug delivery system. The synthesis of MCM-41/hydroxyapatite nanocomposite was carried out at room temperature. The effect of various ageing time on the nanocomposite properties was studied during synthesis process. 0, 24, 36, and 48 h aging times were chosen. Textural properties and microstructure of the nanocomposites were characterized by X-ray diffraction (XRD), Transmission Electron Microscopy (TEM), Energy Dispersive X-ray Spectroscopy (EDS), Electron Diffraction pattern (ED), and N2 adsorption-desorption. Results showed that ageing process led to HA crystals nucleation and growth on the surface of mesoporous silica. At 48 h of aging time, the surface area and total pore volume increased from 36.2 to 334 m2/g and 0.14-0.7 cm3/g, respectively. In contrast, the average pore diameter considerably decreased from 20.1 nm for (MCM-41/HA)24 to 8.39 nm for (MCM-41/HA)48. Furthermore, it was observed more homogeneous pore distribution with increasing the ageing time. In conclusion, the ageing time play an important role on textural properties of MCM-41/HA nanocomposite which could have a major effect on drug delivery properties such as molecular loading and release kinetics.

Adsorption and bioactivity studies of albumin onto hydroxyapatite surface.

PubMed

Mavropoulos, Elena; Costa, Andréa M; Costa, Lilian T; Achete, Carlos A; Mello, Alexandre; Granjeiro, José M; Rossi, Alexandre M

2011-03-01

Bovine serum albumin (BSA) may have an inhibitory or promoter effect on hydroxyapatite (HA) nucleation when apatite is precipitated in a medium containing the protein. In this study we evaluated the influence of BSA on the precipitation of calcium phosphate phases (CP) from simulated body fluid (SBF) when the protein was previously bounded to HA surface. The kinetics of BSA immobilization onto hydroxyapatite surface was performed in different buffers and protein concentrations in order to adjust experimental conditions in which BSA was tightly linked to HA surface for long periods in SBF solution. It was shown that for BSA concentration higher than 0.1mg/mL the adsorption to HA surface followed Langmuir-Freundlich mechanisms, which confirmed the existence of cooperative protein-protein interactions on HA surface. Fourier Transformed Infrared Attenuated Total Reflectance Microscopy (FTIRM-ATR) evidenced changes in BSA conformational state in favor of less-ordered structure. Analyses from high resolution grazing incident X-ray diffraction using synchrotron radiation (GIXRD), Scanning Electron Microscopy (SEM) and Atomic Force Microscopy (AFM) showed that a poorly crystalline calcium phosphate was precipitated on the surface of HA discs coated with BSA, after the immersion in SBF for 4 days. The new bioactive layer had morphological characteristics similar to the one formed on the HA surface without protein. It was identified as a carbonated apatite with preferential crystal growth along apatite 002 direction. The GIXRD results also revealed that BSA layer bound to the surface inhibited the HA dissolution leading to a reduction on the formation of new calcium phosphate phase. 2010 Elsevier B.V. All rights reserved.

Heat treatment's effects on hydroxyapatite powders in water vapor and air atmosphere

NASA Astrophysics Data System (ADS)

Karabulut, A.; Baştan, F. E.; Erdoǧan, G.; Üstel, F.

2015-03-01

Hydroxyapatite (HA; Ca10(PO4)6(OH)2) is the main chemical constituent of bone tissue (~70%) as well as HA which is a calcium phosphate based ceramic material forms inorganic tissue of bone and tooth as hard tissues is used in production of prosthesis for synthetic bone, fractured and broken bone restoration, coating of metallic biomaterials and dental applications because of its bio compatibility. It is known that Hydroxyapatite decomposes with high heat energy after heat treatment. Therefore hydroxyapatite powders that heated in water vapor will less decomposed phases and lower amorphous phase content than in air atmosphere. In this study high purity hydroxyapatite powders were heat treated with open atmosphere furnace and water vapor atmosphere with 900, 1000, 1200 °C. Morphology of same powder size used in this process by SEM analyzed. Chemical structures of synthesized coatings have been examined by XRD. The determination of particle size and morphological structure of has been characterized by Particle Sizer, and SEM analysis, respectively. Weight change of sample was recorded by thermogravimetric analysis (TGA) during heating and cooling.

Improved cell viability and hydroxyapatite growth on nitrogen ion-implanted surfaces

NASA Astrophysics Data System (ADS)

Shafique, Muhammad Ahsan; Murtaza, G.; Saadat, Shahzad; Uddin, Muhammad K. H.; Ahmad, Riaz

2017-08-01

Stainless steel 306 is implanted with various doses of nitrogen ions using a 2 MV pelletron accelerator for the improvement of its surface biomedical properties. Raman spectroscopy reveals incubation of hydroxyapatite (HA) on all the samples and it is found that the growth of incubated HA is greater in higher ion dose samples. SEM profiles depict uniform growth and greater spread of HA with higher ion implantation. Human oral fibroblast response is also found consistent with Raman spectroscopy and SEM results; the cell viability is found maximum in samples treated with the highest (more than 300%) dose. XRD profiles signified greater peak intensity of HA with ion implantation; a contact angle study revealed hydrophilic behavior of all the samples but the treated samples were found to be lesser hydrophilic compared to the control samples. Nitrogen implantation yields greater bioactivity, improved surface affinity for HA incubation and improved hardness of the surface.

Size controlled hydroxyapatite and calcium carbonate particles: synthesis and their application as templates for SERS platform.

PubMed

Parakhonskiy, B V; Svenskaya, Yu I; Yashchenok, A М; Fattah, H A; Inozemtseva, O A; Tessarolo, F; Antolini, R; Gorin, D A

2014-06-01

An elegant route for hydroxyapatite (HA) particle synthesis via ionic exchange reaction is reported. Calcium carbonate particles (CaCO3) were recrystallized into HA beads in water solution with phosphate ions. The size of initial CaCO3 particles was controlled upon the synthesis by varying the amount of ethylene glycol (EG) in aqueous solution. The average size of HA beads ranged from 0.6±0.1 to 4.3±1.1μm. Silver nanoparticles were deposited on the surface of HA and CaCO3 particles via silver mirror reaction. Surface enhanced Raman scattering of silver functionalized beads was demonstrated by detecting Rhodamine B. CaCO3 and HA particles have a great potential for design of carrier which can provide diagnostic and therapeutic functions. Copyright © 2014 Elsevier B.V. All rights reserved.

Melt spinning of poly(lactic acid) and hydroxyapatite composite fibers: influence of the filler content on the fiber properties.

PubMed

Persson, Maria; Lorite, Gabriela S; Cho, Sung-Woo; Tuukkanen, Juha; Skrifvars, Mikael

2013-08-14

Composite fibers from poly(lactic acid) (PLA) and hydroxyapatite (HA) particles were prepared using melt spinning. Different loading concentrations of HA particles (i.e., 5, 10, 15, and 20 wt %) in the PLA fibers and solid-state draw ratios (SSDRs) were evaluated in order to investigate their influence on the fibers' morphology and thermal and mechanical properties. A scanning electron microscopy investigation indicated that the HA particles were homogeneously distributed in the PLA fibers. It was also revealed by atomic force microscopy and Fourier transform infrared spectroscopy that HA particles were located on the fiber surface, which is of importance for their intended application in biomedical textiles. Our results also suggest that the mechanical properties were independent of the loading concentration of the HA particles and that the SSDR played an important role in improving the mechanical properties of the composite fibers.

Preparation, characterization, and in vitro osteoblast functions of a nano-hydroxyapatite/polyetheretherketone biocomposite as orthopedic implant material

PubMed Central

Ma, Rui; Tang, Songchao; Tan, Honglue; Lin, Wentao; Wang, Yugang; Wei, Jie; Zhao, Liming; Tang, Tingting

2014-01-01

A bioactive composite was prepared by incorporating 40 wt% nano-hydroxyapatite (nHA) into polyetheretherketone (PEEK) through a process of compounding, injection, and molding. The mechanical and surface properties of the nHA/PEEK composite were characterized, and the in vitro osteoblast functions in the composite were investigated. The mechanical properties (elastic modulus and compressive strength) of the nHA/PEEK composite increased significantly, while the tensile strength decreased slightly as compared with PEEK. Further, the addition of nHA into PEEK increased the surface roughness and hydrophilicity of the nHA/PEEK composite. In cell tests, compared with PEEK and ultra-high-molecular-weight polyethylene, it was found that the nHA/PEEK composite could promote the functions of MC3T3-E1 cells, including cell attachment, spreading, proliferation, alkaline phosphatase activity, calcium nodule formation, and expression of osteogenic differentiation-related genes. Incorporation of nHA into PEEK greatly improved the bioperformance of PEEK. The nHA/PEEK composite might be a promising orthopedic implant material. PMID:25170265

Synthesis, characterization and modelling of zinc and silicate co-substituted hydroxyapatite

PubMed Central

Friederichs, Robert J.; Chappell, Helen F.; Shepherd, David V.; Best, Serena M.

2015-01-01

Experimental chemistry and atomic modelling studies were performed here to investigate a novel ionic co-substitution in hydroxyapatite (HA). Zinc, silicate co-substituted HA (ZnSiHA) remained phase pure after heating to 1100°C with Zn and Si amounts of 0.6 wt% and 1.2 wt%, respectively. Unique lattice expansions in ZnSiHA, silicate Fourier transform infrared peaks and changes to the hydroxyl IR stretching region suggested Zn and silicate co-substitution in ZnSiHA. Zn and silicate insertion into HA was modelled using density functional theory (DFT). Different scenarios were considered where Zn substituted for different calcium sites or at a 2b site along the c-axis, which was suspected in singly substituted ZnHA. The most energetically favourable site in ZnSiHA was Zn positioned at a previously unreported interstitial site just off the c-axis near a silicate tetrahedron sitting on a phosphate site. A combination of experimental chemistry and DFT modelling provided insight into these complex co-substituted calcium phosphates that could find biomedical application as a synthetic bone mineral substitute. PMID:26040597

Antifungal activity of Ag:hydroxyapatite thin films synthesized by pulsed laser deposition on Ti and Ti modified by TiO2 nanotubes substrates

NASA Astrophysics Data System (ADS)

Eraković, S.; Janković, A.; Ristoscu, C.; Duta, L.; Serban, N.; Visan, A.; Mihailescu, I. N.; Stan, G. E.; Socol, M.; Iordache, O.; Dumitrescu, I.; Luculescu, C. R.; Janaćković, Dj.; Miškovic-Stanković, V.

2014-02-01

Hydroxyapatite (HA) is a widely used biomaterial for implant thin films, largely recognized for its excellent capability to chemically bond to hard tissue inducing the osteogenesis without immune response from human tissues. Nowadays, intense research efforts are focused on development of antimicrobial HA doped thin films. In particular, HA doped with Ag (Ag:HA) is expected to inhibit the attachment of microbes and contamination of metallic implant surface. We herewith report on nano-sized HA and Ag:HA thin films synthesized by pulsed laser deposition on pure Ti and Ti modified with 100 nm diameter TiO2 nanotubes (fabricated by anodization of Ti plates) substrates. The HA-based thin films were characterized by SEM, AFM, EDS, FTIR, and XRD. The cytotoxic activity was tested with HEp2 cells against controls. The antifungal efficiency of the deposited layers was tested against the Candida albicans and Aspergillus niger strains. The Ti substrates modified with TiO2 nanotubes covered with Ag:HA thin films showed the highest antifungal activity.

Interfacial characteristics and determination of cohesive and adhesive strength of plasma-coated hydroxyapatite via nanoindentation and microscratch techniques.

PubMed

McManamon, Colm; de Silva, Johann P; Power, John; Ramirez-Garcia, Sonia; Morris, Michael A; Cross, Graham L W

2014-09-30

We investigate the chemical composition and mechanical properties of plasma-deposited hydroxyapatite on grit-blasted Ti-6Al-4V coupons as models of typical prosthetic hip implants. Nanoindentation is used to extract the mechanical properties of the hydroxyapatite (HA) coating and to evaluate the behavior of the material as a function of distance from the interface. A microscratch technique was used to determine parameters of cohesive and adhesive failure of the material that are critical in determining the functionality of these biomedical devices. This delamination method has not been studied in detail before and is usually considered to be unsuitable because of the thickness of the HA and the roughness of the substrate. However, through cross-section analysis of the scratch test, we can determine the point at which the HA delaminates from the substrate. It was concluded that spallation occurs locally, and there is no evidence of gross spallation, indicating that the coating is well adhered to the substrate.

Development of high strength hydroxyapatite for bone tissue regeneration using nanobioactive glass composites

NASA Astrophysics Data System (ADS)

Shrivastava, Pragya; Dalai, Sridhar; Sudera, Prerna; Sivam, Santosh Param; Vijayalakshmi, S.; Sharma, Pratibha

2013-02-01

With an increasing demand of biocompatible bone substitutes for the treatment of bone diseases and bone tissue regeneration, bioactive glass composites are being tested to improvise the osteoconductive as well as osteoinductive properties. Nanobioactive glass (nBG) composites, having composition of SiO2 70 mol%, CaO 26 mol % and P2O5 4 mol% were prepared by Freeze drying method using PEG-PPG-PEG co-polymer. Polymer addition improves the mechanical strength and porosity of the scaffold of nBG. Nano Bioactive glass composites upon implantation undergo specific reactions leading to the formation of crystalline hydroxyapatite (HA). This is tested in vitro using Simulated Body Fluid (SBF). This high strength hydroxyapatite (HA) layer acts as osteoconductive in cellular environment, by acting as mineral base of bones, onto which new bone cells proliferate leading to new bone formation. Strength of the nBG composites as well as HA is in the range of cortical and cancellous bone, thus proving significant for bone tissue regeneration substitutes.

FLIT-MLO and No. 2 fuel oil: Effects of aerosol applications to mallard eggs on hatchability and behavior of ducklings

USGS Publications Warehouse

Albers, P.H.; Heinz, G.H.

1983-01-01

FLIT-MLO and No. 2 fuel oil are sprayed on wetlands for mosquito control during spring and summer. In one experiment to assess the effects of the spraying on birds, mallard eggs were sprayed with amounts of No. 2 fuel oil equivalent to 2.34, 4.67, or 18.70 liters/ha or FLIT-MLO equivalent to 9.35, 46.75, or 140.25 liters/ha on Day 6 of incubation. In a second experiment, mallard eggs were sprayed with 9.35, 46.75, or 140.25 liters/ha of FLIT-MLO on Days 3, 6, 12, or 18 of incubation. Hatchability of eggs sprayed with the highest treatment level of each substance was significantly lower than that of controls for the first experiment. Hatchability of eggs sprayed with FLIT-MLO in the second experiment was never significantly lower than that of controls. Ducklings from the first experiment, 36-48 hr old, were cold stressed for 1 hr at 8 degrees C and then immediately tested for their ability to respond to a fright stimulus. Ducklings from the group of eggs sprayed with 140.25 liters/ha of FLIT-MLO ran a significantly shorter distance from the fright stimulus than did controls. The effects of the heaviest exposure to FLIT-MLO (140.25 liters/ha) on egg hatchability and behavior of newly hatched young are uncertain because of the contradictory results for hatching success in the two experiments. However, normal applications of FLIT-MLO (9.35-46.75 liters/ha) or No. 2 fuel oil (2.34-4.67 liters/ha) do not appear to pose a threat to the embryos of breeding birds.

Evaluation of thermal stress in hydroxyapatite film fabricated by powder jet deposition.

PubMed

Akatsuka, Ryo; Matsumura, Ken; Noji, Miyoko; Kuriyagawa, Tsunemoto; Sasaki, Keiichi

2013-10-01

This study aimed to create a thick hydroxyapatite (HA) film on the surface of a human tooth via a powder jet deposition (PJD) device for dental handpieces, and to examine the microstructural and mechanical properties of the HA film. In particular, the effects of thermal stress on this film were evaluated. The HA film was created by blasting 3.18-μm HA particles, calcinated at 1,200°C, onto the enamel substrate at room temperature and atmospheric pressure. An HA film with an area of 3 mm × 3 mm was prepared and polished. The following HA film parameters were evaluated from the three-dimensional surface profile: surface roughness, Vickers hardness, and bonding strength before and after artificial aging induced by 500 cycles of thermal cycling (5-55°C). The HA particles in the deposited film were densely packed, and the surface of the HA film was unchanged after thermal cycling. There were also no significant differences in the hardness and the bonding strength of the HA film before and after thermal cycling. The HA film created in this study demonstrated excellent microstructural and mechanical properties, even after the application of thermal stress. © 2013 Eur J Oral Sci.

Structural characterization of nanocrystalline hydroxyapatite and adhesion of pre-osteoblast cells

NASA Astrophysics Data System (ADS)

Zhu, Xiaolong; Eibl, Oliver; Berthold, Christoph; Scheideler, Lutz; Geis-Gerstorfer, Jürgen

2006-06-01

Nanocrystalline hydroxyapatite (Nano HA), a prototype of minerals of bones and teeth, attracts increasing interest in medicine and dentistry. Different parameters for synthesis and post-treatment were investigated to determine their effects on crystallinity of nano HA, and in vitro cell responses to nano HA were studied. XRD and TEM analyses indicate that the crystallinity of nano HA synthesized by a chemical method was within the range of 15-50 nm, which is adapted to natural minerals of hard tissues. Increasing the ageing temperature significantly increased the crystallinity of nano HA, while lengthening the ageing time or varying the post-ageing drying process did not have any influence on its crystallinity. Nano HA annealed between 300 and 900 °C showed a small increase in crystallinity with increasing annealing temperature due to the long-range ordering effect. Cell attachment and spreading on nano HA were lower than those on pure titanium, and decreased as the crystallinity of nano HA increased. However, cells on nano HA demonstrated well-developed filopodia and lamelliopodia, which facilitate migration of the cells on it. This may benefit osteogenesis at the interface between bone and nano HA in vivo.

Microstructural characteristics and biocompatibility of a Type-B carbonated hydroxyapatite coating deposited on NiTi shape memory alloy.

PubMed

Chu, Chenglin; Hu, T; Yin, L H; Pu, Y P; Dong, Y S; Lin, P H; Chung, C Y; Yeung, K W K; Chu, P K

2009-01-01

Microstructural characteristics and biocompatibility of a Type-B carbonated hydroxyapatite (HA) coating prepared on NiTi SMA by biomimetic deposition were characterized using XRD, SEM, XPS, FTIR and in vitro studies including hemolysis test, MTT cytotoxicity test and fibroblasts cytocompatibility test. It is found CO(3)(2-) groups were present as substitution of PO(4)(3-) anions in HA crystal lattice due to Type-B carbonate. The growth of Type-B carbonated HA coating in SBF containing HCO(3)(-) ions is stable during all periods of biomimetic deposition. The carbonated HA coating has better blood compatibility than the chemically-polished NiTi SMA. There was a good cell adhesion to this HA coating surface and cell proliferation in the vicinity of the coating was better than that for the chemically-polished NiTi SMA. Thus biomimetic deposition of this carbonated HA coating is a promising way to improve the biocompatibility of NiTi SMA for implant applications.

Osteoconductive hydroxyapatite coated PEEK for spinal fusion surgery

NASA Astrophysics Data System (ADS)

Hahn, Byung-Dong; Park, Dong-Soo; Choi, Jong-Jin; Ryu, Jungho; Yoon, Woon-Ha; Choi, Joon-Hwan; Kim, Jong-Woo; Ahn, Cheol-Woo; Kim, Hyoun-Ee; Yoon, Byung-Ho; Jung, In-Kwon

2013-10-01

Polyetheretherketone (PEEK) has attracted much interest as biomaterial for interbody fusion cages due to its similar stiffness to bone and good radio-transparency for post-op visualization. Hydroxyapatite (HA) coating stimulates bone growth to the medical implant. The objective of this work is to make an implant consisting of biocompatible PEEK with an osteoconductive HA surface for spinal or orthopedic applications. Highly dense and well-adhered HA coating was developed on medical-grade PEEK using aerosol deposition (AD) without thermal degradation of the PEEK. The HA coating had a dense microstructure with no cracks or pores, and showed good adhesion to PEEK at adhesion strengths above 14.3 MPa. The crystallinity of the HA coating was remarkably enhanced by hydrothermal annealing as post-deposition heat-treatment. In addition, in vitro and in vivo biocompatibility of PEEK, in terms of cell adhesion morphology, cell proliferation, differentiation, and bone-to-implant contact ratio, were remarkably enhanced by the HA coating through AD.

Rapid Obtaining of Nano-Hydroxyapatite Bioactive Films on NiTi Shape Memory Alloy by Electrodeposition Process

NASA Astrophysics Data System (ADS)

Lobo, A. O.; Otubo, J.; Matsushima, J. T.; Corat, E. J.

2011-07-01

Nano-hydroxyapatite (n-HA) crystalline films have been developed in this study by electrodeposition method on NiTi shape memory alloy (SMA). The electrodeposition of the n-HA films was carried out using 0.042 mol/L Ca(NO3)2 · 4H2O + 0.025 mol/L (NH4) · 2HPO4 electrolytes by applying a constant potential of -2.0 V for 120 min and keeping the solution temperature at 70 °C. The characterization of n-HA films is of special importance since bioactive properties related to n-HA have been directly identified with its specific composition and crystalline structure. AFM, XRD, EDX, FEG-SEM and Raman spectroscopy shows a homogeneous film, with high crystallinity, special composition, and bioactivity properties (Ca/P = 1.93) of n-HA on NiTi SMA surfaces. The n-HA coating with special structure would benefit the use of NiTi alloy in orthopedic applications.

Micro-/Nano- sized hydroxyapatite directs differentiation of rat bone marrow derived mesenchymal stem cells towards an osteoblast lineage

NASA Astrophysics Data System (ADS)

Huang, Yan; Zhou, Gang; Zheng, Lisha; Liu, Haifeng; Niu, Xufeng; Fan, Yubo

2012-03-01

Regenerative medicine consisting of cells and materials provides a new way for the repair and regeneration of tissues and organs. Nano-biomaterials are highlighted due to their advantageous features compared with conventional micro-materials. The aim of this study is to investigate the effects of micro-/nano- sized hydroxyapatite (μ/n-HA) on the osteogenic differentiation of rat bone marrow derived mesenchymal stem cells (rBMSCs). μ/n-HA were prepared by a microwave synthesizer and precipitation method, respectively. Different sizes of μ/n-HA were characterized by IR, XRD, SEM, TEM and co-cultured with rBMSCs. It was shown that rBMSCs expressed higher levels of osteoblast-related markers by n-HA than μ-HA stimulation. The size of HA is an important factor for affecting the osteogenic differentiation of rBMSCs. This provides a new avenue for mechanistic studies of stem cell differentiation and a new approach to obtain more committed differentiated cells.

Synthesis and characterization of bovine femur bone hydroxyapatite containing silver nanoparticles for the biomedical applications

NASA Astrophysics Data System (ADS)

Nirmala, R.; Sheikh, Faheem A.; Kanjwal, Muzafar A.; Lee, John Hwa; Park, Soo-Jin; Navamathavan, R.; Kim, Hak Yong

2011-05-01

Bovine femur bone hydroxyapatite (HA) containing silver (Ag) nanoparticles was synthesized by thermal decomposition method and subsequent reduction of silver nitrate with N, N-dimethylformamide (DMF) in the presence of poly(vinylacetate) (PVAc). The structural, morphological, and chemical properties of the HA-Ag nanoparticles were characterized using X-ray diffraction (XRD), scanning electron microscopy (SEM), field-emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), and X-ray photoelectron spectroscopy (XPS). TEM images showed that the Ag nanoparticles with size ranging from 8 to 20 nm and were arranged at the periphery of HA crystals. Bactericidal activity of HA-Ag with different concentration of Ag nanoparticles immobilized on the surface of HA was investigated against gram-positive Staphylococcus aureus ( S. aureus, non-MRSA), Methicillin resistant S. aureus (MRSA) and gram-negative Escherichia coli ( E. coli) by the disc diffusion susceptibility test. The HA-Ag nanoparticles showed that broad spectrum activity against non-MRSA, MRSA, and E. coli bacterial strains.

Thermal Diffusivity in Bone and Hydroxyapatite

NASA Astrophysics Data System (ADS)

Calderón, A.; Peña Rodríguez, G.; Muñoz Hernández, R. A.; Díaz Gongora, J. A. I.; Mejia Barradas, C. M.

2004-09-01

We report thermal diffusivity measurements in bull bone and commercial hydroxyapatite (HA), both in powder form, in order to determinate the thermal compatibility between these materials. Besides this, we report a comparison between these measured values and those of metallic samples frequently used in implants, as high purity titanium and stainless steel. Our results show a good thermal compatibility (74%) between HA and bone, both in powder form. Finally, it was obtained a one order of magnitude difference between the thermal diffusivity values of metallic samples and those corresponding values to bone and HA being this difference greater in titanium than in stainless steel, which is important to consider in some biomedical and dental applications.

Review of ferroelectric hydroxyapatite and its application to biomedicine

NASA Astrophysics Data System (ADS)

Lang, Sidney B.

2016-08-01

Hydroxyapatite (HA) is a major component of bone in humans and animals. Until about 10 years ago, it was considered to have a centrosymmetric crystal structure and could not contribute to the well-known piezoelectric effect in bone. This review describes the theoretical and experimental studies that showed that HA does have a non-centrosymmetric structure. Recent experiments have shown that HA exhibits piezoelectricity, pyroelectricity, and ferroelectricity. It has been made in the form of thick films and as space-charge electrets. It has an important biomedical application as an implant for bone cell attachment and growth. This paper is contributed in honor of the 80th birthday of my long-time friend and colleague, Bozena Hilczer.

Sol-gel derived fluor-hydroxyapatite biocoatings on zirconia substrate.

PubMed

Kim, Hae-Won; Kong, Young-Min; Bae, Chang-Jun; Noh, Yoon-Jung; Kim, Hyoun-Ee

2004-07-01

Fluor-hydroxyapatite (FHA) film was coated on a zirconia (ZrO(2)) substrate by a sol-gel method. An appropriate amount of F ions was incorporated into the hydroxyapatite (HA) during the preparation of the sols. The apatite phase began to crystallize after heat treatment at 400 degrees C, and increased in intensity above 500 degrees C. No decomposition was detected by X-ray diffraction analyses up to 800 degrees C, which illustrates the high thermal stability of the FHA films. The films showed a uniform and dense morphology with a thickness of approximately 1 microm after a precisely controlled heat treatment process. These FHA films adhered firmly to the zirconia substrate, representing notable adhesion strengths of approximately 70 MPa after heat treatment above 500 degrees C. The dissolution rate of the FHA coating layer varied according to the heat treatment temperature, which was closely related to the film crystallinity. The dissolution rate of the FHA film was lower than that of the HA film, suggesting the possibility of a functional gradient coating of HA and FHA. The MG63 cells seeded onto the FHA films proliferated in a similar manner to those seeded onto pure HA ceramic and a plastic control.

Hydroxyapatite formation from cuttlefish bones: kinetics.

PubMed

Ivankovic, H; Tkalcec, E; Orlic, S; Ferrer, G Gallego; Schauperl, Z

2010-10-01

Highly porous hydroxyapatite (Ca(10)(PO(4))(6)·(OH)(2), HA) was prepared through hydrothermal transformation of aragonitic cuttlefish bones (Sepia officinalis L. Adriatic Sea) in the temperature range from 140 to 220°C for 20 min to 48 h. The phase composition of converted hydroxyapatite was examined by quantitative X-ray diffraction (XRD) using Rietveld structure refinement and Fourier transform infrared spectroscopy (FTIR). Johnson-Mehl-Avrami (JMA) approach was used to follow the kinetics and mechanism of transformation. Diffusion controlled one dimensional growth of HA, predominantly along the a-axis, could be defined. FTIR spectroscopy determined B-type substitutions of CO(3) (2-) groups. The morphology and microstructure of converted HA was examined by scanning electron microscopy. The general architecture of cuttlefish bones was preserved after hydrothermal treatment and the cuttlefish bones retained its form with the same channel size (~80 × 300 μm). The formation of dandelion-like HA spheres with diameter from 3 to 8 μm were observed on the surface of lamellae, which further transformed into various radially oriented nanoplates and nanorods with an average diameter of about 200-300 nm and an average length of about 8-10 μm.

The electrolysis time on electrosynthesis of hydroxyapatite with bipolar membrane

NASA Astrophysics Data System (ADS)

Nur, Adrian; Jumari, Arif; Budiman, Anatta Wahyu; Puspitaningtyas, Stella Febianti; Cahyaningrum, Suci; Nazriati, Nazriati; Fajaroh, Fauziatul

2018-02-01

The electrochemical method with bipolar membrane has been successfully used for the synthesis of hydroxyapatite. In this work, we have developed 2 chambers electrolysis system separated by a bipolar membrane. The membrane was used to separate cations (H+ ions produced by the oxidation of water at the anode) and anions (OH- ions produced by the reduction of water at the cathode). With this system, we have designed that OH- ions still stay in the anions chamber because OH- ions was very substantial in the hydroxyapatite particles formation. The aim of this paper was to compare the electrolysis time on electrosynthesis of hydroxyapatite with and without the bipolar membrane. The electrosynthesis was performed at 500 mA/cm2 for 0.5 to 2 hours at room temperature and under ultrasonic cleaner to void agglomeration with and without the bipolar membrane. The electrosynthesis of hydroxyapatite with the bipolar membrane more effective than without the bipolar membrane. The hydroxyapatite has been appeared at 0.5 h of the electrolysis time with the bipolar membrane (at the cathode chamber) while it hasn't been seen without the bipolar membrane. The bipolar membrane prevents OH- ions migrate to the cation chamber. The formation of HA becomes more effective because OH- ions just formed HA particle.

Novel Development of Phosphate Treated Porous Hydroxyapatite.

PubMed

Doi, Kazuya; Abe, Yasuhiko; Kobatake, Reiko; Okazaki, Yohei; Oki, Yoshifumi; Naito, Yoshihito; Prananingrum, Widyasri; Tsuga, Kazuhiro

2017-12-08

Phosphoric acid-etching treatment to the hydroxyapatite (HA) surface can modify the solubility calcium structure. The aim of the present study was to develop phosphate treated porous HA, and the characteristic structures and stimulation abilities of bone formation were evaluated to determine its suitability as a new type of bone graft material. Although the phosphoric acid-etching treatment did not alter the three-dimensional structure, a micrometer-scale rough surface topography was created on the porous HA surface. Compared to porous HA, the porosity of phosphate treated porous HA was slightly higher and the mechanical strength was lower. Two weeks after placement of the cylindrical porous or phosphate treated porous HA in a rabbit femur, newly formed bone was detected in both groups. At the central portion of the bone defect area, substantial bone formation was detected in the phosphate treated porous HA group, with a significantly higher bone formation ratio than detected in the porous HA group. These results indicate that phosphate treated porous HA has a superior surface topography and bone formation abilities in vivo owing to the capacity for both osteoconduction and stimulation abilities of bone formation conferred by phosphoric acid etching.

Novel Development of Phosphate Treated Porous Hydroxyapatite

PubMed Central

Doi, Kazuya; Abe, Yasuhiko; Kobatake, Reiko; Okazaki, Yohei; Oki, Yoshifumi; Naito, Yoshihito; Prananingrum, Widyasri; Tsuga, Kazuhiro

2017-01-01

Phosphoric acid-etching treatment to the hydroxyapatite (HA) surface can modify the solubility calcium structure. The aim of the present study was to develop phosphate treated porous HA, and the characteristic structures and stimulation abilities of bone formation were evaluated to determine its suitability as a new type of bone graft material. Although the phosphoric acid-etching treatment did not alter the three-dimensional structure, a micrometer-scale rough surface topography was created on the porous HA surface. Compared to porous HA, the porosity of phosphate treated porous HA was slightly higher and the mechanical strength was lower. Two weeks after placement of the cylindrical porous or phosphate treated porous HA in a rabbit femur, newly formed bone was detected in both groups. At the central portion of the bone defect area, substantial bone formation was detected in the phosphate treated porous HA group, with a significantly higher bone formation ratio than detected in the porous HA group. These results indicate that phosphate treated porous HA has a superior surface topography and bone formation abilities in vivo owing to the capacity for both osteoconduction and stimulation abilities of bone formation conferred by phosphoric acid etching. PMID:29292788

Production of Poly(ε-Caprolactone)/Hydroxyapatite Composite Scaffolds with a Tailored Macro/Micro-Porous Structure, High Mechanical Properties, and Excellent Bioactivity

PubMed Central

Kim, Jong-Woo; Shin, Kwan-Ha; Koh, Young-Hag; Hah, Min Jin; Moon, Jiyoung; Kim, Hyoun-Ee

2017-01-01

We produced poro-us poly(ε-caprolactone) (PCL)/hydroxyapatite (HA) composite scaffolds for bone regeneration, which can have a tailored macro/micro-porous structure with high mechanical properties and excellent in vitro bioactivity using non-solvent-induced phase separation (NIPS)-based 3D plotting. This innovative 3D plotting technique can create highly microporous PCL/HA composite filaments by inducing unique phase separation in PCL/HA solutions through the non-solvent-solvent exchange phenomenon. The PCL/HA composite scaffolds produced with various HA contents (0 wt %, 10 wt %, 15 wt %, and 20 wt %) showed that PCL/HA composite struts with highly microporous structures were well constructed in a controlled periodic pattern. Similar levels of overall porosity (~78 vol %) and pore size (~248 µm) were observed for all the PCL/HA composite scaffolds, which would be highly beneficial to bone tissue regeneration. Mechanical properties, such as ultimate tensile strength and compressive yield strength, increased with an increase in HA content. In addition, incorporating bioactive HA particles into the PCL polymer led to remarkable enhancements in in vitro apatite-forming ability. PMID:28937605

Hydroxyapatite coatings produced on commercially pure titanium by micro-arc oxidation.

PubMed

Huang, Yong; Wang, Yingjun; Ning, Chengyun; Nan, Kaihui; Han, Yong

2007-09-01

A porous hydroxyapatite (HA) coating on commercially pure titanium was prepared by micro-arc oxidation (MAO) in electrolytic solution containing calcium acetate and beta-glycerol phosphate disodium salt pentahydrate (beta-GP). The thickness, phase, composition morphology and biocompatibility of the oxide coating were characterized by x-ray diffraction (XRD), electron probe microanalysis (EPMA), scanning electron microscopy (SEM) with an energy dispersive x-ray spectrometer (EDS) and cell culture. The thickness of the MAO film was about 20 microm, and the coating was porous and uneven without any apparent interface to the titanium substrates. The result of XRD showed that the porous coating was made up of HA film. The favorable osteoblast cell affinity gives HA film good biocompatibility. HA coatings are expected to have significant uses for medical applications such as dental implants and artificial bone joints.

Anisotropic growth of hydroxyapatite on the silk fibroin films

NASA Astrophysics Data System (ADS)

Li, Yucheng; Cai, Yurong; Kong, Xiangdong; Yao, Juming

2008-12-01

Bombyx mori silk fibroin is of practical interest for its excellent intrinsic properties utilizable in the biotechnological and biomedical fields. Here, the silk fibroin films were pretreated with different methods and then used as the template for the hydroxyapatite (HA) crystal growth. To study the effect of silk films' surface structure on the protein biomineralization, the films were immersed into 1.5 times simulated body fluid (1.5 × SBF) to induce the HA deposition at 37 °C. The results showed that an anisotropic growth of HA crystals was observed on the different films as judging from XRD, TEM and HRTEM data. This was thought that the positions and density of carboxyl groups, C dbnd O and amino groups on the surface of SF films may be different, which play the key effect on HA crystal growth.

Rapid Mix Preparation of Bioinspired Nanoscale Hydroxyapatite for Biomedical Applications

PubMed Central

Wilcock, Caroline J.; Gentile, Piergiorgio; Hatton, Paul V.; Miller, Cheryl A.

2017-01-01

Hydroxyapatite (HA) has been widely used as a medical ceramic due to its good biocompatibility and osteoconductivity. Recently there has been interest regarding the use of bioinspired nanoscale hydroxyapatite (nHA). However, biological apatite is known to be calcium-deficient and carbonate-substituted with a nanoscale platelet-like morphology. Bioinspired nHA has the potential to stimulate optimal bone tissue regeneration due to its similarity to bone and tooth enamel mineral. Many of the methods currently used to fabricate nHA both in the laboratory and commercially, involve lengthy processes and complex equipment. Therefore, the aim of this study was to develop a rapid and reliable method to prepare high quality bioinspired nHA. The rapid mixing method developed was based upon an acid-base reaction involving calcium hydroxide and phosphoric acid. Briefly, a phosphoric acid solution was poured into a calcium hydroxide solution followed by stirring, washing and drying stages. Part of the batch was sintered at 1,000 °C for 2 h in order to investigate the products' high temperature stability. X-ray diffraction analysis showed the successful formation of HA, which showed thermal decomposition to β-tricalcium phosphate after high temperature processing, which is typical for calcium-deficient HA. Fourier transform infrared spectroscopy showed the presence of carbonate groups in the precipitated product. The nHA particles had a low aspect ratio with approximate dimensions of 50 x 30 nm, close to the dimensions of biological apatite. The material was also calcium deficient with a Ca:P molar ratio of 1.63, which like biological apatite is lower than the stoichiometric HA ratio of 1.67. This new method is therefore a reliable and far more convenient process for the manufacture of bioinspired nHA, overcoming the need for lengthy titrations and complex equipment. The resulting bioinspired HA product is suitable for use in a wide variety of medical and consumer health applications. PMID:28287572

Rapid Mix Preparation of Bioinspired Nanoscale Hydroxyapatite for Biomedical Applications.

PubMed

Wilcock, Caroline J; Gentile, Piergiorgio; Hatton, Paul V; Miller, Cheryl A

2017-02-23

Hydroxyapatite (HA) has been widely used as a medical ceramic due to its good biocompatibility and osteoconductivity. Recently there has been interest regarding the use of bioinspired nanoscale hydroxyapatite (nHA). However, biological apatite is known to be calcium-deficient and carbonate-substituted with a nanoscale platelet-like morphology. Bioinspired nHA has the potential to stimulate optimal bone tissue regeneration due to its similarity to bone and tooth enamel mineral. Many of the methods currently used to fabricate nHA both in the laboratory and commercially, involve lengthy processes and complex equipment. Therefore, the aim of this study was to develop a rapid and reliable method to prepare high quality bioinspired nHA. The rapid mixing method developed was based upon an acid-base reaction involving calcium hydroxide and phosphoric acid. Briefly, a phosphoric acid solution was poured into a calcium hydroxide solution followed by stirring, washing and drying stages. Part of the batch was sintered at 1,000 °C for 2 h in order to investigate the products' high temperature stability. X-ray diffraction analysis showed the successful formation of HA, which showed thermal decomposition to β-tricalcium phosphate after high temperature processing, which is typical for calcium-deficient HA. Fourier transform infrared spectroscopy showed the presence of carbonate groups in the precipitated product. The nHA particles had a low aspect ratio with approximate dimensions of 50 x 30 nm, close to the dimensions of biological apatite. The material was also calcium deficient with a Ca:P molar ratio of 1.63, which like biological apatite is lower than the stoichiometric HA ratio of 1.67. This new method is therefore a reliable and far more convenient process for the manufacture of bioinspired nHA, overcoming the need for lengthy titrations and complex equipment. The resulting bioinspired HA product is suitable for use in a wide variety of medical and consumer health applications.

Enhanced Photocatalytic Activity of TiO2 Nanoparticles Supported on Electrically Polarized Hydroxyapatite.

PubMed

Zhang, Xuefei; Yates, Matthew Z

2018-05-23

Fast recombination of photogenerated charge carriers in titanium dioxide (TiO 2 ) remains a challenging issue, limiting the photocatalytic activity. This study demonstrates increased photocatalytic performance of TiO 2 nanoparticles supported on electrically polarized hydroxyapatite (HA) films. Dense and thermally stable yttrium and fluorine co-doped HA films with giant internal polarization were synthesized as photocatalyst supports. TiO 2 nanoparticles deposited on the support were then used to catalyze the photochemical reduction of aqueous silver ions to produce silver nanoparticles. It was found that significantly more silver nanoparticles were produced on polarized HA supports than on depolarized HA supports. In addition, the photodegradation of methyl orange with TiO 2 nanoparticles on polarized HA supports was found to be much faster than with TiO 2 nanoparticles on depolarized HA supports. It is proposed that separation of photogenerated electrons and holes in TiO nanoparticles is promoted by the internal polarization of the HA support, and consequently, the recombination of charge carriers is mitigated. The results imply that materials with large internal polarization can be used in strategies for enhancing quantum efficiency of photocatalysts.

Development of electrophoretically deposited hydroxyapatite coatings on anodized nanotubular TiO2 structures: Corrosion and sintering temperature

NASA Astrophysics Data System (ADS)

Goudarzi, Mona; Batmanghelich, Farhad; Afshar, Abdollah; Dolati, Abolghasem; Mortazavi, Golsa

2014-05-01

Hydroxyapatite (HA) coatings in and onto anodized TiO2 nanotube arrays were presented and prepared by electrophoretic deposition technique (EPD). Coatings were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM). EPD proved to be an innovative and versatile technique to coat HA on and into nanotubular structures of TiO2 with enhanced adhesion between nanotubes and HA particles provided by mechanical interlocking. After EPD of HA on TiO2 layer, samples were sintered at 400 °C, 600 °C and 800 °C for 2 h in an Ar atmosphere. Effect of EPD processing parameters on thickness of the deposits and rate of deposition was elucidated for HA coatings on the nanotubular TiO2 structures. It was shown that higher applied voltages increase deposition rate and thickness of the coatings. Potentiodynamic polarization measurements proved corrosion protection caused by both HA coating and nanotubular TiO2 structure in simulated body fluid (SBF). Effect of sintering temperature on adhesion strength of HA coatings on TiO2 nanotubes and their composition were also studied.

Reinforced Pulsed Laser-Deposited Hydroxyapatite Coating on 316 Stainless Steel

NASA Astrophysics Data System (ADS)

Bajpai, Shubhra; Gupta, Ankur; Pradhan, Siddhartha Kumar; Mandal, Tapendu; Balani, Kantesh

2014-10-01

Hydroxyapatite (HA) is a widely used bioceramic known for its chemical similarity with that of bone and teeth (Ca/P ratio of 1.67). But, owing to its extreme brittleness, α-Al2O3 is reinforced with HA and processed as a coating via pulsed laser deposition (PLD). Reinforcement of α-Al2O3 (50 wt.%) in HA via PLD on 316L steel substrate has shown modulus increase by 4% and hardness increase by 78%, and an improved adhesion strength of 14.2 N (improvement by 118%). Micro-scratching has shown an increase in the coefficient-of-friction from 0.05 (pure HA) to 0.17 (with 50 wt.% Al2O3) with enhancement in the crack propagation resistance (CPR) up to 4.5 times. Strong adherence of PLD HA-Al2O3 coatings (~4.5 times than that of HA coating) is attributed to efficient release of stored tensile strain energy (~17 × 10-3 J/m2) in HA-Al2O3 composites, making it a potential damage-tolerant bone-replacement surface coating.

The usability of ark clam shell (Anadara granosa) as calcium precursor to produce hydroxyapatite nanoparticle via wet chemical precipitate method in various sintering temperature.

PubMed

Khiri, Mohammad Zulhasif Ahmad; Matori, Khamirul Amin; Zainuddin, Norhazlin; Abdullah, Che Azurahanim Che; Alassan, Zarifah Nadakkavil; Baharuddin, Nur Fadilah; Zaid, Mohd Hafiz Mohd

2016-01-01

This paper reported the uses of ark clam shell calcium precursor in order to form hydroxyapatite (HA) via the wet chemical precipitation method. The main objective of this research is to acquire better understanding regarding the effect of sintering temperature in the fabrication of HA. Throughout experiment, the ratio of Ca:P were constantly controlled, between 1.67 and 2.00. The formation of HA at these ratio was confirmed by means of energy-dispersive X-ray spectroscopy analysis. In addition, the effect of sintering temperature on the formation of HA was observed using X-ray diffraction analysis, while the structural and morphology was determined by means of field emission scanning electron microscopy. The formation of HA nanoparticle was recorded (~35-69 nm) in the form of as-synthesize HA powder. The bonding compound appeared in the formation of HA was carried out using Fourier transform infrared spectroscopy such as biomaterials that are expected to find potential applications in orthopedic and biomedical industries .

Mechanical, Rheological, and Bioactivity Properties of Ultra High-Molecular-Weight Polyethylene Bioactive Composites Containing Polyethylene Glycol and Hydroxyapatite

PubMed Central

Ahmad, Mazatusziha; Wahit, Mat Uzir; Abdul Kadir, Mohammed Rafiq; Mohd Dahlan, Khairul Zaman

2012-01-01

Ultrahigh-molecular-weight polyethylene/high-density polyethylene (UHMWPE/HDPE) blends prepared using polyethylene glycol PEG as the processing aid and hydroxyapatite (HA) as the reinforcing filler were found to be highly processable using conventional melt blending technique. It was demonstrated that PEG reduced the melt viscosity of UHMWPE/HDPE blend significantly, thus improving the extrudability. The mechanical and bioactive properties were improved with incorporation of HA. Inclusion of HA from 10 to 50 phr resulted in a progressive increase in flexural strength and modulus of the composites. The strength increment is due to the improvement on surface contact between the irregular shape of HA and polymer matrix by formation of mechanical interlock. The HA particles were homogenously distributed even at higher percentage showed improvement in wetting ability between the polymer matrix and HA. The inclusion of HA enhanced the bioactivity properties of the composite by the formation of calcium phosphate (Ca-P) precipitates on the composite surface as proven from SEM and XRD analysis. PMID:22666129

Preparation of micro-porous bioceramic containing silicon-substituted hydroxyapatite and beta-tricalcium phosphate.

PubMed

Fuh, Lih-Jyh; Huang, Ya-Jing; Chen, Wen-Cheng; Lin, Dan-Jae

2017-06-01

Dimensional instability caused by sintering shrinkage is an inevitable drawback for conventional processing of hydroxyapatite (HA). A new preparation method for biphasic calcium phosphates was developed to increase micro pores and biodegradation without significant dimensional change. Powder pressed HA discs, under 100MPa, were immersed in a colloidal mixture of tetraethoxysilane (TEOS) and ammonium hydroxide for 10min, followed by drying, and then were sintered at 900°C, 1050°C, and 1200°C, respectively. Comparing with pure HA discs, the newly prepared product sintered up to 1200°C contained silicon substituted HA, beta-tricalcium phosphate, and calcium silicate with better micro-porosity, high specific surface area, less sintering shrinkage and the strength maintained. The cytocompatibility test demonstrated a better viability for D1 mice stem cells cultured on TEOS treated HA for 14days compared to the pure HA. This simple TEOS sol-gel pretreatment has the potential to be applied to any existing manufacturing process of HA scaffold for better control of sintering shrinkage, create micropores, and increase biodegradation. Copyright © 2017 Elsevier B.V. All rights reserved.

In vitro investigation of nanohydroxyapatite/poly(L-lactic acid) spindle composites used for bone tissue engineering.

PubMed

Yan, W; Zhang, C Y; Xia, L L; Zhang, T; Fang, Q F

2016-08-01

Calcium phosphate ceramics such as synthetic hydroxyapatite and tricalcium phosphate are widely used in the clinic, but they stimulate less bone regeneration. In this paper, nano-hydroxyapatite/poly(L-lactic acid) (nano-HA/PLLA) spindle composites with good mechanical performance were fabricated by a modified in situ precipitation method. The HA part of composite, distributing homogenously in PLLA matrix, is spindle shape with size of 10-30 nm in diameter and 60-100 nm in length. The molar ratio of Ca/P in the synthesized nano-HA spindles was deduced as 1.52 from the EDS spectra, which is close to the stoichiometric composition of HA (Ca/P & 1.67). The compress strength is up to 150 MPa when the HA content increase to 20 %. The in vitro tests indicate that HA/PLLA bio-composites have good biodegradability and bioactivity when immersed in simulated body fluid solutions. All the results suggested that HA/PLLA nano-biocomposites are appropriate to be applied as bone substitute in bone tissue engineering.

Hierarchically nanostructured hydroxyapatite: hydrothermal synthesis, morphology control, growth mechanism, and biological activity

PubMed Central

Ma, Ming-Guo

2012-01-01

Hierarchically nanosized hydroxyapatite (HA) with flower-like structure assembled from nanosheets consisting of nanorod building blocks was successfully synthesized by using CaCl2, NaH2PO4, and potassium sodium tartrate via a hydrothermal method at 200°C for 24 hours. The effects of heating time and heating temperature on the products were investigated. As a chelating ligand and template molecule, the potassium sodium tartrate plays a key role in the formation of hierarchically nanostructured HA. On the basis of experimental results, a possible mechanism based on soft-template and self-assembly was proposed for the formation and growth of the hierarchically nanostructured HA. Cytotoxicity experiments indicated that the hierarchically nanostructured HA had good biocompatibility. It was shown by in-vitro experiments that mesenchymal stem cells could attach to the hierarchically nanostructured HA after being cultured for 48 hours. Objective The purpose of this study was to develop facile and effective methods for the synthesis of novel hydroxyapatite (HA) with hierarchical nanostructures assembled from independent and discrete nanobuilding blocks. Methods A simple hydrothermal approach was applied to synthesize HA by using CaCl2, NaH2PO4, and potassium sodium tartrate at 200°C for 24 hours. The cell cytotoxicity of the hierarchically nanostructured HA was tested by MTT (3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide) assay. Results HA displayed the flower-like structure assembled from nanosheets consisting of nanorod building blocks. The potassium sodium tartrate was used as a chelating ligand, inducing the formation and self-assembly of HA nanorods. The heating time and heating temperature influenced the aggregation and morphology of HA. The cell viability did not decrease with the increasing concentration of hierarchically nanostructured HA added. Conclusion A novel, simple and reliable hydrothermal route had been developed for the synthesis of hierarchically nanosized HA with flower-like structure assembled from nanosheets consisting of nanorod building blocks. The HA with the hierarchical nanostructure was formed via a soft-template assisted self-assembly mechanism. The hierarchically nanostructured HA has a good biocompatibility and essentially no in-vitro cytotoxicity. PMID:22619527

Pyroelectric, piezoelectric, and photoeffects in hydroxyapatite thin films on silicon

NASA Astrophysics Data System (ADS)

Lang, S. B.; Tofail, S. A. M.; Gandhi, A. A.; Gregor, M.; Wolf-Brandstetter, C.; Kost, J.; Bauer, S.; Krause, M.

2011-03-01

Hydroxyapatite (HA) is the major component of bone and is used in artificial form in many biomedical applications. It was once believed to have a centrosymmetric crystal structure. In theoretical and experimental studies published in 2005, it was shown to have a monoclinic P21 structure. In the work reported here, 500 nm films of HA were spin-coated on silicon wafers. The materials were not poled. They had a nonuniform polarization distribution and exhibited pyroelectricity, piezoelectricity, and photoeffects. Structures of this type may have a number of technological applications.

Chlorhexidine-loaded hydroxyapatite microspheres as an antimicrobial delivery system and its effect on in vivo osteo-conductive properties.

PubMed

Soriano-Souza, Carlos Alberto; Rossi, Andre L; Mavropoulos, Elena; Hausen, Moema A; Tanaka, Marcelo N; Calasans-Maia, Mônica D; Granjeiro, Jose M; Rocha-Leão, Maria Helena M; Rossi, Alexandre M

2015-04-01

Hydroxyapatite (HA) has been investigated as a delivery system for antimicrobial and antibacterial agents to simultaneously stimulate bone regeneration and prevent infection. Despite evidence supporting the bactericidal efficiency of these HA carriers, few studies have focused on the effect of this association on bone regeneration. In this work, we evaluated the physico-chemical properties of hydroxyapatite microspheres loaded with chlorhexidine (CHX) at two different concentrations, 0.9 and 9.1 μgCHX/cm2 HA, and characterized their effects on in vitro osteoblast viability and bone regeneration. Ultraviolet-visible spectroscopy, scanning and transmission electron microscopy associated with energy-dispersive X-ray spectroscopy and electron energy loss spectroscopy were used to characterize the association of CHX and HA nanoparticles. The high CHX loading dose induced formation of organic CHX plate-like aggregates on the HA surface, whereas a Langmuir film was formed at the low CHX surface concentration. Quantitative evaluation of murine osteoblast viability parameters, including adhesion, mitochondrial activity and membrane integrity of cells exposed to HA/CHX extracts, revealed a cytotoxic effect for both loading concentrations. Histomorphological analysis upon implantation into the dorsal connective tissues and calvaria of rats for 7 and 42 days showed that the high CHX concentration induced the infiltration of inflammatory cells, resulting in retarded bone growth. Despite a strong decrease in in vitro cell viability, the low CHX loading dose did not impair the biocompatibility and osteoconductivity of HA during bone repair. These results indicate that high antimicrobial doses may activate a strong local inflammatory response and disrupt the long-term osteoconductive properties of CHX-HA delivery systems.

Characterization of Nano-Hydroxyapatite Synthesized from Sea Shells Through Wet Chemical Method

NASA Astrophysics Data System (ADS)

Santhosh, S.; Prabu, S. Balasivanandha

2012-10-01

Nano-hydroxyapatite (HA) was synthesized by a wet chemical reaction using powdered sea shells (CaO) as starting material which was converted to calcium hydroxide (Ca(OH)2) and subsequently reacted with phosphoric acid (H3PO4). Initially raw sea shells (CaCO3) were thermally converted to amorphous calcium oxide by heat treatment. Two sets of experiments were done; in the first experiment, HA powder was dried in an electric furnace and in the second experiment, the reactants were irradiated in a domestic microwave oven followed by microwave drying. In each set of experiments, the concentrations of the reactants were decreased gradually. HA was synthesized by slow addition of phosphoric acid (H3PO4) in to calcium hydroxide (Ca(OH)2) maintaining the pH of the solution at 10 to avoid the formation of calcium deficient apatites. In both the experiments, Ca:P ratio of 1.67 was maintained for the reagents. The synthesized samples showed X-ray diffraction (XRD) patterns corresponding to hydroxyapatite. The wet chemical process with furnace drying resulted in HA particles of size 7-34 nm, whereas microwave irradiated process yielded HA particles of size 34-102 nm as evidenced from XRD analyses. The above experimental work done by wet chemical synthesis to produce HA powder from sea shells is a simple processing method at room temperature. Microwave irradiation leads to uniform crystallite sizes as evident from this study, at differing concentrations of the reactants and is a comparatively easy method to synthesize HA. The high resolution scanning electron microscopy (HRSEM)/transmission electron microscopic (TEM) analyses revealed the characteristic rod-shaped nanoparticles of HA for the present study.

The thermal stability of hydroxyapatite in biphasic calcium phosphate ceramics.

PubMed

Nilen, R W N; Richter, P W

2008-04-01

Biphasic calcium phosphate ceramics (BCP) comprising a mix of non-resorbable hydroxyapatite (HA) and resorbable beta-tricalcium phosphate (beta-TCP) are particularly suitable materials for synthetic bone substitute applications. In this study, HA synthesised by solid state reaction was mechanically mixed with beta-TCP, then sintered to form a suite of BCP materials with a wide range of HA/beta-TCP phase content ratios. The influence of sintering temperature and composition on the HA thermal stability was quantified by X-ray diffraction (XRD). The pre-sinter beta-TCP content was found to strongly affect the post-sinter HA/beta-TCP ratio by promoting the thermal decomposition of HA to beta-TCP, even at sintering temperatures as low as 850 degrees C. For BCP material with pre-sinter HA/beta-TCP = 40/60 wt%, approximately 80% of the HA decomposed to beta-TCP during sintering at 1000 degrees C. Furthermore, the HA content appeared to influence the reverse transformation of alpha-TCP to beta-TCP expected upon gradual cooling from sintering temperatures greater than 1125 degrees C. Because the HA/beta-TCP ratio dominantly determines the rate and extent of BCP resorption in vivo, the possible thermal decomposition of HA during BCP synthesis must be considered, particularly if high temperature treatments are involved.

Nano-hydroxyapatite/chitosan-starch nanocomposite as a novel bone construct: Synthesis and in vitro studies.

PubMed

Shakir, Mohammad; Jolly, Reshma; Khan, Mohd Shoeb; Iram, Noor e; Khan, Haris M

2015-09-01

A novel ternary nanocomposite system incorporating hydroxyapatite, chitosan and starch (n-HA/CS-ST) has been synthesized by co-precipitation method at room temperature, addressing the issues of biocompatibility, mechanical strength and cytotoxicity required for bone tissue engineering. The interactions, crystallite size, surface morphology and thermal stability against n-HA/CS nanocomposite have been obtained by comparing the results of FTIR, SEM, TEM, DLS, XRD and TGA/DTA. A comparative study of bioactivity and thermal stability of n-HA/CS and n-HA/CS-ST nanocomposites revealed that the incorporation of starch as templating agent enhanced these properties in n-HA/CS-ST nanocomposite. A lower swelling rate of n-HA/CS-ST relative to n-HA/CS indicates a higher mechanical strength supportive of bone tissue ingrowths. The MTT assay on murine fibroblast L929 and human osteoblasts-like MG-63 cells and in vitro bioactivity of n-HA/CS-ST matrix referred superior non-toxic nature of n-HA/CS-ST nanocomposite and greater possibility of osteointegration in vivo respectively. Furthermore n-HA/CS-ST exhibited improved antibacterial property against both Gram-positive and Gram-negative bacteria relative to n-HA/CS. Copyright © 2015. Published by Elsevier B.V.

Bone tissue engineering with a collagen–hydroxyapatite scaffold and culture expanded bone marrow stromal cells

PubMed Central

Villa, Max M.; Wang, Liping; Huang, Jianping; Rowe, David W.; Wei, Mei

2015-01-01

Osteoprogenitor cells combined with supportive biomaterials represent a promising approach to advance the standard of care for bone grafting procedures. However, this approach faces challenges, including inconsistent bone formation, cell survival in the implant, and appropriate biomaterial degradation. We have developed a collagen–hydroxyapatite (HA) scaffold that supports consistent osteogenesis by donor derived osteoprogenitors, and is more easily degraded than a pure ceramic scaffold. Herein, the material properties are characterized as well as cell attachment, viability, and progenitor distribution in vitro. Furthermore, we examined the biological performance in vivo in a critical-size mouse calvarial defect. To aid in the evaluation of the in-house collagen–HA scaffold, the in vivo performance was compared with a commercial collagen–HA scaffold (Healos®, Depuy). The in-house collagen–HA scaffold supported consistent bone formation by predominantly donor-derived osteoblasts, nearly completely filling a 3.5 mm calvarial defect with bone in all samples (n=5) after 3 weeks of implantation. In terms of bone formation and donor cell retention at 3 weeks postimplantation, no statistical difference was found between the in-house and commercial scaffold following quantitative histomorphometry. The collagen–HA scaffold presented here is an open and well-defined platform that supports robust bone formation and should facilitate the further development of collagen–hydroxyapatite biomaterials for bone tissue engineering. PMID:24909953

Fabrication and mechanical evaluation of hydroxyapatite/oxide nano-composite materials.

PubMed

Mohamed, Khaled R; Beherei, Hanan H; El Bassyouni, Gehan T; El Mahallawy, Nahed

2013-10-01

In the current study, the semiconducting metal oxides such as nano-ZnO and SiO2 powders were prepared via sol-gel technique and conducted on nano-hydroxyapatite (nHA) which was synthesized by chemical precipitation. The properties of fabricated nano-structured composites containing different ratios of HA, ZnO and SiO2 were examined using X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy, scanning electron microscope (SEM) and transmission electron microscope (TEM) techniques. The effect of the variation of ratios between the three components on mechanical, microstructure and in-vitro properties was assessed to explore the possibility of enhancing these properties. The results proved that the mechanical properties exhibited an increment with increasing the ZnO content at the extent of HA. In-vitro study proved the formation and nucleation of apatite onto the surface of the fabricated composites after one week of immersion. It is concluded that HA composites containing SiO2 or SiO2/ZnO content had a suitable mechanical properties and ability to form apatite particles onto the composite surface. Based on bioactivity behavior, Si-HA is more bioactive than pure hydroxyapatite and nano-arrangements will provide an interface for better bone formation. Therefore, these nano-composites will be promising as bone substitutes especially in load bearing sites. Copyright © 2013 Elsevier B.V. All rights reserved.

Field evaluation of a botanical formulation from the milky mangrove Excoecaria agallocha L. against Helicoverpa armigera Hübner. in Abelmoschus esculentus (lady's finger) and Cajanus cajan (pigeon pea).

PubMed

Santhanam, Satyan Ramachandran; Egigu, Meseret C

2014-09-01

To evaluate a formulation from the milky mangrove tree Excoecaria agallocha L. (E. agallocha) against Helicoverpa armigera Hubner (H. armigera). About 3% aqueous ethanolic spray formulation derived from the lipophilic extract of E. agallocha (dry leaf) was evaluated against H. armigera in Abelmoschus esculentus (lady's finger) and Cajanus cajan (C. cajan) (pigeon pea), under field conditions. On the 9th day of the 4th spray the larval count in the plot treated with 3% E. agallocha formulation drastically came down to 0.23 larva/plant, compared to 1.63 in the ethanol control plot and 1.60 in the unsprayed plot. Blocks sprayed with 3% E. agallocha formulation yielded 35.8 quintals/hectare (q/ha) of healthy pods compared to Ekalux® (pod yield: 60.7 q/ha), 3% Vijay Neem® (60.22 q/ha), yield plot (6 q/ha) and ethanol control (7 q/ha). In C. cajan, 1% E. agallocha, 3% Nimbecidine® and 0.07% indoxacarb were equally potent in reducing the larval population of H. armigera and the non-target pest Spilosoma obliqua to 0%, from the 9th day (3rd spray). Indoxacarb plot recorded the maximum yield of 16.1 q/ha with 2.4% pod damage. Plots sprayed with 1% E. agallocha yielded 14.7 q/ha with 2.32% pod damage. The effect of 3% Nimbecidine® spray (14.35 q/ha) was comparable to E. agallocha formulation. Unsprayed and ethanol control plots yielded 12.41 and 11.2 q/ha of pods with an average pod damage of 4.7%. E. agallocha formulation was found to be promising for the control of H. armigera, under field conditions. Copyright © 2014 Hainan Medical College. Published by Elsevier B.V. All rights reserved.

Hydroxyapatite/poly(epsilon-caprolactone) composite coatings on hydroxyapatite porous bone scaffold for drug delivery.

PubMed

Kim, Hae-Won; Knowles, Jonathan C; Kim, Hyoun-Ee

2004-01-01

Hydroxyapatite (HA) porous scaffold was coated with HA and polycaprolactone (PCL) composites, and antibiotic drug tetracycline hydrochloride was entrapped within the coating layer. The HA scaffold obtained by a polymeric reticulate method, possessed high porosity ( approximately 87%) and controlled pore size (150-200 microm). Such a well-developed porous structure facilitated usage in a drug delivery system due to its high surface area and blood circulation efficiency. The PCL polymer, as a coating component, was used to improve the brittleness and low strength of the HA scaffold, as well to effectively entrap the drug. To improve the osteoconductivity and bioactivity of the coating layer, HA powder was hybridized with PCL solution to make the HA-PCL composite coating. With alteration in the coating concentration and HA/PCL ratio, the morphology, mechanical properties, and biodegradation behavior were investigated. Increasing the concentration rendered the stems thicker and some pores to be clogged; as well increasing the HA/PCL ratio made the coating surface be rough due to the large amount of HA particles. However, for all concentrations and compositions, uniform coatings were formed, i.e., with the HA particles being dispersed homogeneously in the PCL sheet. With the composite coating, the mechanical properties, such as compressive strength and elastic modulus were improved by several orders of magnitude. These improvements were more significant with thicker coatings, while little difference was observed with the HA/PCL ratio. The in vitro biodegradation of the composite coatings in the phosphate buffered saline solution increased linearly with incubation time and the rate differed with the coating concentration and the HA/PCL ratio; the higher concentration and HA amount caused the increased biodegradation. At short period (<2 h), about 20-30% drug was released especially due to free drug at the coating surface. However, the release rate was sustained for prolonged periods and was highly dependent on the degree of coating dissolution, suggesting the possibility of a controlled drug release in the porous scaffold with HA+PCL coating.

Comparing Two Antibacterial Treatments for Bioceramic Coatings at Short Culture Times

NASA Astrophysics Data System (ADS)

Melero, H.; Madrid, C.; Fernández, J.; Guilemany, J. M.

2014-04-01

Plasma-sprayed hydroxyapatite coatings were employed industrially for decades to improve osteointegration of articular implants, but many studies have warned about the problems inherent to this procedure (mechanical properties, harmful phases). Consequently, a combination of hydroxyapatite with TiO2 sprayed by high velocity oxy-fuel spray was considered in this study. As infection after joint replacement surgery is one of the most critical concerns when considering implant performance, it is necessary to study possible ways to reduce or eliminate it. Two coating treatments were chosen for this study: addition of a percentage of ZnO and immersion in gentamicin for 24 h. Furthermore, three bacteria were considered: Escherichia coli, Pseudomonas aeruginosa, and Staphylococcus aureus. The evolution of bacteria viability in solution was measured at 0, 2, and 4 h; and plate assays were performed to study antibacterial effects by diffusion. The results show an important antibacterial effect of the as-sprayed coating, attributed to the presence of -OH radicals on the surface. The presence of ZnO did not have any additional influence on bacteria viability, but gentamicin-treated samples showed an improvement in antibacterial behavior for Gram-negative bacteria in solution, as well as a bactericidal effect in diffusion conditions.

Peptide Probe for Crystalline Hydroxyapatite: In Situ Detection of Biomineralization

NASA Astrophysics Data System (ADS)

Cicerone, Marcus; Becker, Matthew; Simon, Carl; Chatterjee, Kaushik

2009-03-01

While cells template mineralization in vitro and in vivo, specific detection strategies that impart chemical and structural information on this process have proven elusive. Recently we have developed an in situ based peptide probe via phage display methods that is specific to crystalline hydroxyapatite (HA). We are using this in fluorescence based assays to characterize mineralization. One application being explored is the screening of tissue engineering scaffolds for their ability to support osteogenesis. Specifically, osteoblasts are being cultured in hydrogel scaffolds possessing property gradients to provide a test bed for the HA peptide probe. Hydrogel properties that support osteogenesis and HA deposition will be identified using the probe to demonstrate its utility in optimizing design of tissue scaffolds.

Magnetic apatite for structural insights on the plasma membrane

NASA Astrophysics Data System (ADS)

Stanca, Sarmiza E.; Müller, Robert; Dellith, Jan; Nietzsche, Sandor; Stöckel, Stephan; Biskup, Christoph; Deckert, Volker; Krafft, Christoph; Popp, Jürgen; Fritzsche, Wolfgang

2015-01-01

The iron oxide-hydroxyapatite (FeOxHA) nanoparticles reported here differ from those reported before by their advantage of homogeneity and simple preparation; moreover, the presence of carboxymethyldextran (CMD), together with hydroxyapatite (HA), allows access to the cellular membrane, which makes our magnetic apatite unique. These nanoparticles combine magnetic behavior, Raman label ability and the property of interaction with the cellular membrane; they therefore represent an interesting material for structural differentiation of the cell membrane. It was observed by Raman spectroscopy, scanning electron microscopy (SEM) and fluorescence microscopy that FeOxHA adheres to the plasma membrane and does not penetrate the membrane. These insights make the nanoparticles a promising material for magnetic cell sorting, e.g. in microfluidic device applications.

Surface phenomena of hydroxyapatite film on the nanopore formed Ti-29Nb-xZr alloy by anodization for bioimplants.

PubMed

Kim, Eun-Ju; Jeong, Yong-Hoon; Choe, Han-Cheol

2013-03-01

In this study, surface phenomena of hydroxyapatite (HA) film on the nanopore formed Ti-29Nb-xZr alloy by anodization for bioimplants have been investigated by electron beam physical vapor deposition (EB-PVD), field emission scanning electron microscope (FE-SEM), X-ray diffractometer (XRD), potentiostat and contact angle. The microstructure of Ti-29Nb-xZr alloys exhibited equiaxed structure and alpha" phase decreased, whereas beta phase increased as Zr content increased. The increment of Zr contents in HA coated nanotubular Ti-29Nb-xZr alloys showed good corrosion potential in 0.9% NaCI solution. The wettability of HA coated nanotubular surface was higher than that of non-coated samples.

Magnetic apatite for structural insights on the plasma membrane.

PubMed

Stanca, Sarmiza E; Müller, Robert; Dellith, Jan; Nietzsche, Sandor; Stöckel, Stephan; Biskup, Christoph; Deckert, Volker; Krafft, Christoph; Popp, Jürgen; Fritzsche, Wolfgang

2015-01-21

The iron oxide-hydroxyapatite (FeOxHA) nanoparticles reported here differ from those reported before by their advantage of homogeneity and simple preparation; moreover, the presence of carboxymethyldextran (CMD), together with hydroxyapatite (HA), allows access to the cellular membrane, which makes our magnetic apatite unique. These nanoparticles combine magnetic behavior, Raman label ability and the property of interaction with the cellular membrane; they therefore represent an interesting material for structural differentiation of the cell membrane. It was observed by Raman spectroscopy, scanning electron microscopy (SEM) and fluorescence microscopy that FeOxHA adheres to the plasma membrane and does not penetrate the membrane. These insights make the nanoparticles a promising material for magnetic cell sorting, e.g. in microfluidic device applications.

Matched Comparison of Fusion Rates between Hydroxyapatite Demineralized Bone Matrix and Autograft in Lumbar Interbody Fusion.

PubMed

Kim, Dae Hwan; Lee, Nam; Shin, Dong Ah; Yi, Seong; Kim, Keung Nyun; Ha, Yoon

2016-07-01

To compare the fusion rate of a hydroxyapatite demineralized bone matrix (DBM) with post-laminectomy acquired autograft in lumbar interbody fusion surgery and to evaluate the correlation between fusion rate and clinical outcome. From January 2013 to April 2014, 98 patients underwent lumbar interbody fusion surgery with hydroxyapatite DBM (HA-DBM group) in our institute. Of those patients, 65 received complete CT scans for 12 months postoperatively in order to evaluate fusion status. For comparison with autograft, we selected another 65 patients who underwent lumbar interbody fusion surgery with post-laminectomy acquired autograft (Autograft group) during the same period. Both fusion material groups were matched in terms of age, sex, body mass index (BMI), and bone mineral density (BMD). To evaluate the clinical outcomes, we analyzed the results of visual analogue scale (VAS), Oswestry Disability Index (ODI), and Short Form Health Survey (SF-36). We reviewed the CT scans of 149 fusion levels in 130 patients (HA-DBM group, 75 levels/65 patients; Autograft group, 74 levels/65 patients). Age, sex, BMI, and BMD were not significantly different between the groups (p=0.528, p=0.848, p=0.527, and p=0.610, respectively). The HA-DBM group showed 39 of 75 fused levels (52%), and the Autograft group showed 46 of 74 fused levels (62.2%). This difference was not statistically significant (p=0.21). In the HA-DBM group, older age and low BMD were significantly associated with non-fusion (61.24 vs. 66.68, p=0.027; -1.63 vs. -2.29, p=0.015, respectively). VAS and ODI showed significant improvement after surgery when fusion was successfully achieved in both groups (p=0.004, p=0.002, HA-DBM group; p=0.012, p=0.03, Autograft group). The fusion rates of the hydroxyapatite DBM and Autograft groups were not significantly different. In addition, clinical outcomes were similar between the groups. However, older age and low BMD are risk factors that might induce non-union after surgery with hydroxyapatite DBM.

Matched Comparison of Fusion Rates between Hydroxyapatite Demineralized Bone Matrix and Autograft in Lumbar Interbody Fusion

PubMed Central

Kim, Dae Hwan; Lee, Nam; Shin, Dong Ah; Yi, Seong; Kim, Keung Nyun

2016-01-01

Objective To compare the fusion rate of a hydroxyapatite demineralized bone matrix (DBM) with post-laminectomy acquired autograft in lumbar interbody fusion surgery and to evaluate the correlation between fusion rate and clinical outcome. Methods From January 2013 to April 2014, 98 patients underwent lumbar interbody fusion surgery with hydroxyapatite DBM (HA-DBM group) in our institute. Of those patients, 65 received complete CT scans for 12 months postoperatively in order to evaluate fusion status. For comparison with autograft, we selected another 65 patients who underwent lumbar interbody fusion surgery with post-laminectomy acquired autograft (Autograft group) during the same period. Both fusion material groups were matched in terms of age, sex, body mass index (BMI), and bone mineral density (BMD). To evaluate the clinical outcomes, we analyzed the results of visual analogue scale (VAS), Oswestry Disability Index (ODI), and Short Form Health Survey (SF-36). Results We reviewed the CT scans of 149 fusion levels in 130 patients (HA-DBM group, 75 levels/65 patients; Autograft group, 74 levels/65 patients). Age, sex, BMI, and BMD were not significantly different between the groups (p=0.528, p=0.848, p=0.527, and p=0.610, respectively). The HA-DBM group showed 39 of 75 fused levels (52%), and the Autograft group showed 46 of 74 fused levels (62.2%). This difference was not statistically significant (p=0.21). In the HA-DBM group, older age and low BMD were significantly associated with non-fusion (61.24 vs. 66.68, p=0.027; -1.63 vs. -2.29, p=0.015, respectively). VAS and ODI showed significant improvement after surgery when fusion was successfully achieved in both groups (p=0.004, p=0.002, HA-DBM group; p=0.012, p=0.03, Autograft group). Conclusion The fusion rates of the hydroxyapatite DBM and Autograft groups were not significantly different. In addition, clinical outcomes were similar between the groups. However, older age and low BMD are risk factors that might induce non-union after surgery with hydroxyapatite DBM. PMID:27446517

Employing the cyclophosphate to accelerate the degradation of nano-hydroxyapatite/poly(amino acid) (n-HA/PAA) composite materials.

PubMed

Jing, Linjing; Chen, Li; Peng, Haitao; Ji, Mizhi; Xiong, Yi; Lv, Guoyu

2017-12-01

Owing to the good degradability and biocompatibility of polyphosphoesters (PPEs), the aim of the current study was to investigate a novel degradable composite of nano-hydroxyapatite/poly(amino acid) (n-HA/PAA) with cyclophosphate (CPE) via in situ melting polymerization to improve the degradation of n-HA/PAA. The structure of each composite was characterized via Fourier transform infrared spectroscopy, X-ray diffraction, and X-ray photoelectron spectroscopy. The degradation properties were studied in terms of the weight loss and pH in a phosphate-buffered saline (PBS) solution, while the surface morphology was examined using a scanning electron microscope-energy dispersive spectrometer (SEM-EDS) after soaking the surface in simulated body fluid (SBF). The cell proliferation, cell adhesion, and alkaline phosphatase (ALP) activity were used for the analysis of cytocompatibility. The weight loss results showed that the n-HA/PAA composite was 9.98 wt%, weighed after soaking in the PBS solution for 12 weeks, whereas the nano-hydroxyapatite/polyphosphoester-amino acid (n-HA/PPE-AA) composite was 46.94 wt%. The pH of the composites was in a suitable range between 6.64 to 7.06 and finally stabilized at 7.39. The SEM and EDS results revealed the formation of an apatite-like layer on the surface of the n-HA/PPE-AA composites after soaking in SBF for one week. The cell counting Kit 8 (CCK-8) assay of the cell culture in the leaching liquid of the n-HA/PPE-AA composites exhibited non-cytotoxicity and high-proliferation, and the cell adhesion showed the well spreading and normal phenotype extension of the cells on the n-HA/PPE-AA composites surface. Concurrently, the co-culture results of the composites and cells confirmed that the n-HA/PPE-AA composites exhibited a higher ALP activity. In summary, the results demonstrated that the n-HA/PPE-AA composites had a controllable degradation property, good bioactivity, and cytocompatibility.

On the use of superparamagnetic hydroxyapatite nanoparticles as an agent for magnetic and nuclear in vivo imaging.

PubMed

Adamiano, Alessio; Iafisco, Michele; Sandri, Monica; Basini, Martina; Arosio, Paolo; Canu, Tamara; Sitia, Giovanni; Esposito, Antonio; Iannotti, Vincenzo; Ausanio, Giovanni; Fragogeorgi, Eirini; Rouchota, Maritina; Loudos, George; Lascialfari, Alessandro; Tampieri, Anna

2018-06-01

The identification of alternative biocompatible magnetic NPs for advanced clinical application is becoming an important need due to raising concerns about iron accumulation in soft issues associated to the administration of superparamagnetic iron oxide nanoparticles (NPs). Here, we report on the performance of previously synthetized iron-doped hydroxyapatite (FeHA) NPs as contrast agent for magnetic resonance imaging (MRI). The MRI contrast abilities of FeHA and Endorem® (dextran coated iron oxide NPs) were assessed by 1 H nuclear magnetic resonance relaxometry and their performance in healthy mice was monitored by a 7 Tesla scanner. FeHA applied a higher contrast enhancement, and had a longer endurance in the liver with respect to Endorem® at iron equality. Additionally, a proof of concept of FeHA use as scintigraphy imaging agent for positron emission tomography (PET) and single photon emission computed tomography (SPECT) was given labeling FeHA with 99m Tc-MDP by a straightforward surface functionalization process. Scintigraphy/x-ray fused imaging and ex vivo studies confirmed its dominant accumulation in the liver, and secondarily in other organs of the mononuclear phagocyte system. FeHA efficiency as MRI-T 2 and PET-SPECT imaging agent combined to its already reported intrinsic biocompatibility qualifies it as a promising material for innovative nanomedical applications. The ability of iron-doped hydroxyapatite nanoaprticles (FeHA) to work in vivo as imaging agents for magnetic resonance (MR) and nuclear imaging is demonstrated. FeHA applied an higher MR contrast in the liver, spleen and kidneys of mice with respect to Endorem®. The successful radiolabeling of FeHA allowed for scintigraphy/X-ray and ex vivo biodistribution studies, confirming MR results and envisioning FeHA application for dual-imaging. Copyright © 2018 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Modulating protein adsorption onto hydroxyapatite particles using different amino acid treatments

PubMed Central

Lee, Wing-Hin; Loo, Ching-Yee; Van, Kim Linh; Zavgorodniy, Alexander V.; Rohanizadeh, Ramin

2012-01-01

Hydroxyapatite (HA) is a material of choice for bone grafts owing to its chemical and structural similarities to the mineral phase of hard tissues. The combination of osteogenic proteins with HA materials that carry and deliver the proteins to the bone-defective areas will accelerate bone regeneration. The study investigated the treatment of HA particles with different amino acids such as serine (Ser), asparagine (Asn), aspartic acid (Asp) and arginine (Arg) to enhance the adsorption ability of HA carrier for delivering therapeutic proteins to the body. The crystallinity of HA reduced when amino acids were added during HA preparation. Depending on the types of amino acid, the specific surface area of the amino acid-functionalized HA particles varied from 105 to 149 m2 g–1. Bovine serum albumin (BSA) and lysozyme were used as model proteins for adsorption study. The protein adsorption onto the surface of amino acid-functionalized HA depended on the polarities of HA particles, whereby, compared with lysozyme, BSA demonstrated higher affinity towards positively charged Arg-HA. Alternatively, the binding affinity of lysozyme onto the negatively charged Asp-HA was higher when compared with BSA. The BSA and lysozyme adsorptions onto the amino acid-functionalized HA fitted better into the Freundlich than Langmuir model. The amino acid-functionalized HA particles that had higher protein adsorption demonstrated a lower protein-release rate. PMID:21957116

Synthesis, characterization and modelling of zinc and silicate co-substituted hydroxyapatite.

PubMed

Friederichs, Robert J; Chappell, Helen F; Shepherd, David V; Best, Serena M

2015-07-06

Experimental chemistry and atomic modelling studies were performed here to investigate a novel ionic co-substitution in hydroxyapatite (HA). Zinc, silicate co-substituted HA (ZnSiHA) remained phase pure after heating to 1100 °C with Zn and Si amounts of 0.6 wt% and 1.2 wt%, respectively. Unique lattice expansions in ZnSiHA, silicate Fourier transform infrared peaks and changes to the hydroxyl IR stretching region suggested Zn and silicate co-substitution in ZnSiHA. Zn and silicate insertion into HA was modelled using density functional theory (DFT). Different scenarios were considered where Zn substituted for different calcium sites or at a 2b site along the c-axis, which was suspected in singly substituted ZnHA. The most energetically favourable site in ZnSiHA was Zn positioned at a previously unreported interstitial site just off the c-axis near a silicate tetrahedron sitting on a phosphate site. A combination of experimental chemistry and DFT modelling provided insight into these complex co-substituted calcium phosphates that could find biomedical application as a synthetic bone mineral substitute. © 2015 The Author(s) Published by the Royal Society. All rights reserved.

Physical Properties and Cellular Responses to Crosslinkable Poly(Propylene Fumarate)/Hydroxyapatite Nanocomposites

PubMed Central

Lee, Kee-Won; Wang, Shanfeng; Yaszemski, Michael J.; Lu, Lichun

2008-01-01

A series of crosslinkable nanocomposites has been developed using hydroxyapatite (HA) nanoparticles and poly(propylene fumarate) (PPF). PPF/HA nanocomposites with four different weight fractions of HA nanoparticles have been characterized in terms of thermal and mechanical properties. To assess surface chemistry of crosslinked PPF/HA nanocomposites, their hydrophilicity and capability of adsorbing proteins have been determined using static contact angle measurement and MicroBCA protein assay kit after incubation with 10% fetal bovine serum (FBS), respectively. In vitro cell studies have been performed using MC3T3-E1 mouse pre-osteoblast cells to investigate the ability of PPF/HA nanocomposites to support cell attachment, spreading, and proliferation after 1, 4, and 7 days. By adding HA nanoparticles to PPF, the mechanical properties of crosslinked PPF/HA nanocomposites have not been increased due to the initially high modulus of crosslinked PPF. However, hydrophilicity and serum protein adsorption on the surface of nanocomposites have been significantly increased, resulting in enhanced cell attachment, spreading, and proliferation after 4 days of cell seeding. These results indicate that crosslinkable PPF/HA nanocomposites are useful for hard tissue replacement because of excellent mechanical strength and osteoconductivity. PMID:18403013

Strontium-doped hydroxyapatite polysaccharide materials effect on ectopic bone formation

PubMed Central

Aid-Launais, R.; Sagardoy, T.; Siadous, R.; Bareille, R.; Rey, S.; Pechev, S.; Etienne, L.; Kalisky, J.; de Mones, E.; Letourneur, D.; Amedee Vilamitjana, J.

2017-01-01

Previous studies performed using polysaccharide-based matrices supplemented with hydroxyapatite (HA) particles showed their ability to form in subcutaneous and intramuscular sites a mineralized and osteoid tissue. Our objectives are to optimize the HA content in the matrix and to test the combination of HA with strontium (Sr-HA) to increase the matrix bioactivity. First, non-doped Sr-HA powders were combined to the matrix at three different ratios and were implanted subcutaneously for 2 and 4 weeks. Interestingly, matrices showed radiolucent properties before implantation. Quantitative analysis of micro-CT data evidenced a significant increase of mineralized tissue formed ectopically with time of implantation and allowed us to select the best ratio of HA to polysaccharides of 30% (w/w). Then, two Sr-substitution of 8% and 50% were incorporated in the HA powders (8Sr-HA and 50Sr-HA). Both Sr-HA were chemically characterized and dispersed in matrices. In vitro studies performed with human mesenchymal stem cells (MSCs) demonstrated the absence of cytotoxicity of the Sr-doped matrices whatever the amount of incorporated Sr. They also supported osteoblastic differentiation and activated the expression of one late osteoblastic marker involved in the mineralization process i.e. osteopontin. In vivo, subcutaneous implantation of these Sr-doped matrices induced osteoid tissue and blood vessels formation. PMID:28910401

Effect of foliar application of micronutrients on the yield and quality of sweet orange (Citrus Sinensis L.).

PubMed

Tariq, M; Sharif, M; Shah, Z; Khan, R

2007-06-01

An experiment was designed to study the effect of foliar application of micronutrients on the yield, quality and leaf composition of sweet orange, Blood red variety at Shabazgari, Mardan. The experiment was laid out in a randomized complete block design in 2) factorial arrangement. Zinc, manganese and boron were applied as foliar spray at the rate of 0.4, 0.2 and 0.04 kg ha(-1), respectively in the presence of 1.56 kg N ha(-1) as urea and 0.4 kg surfactance ha(-1) (as wetting agent) in 400 L of water. The maximum fruit yield was obtained, when 0.4 kg Zn ha(-1) and 0.2 kg Mn ha(-1) was sprayed along with 1.56 kg N ha(-1) and 0.4 kg surfactance ha(-1) in 400 L of water. The minimum % peel was obtained with B alone and minimum % rag with Zn + Mn, maximum fruit size with Zn + B and maximum fruit volume with Zn + Mn. Similarly, % juice in sweet oranges was increased significantly by B alone, reducing sugar by Mn alone and vitamin C contents by Zn + B through foliar spray, suggested that each micronutrient had different role on the quality of citrus fruit. Foliar spray of Zn, Mn and B along with urea significantly increased the concentration of Zn and Mn in citrus leaves, while the concentration of B was not affected with foliar spray, perhaps due to dilution within the citrus tissues. Therefore, it is suggested that either Zn+Mn or Zn+B may be applied as foliar spray in combination with urea and surfactance for getting the maximum yield and improved quality of citrus fruit under prevailing conditions.

A biodegradable AZ91 magnesium alloy coated with a thin nanostructured hydroxyapatite for improving the corrosion resistance.

PubMed

Mukhametkaliyev, T M; Surmeneva, M A; Vladescu, A; Cotrut, C M; Braic, M; Dinu, M; Vranceanu, M D; Pana, I; Mueller, M; Surmenev, R A

2017-06-01

The main aim of this study was to investigate the properties of an AZ91 alloy coated with nanostructured hydroxyapatite (HA) prepared by radio frequency (RF) magnetron sputtering. The bioactivity and biomineralization of the AZ91 magnesium alloy coated with HA were investigated in simulated body fluid (SBF) via an in vitro test. Scanning electron microscopy (SEM), Fourier transform infrared (FTIR) spectroscopy, and X-ray diffraction (XRD) analyses were performed. The samples were immersed in SBF to study the ability of the surface to promote the formation of an apatite layer as well as corrosion resistance and mass change of the HA-coated AZ91 alloy. Electrochemical tests were performed to estimate the corrosion behaviour of HA-coated and uncoated samples. The results revealed the capability of the HA coating to significantly improve the corrosion resistance of the uncoated AZ91 alloy. Copyright © 2017 Elsevier B.V. All rights reserved.

Use of quartz crystal nanobalance to study the binding and stabilization of albumin and doxycycline on a thin layer of hydroxyapatite

NASA Astrophysics Data System (ADS)

Victor, Sunita Prem; Sharma, Chandra P.; Sreenivasan, K.

2011-12-01

This study reports the use of quartz crystal nanobalance (QCN) to study the adsorption of two model molecules namely albumin and doxycycline by hydroxyapatite (HA). The work focuses on the deposition of a stable coating of HA on the quartz crystal, modification of the coating using doxycycline and its subsequent effects on albumin adsorption. The uniformity and thickness of the HA coating has been studied using atomic force microscopy (AFM). The functional groups to ascertain the presence of the selected moieties have been characterized by Raman spectroscopy. The results indicate that the mass of albumin deposited on the surface of the HA coated quartz crystal functionalized with doxycycline shows a substantial increase when compared to the standard HA coated quartz crystal. The adsorbed albumin has also been found to be retained for an enhanced period of time. This surface immobilization of doxycycline and subsequent albumin adsorption seem to be a promising approach to confer biomaterials with antithrombogenic and antibacterial surfaces.

Evaluation of calcination temperature and phase composition ratio for new hyroxyapatite

NASA Astrophysics Data System (ADS)

Salimi, M. N. Ahmad; Chin, H. S.

2017-10-01

The demand of production of hydroxyapatite (HA) has been increasing for the purpose of medical and dental application. HA possesses the excellent properties leads to the priority choice for ceramic bone replacement. Synthesis route by wet chemical precipitation is commonly practised in industrial scale. Calcium hydroxide and Orthophosphoric acid are the precursors for production scale. The synthesis of HA is conducted by varying the synthetic condition: stirring rate, calcium-phosphate and calcination temperature. This paper is focused on the properties of HA produced by regulating the synthetic condition so that the qualities of HA can be well performed. Characterization studies were also carried out by Fourier Transform Infrared Spectroscopy (FT-IR) for functional group identification, Scanning Electron Microscope (SEM) for surface morphology analysis and X-Ray Diffraction (XRD) for phase composition and crystallinity respectively. Narrow particle size distribution contributed to better quality of hydroxyapatite for bone replacement. Both calcium-phosphate ratio and calcination temperature would affect the phase composition of calcium phosphate.

In vitro biomechanical and biocompatible evaluation of natural hydroxyapatite/chitosan composite for bone repair.

PubMed

Lü, Xiaoying; Zheng, Buzhong; Tang, Xiaojun; Zhao, Lifeng; Lu, Jieyan; Zhang, Zhiwei; Zhang, Jizhong; Cui, Wei

2011-01-01

To evaluate the biomechanical properties and biocompatibility of natural hydroxyapatite/chitosan (HA/CS) composites. The natural HA/CS composites with a different proportion of HA and CS were prepared by the cross-linking method, and then the compressive strength, microstructure and pH values of extracts from these composites were measured by SEM and pH meter, respectively. Subsequently, the biocompatibility of the composites was evaluated by means of a series of biological tests, including MTT, acute systemic toxicity, heat source, and hemolysis tests in vitro. The chitosan content in the composites had significantly influenced the mechanical properties and microstructure of the composites. The pH value of the composite extract was approximately 7.0, which was very close to that of human plasma. Furthermore, the natural HA/CS composites showed no cytotoxicity, irritation, teratogenicity, carcinogenicity and special pyrogen. These results indicated that the natural HA/CS composite may be a potential bone repair material.

Hydroxyapatite nanocrystals functionalized with alendronate as bioactive components for bone implant coatings to decrease osteoclastic activity

NASA Astrophysics Data System (ADS)

Bosco, Ruggero; Iafisco, Michele; Tampieri, Anna; Jansen, John A.; Leeuwenburgh, Sander C. G.; van den Beucken, Jeroen J. J. P.

2015-02-01

The integration of bone implants within native bone tissue depends on periprosthetic bone quality, which is severely decreased in osteoporotic patients. In this work, we have synthesized bone-like hydroxyapatite nanocrystals (nHA) using an acid-base neutralization reaction and analysed their physicochemical properties. Subsequently, we have functionalized the nHA with alendronate (nHAALE), a well-known bisphosphonate drug used for the treatment of osteoporosis. An in vitro osteoclastogenesis test was carried out to evaluate the effect of nHAALE on the formation of osteoclast-like cells from monocytic precursor cells (i.e. RAW264.7 cell line) showing that nHAALE significantly promoted apoptosis of osteoclast-like cells. Subsequently, nHA and nHAALE were deposited on titanium disks using electrospray deposition (ESD), for which characterisation of the deposited coatings confirmed the presence of alendronate in nHAALE coatings with nanoscale thickness of about 700 nm. These results indicate that alendronate linked to hydroxyapatite nanocrystals has therapeutic potential and nHAALE can be considered as an appealing coating constituent material for orthopaedic and oral implants for application in osteoporotic patients.

Biopolymers for Medical Applications: Polyglycerol Sebacate (PGS) doped Hydroxyapatite (HA)

NASA Astrophysics Data System (ADS)

Teruel, Maria; Kuthirummal, Narayanan; Levi, Nicole; Wake College Team

2011-04-01

In the investigation to engineer the ideal scaffolding device for cleft palate repair, polyglycerol sebacate (PGS) doped with hydroxyapatite (HA) were chosen for their elastomeric and biodegradable properties, as well as their cost-effective synthesis. Hydroxyapatite was integrated into the PGS to form a composite with high porosity and improved mechanical properties yielding a good substrate for cell attachment during the repair process. FT-IR scans were performed to characterize the composite polymer. Differential Scanning Calorimetry (DSC) was utilized to identify an acceptable glass transition temperature (Tg), between -18 and - 21°C. At this Tg, it was determined that the material was sufficiently polymerized to a point where it was durable yet pliable enough to use for cleft palate devices. In the synthesis of PGS 3% and 5% HA, a Tg of - 20.10°C and - 21.72°C, respectively, was achieved and further analytical tests were then performed on the polymers. Methods of analysis included X-Ray Diffraction and Tensile Strength Testing. Acknowledgements to the Research Department of Plastic and Reconstructive Surgery, Wake Forest University and College of Charleston.

[Histocompatibility of nano-hydroxyapatite/poly-co-glycolic acid tissue engineering bone modified by mesenchymal stem cells with vascular endothelial frowth factor].

PubMed

Zhang, Minglei; Wang, Dapeng; Yin, Ruofeng

2015-10-06

To explorec Histocompatibility of nano-hydroxyapatite/poly-co-glycolic acid tissue engineering bone modified by mesenchymal stem cells with vascular endothelial frowth factor transinfected. Rat bone marrow mesenchymal stem cells (BMSCs) was separated, using BMSCs as target cells, and then vascular endothelial growth factor (VEGF) gene was transfected. Composite bone marrow mesenchymal stem cells and cells transfected with nano-hydroxyapatite (HA)/polylactic-co-glycolic acid (PLGA). The composition of cell and scaffold was observed. The blank plasmid transfection was 39.1%, 40.1% in VEGF group. The cell adhesion and growth was found on the scaffold pore wall after 5 days, and the number of adherent cells in the nano-HA/PLGA composite scaffold material basically had no significant difference in both. Although the nano-HA/PLGA scaffold material is still not fully meet the requirements of the matrix material for bone tissue engineering, but good biocompatibility, structure is its rich microporous satisfaction in material mechanics, toughening, enhanced obviously. Composition scaffold with BMSCs transfected by VEGF plasmid, the ability of angiogenesis is promoted.

Comparison of physical characteristics and cell culture test of hydroxyapatite/collagen composite coating on NiTi SMA: electrochemical deposition and chemically biomimetic growth

NASA Astrophysics Data System (ADS)

Hu, Kai; Yang, Xianjin; Cai, Yanli; Cui, Zhenduo; Wei, Qiang

2007-07-01

A hydroxyapatite (HA)/collagen (COL) composite coating on NiTi shape memory alloy (SMA) was prepared by eletrochemical deposition (ELD) in modified simulated body fluid (MSBF). To draw comparisons of physical characteristics and bioactivity of the composite coating, the HA/COL composite coating was also prepared by chemically biomimetic growth (BG) and the ELD coating was re-soaked in MSBF again for further biomimetic growth (called EBG method in this paper). It was indicated that the c-axis of HA crystals was oriented parallel to the longitudinal direction of the COL fibril in BG and EBG coating, which could not found in ELD coating. The EBG method could induce a denser, thicker and better crystallized HA/COL coating. The cell culture test indicated that the BG coating presented better cell biocompatibility.

Comparative NEXAFS study of the selected icefish hard tissues and hydroxyapatite

NASA Astrophysics Data System (ADS)

Petrova, O. V.; Nekipelov, S. V.; Sivkov, D. V.; Mingaleva, A. E.; Nikolaev, A.; Frank-Kamenetskaya, O. V.; Bazhenov, V. V.; Vyalikh, D. V.; Molodtsov, S. L.; Sivkov, V. N.; Ehrlich, H.

2017-11-01

The structure of native Champsocephalus gunnari icefish otoliths, scales, teeth, bones and pristine hydroxyapatite (HA) were examined using Near Edge X-ray Absorption Fine Structure (NEXAFS) spectroscopy. NEXAFS Cls-absorption spectra of the selected icefish hard tissues indicate that otoliths contain anion [CO3]2-. NEXAFS P2p-spectra clearly indicate the absence of phosphorus atoms only within otoliths and scales samples. However, the icefish teeth and bones P2p-spectra demonstrate identical spectral feature typical for the HA. NEXAFS Ca2p-spectra of the icefish hard tissues studied also shows features, which are in good correspondence with HA spectra. Interestingly, there is a red shift ≈ 0.1 eV of the 2p1/2,3/2 → 3d transition energies in NEXAFS Ca2p-spectra of teethes and bones of the C. gunnari in comparison to HA.

Production of morphology-controllable porous hyaluronic acid particles using a spray-drying method.

PubMed

Iskandar, Ferry; Nandiyanto, Asep Bayu Dani; Widiyastuti, W; Young, Lee Sin; Okuyama, Kikuo; Gradon, Leon

2009-05-01

Hyaluronic acid (HA) porous particles with controllable porosity and pore size, ranging from 100 to 300 nm, were successfully prepared using a colloidal templating and spray-drying method. HA powder and polystyrene latex (PSL) particles, which were used as the precursor and templating agent, respectively, were mixed in aqueous solution and spray-dried using a two-fluid nozzle system to produce HA and PSL composite particles. Water was evaporated during spray-drying using heated air with a temperature of 120 degrees C. This simple process was completed within several seconds. The prepared particles were collected and washed with an organic solvent to dissolve the PSL templating agent. The porosity and pore size of the resulting particles were easily controlled by changing the initial mass ratio of precursor to templating agent, i.e., HA to PSL, and by altering the size of the PSL template particles.

Effect of spray volume on the deposition, viability and infectivity of entomopathogenic nematodes in a foliar spray on vegetables.

PubMed

Brusselman, Eva; Beck, Bert; Pollet, Sabien; Temmerman, Femke; Spanoghe, Pieter; Moens, Maurice; Nuyttens, David

2012-10-01

Spray volume can influence the amount of free water on the leaf surface and subsequently the ability of entomopathogenic nematodes (EPNs) to move. In this study, an investigation was made of the effect of spray volume (548, 730 and 1095 L ha(-1) ) on the deposition, viability and infectivity of EPNs against Galleria mellonella on savoy cabbage, cauliflower and leek. Increasing spray volume decreased nematode deposition on 7.1 cm2 leek leaf discs at a 15° angle with the spray nozzle. Although the number of living nematodes observed on leek after 240 min of exposure was not significantly different between the low-volume application (548 L ha(-1) ) and the high-volume application (1095 L ha(-1) ), a greater infectivity was obtained in the latter application. The higher number of droplets deposited on the leek discs in the high-volume application may have stimulated nematode movement. No significant effect of spray volume was observed on the relative deposition of Steinernema carpocapsae on the bottom side of cauliflower and savoy cabbage leaf discs. In spite of the low S. carpocapsae deposition on the bottom side of the savoy cabbage discs, high infectivity was obtained against G. mellonella. Using the lowest spray volume on savoy cabbage, infectivity decreased with increasing exposure time, while infectivity was not affected by exposure time when a spray volume of 730 L ha(-1) or more was used. Spray volume is an important application parameter, as it affects nematode infectivity. Future research should investigate the effect of spray volume in the field and its influence on the effect of adjuvants. Copyright © 2012 Society of Chemical Industry.

Coatings of needle/stripe-like fluoridated hydroxyapatite on H2O2-treated carbon/carbon composites prepared by induction heating and hydrothermal methods

NASA Astrophysics Data System (ADS)

Xiong, Xin-Bo; Huang, Jian-Feng; Zeng, Xie-Rong; Liang, Ping; Zou, Ji-Zhao

2012-06-01

A hydroxyapatite (HA) coating was achieved on H2O2-treated carbon/carbon (C/C) composite through hydrothermally treating and induction heating deposited CaHPO4 coating in an ammonia solution under ultrasonic water bath. Then, this HA coating was placed in a NH4F solution and hydrothermally treated again to fabricate fluorinated hydroxyapatite (FHA) coatings for 24 h at 353, 373, 393 and 413 K, respectively. The structure, morphology and chemical composition of the HA and FHA coatings were characterized by SEM, XRD, EDS and FTIR, and the adhesiveness and chemical stability of these FHA coatings were examined by a scratch test and an immersion test, respectively. The results showed that the as-prepared FHA coatings contained needle-like or stripe-like crystals, different from those of the HA coating. As the fluoridation temperature rose, the adhesiveness of the FHA coating first increased from 34.8 to 40.9 N at a temperature between 353 and 393 K, and then decreased to 24.2 N at 413 K, while the dissolution rate of the FHA coating decreased steadily. The reasons for the property variation of the FHA coatings were proposed by analyzing the morphology, composition and structure of the coatings.

Effect of aging temperature on formation of sol-gel derived fluor-hydroxyapatite nanoparticles.

PubMed

Joughehdoust, S; Behnamghader, A; Jahandideh, R; Manafi, S

2010-04-01

Synthetic hydroxyapatite (HA) has been recognized as one of the most important bone substitute materials in orthopaedics and dentistry over past few decades because of its chemical and biological similarity to the mineral phase of human bone. One solution for reduction the solubility of HA in biological environments is replacing F- by OH in HA structure and forming fluor-hydroxyapatite (FHA) solid solution. In this paper, FHA nanoparticles were successfully synthesized by a sol-gel method. Also, the influence of aging temperature on formation of FHA powder was studied. Equimolar solutions of calcium nitrate tetrahydrate, triethyl phosphite and ammonium fluoride in ethanol were used as Ca, P and F precursors. After aging at different temperatures, the synthesized powders were heat treated at 550 degrees C. The powders were investigated with X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), transmission electron microscopy (TEM), selected area electron diffraction pattern (SAED), energy dispersive analysis of X-ray (EDAX) and zetasizer measurement. The results of XRD proved the presence of fluorapatite (FA) and HA in all samples. In addition, the formation of FHA was confirmed by FT-IR results. XRD studies also showed that the crystallites were in nanometric scale. At the same time, this result was in good agreement with the result of zetasizer analysis.

Preparation, in vitro degradability, cytotoxicity, and in vivo biocompatibility of porous hydroxyapatite whisker-reinforced poly(L-lactide) biocomposite scaffolds.

PubMed

Xie, Lu; Yu, Haiyang; Yang, Weizhong; Zhu, Zhuoli; Yue, Li

2016-01-01

Biodegradable and bioactive scaffolds with interconnected macroporous structures, suitable biodegradability, adequate mechanical property, and excellent biocompatibility have drawn increasing attention in bone tissue engineering. Hence, in this work, porous hydroxyapatite whisker-reinforced poly(L-lactide) (HA-w/PLLA) composite scaffolds with different ratios of HA and PLLA were successfully developed through compression molding and particle leaching. The microstructure, in vitro mineralization, cytocompatibility, hemocompatibility, and in vivo biocompatibility of the porous HA-w/PLLA were investigated for the first time. The SEM results revealed that these HA-w/PLLA scaffolds possessed interconnected pore structures. Compared with porous HA powder-reinforced PLLA (HA-p/PLLA) scaffolds, HA-w/PLLA scaffolds exhibited better mechanical property and in vitro bioactivity, as more formation of bone-like apatite layers were induced on these scaffolds after mineralization in SBF. Importantly, in vitro cytotoxicity displayed that porous HA-w/PLLA scaffold with HA/PLLA ratio of 1:1 (HA-w1/PLLA1) produced no deleterious effect on human mesenchymal stem cells (hMSCs), and cells performed elevated cell proliferation, indicating a good cytocompatibility. Simultaneously, well-behaved hemocompatibility and favorable in vivo biocompatibility determined from acute toxicity test and histological evaluation were also found in the porous HA-w1/PLLA1 scaffold. These findings may provide new prospects for utilizing the porous HA whisker-based biodegradable scaffolds in bone repair, replacement, and augmentation applications.

Zinc-substituted hydroxyapatite: a biomaterial with enhanced bioactivity and antibacterial properties.

PubMed

Thian, E S; Konishi, T; Kawanobe, Y; Lim, P N; Choong, C; Ho, B; Aizawa, M

2013-02-01

Hydroxyapatite (HA) is a synthetic biomaterial and has been found to promote new bone formation when implanted in a bone defect site. However, its use is often limited due to its slow osteointegration rate and low antibacterial activity, particularly where HA has to be used for long term biomedical applications. This work will describe the synthesis and detailed characterization of zinc-substituted HA (ZnHA) as an alternative biomaterial to HA. ZnHA containing 1.6 wt% Zn was synthesized via a co-precipitation reaction between calcium hydroxide, orthophosphoric acid and zinc nitrate hexahydrate. Single-phase ZnHA particles with a rod-like morphology measuring ~50 nm in length and ~15 nm in width, were obtained and characterized using transmission electron microscopy and X-ray diffraction. The substitution of Zn into HA resulted in a decrease in both the a- and c-axes of the unit cell parameters, thereby causing the HA crystal structure to alter. In vitro cell culture work showed that ZnHA possessed enhanced bioactivity since an increase in the growth of human adipose-derived mesenchymal stem cells along with the bone cell differentiation markers, were observed. In addition, antibacterial work demonstrated that ZnHA exhibited antimicrobial capability since there was a significant decrease in the number of viable Staphylococcus aureus bacteria after in contact with ZnHA.

In vitro study of biocompatibility of a graphene composite with gold nanoparticles and hydroxyapatite on human osteoblasts.

PubMed

Crisan, Liana; Crisan, Bogdan; Soritau, Olga; Baciut, Mihaela; Biris, Alexandru Radu; Baciut, Grigore; Lucaciu, Ondine

2015-10-01

The purpose of this study was to evaluate the biocompatibility of some composites consisting of different proportions of graphene in combination with gold nanoparticles (AuNPs) and nanostructured hydroxyapatite (HA) on osteoblast viability, proliferation and differentiation. Au/HA@graphene composites synthesized by the catalytic chemical vapor deposition induction heating method with acetylene as the carbon source and over an Au/HA catalyst, were characterized by transmission electron microscopy, thermogravimetric analysis and Raman spectroscopy and showed that the few-layer graphene was grown over the Au/HA catalyst. The cytocompatibility study was performed using the fluorescein diacetate assay for assessment of the viability and proliferation of osteoblasts cultivated in the presence of HA, Au/HA and Au/HA@graphene composites as colloidal suspensions or as substrates. The most favorable composites for cell adhesion and proliferation were HA, Au/HA and Au/HA composites with 1.6% and 3.15% concentration of graphenes. Immunocytochemical staining performed after 19 days of osteoblasts cultivation on substrates showed that the graphene composites induced low expression of alkaline phosphatase compared to the control group and HA and Au/HA substrates. The presence of graphene in the substrate composition also induced an increased level of intracellular osteopontin and cytoskeleton reorganization (actin-F) depending on graphene concentration, suggesting cell activation, increased cellular adhesion and acquisition of a mechanosensorial osteocyte phenotype. Copyright © 2015 John Wiley & Sons, Ltd.

Preparation and characterization of collagen-hydroxyapatite/pectin composite.

PubMed

Wenpo, Feng; Gaofeng, Liang; Shuying, Feng; Yuanming, Qi; Keyong, Tang

2015-03-01

Pectin, a kind of plant polysaccharide, was introduced into collagen-hydroxyapatite composite system, and prepared collagen-hydroxyapatite/pectin (Col-HA/pectin) composite in situ. The structure of the composite was investigated by XRD, SEM, and FT-IR. The mechanical properties, water absorption, enzyme degradation, and cytotoxicity of the composite were investigated as well. The results show that the inorganic substance in the composite materials is hydroxyapatite in relatively low crystallinity. A new interface appeared by the interaction among hydroxyapatite and collagen-pectin, and formed smooth fine particles. The mechanical properties, water absorption, enzyme degradation, and cytotoxicity indicate a potential use in bone replacement for the new composite. Copyright © 2014 Elsevier B.V. All rights reserved.

Bio resorbability of the modified hydroxyapatite in Tris-HCL buffer

NASA Astrophysics Data System (ADS)

Golovanova, O. A.; Izmailov, R. R.; Ghyngazov, S. A.

2016-02-01

The solubility of carbonated hydroxyapatite powders and granulated carbonated hydroxyapatite produced from the synovial biofluid model solution has been studied. The kinetic characteristics of dissolution were determined. It was found that the solubility of carbonated hydroxyapatite is higher as compared to that of hydroxyapatite. The impact of the organic matrix on the rate of sample dissolution was revealed. For HA-gelatin composites, as the gelatin concentration grows, the dissolution rate becomes greater, and a sample of 6.0 g / L concentration has higher resorbability. The results of the research can be used to study the kinetics of dissolution and the biocompatibility of ceramic materials for medicine, namely for reconstructive surgery, dentistry, and development of drug delivery systems.

Bone regeneration in the presence of a synthetic hydroxyapatite/silica oxide-based and a xenogenic hydroxyapatite-based bone substitute material.

PubMed

Kruse, A; Jung, R E; Nicholls, F; Zwahlen, R A; Hämmerle, C H F; Weber, F E

2011-05-01

A comparison of synthetic hydroxyapatite/silica oxide, xenogenic hydroxyapatite-based bone substitute materials with empty control sites in terms of bone regeneration enhancement in a rabbit calvarial four non-critical-sized defect model. In each of six rabbits, four bicortical calvarial bone defects were generated. The following four treatment modalities were randomly allocated: (1) empty control site, (2) synthetic hydroxyapatite/silica oxide-based (HA/SiO) test granules, (3) xenogenic hydroxyapatite -based granules, (4) synthetic hydroxyapatite/silica oxide -based (HA/SiO) test two granules. The results of the latter granules have not been reported due to their size being three times bigger than the other two granule types. After 4 weeks, the animals were sacrificed and un-decalcified sections were obtained for histological analyses. For statistical analysis, the Kruskal-Wallis test was applied (P<0.05). Histomorphometric analysis showed an average area fraction of newly formed bone of 12.32±10.36% for the empty control, 17.47±6.42% for the xenogenic hydroxyapatite -based granules group, and 21.2±5.32% for the group treated with synthetic hydroxyapatite/silica oxide -based granules. Based on the middle section, newly formed bone bridged the defect to 38.33±37.55% in the empty control group, 54.33±22.12% in the xenogenic hydroxyapatite -based granules group, and to 79±13.31% in the synthetic hydroxyapatite/silica oxide -based granules group. The bone-to-bone substitute contact was 46.38±18.98% for the xenogenic and 59.86±14.92% for the synthetic hydroxyapatite/silica oxide-based granules group. No significant difference in terms of bone formation and defect bridging could be detected between the two bone substitute materials or the empty defect. There is evidence that the synthetic hydroxyapatite/silica oxide granules provide comparable results with a standard xenogenic bovine mineral in terms of bone formation and defect bridging in non-critical size defects. © 2010 John Wiley & Sons A/S.

Mechanical strength of [HA/Bioplastic/Sericin] composite part printed by bioprinter

DOE Office of Scientific and Technical Information (OSTI.GOV)

Tontowi, Alva Edy, E-mail: alvaedytontowi@ugm.ac.id; Setiawan, Agris

The aim of this research was to determine the effect of hydroxyapatite (HA) content in printed biocomposite to its mechanical strength. The biocomposite paste was prepared by composing HA, bioplastic and sericin with various ratios of [HA/Bioplastic]: 40/60, 50/50, 60,40 and 70/30. Sericin of 0.3% weight was added to the biocomposite. Mechanical test was conducted to observe tensile (ASTM D 638 type 4) and flexural strength (ASTM D 790). Both type of specimens were fabricated using 3D Printer. Printing process parameter (infill speed, print speed and layer height) were set up as 60 mm/s, 10 mm/s, 0.35 mm, respectively. Resultsmore » showed that biocomposite with [HA/Biplastic]. weight ratio of 60/40(w/w) has an optimum tensile (3.89 ± 1.26 MPa) and flexural strength (2.51 ± 0.45 MPa). Scanning electron microscope observation indicated that microstructure of specimen was influenced by the percentage of the hydroxyapatite. There was no agglomeration of HA particle within the composite.« less

Morphological structure and characteristics of hydroxyapatite/β-cyclodextrin composite nanoparticles synthesized at different conditions.

PubMed

Son, Kyoung Dan; Kim, Young-Jin

2013-01-01

Hydroxyapatite (HA) nanoparticles were prepared simply in the presence of β-cyclodextrin (β-CD). Mixing sequence of ion precursors during the synthesis of HA greatly affected the morphological structure of nanoparticles. Ca-P showed only the sphere-like structure, however P-Ca exhibited the mixture of spherical and rod-like nanoparticles. The size of nanoparticles slightly decreased with increasing the content of β-CD. The HAs synthesized in the presence of β-CD agglomerated, leading to the formation of aggregates with a size of hundreds nanometer and narrow size distribution. FT-IR, XRD and XRF analyses confirmed that the HA nanoparticles could be synthesized with using β-CD, in which the Ca/P molar ratio was ranged from 1.72 to 1.70. The crystalline phase of these HA nanoparticles was similar to that of the stoichiometric HA. In addition, the content of β-CD contained in the products could influence the initial deposition rate of bone-like apatite on the surface of HA nanoparticles in simulated body fluid (SBF). Copyright © 2012 Elsevier B.V. All rights reserved.

The influence of Ca/P ratio on the properties of hydroxyapatite bioceramics

NASA Astrophysics Data System (ADS)

Ramesh, S.; Tan, C. Y.; Hamdi, M.; Sopyan, I.; Teng, W. D.

2007-07-01

The paper reports on the effect of Ca/P ratio (1.57, 1.67 and 1.87) on the densification behaviour of nanocrystalline hydroxyapatite (HA) prepared by a chemical precipitation method. Green compacts were prepared and sintered at temperatures ranging from 1000°C to 1350°C. The sintered samples were characterized to determine the HA phase stability, bulk density, hardness, fracture toughness and Young's modulus. XRD analysis revealed that the phase stability was not disrupted throughout the sintering regime employed for HA having Ca/P ratio of 1.57 and 1.67. However, secondary phases were observed for HA having a Ca/P ratio of 1.87 when sintered at high temperatures. In general, regardless of Ca/P ratio, the HA bodies achieved > 95% relative density when sintered at 1100°C-1250°C. The results indicated that the stoichiometric HA (Ca/P ratio = 1.67) exhibited the overall best properties, with the highest hardness of 7.23 GPa and fracture toughness of 1.28 MPam1/2 being attained when sintered at 1000°C-1050°C.

Fabrication of DNA/Hydroxyapatite nanocomposites by simulated body fluid for gene delivery

NASA Astrophysics Data System (ADS)

Takeshita, Takayuki; Okamoto, Masami

2015-05-01

The hydroxyapatite (HA) formation on the surface of DNA molecules in simulated body fluid (SBF) was examined. The osteoconductivity is estimated using SBF having ion concentrations approximately equal to those of human blood plasma. After immersion for 4 weeks in SBF at 36.5 °C, the HA crystallites possessing 1-14 micrometer in diameter grew on the surface of DNA molecules. The leaf flake-like and spherical shapes morphologies were observed through scanning electron microscopy analysis. Original peaks of both of DNA and HA were characterized by fourier transform infrared spectroscopy. The Ca/P ratio (1.1-1.5) in HA was estimated by energy dispersive X-ray analysis. After biomineralization, the calculated weight ratio of DNA/HA was 18/82 by thermogravimetry/differential thermal analysis. The molecular orbital computer simulation has been used to probe the interaction of DNA with two charge-balancing ions, CaOH+ and C a H2P O4+ . The adsorption enthalpy of the two ions on DNA having negative value was the evidence for the interface in mineralization of HA in SBF.

In vitro and in vivo investigation of bisphosphonate-loaded hydroxyapatite particles for peri-implant bone augmentation.

PubMed

Kettenberger, Ulrike; Luginbuehl, Vera; Procter, Philip; Pioletti, Dominique P

2017-07-01

Locally applied bisphosphonates, such as zoledronate, have been shown in several studies to inhibit peri-implant bone resorption and recently to enhance peri-implant bone formation. Studies have also demonstrated positive effects of hydroxyapatite (HA) particles on peri-implant bone regeneration and an enhancement of the anti-resorptive effect of bisphosphonates in the presence of calcium. In the present study, both hydroxyapatite nanoparticles (nHA) and zoledronate were combined to achieve a strong reinforcing effect on peri-implant bone. The nHA-zoledronate combination was first investigated in vitro with a pre-osteoclastic cell assay (RAW 264.7) and then in vivo in a rat model of postmenopausal osteoporosis. The in vitro study confirmed that the inhibitory effect of zoledronate on murine osteoclast precursor cells was enhanced by loading the drug on nHA. For the in vivo investigation, either zoledronate-loaded or pure nHA were integrated in hyaluronic acid hydrogel. The gels were injected in screw holes that had been predrilled in rat femoral condyles before the insertion of miniature screws. Micro-CT-based dynamic histomorphometry and histology revealed an unexpected rapid mineralization of the hydrogel in vivo through formation of granules, which served as scaffold for new bone formation. The delivery of zoledronate-loaded nHA further inhibited a degradation of the mineralized hydrogel as well as a resorption of the peri-implant bone as effectively as unbound zoledronate. Hyaluronic acid with zoledronate-loaded nHA, thanks to its dual effect on inducing a rapid mineralization and preventing resorption, is a promising versatile material for bone repair and augmentation. Copyright © 2015 John Wiley & Sons, Ltd. Copyright © 2015 John Wiley & Sons, Ltd.

Cytocompatibility and biocompatibility of nanostructured carbonated hydroxyapatite spheres for bone repair

PubMed Central

CALASANS-MAIA, Mônica Diuana; de MELO, Bruno Raposo; ALVES, Adriana Terezinha Neves Novellino; RESENDE, Rodrigo Figueiredo de Brito; LOURO, Rafael Seabra; SARTORETTO, Suelen Cristina; GRANJEIRO, José Mauro; ALVES, Gutemberg Gomes

2015-01-01

ABSTRACT Objective The aim of this study was to investigate the in vitro and in vivo biological responses to nanostructured carbonated hydroxyapatite/calcium alginate (CHA) microspheres used for alveolar bone repair, compared to sintered hydroxyapatite (HA). Material and Methods The maxillary central incisors of 45 Wistar rats were extracted, and the dental sockets were filled with HA, CHA, and blood clot (control group) (n=5/period/group). After 7, 21 and 42 days, the samples of bone with the biomaterials were obtained for histological and histomorphometric analysis, and the plasma levels of RANKL and OPG were determined via immunoassay. Statistical analysis was performed by Two-Way ANOVA with post-hoc Tukey test at 95% level of significance. Results The CHA and HA microspheres were cytocompatible with both human and murine cells on an in vitro assay. Histological analysis showed the time-dependent increase of newly formed bone in control group characterized by an intense osteoblast activity. In HA and CHA groups, the presence of a slight granulation reaction around the spheres was observed after seven days, which was reduced by the 42nd day. A considerable amount of newly formed bone was observed surrounding the CHA spheres and the biomaterials particles at 42-day time point compared with HA. Histomorphometric analysis showed a significant increase of newly formed bone in CHA group compared with HA after 21 and 42 days from surgery, moreover, CHA showed almost 2-fold greater biosorption than HA at 42 days (two-way ANOVA, p<0.05) indicating greater biosorption. An increase in the RANKL/OPG ratio was observed in the CHA group on the 7th day. Conclusion CHA spheres were osteoconductive and presented earlier biosorption, inducing early increases in the levels of proteins involved in resorption. PMID:26814461

Comparison of bioactive glass coated and hydroxyapatite coated titanium dental implants in the human jaw bone.

PubMed

Mistry, S; Kundu, D; Datta, S; Basu, D

2011-03-01

Current trends in clinical dental implant therapy include modification of titanium surfaces for the purpose of improving osseointegration by different additive (bioactive coatings) and subtractive processes (acid etching, grit-blasting). The aim of this study was to evaluate and compare the behaviour of hydroxyapatite and the newly developed bioactive glass coated implants (62 implants) in osseous tissue following implantation in 31 patients. Bioactive glass and hydroxyapatite was suitably coated on titanium alloy. Hydroxyapatite coating was applied on the implant surface by air microplasma spray technique and bioactive glass coating was applied by vitreous enamelling technique. The outcome was assessed up to 12 months after prosthetic loading using different clinical and radiological parameters. Hydroxyapatite and bioactive glass coating materials were non-toxic and biocompatible. Overall results showed that bioactive glass coated implants were as equally successful as hydroxyapatite in achieving osseointegration and supporting final restorations. The newly developed bioactive glass is a good alternative coating material for dental implants. © 2011 Australian Dental Association.

Nano-hydroxyapatite and its applications in preventive, restorative and regenerative dentistry: a review of literature.

PubMed

Pepla, Erlind; Besharat, Lait Kostantinos; Palaia, Gaspare; Tenore, Gianluca; Migliau, Guido

2014-07-01

This study aims to critically summarize the literature about nano-hydroxyapatite. The purpose of this work is to analyze the benefits of using nano-hydroxyapatite in dentistry, especially for its preventive, restorative and regenerative applications. We also provide an overview of new dental materials, still experimental, which contain the nano-hydroxyapatite in its nano-crystalline form. Hydroxyapatite is one of the most studied biomaterials in the medical field for its proven biocompatibility and for being the main constituent of the mineral part of bone and teeth. In terms of restorative and preventive dentistry, nano-hydroxyapatite has significant remineralizing effects on initial enamel lesions, certainly superior to conventional fluoride, and good results on the sensitivity of the teeth. The nano-HA has also been used as an additive material, in order to improve already existing and widely used dental materials, in the restorative field (experimental addition to conventional glass ionomer cements, that has led to significant improvements in their mechanical properties). Because of its unique properties, such as the ability to chemically bond to bone, to not induce toxicity or inflammation and to stimulate bone growth through a direct action on osteoblasts, nano-HA has been widely used in periodontology and in oral and maxillofacial surgery. Its use in oral implantology, however, is a widely used practice established for years, as this substance has excellent osteoinductive capacity and improves bone-to-implant integration.

Nano-hydroxyapatite particles induce apoptosis on MC3T3-E1 cells and tissue cells in SD rats

NASA Astrophysics Data System (ADS)

Wang, Liting; Zhou, Gang; Liu, Haifeng; Niu, Xufeng; Han, Jingyun; Zheng, Lisha; Fan, Yubo

2012-04-01

While the advantages of nanomaterials are being increasingly recognized, their potential toxicity is drawing more and more attention and concern. In this study, we explore the toxicity mechanism of 20-30 nm rod-shaped hydroxyapatite (HA) nanoparticles in vitro and in vivo. The nanoparticles were prepared by precipitation and characterized by IR, XRD and TEM. Concentrations of 0 μg mL-1, 10 μg mL-1, 100 μg mL-1, 1 mg mL-1, and 10 mg mL-1 were applied to the MC3T3-E1 cells for viability (MTT-test). Based on the characteristic differences of the two methods of cell death, the morphological features of the MC3T3-E1 cell line co-cultured with nano-hydroxyapatite (n-HA) (10 mg mL-1) for 24 h were also observed by TEM. Furthermore, important serum biochemical markers and histopathological examinations were used to evaluate the potential toxicological effect of n-HA on the major organs of SD rats injected intraperitoneally with n-HA (33.3 mg kg-1 body weight). In the results, we found cell growth inhibition and apoptosis in MC3T3-E1 cells co-cultured with n-HA. Moreover, apoptosis but not necrosis was illustrated in liver and renal tissue by using histopathology slices and serum biochemical markers. It suggests that apoptosis may be the possible mechanism of n-HA toxicity and provides a better understanding of the biocompatibility of nanomaterials applied in human bone repair.

Hydroxyapatite, fluor-hydroxyapatite and fluorapatite produced via the sol-gel method: dissolution behaviour and biological properties after crystallisation.

PubMed

Tredwin, Christopher J; Young, Anne M; Abou Neel, Ensanya A; Georgiou, George; Knowles, Jonathan C

2014-01-01

Hydroxyapatite (HA), fluor-hydroxyapatite (FHA) with varying levels of fluoride ion substitution and fluorapatite (FA) were synthesised by the sol-gel method as possible implant coating or bone-grafting materials. Calcium nitrate and triethyl phosphite were used as precursors under an ethanol-water based solution. Different amounts of ammonium fluoride were incorporated for the preparation of the FHA and FA sol-gels. After heating and powdering the sol-gels, dissolution behaviour was assessed using ion chromatography to measure Ca(2+) and PO4 (3-) ion release. Biological behaviour was assessed using cellular proliferation with human osteosarcoma cells and alamarBlue™ assay. Statistical analysis was performed with a two way analysis of variance and post hoc testing with a Bonferroni correction. Increasing fluoride substitution into an apatite structure decreased the dissolution rate. Increasing the firing temperature of the HA, FHA and FA sol-gels up to 1,000 °C decreased the dissolution rate. There was significantly higher cellular proliferation on highly substituted FHA and FA than on HA or Titanium. The properties of an implant coating or bone grafting material can be tailored to meet specific requirements by altering the amount of fluoride that is incorporated into the original apatite structure. The dissolution behaviour can further be altered by the temperature at which the sol-gel is fired.

Effect of negatively charged cellulose nanofibers on the dispersion of hydroxyapatite nanoparticles for scaffolds in bone tissue engineering.

PubMed

Park, Minsung; Lee, Dajung; Shin, Sungchul; Hyun, Jinho

2015-06-01

Nanofibrous 2,2,6,6-tetramethylpiperidine-1-oxyl(TEMPO)-oxidized bacterial cellulose (TOBC) was used as a dispersant of hydroxyapatite (HA) nanoparticles in aqueous solution. The surfaces of TOBC nanofibers were negatively charged after the reaction with the TEMPO/NaBr/NaClO system at pH 10 and room temperature. HA nanoparticles were simply adsorbed on the TOBC nanofibers (HA-TOBC) and dispersed well in DI water. The well-dispersed HA-TOBC colloidal solution formed a hydrogel after the addition of gelatin, followed by crosslinking with glutaraldehyde (HA-TOBC-Gel). The chemical modification of the fiber surfaces and the colloidal stability of the dispersion solution confirmed TOBC as a promising HA dispersant. Both the Young's modulus and maximum tensile stress increased as the amount of gelatin increased due to the increased crosslinking of gelatin. In addition, the well-dispersed HA produced a denser scaffold structure resulting in the increase of the Young's modulus and maximum tensile stress. The well-developed porous structures of the HA-TOBC-Gel composites were incubated with Calvarial osteoblasts. The HA-TOBC-Gel significantly improved cell proliferation as well as cell differentiation confirming the material as a potential candidate for use in bone tissue engineering scaffolds. Copyright © 2015 Elsevier B.V. All rights reserved.

Evaluation of Heating and Shearing on the Viscoelastic Properties of Calcium Hydroxyapatite Used in Injection Laryngoplasty.

PubMed

Mahboubi, Hossein; Mohraz, Ali; Verma, Sunil P

2016-03-01

To compare the viscoelastic properties of calcium hydroxyapatite (CaHA) to carboxymethylcellulose (CMC) injectables used for injection laryngoplasty and determine if they are affected by heating and shearing. Experimental. University laboratory. Vocal fold injection laryngoplasty with CaHA is oftentimes challenging due to the amount of pressure necessary to push the injectate through a needle. Anecdotal techniques, such as heating the product, have been suggested to facilitate injection. The viscoelastic properties of CaHA and CMC were measured with a rheometer. The effects of heating and shearing on sample viscoelasticity were recorded. CaHA was 9.5 times more viscous than CMC (43,100 vs 4540 Pa·s). Heating temporarily decreased the viscosity of CaHA by 32%. However, it also caused the viscosity to subsequently increase after time. Shearing of CaHA reduced its viscosity by 26%. Heating and shearing together temporarily reduced the viscosity of CaHA by 52%. A combination of heating and shearing had a more profound effect than heating or shearing alone on the viscosity of CaHA, potentially making it easier to inject temporarily. Long-term and in vivo studies are required to further analyze the effect of heating and shearing on CaHA injectables. © American Academy of Otolaryngology—Head and Neck Surgery Foundation 2016.

Preparation and Properties of Nano-Hydroxyapatite/Gelatin/Poly(vinyl alcohol) Composite Membrane.

PubMed

Liao, Haotian; Shi, Kun; Peng, Jinrong; Qu, Ying; Liao, Jinfeng; Qian, Zhiyong

2015-06-01

In this study, the bone-like composite membrane based on blends of gelatin (Gel), nano-hydroxyapatite (n-HA) and poly(vinyl alcohol) (PVA) was fabricated by solvent casting and evaporation methods. The effect of n-HA content and the ratio of Gel/PVA on the properties of the composite was investigated. The Gel/PVA and n-HA/Gel/PVA composite membranes were characterized by Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), water contact angle measurement and scanning electron microscopy (SEM). The mechanical properties of the composites were determined by tensile tests. The as prepared composite membranes exhibited hydrophobility, the water contact angle of composite membrane was 126.6 when its mass ratio of n-HA/Gel/PVA was 10/50/40. The tensile strength of composite membranes was greatly increased due to the introduction of n-HA, and the tensile strength was increased to 74.92 MPa when the mass ratio of n-HA/Gel/PVA was 10/50/40. SEM observation indicated that n-HA was dispersed in the membranes and a sea-island structure was formed in the n-HA/Gel/PVA composite membranes, resulting in a significant increase in tensile strength. The as-prepared n-HA/Gel/PVA composite membranes may be applied in the field of bone tissue engineering.

Carbon fibers with a nano-hydroxyapatite coating as an excellent biofilm support for bioreactors

NASA Astrophysics Data System (ADS)

Liu, Qijie; Zhang, Chao; Bao, Yanling; Dai, Guangze

2018-06-01

A biofilm support with high biocompatibility is needed for bioreactors. A nano-hydroxyapatite (HA) coating on carbon fibers (CFs) was prepared by electrochemical deposition (ECD). The sludge immobilization assays, bacterial cells adhesion assays and Derjaguin-Landau-Verwey-Overbeek (DLVO) theory were used to evaluate the capacity of CF supports to immobilize activated sludge and bacterial cells. The sludge immobilization and bacterial cells adhesion assays illustrated that HA coating could enhance the capacity of CFs to immobilize microorganisms. SEM images showed that HA and bacterial cells formed a dense film on CFs surface. In addition, HA, acting as a glue, could combine CFs with bacterial cells or between cells, which helped CFs capture more bacterial cells. DLVO theory illustrated that CFs with HA coating had a lower total interaction energy than CFs without handling, explaining the higher capacity of CFs with HA coating to immobilize bacterial cells. This result was owning to the less negative zeta potential and higher hydrophilicity of CFs with HA coating, and the hydrophilicity made a greater contribution to the lower total interaction energy. Experiments and theory reveal that HA coating could enhance the biocompatibility of CFs, and CFs with HA coating could be used as an excellent biofilm support for bioreactors.

Beneficial effects of hydroxyapatite on enamel subjected to 30% hydrogen peroxide.

PubMed

Jiang, Tao; Ma, Xiao; Wang, Zhejun; Tong, Hua; Hu, Jiming; Wang, Yining

2008-11-01

To evaluate the effect of combination of hydroxyapatite (HA) and hydrogen peroxide (HP) on color, microhardness and morphology of human tooth enamel. Forty-eight human dental blocks were obtained from 12 pairs of premolars and were randomly divided into four groups. Group DW was treated with distilled water, group HP with 30% HP, group HA+DW with HA mixed with distilled water and group HA+HP with HA mixed with 30% HP. Baseline and final color measurements and microhardness test were carried out before and after bleaching experiments. Two specimens from each group were selected for morphological investigation after final tests. The DeltaE of group HP and HA+HP were significantly higher than those of group DW (p=0.000 and p=0.000) and group HA+DW (p=0.000 and p=0.000). The percentage microhardness loss of group HA+HP was significantly lower than that of group HP (p=0.047), but significantly higher than those of group DW (p=0.000) and group HA+DW (p=0.000). The obvious variation of morphology was only observed on enamel surfaces in group HP. This study suggested that combination of HA and HP was effective in tooth whitening. HA could significantly reduce the microhardness loss of enamel caused by 30% HP and keep enamel surface morphology almost unchanged.

Development of nanosized silver-substituted apatite for biomedical applications: A review.

PubMed

Lim, Poon Nian; Chang, Lei; Thian, Eng San

2015-08-01

The favorable biocompatibility of hydroxyapatite (HA) makes it a popular bone graft material as well as a coating layer on metallic implant. To reduce implant-related infections, silver ions were either incorporated into the apatite during co-precipitation process (AgHA-CP) or underwent ion-exchange with the calcium ions in the apatite (AgHA-IE). However, the distribution of silver ions in AgHA-CP and AgHA-IE was different, thus affecting the antibacterial action. Several studies reported that nanosized AgHA-CP containing 0.5 wt.% of silver provided an optimal trade-off between antibacterial properties and cytotoxicity. Nevertheless, nanosized AgHA and AgHA nanocoatings could not function ideally due to the compromise in the bone differentiation of mesenchymal stem cells, as evidenced in the reduced alkaline phosphatase, type I collagen and osteocalcin. Preliminary studies showed that biological responses of nanosized AgHA and AgHA nanocoatings could be improved with the addition of silicon. This review will discuss on nanosized AgHA and AgHA nanocoatings. In many patients needing bone graft material, hydroxyapatite (HA) has proven to be a popular choice. Nonetheless, implant-related infections remain a major concern. Hence, effective preventive measures are needed. In this review article, the authors discussed the application of incorporating silver nanoparticles in HA and its use as bone graft biomaterials together with the addition of silica. Copyright © 2015 Elsevier Inc. All rights reserved.

Bone ingrowth in bFGF-coated hydroxyapatite ceramic implants.

PubMed

Schnettler, Reinhard; Alt, Volker; Dingeldein, Elvira; Pfefferle, Hans-Joachim; Kilian, Olaf; Meyer, Christof; Heiss, Christian; Wenisch, Sabine

2003-11-01

This experimental study was performed to evaluate angiogenesis, bone formation, and bone ingrowth in response to osteoinductive implants of bovine-derived hydroxyapatite (HA) ceramics either uncoated or coated with basic fibroblast growth factor (bFGF) in miniature pigs. A cylindrical bone defect was created in both femur condyles of 24 miniature pigs using a saline coated trephine. Sixteen of the 48 defects were filled with HA cylinders coated with 50 microg rhbFG, uncoated HA cylinders, and with autogenous transplants, respectively. Fluorochrome labelled histological analysis, histomorphometry, and scanning electron microscopy were performed to study angiogenesis, bone formation and bone ingrowth. Complete bone ingrowth into bFGF-coated HA implants and autografts was seen after 34 days compared to 80 days in the uncoated HA group. Active ring-shaped areas of fluorochrome labelled bone deposition with dynamic bone remodelling were found in all cylinders. New vessels could be found in all cylinders. Histomorphometric analysis showed no difference in bone ingrowth over time between autogenous transplants and bFGF-coated HA implants. The current experimental study revealed comparable results of bFGF-coated HA implants and autogenous grafts regarding angiogenesis, bone synthesis and bone ingrowth.

Combined effect of pulse electron beam treatment and thin hydroxyapatite film on mechanical features of biodegradable AZ31 magnesium alloy

NASA Astrophysics Data System (ADS)

Surmeneva, M. A.; Tyurin, A. I.; Teresov, A. D.; Koval, N. N.; Pirozhkova, T. S.; Shuvarin, I. A.; Surmenev, R. A.

2015-11-01

The morphology, elemental, phase composition, nanohardness, and Young's modulus of the hydroxyapatite (HA) coating deposited via radio frequency (RF) magnetron sputtering onto the AZ31 surface were investigated by atomic force microscopy (AFM), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), X-ray diffraction (XRD), and nanoindentationtechniques. The calcium phosphate (Ca/P) molar ratio of the HA coating deposited via RF-magnetron sputtering onto AZ31 substrates according to EDX was 1.57+0.03. The SEM experiments revealed significant differences in the morphology of the HA film deposited on untreated and treated with the pulsed electron beam (PEB) AZ31 substrate. Nanoindentation studies demonstrated significant differences in the mechanical responses of the HA film deposited on the initial and PEB-modified AZ31 substrates. The nanoindentation hardness and the Young's modulus of the HA film on the magnesium alloy modified using the PEB treatment were higher than that of the HA layer on the untreated substrate. Moreover, the HA film fabricated onto the PEB-treated surface was more resistant to plastic deformation than the same film on the untreated AZ31 surface.

Osteogenic Responses to Zirconia with Hydroxyapatite Coating by Aerosol Deposition

PubMed Central

Cho, Y.; Hong, J.; Ryoo, H.; Kim, D.; Park, J.

2015-01-01

Previously, we found that osteogenic responses to zirconia co-doped with niobium oxide (Nb2O5) or tantalum oxide (Ta2O5) are comparable with responses to titanium, which is widely used as a dental implant material. The present study aimed to evaluate the in vitro osteogenic potential of hydroxyapatite (HA)-coated zirconia by an aerosol deposition method for improved osseointegration. Surface analysis by scanning electron microscopy and x-ray diffraction proved that a thin as-deposited HA film on zirconia showed a shallow, regular, crater-like surface. Deposition of dense and uniform HA films was measured by SEM, and the contact angle test demonstrated improved wettability of the HA-coated surface. Confocal laser scanning microscopy indicated that MC3T3-E1 pre-osteoblast attachment did not differ notably between the titanium and zirconia surfaces; however, cells on the HA-coated zirconia exhibited a lower proliferation than those on the uncoated zirconia late in the culture. Nevertheless, ALP, alizarin red S staining, and bone marker gene expression analysis indicated good osteogenic responses on HA-coated zirconia. Our results suggest that HA-coating by aerosol deposition improves the quality of surface modification and is favorable to osteogenesis. PMID:25586588

Effect of hydroxyapatite nano-particles on morphology, rheology and thermal behavior of poly(caprolactone)/chitosan blends.

PubMed

Ghorbani, Fereshte Mohammad; Kaffashi, Babak; Shokrollahi, Parvin; Akhlaghi, Shahin; Hedenqvist, Mikael S

2016-02-01

The effect of hydroxyapatite nano-particles (nHA) on morphology, and rheological and thermal properties of PCL/chitosan blends was investigated. The tendency of nHA to reside in the submicron-dispersed chitosan phase is determined using SEM and AFM images. The presence of electrostatic interaction between amide sites of chitosan and ionic groups on the nHA surface was proved by FTIR. It is shown that the chitosan phase is thermodynamically more favorable for the nano-particles to reside than the PCL phase. Lack of implementation of Cox-Merz theory for this system shows that the polymer-nano-particle network is destructed by the flow. Results from dynamic rheological measurements and Zener fractional model show that the presence of nHA increases the shear moduli and relaxation time of the PCL/chitosan blends. DSC measurements showed that nHA nano-particles are responsible for the increase in melting and crystallization characteristics of the PCL/chitosan blends. Based on thermogravimetric analysis, the PCL/chitosan/nHA nano-composites exhibited a greater thermal stability compared to the nHA-free blends. Copyright © 2015 Elsevier B.V. All rights reserved.

Combination of high-intensity focused ultrasound irradiation and hydroxyapatite nanoparticle injection to injure normal goat liver tissue in vivo without costal bone incision.

PubMed

Liu, L; Xiao, Z; Xiao, Y; Wang, Z; Li, F; Li, M; Peng, X

2014-10-20

The aims of this study were to evaluate the in vivo safety of intravenous nano-hydroxyapatite (nano-HA), to explore how nano-HA might influence the effects of high-intensity focused ultrasound (HIFU) on normal liver tissue, and to investigate whether intravenous nano-HA could enhance HIFU for hepatocellular carcinoma ablation in a goat model. The present study, for the first time, indicated that the delivery of abundant nano-HA into the body over short periods of time could be assembled by the hepatic reticuloendothelial system, subsequently leading to a rapid rise of ultrasound-induced overheating, and ultimately resulting in enlargement of the coagulation necrotic area for ablated hepatocellular carcinoma in goats both in vivo and ex vivo. On the other hand, therapeutic doses of nano-HA were much lower than the lethal dose, and consequently presented transient and mild abnormalities of hepatic enzymes and renal function during the first 24 h after nano-HA injection. These results suggested that the combined application of nano-HA and HIFU is potentially a more effective alternative option compared to surgery for hepatocellular carcinoma local ablation in a safe and feasible manner.

Electrophoretic deposition of graphene oxide reinforced chitosan-hydroxyapatite nanocomposite coatings on Ti substrate.

PubMed

Shi, Y Y; Li, M; Liu, Q; Jia, Z J; Xu, X C; Cheng, Y; Zheng, Y F

2016-03-01

Electrophoretic deposition (EPD) is a facile and feasible technique to prepare functional nanocomposite coatings for application in orthopedic-related implants. In this work, a ternary graphene oxide-chitosan-hydroxyapatite (GO-CS-HA) composite coating on Ti substrate was successfully fabricated by EPD. Coating microstructure and morphologies were investigated by scanning electron microscopy, contact angle test, Raman spectroscopy, Fourier transform infrared spectroscopy and thermogravimetric analysis. It was found GO-CS surface were uniformly decorated by HA nanoparticles. The potentiodynamic polarization test in simulated body fluid indicated that the GO-CS-HA coatings could provide effective protection of Ti substrate from corrosion. This ternary composite coating also exhibited good biocompatibility during incubation with MG63 cells. In addition, the nanocomposite coatings could decrease the attachment of Staphylococcus aureus.

Powder Metallurgical Synthesis of Biodegradable Mg-Hydroxyapatite Composites for Biomedical Applications

NASA Astrophysics Data System (ADS)

Stüpp, Cesar Augusto; Szakács, Gábor; Mendis, Chamini Lakshi; Gensch, Felix; Müller, Sören; Feyerabend, Frank; Hotza, Dachamir; Fredel, Marcio Celso; Hort, Norbert

Magnesium alloys with acceptable or even controllable corrosion rates, where mechanical properties are not significantly modified or worsened, have been increasingly investigated in the last decade for use as biomaterials. This work shows an approach with a magnesium metal matrix composite (Mg-MMC), composed of ZK60 as base material and hydroxyapatite (HA) particles. The composite was produced by mechanical alloying followed by hot extrusion, as HA in contact with molten magnesium releases toxic gases such as phosphine (PH3). This work will present the influence of different amounts of HA on corrosion behaviour and mechanical properties of the investigated composites. Compared to the ZK60 alloy, corrosion is expected to be delayed, without localized corrosion. The mechanical properties are not expected to be compromised with such composite during tissue's healing period.

Poly(vinyl alcohol) hydrogel coatings with tunable surface exposure of hydroxyapatite

PubMed Central

Moreau, David; Villain, Arthur; Ku, David N; Corté, Laurent

2014-01-01

Insufficient bone anchoring is a major limitation of artificial substitutes for connective osteoarticular tissues. The use of coatings containing osseoconductive ceramic particles is one of the actively explored strategies to improve osseointegration and strengthen the bone-implant interface for general tissue engineering. Our hypothesis is that hydroxyapatite (HA) particles can be coated robustly on specific assemblies of PVA hydrogel fibers for the potential anchoring of ligament replacements. A simple dip-coating method is described to produce composite coatings made of microscopic hydroxyapatite (HA) particles dispersed in a poly(vinyl alcohol) (PVA) matrix. The materials are compatible with the requirements for implant Good Manufacturing Practices. They are applied to coat bundles of PVA hydrogel fibers used for the development of ligament implants. By means of optical and electronic microscopy, we show that the coating thickness and surface state can be adjusted by varying the composition of the dipping solution. Quantitative analysis based on backscattered electron microscopy show that the exposure of HA at the coating surface can be tuned from 0 to over 55% by decreasing the weight ratio of PVA over HA from 0.4 to 0.1. Abrasion experiments simulating bone-implant contact illustrate how the coating cohesion and wear resistance increase by increasing the content of PVA relative to HA. Using pullout experiments, we find that these coatings adhere well to the fiber bundles and detach by propagation of a crack inside the coating. These results provide a guide to select coated implants for anchoring artificial ligaments. PMID:25482413

Thermal Spraying of Bioactive Polymer Coatings for Orthopaedic Applications

NASA Astrophysics Data System (ADS)

Chebbi, A.; Stokes, J.

2012-06-01

Flame sprayed biocompatible polymer coatings, made of biodegradable and non-biodegradable polymers, were investigated as single coatings on titanium and as top coatings on plasma sprayed Hydroxyapatite. Biocompatible polymers can act as drug carriers for localized drug release following implantation. The polymer matrix consisted of a biodegradable polymer, polyhydroxybutyrate 98%/ polyhydroxyvalerate 2% (PHBV) and a non-biodegradable polymer, polymethylmethacrylate (PMMA). Screening tests were performed to determine the suitable range of spraying parameters, followed by a Design of Experiments study to determine the effects of spraying parameters on coating characteristics (thickness, roughness, adhesion, wettability), and to optimize the coating properties accordingly. Coatings characterization showed that optimized flame sprayed biocompatible polymers underwent little chemical degradation, did not produce acidic by-products in vitro, and that cells proliferated well on their surface.

Silver oxide-containing hydroxyapatite coating supports osteoblast function and enhances implant anchorage strength in rat femur.

PubMed

Eto, Shuichi; Miyamoto, Hiroshi; Shobuike, Takeo; Noda, Iwao; Akiyama, Takayuki; Tsukamoto, Masatsugu; Ueno, Masaya; Someya, Shinsuke; Kawano, Shunsuke; Sonohata, Motoki; Mawatari, Masaaki

2015-09-01

Antibacterial silver with hydroxyapatite (Ag-HA) is a promising coating material for imparting antibacterial properties to implants. We previously reported that 3% (w/w) silver with HA (3% Ag-HA) has both antibacterial activity and osteoconductivity. In this study, we investigated the effects of Ag-HA on the in vitro osteoblast function and the in vivo anchorage strength and osteoconductivity of implants. Production of the osteoblast marker alkaline phosphatase, but not cytotoxicity, was observed in cells of the osteoblast cell line MC3T3-E1 cultured on the 3% Ag-HA-coated surface. These results were similar to those observed with silver-free HA coating. In contrast, a significant high level of cytotoxicity was observed when the cells were cultured on a 50% Ag-HA-coated surface. The anchorage strength of implants inserted into the femur of Sprague-Dawley (SD) rats was enhanced by coating the implants with 3% Ag-HA. On the 3% Ag-HA-coated surface, both metaphyseal and diaphyseal areas were largely covered with new bone and had adequate osteoconductivity. These results suggest that 3% Ag-HA, like conventional HA, promotes osteogenesis by supporting osteoblast viability and function and thereby contributes to sufficient anchorage strength of implants. Application of 3% Ag-HA, which combines the osteoconductivity of HA and the antibacterial activity of silver, to prosthetic joints will help prevent postoperative infections. © 2015 Orthopaedic Research Society. Published by Wiley Periodicals, Inc.

Osteoblast and osteoclast responses to A/B type carbonate-substituted hydroxyapatite ceramics for bone regeneration.

PubMed

Germaini, Marie-Michèle; Detsch, Rainer; Grünewald, Alina; Magnaudeix, Amandine; Lalloue, Fabrice; Boccaccini, Aldo R; Champion, Eric

2017-06-06

The influence of carbonate substitution (4.4 wt%, mixed A/B type) in hydroxyapatite ceramics for bone remodeling scaffolds was investigated by separately analyzing the response of pre-osteoblasts and osteoclast-like cells. Carbonated hydroxyapatite (CHA) (Ca 9.5 (PO 4 ) 5.5 (CO 3 ) 0.5 (OH)(CO 3 ) 0.25 -CHA), mimicking the chemical composition of natural bone mineral, and pure hydroxyapatite (HA) (Ca 10 (PO 4 ) 6 (OH) 2 -HA) porous ceramics were processed to obtain a similar microstructure and surface physico-chemical properties (grain size, porosity ratio and pore size, surface roughness and zeta potential). The biological behavior was studied using MC3T3-E1 pre-osteoblastic and RAW 264.7 monocyte/macrophage cell lines. Chemical dissolution in the culture media and resorption lacunae produced by osteoclasts occur with both HA and CHA ceramics, but CHA exhibits much higher dissolution and greater bioresorption ability. CHA ceramics promoted a significantly higher level of pre-osteoblast proliferation. Osteoblastic differentiation, assessed by qRT-PCR of RUNX2 and COLIA2, and pre-osteoclastic proliferation and differentiation were not significantly different on CHA or HA ceramics but cell viability and metabolism were significantly greater on CHA ceramics. Thus, the activity of both osteoclast-like and osteoblastic cells was influenced by the carbonate substitution in the apatite structure. Furthermore, CHA showed a particularly interesting balance between biodegradation, by osteoclasts and chemical dissolution, and osteogenesis through osteoblasts' activity, to stimulate bone regeneration. It is hypothesized that this amount of 4.4 wt% carbonate substitution leads to an adapted concentration of calcium in the fluid surrounding the ceramic to stimulate the activity of cells. These results highlight the superior biological behavior of microporous 4.4 wt% A/B CHA ceramics that could beneficially replace the commonly used HA of biphasic calcium phosphates for future applications in bone tissue engineering.

Removal of Uranium in Drinking Water: Brimac Environmental Services, Inc. Brimac HA 216 Adsorptive Media

EPA Science Inventory

The Brimac HA 216 Adsorptive Media was tested for uranium (U) removal from a drinking water source (well water) at Grappone Toyota located in Bow, New Hampshire. The HA 216 media is a hydroxyapatite-based material. A pilot unit, consisting of a TIGG Corporation Cansorb® C-5 ste...

Development of gelatin-chitosan-hydroxyapatite based bioactive bone scaffold with controlled pore size and mechanical strength.

PubMed

Maji, Kanchan; Dasgupta, Sudip; Kundu, Biswanath; Bissoyi, Akalabya

2015-01-01

Hydroxyapatite-chitosan/gelatin (HA:Chi:Gel) nanocomposite scaffold has potential to serve as a template matrix to regenerate extra cellular matrix of human bone. Scaffolds with varying composition of hydroxyapatite, chitosan, and gelatin were prepared using lyophilization technique where glutaraldehyde (GTA) acted as a cross-linking agent for biopolymers. First, phase pure hydroxyapatite-chitosan nanocrystals were in situ synthesized by coprecipitation method using a solution of 2% acetic acid dissolved chitosan and aqueous solution of calcium nitrate tetrahydrate [Ca(NO3)2,4H2O] and diammonium hydrogen phosphate [(NH4)2H PO4]. Keeping solid loading constant at 30 wt% and changing the composition of the original slurry of gelatin, HA-chitosan allowed control of the pore size, its distribution, and mechanical properties of the scaffolds. Microstructural investigation by scanning electron microscopy revealed the formation of a well interconnected porous scaffold with a pore size in the range of 35-150 μm. The HA granules were uniformly dispersed in the gelatin-chitosan network. An optimal composition in terms of pore size and mechanical properties was obtained from the scaffold with an HA:Chi:Gel ratio of 21:49:30. The composite scaffold having 70% porosity with pore size distribution of 35-150 μm exhibited a compressive strength of 3.3-3.5 MPa, which is within the range of that exhibited by cancellous bone. The bioactivity of the scaffold was evaluated after conducting mesenchymal stem cell (MSC) - materials interaction and MTT (3-[4,5-dimethylthiazol-2-yl]-2,5-diphenyltetrazolium bromide) assay using MSCs. The scaffold found to be conducive to MSC's adhesion as evident from lamellipodia, filopodia extensions from cell cytoskeleton, proliferation, and differentiation up to 14 days of cell culture.

Nanoporous hydroxyapatite/sodium titanate bilayer on titanium implants for improved osteointegration.

PubMed

Carradò, A; Perrin-Schmitt, F; Le, Q V; Giraudel, M; Fischer, C; Koenig, G; Jacomine, L; Behr, L; Chalom, A; Fiette, L; Morlet, A; Pourroy, G

2017-03-01

The aim of this study was to improve the strength and quality of the titanium-hydroxyapatite interface in order to prevent long-term failure of the implanted devices originating from coating delamination and to test it in an in-vivo model. Ti disks and dental commercial implants were etched in Kroll solution. Thermochemical treatments of the acid-etched titanium were combined with sol-gel hydroxyapatite (HA) coating processes to obtain a nanoporous hydroxyapatite/sodium titanate bilayer. The sodium titanate layer was created by incorporating sodium ions onto the Ti surface during a NaOH alkaline treatment and stabilized using a heat treatment. HA layer was added by dip-coating in a sol-gel solution. The bioactivity was assessed in vitro with murine MC3T3-E1 and human SaOs-2 cells. Functional and histopathological evaluations of the coated Ti implants were performed at 22, 34 and 60days of implantation in a dog lower mandible model. Nanoporous hydroxyapatite/sodium titanate bilayer on titanium implants was sensitive neither to crack propagation nor to layer delamination. The in vitro results on murine MC3T3-E1 and human SaOs-2 cells confirm the advantage of this coating regarding the capacity of cell growth and differentiation. Signs of progressive bone incorporation, such as cancellous bone formed in contact with the implant over the existing compact bone, were notable as early as day 22. Overall, osteoconduction and osteointegration mean scores were higher for test implants compared to the controls at 22 and 34 days. Nanoporous hydroxyapatite/sodium titanate bilayer improves the in-vivo osteoconduction and osteointegration. It prevents the delamination during the screwing and it could increase HA-coated dental implant stability without adhesive failures. The combination of thermochemical treatments with dip coating is a low-cost strategy. Copyright © 2017 The Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Mixed zirconia calcium phosphate coatings for dental implants: tailoring coating stability and bioactivity potential.

PubMed

Pardun, Karoline; Treccani, Laura; Volkmann, Eike; Streckbein, Philipp; Heiss, Christian; Li Destri, Giovanni; Marletta, Giovanni; Rezwan, Kurosch

2015-03-01

Enhanced coating stability and adhesion are essential for long-term success of orthopedic and dental implants. In this study, the effect of coating composition on mechanical, physico-chemical and biological properties of coated zirconia specimens is investigated. Zirconia discs and dental screw implants are coated using the wet powder spraying (WPS) technique. The coatings are obtained by mixing yttria-stabilized zirconia (TZ) and hydroxyapatite (HA) in various ratios while a pure HA coating served as reference material. Scanning electron microscopy (SEM) and optical profilometer analysis confirm a similar coating morphology and roughness for all studied coatings, whereas the coating stability can be tailored with composition and is probed by insertion and dissections experiments in bovine bone with coated zirconia screw implants. An increasing content of calcium phosphate (CP) resulted in a decrease of mechanical and chemical stability, while the bioactivity increased in simulated body fluid (SBF). In vitro experiments with human osteoblast cells (HOB) revealed that the cells grew well on all samples but are affected by dissolution behavior of the studied coatings. This work demonstrates the overall good mechanical strength, the excellent interfacial bonding and the bioactivity potential of coatings with higher TZ contents, which provide a highly interesting coating for dental implants. Copyright © 2014 Elsevier B.V. All rights reserved.

Nucleation and growth of hydroxyapatite on arc-deposited TiO2 surfaces studied by quartz crystal microbalance with dissipation

NASA Astrophysics Data System (ADS)

Lilja, Mirjam; Butt, Umer; Shen, Zhijian; Bjöörn, Dorota

2013-11-01

Understanding of nucleation and growth kinetics of biomimetically deposited hydroxyapatite (HA) on crystalline TiO2 surfaces is important with respect to the application and performance of HA as functional implant coatings. Arc-evaporation was used to deposit TiO2 coatings dominated by anatase phase, rutile phase or their mixtures. Subsequent formation of HA from phosphate buffered saline solution (PBS) was investigated in real-time using in situ quartz crystal microbalance with dissipation technique (QCM-D). Scanning electron microscopy (SEM) and X-ray diffraction (XRD) were employed to characterize the presence, morphology and crystal structure of TiO2 coatings and the formed HA. Increasing temperature of the PBS, increasing flow rate and applying a higher ion concentration in solution were found to accelerate HA nucleation process and hence affect growth kinetics. Lower PBS temperature resulted in the formation of HA coatings with flake-like morphology and increasing HA porosity. All TiO2 coatings under study enabled HA formation at body temperature, while in contrast Ti reference surfaces only supported HA nucleation and growth at elevated temperatures. QCM-D technique is a powerful tool for studying the impact of process parameters during biomimetic coating deposition on coating structure evolution in real time and provides valuable information for understanding, optimizing as well as tailoring the biomimetic HA growth processes.

Synthesis and investigation of physico-chemical, antibacterial, biomymetic properties of silver and zinc containing hydroxyapatite

NASA Astrophysics Data System (ADS)

Zhuk, Ilya; Rasskazova, Lyudmila; Korotchenko, Natalia; Kozik, Vladimir; Kurzina, Irina

2017-11-01

In the work we carried out microwave synthesis of modified hydroxyapatites (HA) with different content of ions. A solid solution based on HA remains a single-phase sample when the calcium ions are substituted by silver and zinc ions up to 5 % by weight (0.5 mole fraction). The microstructure parameters, morphology and the particle powders size were studied by X-ray diffraction analysis, IR spectroscopy, and scanning electron microscopy (SEM). It is shown that the modification of HA by silver (AgHA) and zinc (ZnHA) ions increases the size of its particles, the degree of crystallinity, and the pore sizes of the samples while reducing their specific surface and uniformity of their forms. Elemental analysis and distribution of elements over the surface of HA, AgHA, and ZnHA powders were performed by X-ray spectral microanalysis (RSMA). The ratio of Ca/P is within the range of 1.66-1.77 and corresponds to the ratio of Ca/P in stoichiometric HA and the HA entering bone tissue. The ability of AgHA- and ZnHA-substrates to form on their surface a calcium-phosphate layer from the simulated body fluid (SBF) at 37 °C is determined. This ability decreases in the order: in ZnHA it is less than in AgHA, but greater than in HA. The antibacterial activity of the samples was analyzed. The AgHA sample has both bactericidal and persistent bacteriostatic properties in the case of direct contact with Escherichia coli cells.

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

PubMed Central

Lou, Weiwei; Dong, Yiwen; Zhang, Hualin; Jin, Yifan; Hu, Xiaohui; Ma, Jianfeng; Liu, Jinsong; Wu, Gang

2015-01-01

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. PMID:26404255

Template-directed hydrothermal synthesis of hydroxyapatite as a drug delivery system for the poorly water-soluble drug carvedilol

NASA Astrophysics Data System (ADS)

Zhao, Qinfu; Wang, Tianyi; Wang, Jing; Zheng, Li; Jiang, Tongying; Cheng, Gang; Wang, Siling

2011-09-01

In order to improve the dissolution rate and increase the bioavailability of a poorly water-soluble drug, intended to be administered orally, the biocompatible and bioactive mesoporous hydroxyapatite (HA) was successfully synthesized. In the present study, mesoporous HA nanoparticles were produced using Pluronic block co-polymer F127 and cetyltrimethylammonium bromide (CTAB) as templates by the hydrothermal method. The obtained mesoporous HA was employed as a drug delivery carrier to investigate the drug storage/release properties using carvedilol (CAR) as a model drug. Characterizations of the raw CAR powder, mesoporous HA and CAR-loaded HA were carried out by the scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray powder diffraction (XRPD), differential scanning calorimetry (DSC), Fourier transform infrared (FT-IR) spectroscopy, N2 adsorption/desorption, thermogravimetric analysis (TGA), and UV-VIS spectrophotometry. The results demonstrated that CAR was successfully incorporated into the mesoporous HA host. In vitro drug release studies showed that mesoporous HA had a high drug load efficiency and provided immediate release of CAR compared with micronized raw drug in simulated gastric fluid (pH 1.2) and intestinal fluid (pH 6.8). Consequently, mesoporous HA is a good candidate as a drug carrier for the oral delivery of poorly water-soluble drugs.

Evaluation of nanoparticles of hydroxyapatite and MWCNT’s in scaffolds of poly lactic acid

NASA Astrophysics Data System (ADS)

Román-Doval, R.; Morales-Corona, J.; Olayo, R.; Escamilla-Rivera, V.; Uribe-Ramírez, M.; Ortega-López, M.

2016-12-01

In the tissue engineering, the cytotoxicity test is an important part of the biomaterials performance. This research reports the production and characterization of polylactic acid (PLA)-supported hydroxyapatite (HA) and multiwalled carbon nanotubes (MWCNT) scaffolds as a bone graft material. Samples containing different HA/MWCNT wt% ratios were prepared by electrospinning. The obtained samples displayed valuable characteristics for the cell adhesion because of their porous-spongy bone-like morphology. The Fourier transforms infrared and Raman analyses indicated no chemical interaction of HA and MWCNT with PLA molecules, but they appear to be only embedded into the PLA fibers. As indicated by x-ray diffraction, crystalline HA and MWCNT’s are supported in the amorphous PLA fibers. Under tensile stress, scaffolds display a Young’s Modulus about 86 MPa, whilst the scaffolds resistance increases with the HA-MWCNT’s ratio. However, the MTS in-vitro assays using the hFOB 1.19 (ATCC CRL-11372) cells, for cell exposure time of 24 and 48 h, revealed that viability reduces for HA-MWCNT’s ratio values over 25 wt%. Our results suggest that a maximum HA/MWCNT’s ratio of 19:1 could be acceptable for cell proliferation while maintaining HA at 200 mg.

Silver/hydroxyapatite composite coatings on porous titanium surfaces by sol-gel method.

PubMed

Qu, Jie; Lu, Xiong; Li, Dan; Ding, Yonghui; Leng, Yang; Weng, Jie; Qu, Shuxin; Feng, Bo; Watari, Fumio

2011-04-01

Hydroxyapatite (HA) coatings loaded with nanosilver particles is an attractive method to impart the HA coating with antibacterial properties. Producing Ag/HA coatings on porous Ti substrates have been an arduous job since commonly used line-of-sight techniques are not able to deposit uniform coatings on the inner pore surfaces of the porous Ti. In this study, porous Ti scaffolds with high porosity and interconnected structures were prepared by polymer impregnating method. A sol-gel process was used to produce uniform Ag/HA composite coatings on the surfaces of porous Ti substrates. Ca(NO(3) )(2) ·4H(2) O and P(2) O(5) in an ethyl alcohol based system was selected to prepare the sol, which ensured the homogeneous distribution of Ag in the sol. The characterization revealed that silver particles uniformly distributed in the coatings without agglomeration. High antibacterial ratio (>95%), against E. coli and S. albus was expressed by the silver-containing coatings (Ag/HA 0.8 and 1.6 wt %). The biocompatibility of the Ag/HA 0.8 surfaces was as good as that of pure HA surface, as revealed by culturing osteoblasts on them. The results indicated that Ag/HA 0.8 had the good balance between the biocompatibility and antibacterial properties of the coatings. Copyright © 2011 Wiley Periodicals, Inc.

Comparison of nanoparticular hydroxyapatite pastes of different particle content and size in a novel scapula defect model

PubMed Central

Hruschka, Veronika; Tangl, Stefan; Ryabenkova, Yulia; Heimel, Patrick; Barnewitz, Dirk; Möbus, Günter; Keibl, Claudia; Ferguson, James; Quadros, Paulo; Miller, Cheryl; Goodchild, Rebecca; Austin, Wayne; Redl, Heinz; Nau, Thomas

2017-01-01

Nanocrystalline hydroxyapatite (HA) has good biocompatibility and the potential to support bone formation. It represents a promising alternative to autologous bone grafting, which is considered the current gold standard for the treatment of low weight bearing bone defects. The purpose of this study was to compare three bone substitute pastes of different HA content and particle size with autologous bone and empty defects, at two time points (6 and 12 months) in an ovine scapula drillhole model using micro-CT, histology and histomorphometry evaluation. The nHA-LC (38% HA content) paste supported bone formation with a high defect bridging-rate. Compared to nHA-LC, Ostim® (35% HA content) showed less and smaller particle agglomerates but also a reduced defect bridging-rate due to its fast degradation The highly concentrated nHA-HC paste (48% HA content) formed oversized particle agglomerates which supported the defect bridging but left little space for bone formation in the defect site. Interestingly, the gold standard treatment of the defect site with autologous bone tissue did not improve bone formation or defect bridging compared to the empty control. We concluded that the material resorption and bone formation was highly impacted by the particle-specific agglomeration behaviour in this study. PMID:28233833

Facile synthesis of both needle-like and spherical hydroxyapatite nanoparticles: effect of synthetic temperature and calcination on morphology, crystallite size and crystallinity.

PubMed

Wijesinghe, W P S L; Mantilaka, M M M G P G; Premalal, E V A; Herath, H M T U; Mahalingam, S; Edirisinghe, M; Rajapakse, R P V J; Rajapakse, R M G

2014-09-01

Synthetic hydroxyapatite (HA) nanoparticles, that mimic natural HA, are widely used as biocompatible coatings on prostheses to repair and substitute human bones. In this study, HA nanoparticles are prepared by precipitating them from a precursor solution containing calcium sucrate and ammonium dihydrogen orthophosphate, at a Ca/P mole ratio of 1.67:1, at temperatures, ranging from 10°C to 95°C. A set of products, prepared at different temperatures, is analyzed for their crystallinity, crystallite size, morphology, thermal stability and composition, by X-ray diffraction (XRD), scanning electron microscopy (SEM), thermogravimetric analysis (TGA) and Fourier transform infrared (FT-IR) spectroscopic techniques, while the other set is analyzed after calcining the respective products, soon after their synthesis, for 3h, at 700°C. The as-prepared products, after 2h of drying, without any calcination, are not crystalline, but they grow very slowly into needle-like morphologies, as they are ripened with time. The percentage crystallinity of the final products increases from 15% to 52%, with increasing the preparative temperature. The calcined samples always produce spherical nanoparticles of essentially the same diameter, between 90 nm and 100 nm, which does not change due to aging and preparative temperatures. Therefore, the same method can be utilized to synthesize both spherical and needle-like nanoparticles of hydroxyapatite, with well-defined sizes and shapes. The ability to use readily available cheap raw materials, for the synthesis of such well-defined crystallites of hydroxyapatite, is an added advantage of this method, which may be explored further for the scaling up of the procedures to suit to industrial scale synthesis of such hydroxyapatite nanoparticles. Copyright © 2014 Elsevier B.V. All rights reserved.

Nano hydroxyapatite-blasted titanium surface affects pre-osteoblast morphology by modulating critical intracellular pathways.

PubMed

Bezerra, Fábio; Ferreira, Marcel R; Fontes, Giselle N; da Costa Fernandes, Célio Jr; Andia, Denise C; Cruz, Nilson C; da Silva, Rodrigo A; Zambuzzi, Willian F

2017-08-01

Although, intracellular signaling pathways are proposed to predict the quality of cell-surface relationship, this study addressed pre-osteoblast behavior in response to nano hydroxyapatite (HA)-blasted titanium (Ti) surface by exploring critical intracellular pathways and pre-osteoblast morphological change. Physicochemical properties were evaluated by atomic force microscopy (AFM) and wettability considering water contact angle of three differently texturized Ti surfaces: Machined (Mac), Dual acid-etching (DAE), and nano hydroxyapatite-blasted (nHA). The results revealed critical differences in surface topography, impacting the water contact angle and later the osteoblast performance. In order to evaluate the effect of those topographical characteristics on biological responses, we have seeded pre-osteoblast cells on the Ti discs for up to 4 h and subjected the cultures to biological analysis. First, we have observed pre-osteoblasts morphological changes resulting from the interaction with the Ti texturized surfaces whereas the cells cultured on nHA presented a more advanced spreading process when compared with the cells cultured on the other surfaces. These results argued us for analyzing the molecular machinery and thus, we have shown that nHA promoted a lower Bax/Bcl2 ratio, suggesting an interesting anti-apoptotic effect, maybe explained by the fact that HA is a natural element present in bone composition. Thereafter, we investigated the potential effect of those surfaces on promoting pre-osteoblast adhesion and survival signaling by performing crystal violet and immunoblotting approaches, respectively. Our results showed that nHA promoted a higher pre-osteoblast adhesion supported by up-modulating FAK and Src activations, both signaling transducers involved during eukaryotic cell adhesion. Also, we have shown Ras-Erk stimulation by the all evaluated surfaces. Finally, we showed that all Ti-texturing surfaces were able to promote osteoblast differentiation up to 10 days, when alkaline phosphatase (ALP) activity and osteogenic transcription factors were up-modulated. Altogether, our results showed for the first time that nano hydroxyapatite-blasted titanium surface promotes crucial intracellular signaling network responsible for cell adapting on the Ti-surface.Biotechnol. Bioeng. 2017;114: 1888-1898. © 2017 Wiley Periodicals, Inc. © 2017 Wiley Periodicals, Inc.

Hydroxyapatite clay for gap filling and adequate bone ingrowth.

PubMed

Maruyama, M; Terayama, K; Ito, M; Takei, T; Kitagawa, E

1995-03-01

In uncemented total hip arthroplasty, a complete filling of the gap between femoral prosthesis and the host bone is difficult and defects would remain, because the anatomy of the reamed intramedullary canal cannot fit the prosthesis. Therefore, it seems practical to fill the gap with a clay containing hydroxyapatite (HA), which has an osteoconductive character. The clay (HA clay) is made by mixing HA granules (size 0.1 mm or more) having a homogeneous pore distribution and a porosity of 35-48 vol%, and a viscous substance such as a saline solution of sodium alginate (SSSA). In the first experiment, the ratio of HA granules and sodium alginate in SSSA is set for the same handling properties of HA clay and polymethylmethacrylate bone cement (standard viscosity) before hardening. As a result, the ratio is set for 55 wt% of HA in the clay and 12.5 wt% of sodium alginate in SSSA (i.e., HA:sodium alginate:saline solution = 9.8:1:7). In the second study, the gap between the femoral stem and bone model is completely filled with HA clay. However, the gap is not filled only with HA granules or HA granules mixed with saline solution. In the third animal experiment, using an unloaded model, histology shows that HA clay has an osteoconductive property bridging the gap between the implant and the cortical bone without any adverse reaction. HA clay is considered a useful biomaterial to fill the gap with adequate bone ingrowth.

In vitro characterisation of a sol-gel derived in situ silica-coated silicate and carbonate co-doped hydroxyapatite nanopowder for bone grafting.

PubMed

Latifi, Seyed Mohsen; Fathi, Mohammadhossein; Sharifnabi, Ali; Varshosaz, Jaleh

2017-06-01

Design and synthesis of materials with better properties and performance are essential requirements in the field of biomaterials science that would directly improve patient quality of life. For this purpose, in situ silica-coated silicate and carbonate co-doped hydroxyapatite (Sc/S.C.HA) nanopowder was synthesized via the sol-gel method. Characterisation of the prepared nanopowder was carried out by XRD, FTIR, TEM, SEM, EDX, ICP, zeta potential, acid dissolution test, and cell culture test. The substitution of the silicate and carbonate ions into hydroxyapatite structure was confirmed by FTIR analysis. XRD analysis showed that silica is an amorphous phase, which played a role in covering the surface of the S.C.HA nanoparticles as confirmed by acid dissolution test. Low thickness and low integrity of the amorphous silica surface layer facilitated ions release from S.C.HA nanoparticles into physiological saline solution. Zeta potential of the prepared nanopowder suspended in physiological saline solution was -27.3±0.2mV at pH7.4. This negatively charged surface, due to the presence of amorphous silica layer upon the S.C.HA nanoparticles, not only had an accelerating effect on in vitro biomineralization of apatite, but also had a positive effect on cell attachment. Copyright © 2017 Elsevier B.V. All rights reserved.

Sectioning studies of biomimetic collagen-hydroxyapatite coatings on Ti-6Al-4V substrates using focused ion beam

NASA Astrophysics Data System (ADS)

Hu, Changmin; Yu, Le; Wei, Mei

2018-06-01

A biomimetic bone-like collagen-hydroxyapatite (Col-HA) composite coating was formed on a surface-treated Ti-6Al-4V alloy substrate via simultaneous collagen self-assembly and hydroxyapatite nucleation. The coating process has been carried out by immersing sand-blasted, acid-etched and UV irradiated Ti-6Al-4V alloy in type I collagen-containing modified simulated body fluid (m-SBF). The surface morphology and phase composition of the coating were characterized using various techniques. More importantly, dual-beam FIB/SEMs with either gallium ion source (GFIB) or xenon plasma ion source (PFIB) were used to investigate the cross-sectional features of the biomimetic Col-HA composite coating in great details. As a result, the cross-sectional images and thin transmission electron microscopy (TEM) specimens were successfully obtained from the composite coating with no obvious damages or milling ion implantations. Both the cross-sectional SEM and TEM results have confirmed that the Col-HA coating demonstrates a similar microstructure to that of pure HA coating with homogeneously distributed elements across the whole cross section. Both coatings consist of a uniform, crack-free gradient structure with a dense layer adjacent to the interface between the Ti-6Al-4V substrate and the coating facilitating a strong bonding, while a porous structure at the coating surface aiding cell attachment.

Coating hydroxiapatite on stainless steel 316 L by using sago starch as binder with dip-coating method

NASA Astrophysics Data System (ADS)

Fadli, A.; Akbar, F.; Prabowo, A.; Hidayah, P. H.

2018-04-01

Hydroxyapatite (HA) is a mineral form of naturally occurring apatite calcium with Ca10(PO4)6(OH)2 formula. One of the major innovations in the field of bone reconstruction is to apply HA as a surface coating on a mechanically strong implant metal and to improve the stability of bone implants thereby increasing the lifetime of the metal implants. Pure hydroxyapatite has poor mechanical properties so it is necessary to add sago starch as a binder to combine the strength and hardness of metal surfaces with bioactive properties of hydroxyapatite by Dip Coating method. Stainless steel 316L is the most commonly used alloy as an implant for bones and teeth due to its excellent corrosion and oxidation resistance and is easily formed. In this study, hydroxyapatite coatings used fixed variables as hydroxyapatite mass (10 grams), aquades mass (20 grams), dipping time (20 seconds), and calcination conditions (800°C, 1 hour). The variables are sago starch mass (1, 1.25, 1.5 gram) and stirring time (16, 20, 24 hours). The shear strength value is higher in the addition of 1.25, 10, 20, and again in the binder ratio of 1.5; 10; 20. The addition of stirring time causes a decrease in shear strength. The highest shear strength value obtained was 3.07 MPa. The layer attached to the substrate is a hydroxyapatite with a composition of 99.4% as evidenced by the results of XRD analysis.

Behavior of osteoblast-like cells on calcium-deficient hydroxyapatite ceramics composed of particles with different shapes and sizes.

PubMed

Kamitakahara, Masanobu; Uno, Yuika; Ioku, Koji

2014-01-01

In designing the biomaterials, it is important to control their surface morphologies, because they affect the interactions between the materials and cells. We previously reported that porous calcium-deficient hydroxyapatite (HA) ceramics composed of rod-like particles had advantages over sintered porous HA ceramics; however, the effects of the surface morphology of calcium-deficient HA ceramics on cell behavior have remained unclear. Using a hydrothermal process, we successfully prepared porous calcium-deficient HA ceramics with different surface morphologies, composed of plate-like particles of 200-300, 500-800 nm, or 2-3 μm in width and rod-like particles of 1 or 3-5 μm in width, respectively. The effects of these surface morphologies on the behavior of osteoblast-like cells were examined. Although the numbers of cells adhered to the ceramic specimens did not differ significantly among the specimens, the proliferation rates of cells on the ceramics decreased with decreasing particle size. Our results reveal that controlling the surface morphology that is governed by particle shape and size is important for designing porous calcium-deficient HA ceramics.

Fabrication and characterization of electrospun cellulose/nano-hydroxyapatite nanofibers for bone tissue engineering.

PubMed

Ao, Chenghong; Niu, Yan; Zhang, Ximu; He, Xu; Zhang, Wei; Lu, Canhui

2017-04-01

Nanofibrous scaffolds from cotton cellulose and nano-hydroxyapatite (nano-HA) were electrospun for bone tissue engineering. The solution properties of cellulose/nano-HA spinning dopes and their associated electrospinnability were characterized. Morphological, thermal and mechanical properties of the electrospun cellulose/nano-HA nanocomposite nanofibers (ECHNN) were measured and the biocompatibility of ECHNN with human dental follicle cells (HDFCs) was evaluated. Scanning electron microscope (SEM) images indicated that the average diameter of ECHNN increased with a higher nano-HA loading and the fiber diameter distributions were well within the range of natural ECM (extra cellular matrix) fibers (50-500nm). The ECHNN exhibited extraordinary mechanical properties with a tensile strength and a Young's modulus up to 70.6MPa and 3.12GPa respectively. Moreover, it was discovered that the thermostability of the ECHNN could be enhanced with the incorporation of nano-HA. Cell culture experiments demonstrated that the ECHNN scaffolds were quite biocompatible for HDFCs attachment and proliferation, suggesting their great potentials as scaffold materials in bone tissue engineering. Copyright © 2017 Elsevier B.V. All rights reserved.

An efficient method to prepare magnetic hydroxyapatite-functionalized multi-walled carbon nanotubes nanocomposite for bone defects.

PubMed

Afroze, J D; Abden, M J; Islam, M A

2018-05-01

Hydroxyapatite-functionalized multi-walled carbon nanotube (HA-fMWCNT) magnetic nanocomposite was successfully prepared using a novel slurry-compounding method. The prepared HA-fMWCNT nanocomposite with the addition of small amount (0.5 wt%) of fMWCNT exhibited much greater improvement in mechanical properties due to strong interfacial adhesion between acid-treated MWCNTs fillers and HA matrix, thus efficient stress transfer to nanotubes from the matrix. The nanocomposite exhibited excellent haemocompatibility. Fractographic analysis was performed in order to understand the fracture behavior and toughening mechanisms. The fracture mechanisms and micro-deformation were examined by studying the microstructure of arrested crack tips using field emission scanning electron microscopy (FESEM). The origination and formation of micro-cracks are the dominant fracture mechanisms and micro-deformation in the HA-fMWCNTs nanocomposite. The developed new method enables to the fabrication of magnetic HA-fMWCNTs nanocomposite with superior mechanical performance may be potential for application as high load-bearing bone implants in the biomedical field. Copyright © 2018 Elsevier B.V. All rights reserved.

Mechanochemical Synthesis of Hydroxyapatite and Its Modifications: Composition, Structure, and Properties

NASA Astrophysics Data System (ADS)

Chaikina, M. V.; Bulina, N. V.; Ishchenko, A. V.; Prosanov, I. Yu.

2014-02-01

The mechanochemical method is used to synthesize samples of hydroxyapatite (HA) with substitution of the phosphate ion by silicate and zirconate ions, and substitution of calcium ions by copper ions. In the process of mechanochemical synthesis, carbonate ions and water molecules are incorporated into the structure of HA due to interaction of components of the reaction mixture with air. Intrusion of carbonate into the structure of HA is a competing process with modification of apatite by silicate and zirconate anions; therefore, the composition of the product during synthesis differs from the prescribed one. After annealing of the samples, the composition of the anion-modified HA can be described by the formula Са10(РО4)6- х (АО4) х (ОН)2- х , where (АО4)4- is the modifying anion. Substitution of calcium by copper ions localized at the Са1 position has been detected. Silver ions are not incorporated into the structure of HA, but are distributed in the apatite matrix in the form of nanocrystals of metallic silver.

Synthesis, structure and temperature dependent luminescence of Eu3+ doped hydroxyapatite

NASA Astrophysics Data System (ADS)

Luo, Xiaobing; Luo, Xiaoxia; Wang, Hongwei; Deng, Yue; Yang, Peixin; Tian, Yili

2018-01-01

A series of Eu3+ substituted hydroxyapatite (HA) were prepared by co-precipitation reactions. The phase, fluorescence and temperature dependent luminescence of the phosphors were investigated by X-ray diffraction (XRD) and photoluminescence (PL). It is found that the doped Eu3+ ions have entered the hexagonal lattice with no obvious secondary phase were detected by XRD. The 5D0 → 7F0 transition was clearly split into two even at room temperature. The predominate 573 nm peak illustrates Eu3+ ions occupy more Ca(II) sites. The temperature dependent luminescent results show HA:xEu might be applied as one potential optical thermometry material.

Sol-Gel Derived Hydroxyapatite Coating on Mg-3Zn Alloy for Orthopedic Application

NASA Astrophysics Data System (ADS)

Singh, Sanjay; Manoj Kumar, R.; Kuntal, Kishor Kumar; Gupta, Pallavi; Das, Snehashish; Jayaganthan, R.; Roy, Partha; Lahiri, Debrupa

2015-04-01

In recent years, magnesium and its alloys have gained a lot of interest as orthopedic implant constituents because their biodegradability and mechanical properties are closer to that of human bone. However, one major concern with Mg in orthopedics is its high corrosion rate that results in the reduction of mechanical integrity before healing the bone tissue. The current study evaluates the sol-gel-derived hydroxyapatite (HA) coating on a selected Mg alloy (Mg-3Zn) for decreasing the corrosion rate and increasing the bioactivity of the Mg surface. The mechanical integrity of the coating is established as a function of the surface roughness of the substrate and the sintering temperature of the coating. Coating on a substrate roughness of 15-20 nm and sintering at 400°C shows the mechanical properties in similar range of bone, thus making it suitable to avoid the stress-shielding effect. The hydroxyapatite coating on the Mg alloy surface also increases corrosion resistance very significantly by 40 times. Bone cells are also found proliferating better in the HA-coated surface. All these benefits together establish the candidature of sol-gel HA-coated Mg-3Zn alloy in orthopedic application.

Direct cytotoxicity evaluation of 63S bioactive glass and bone-derived hydroxyapatite particles using yeast model and human chondrocyte cells by microcalorimetry.

PubMed

Doostmohammadi, A; Monshi, A; Fathi, M H; Karbasi, S; Braissant, O; Daniels, A U

2011-10-01

In this study, the cytotoxicity evaluation of prepared 63S bioactive glass and bone-derived hydroxyapatite particles with yeast and human chondrocyte cells was carried out using isothermal micro-nano calorimetry (IMNC), which is a new method for studying cell/biomaterial interactions. Bioactive glass particles were made via sol-gel method and hydroxyapatite was obtained from bovine bone. Elemental analysis was carried out by XRF and EDXRF. Amorphous structure of the glass and completely crystalline structure of HA were detected by XRD analysis. Finally, the cytotoxicity of bioactive glass and bone-derived HA particles with yeast and cultured human chondrocyte cells was evaluated using IMNC. The results confirmed the viability, growth and proliferation of human chondrocyte cells in contact with 63S bioactive glass, and bone-derived HA particles. Also the results indicated that yeast model which is much easier to handle, can be considered as a good proxy and can provide a rapid primary estimate of the ranges to be used in assays involving human cells. All of these results confirmed that IMNC is a convenient method which caters to measuring the cell-biomaterial interactions alongside the current methods.

A combined chitosan/nano-size hydroxyapatite system for the controlled release of icariin.

PubMed

Fan, Junjun; Bi, Long; Wu, Tao; Cao, Liangguo; Wang, Dexin; Nan, Kaihui; Chen, Jingdi; Jin, Dan; Jiang, Shan; Pei, Guoxian

2012-02-01

Icariin, a plant-derived flavonol glycoside, has been proved as an osteoinductive agent for bone regeneration. For this reason, we developed an icariin-loaded chitosan/nano-sized hydroxyapatite (IC-CS/HA) system which controls the release kinetics of icariin to enhance bone repairing. First, by Fourier transform infrared spectroscopy, we found that icariin was stable in the system developed without undergoing any chemical changes. On the other hand, X-ray diffraction, scanning electron microscopy and mechanical test revealed that the introduction of icariin did not remarkably change the phase, morphology, porosity and mechanical strength of the CS/HA composite. Then the hydrolytic degradation and drug release kinetics in vitro were investigated by incubation in phosphate buffered saline solution. The results indicated that the icariin was released in a temporally controlled manner and the release kinetics could be governed by degradation of both chitosan and hydroxyapatite matrix. Finally the in vitro bioactivity assay revealed that the loaded icariin was biologically active as evidenced by stimulation of bone marrow derived stroma cell alkaline phosphatase activity and formation of mineralized nodules. This successful IC-CS/HA system offers a new delivery method of osteoinductive agents and a useful scaffold design for bone regeneration.

Effects of nozzle types and 2,4-D formulations on spray deposition.

PubMed

Contiero, Robinson L; Biffe, Denis F; Constantin, Jamil; de Oliveira, Rubem S; Braz, Guilherme B P; Lucio, Felipe R; Schleier, Jerome J

2016-12-01

The objective of this study was to evaluate the effects of nozzle types and 2,4-D formulations on spray deposition on different targets. Two field experiments were carried out in a completely randomized design, and treatments were arranged in a factorial scheme. Species in experiment 1 were Sumatran fleabane (Conyza sumatrensis) and Brazil pusley (Richardia brasiliensis) and in experiment 2 were soybeans (Glycine max) and Benghal dayflower (Commelina benghalensis). For both experiments, the first factor corresponded to spray nozzles with different settings (AD 110.015 - 61 and 105 L ha -1 ; AD 015-D - 75 and 146 L ha -1 ; XR 110.0202 - 200 L ha -1 ; and ADIA-D 110.02 - 208 L ha -1 ) and the second factor consisted of two formulations of 2,4-D (amine and choline). The formulation of 2,4-D choline has contained Colex-D™ Technology. Similar or higher spray deposition was observed on the leaves and artificial targets when using 2,4-D choline as compared to the 2,4-D amine formulation, and these differences in deposition were more evident for nozzles applying lower spray volumes. Deposition was more affected by nozzle type when amine formulation was used, compared to choline formulation.

Development and characterization of titanium-containing hydroxyapatite for medical applications.

PubMed

Huang, J; Best, S M; Bonfield, W; Buckland, Tom

2010-01-01

Hydroxyapatite containing levels of titanium (TiHA) of up to 1.6 wt.% has been produced via a chemical co-precipitation route. The distribution of Ti was seen by transmission electron microscopy/energy-dispersive X-ray analysis to be uniform throughout as-prepared nanosized TiHA particles (20 nm x 100 nm). The incorporation of Ti into the HA structure was found to influence the ceramic microstructure on sintering and the grain size was found to decrease from 0.89 microm with HA to 0.63 microm with 0.8 wt.% TiHA (0.8 TiHA) and 0.45 microm with 1.6 wt.% TiHA (1.6 TiHA). Rietveld refinement analysis showed that there was a proportional increase in both the a and c axis with incorporation of Ti into the HA lattice structure, leading to an increase in the cell volume with the addition of Ti. Fourier transform-Raman analysis showed a slight increase in the ratio of O-H/P-O peaks on TiHA, in comparison with HA. A bone-like apatite layer was formed on the surface of TiHA after immersion in simulated body fluid for 3 days, which demonstrated the high in vitro bioactivity of TiHA. In vitro culture with primary human osteoblast (HOB) cells revealed that TiHA was able to support the growth and proliferation of HOB cells in vitro, with a significantly higher cell activity being observed on 0.8 TiHA after 7 days of culture in comparison with that on HA. Well-organized actin cytoskeletal protein was developed after 1 day of culture, and an increase in cell filopodia (attachment) was observed on TiHA sample surfaces. The results indicate that TiHA has great potential for biomedical applications.

Diversity of multinucleated giant cells by microstructures of hydroxyapatite and plasma components in extraskeletal implantation model.

PubMed

Morishita, Kota; Tatsukawa, Eri; Shibata, Yasuaki; Suehiro, Fumio; Kamitakahara, Masanobu; Yokoi, Taishi; Ioku, Koji; Umeda, Masahiro; Nishimura, Masahiro; Ikeda, Tohru

2016-07-15

Foreign body giant cells (FBGCs) and osteoclasts are multinucleated giant cells (MNGCs), both of which are formed by the fusion of macrophage-derived mononuclear cells. Osteoclasts are distinct from FBGCs due to their bone resorption ability; however, not only morphological, but also functional similarities may exist between these cells. The characterization and diversity of FBGCs that appear in an in vivo foreign body reaction currently remain incomplete. In the present study, we investigated an in vivo foreign body reaction using an extraskeletal implantation model of hydroxyapatite (HA) with different microstructures. The implantation of HA granules in rat subcutaneous tissue induced a foreign body reaction that was accompanied by various MNGCs. HA granules composed of rod-shaped particles predominantly induced cathepsin K (CTSK)-positive FBGCs, whereas HA granules composed of globular-shaped particles predominantly induced CTSK-negative FBGCs. Plasma, which was used as the binder of ceramic granules, stimulated the induction of CTSK-positive FBGCs more strongly than purified fibrin. Furthermore, the implantation of HA composed of rod-shaped particles with plasma induced tartrate-resistant acid phosphatase (TRAP)-positive MNGCs in contrast to HA composed of globular-shaped particles with purified fibrin, which predominantly induced CTSK-negative and TRAP-negative typical FBGCs. These results suggest that CTSK-positive, TRAP-positive, and CTSK- and TRAP-negative MNGCs are induced in this subcutaneous implantation model in a manner that is dependent on the microstructure of HA and presence or absence of plasma. We attempted to elucidate the mechanisms responsible for the foreign body reaction induced by the implantation of hydroxyapatite granules with different microstructures in rat subcutaneous tissue with or without plasma components as the binder of ceramic granules. By analyzing the expression of two reliable osteoclast markers, we detected tartrate-resistant acid phosphatase-positive multinucleated giant cells, cathepsin K-positive multinucleated giant cells, and tartrate-resistant acid phosphatase- and cathepsin K-negative multinucleated giant cells. The induction of tartrate-resistant acid phosphatase-positive multinucleated giant cells was plasma component-dependent while the induction of cathepsin K-positive multinucleated giant cells was influenced by the microstructure of hydroxyapatite. This is the first study to show the conditions dividing the three kinds of multinucleated giant cells in the foreign body reaction. Copyright © 2016 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Biomedical potential of chitosan/HA and chitosan/β-1,3-glucan/HA biomaterials as scaffolds for bone regeneration--A comparative study.

PubMed

Przekora, Agata; Palka, Krzysztof; Ginalska, Grazyna

2016-01-01

The aim of this work was to compare biomedical potential of chitosan/hydroxyapatite (chit/HA) and novel chitosan/β-1,3-glucan/hydroxyapatite (chit/glu/HA) materials as scaffolds for bone regeneration via characterization of their biocompatibility, porosity, mechanical properties, and water uptake behaviour. Biocompatibility of the scaffolds was assessed in direct-contact with the materials using normal human foetal osteoblast cell line. Cytotoxicity and osteoblast proliferation rate were evaluated. Porosity was assessed using computed microtomography analysis and mechanical properties were determined by compression testing. Obtained results demonstrated that chit/HA scaffold possessed significantly better mechanical properties (compressive strength: 1.23 MPa, Young's modulus: 0.46 MPa) than chit/glu/HA material (compressive strength: 0.26 MPa, Young's modulus: 0.25 MPa). However, addition of bacterial β-1,3-glucan to the chit/HA scaffold improved its flexibility and porosity. Moreover, chit/glu/HA scaffold revealed significantly higher water uptake capability (52.6% after 24h of soaking) compared to the chit/HA (30.7%) and thus can serve as a very good drug delivery carrier. Chit/glu/HA scaffold was also more favourable to osteoblast survival (near 100% viability after 24-h culture), proliferation, and spreading compared to the chit/HA (63% viability). The chit/glu/HA possesses better biomedical potential than chit/HA scaffold. Nevertheless, poor mechanical properties of the chit/glu/HA limit its application to non-load bearing implantation area. Copyright © 2015 Elsevier B.V. All rights reserved.

Mechanical parameters of strontium doped hydroxyapatite sintered using microwave and conventional methods.

PubMed

Curran, Declan J; Fleming, Thomas J; Towler, Mark R; Hampshire, Stuart

2011-11-01

The effects of ion substitution in hydroxyapatite (HA) on crystal structure and lattice stability is investigated in the green state and post sintering. The effects of ion incorporation on the biaxial flexural strength and hardness are also investigated. Sintering is carried out at 1200 °C using comparative conventional and microwave regimes. Post sintering, the effects of ion incorporation manifest as an increase in the lattice d-spacings and a reduction of the crystallite size. Some HA decomposition occurs with β-TCP stabilisation in conventional sintering (CS), but this phase is destabilised during microwave sintering (MS), generating α-TCP. Conventional sintering (CS) allows higher densification in the undoped samples. Overall, for the Sr-doped compositions, the MS samples retain higher amounts of HA and experience higher density levels compared to the CS samples. Published by Elsevier Ltd.

Electrophoretic deposition and electrochemical behavior of novel graphene oxide-hyaluronic acid-hydroxyapatite nanocomposite coatings

NASA Astrophysics Data System (ADS)

Li, Ming; Liu, Qian; Jia, Zhaojun; Xu, Xuchen; Shi, Yuying; Cheng, Yan; Zheng, Yufeng; Xi, Tingfei; Wei, Shicheng

2013-11-01

Novel ternary graphene oxide-hyaluronic acid-hydroxyapatite (GO-HY-HA) nanocomposite coatings were prepared on Ti substrate using anodic electrophoretic deposition (EPD). Hyaluronic acid was employed as charging additive and dispersion agent during EPD. The kinetics and mechanism of the deposition, and the microstructure of the coated samples were investigated using scanning electron microscopy, X-ray diffraction, Raman spectrum, thermo-gravimetric analysis, and microscopic Fourier transform infrared analysis. The results showed that the addition of GO sheets into the HY-HA suspensions could increase the deposition rate and inhibit cracks creation and propagation in the coatings. The corrosion resistant of the resulting samples were evaluated using potentiodynamic polarization method in simulated body fluid, and the GO-HY-HA coatings could effectively improve the anti-corrosion property of the Ti substrate.

Joining of ceramics of different biofunction by hot isostatic pressing

DOE Office of Scientific and Technical Information (OSTI.GOV)

Li, Jianguo; Harmansson, L.; Soeremark, R.

1993-10-01

Monolithic zirconia (Z) and zirconia-hydroxyapatite (Z/HA) composites were joined by cold isostatic pressing (CIP at 300 MPa) and subsequently by glass-encapsulated hot isostatic pressing (HIP at 1225 C, 1 h and 200 MPa). The physical and mechanical properties of the materials were measured. The fracture surface was studied using a light microscope. The results indicate a strength level of the joint similar to that of the corresponding composite material (Z/HA), 845 and 860 MPa, respectively. Similar experiments with monolithic alumina (A) and alumina-hydroxyapatite (A/HA) were carried out without success. Cracking occurred in the joint area during the cold isostatic pressingmore » process. It seems that ceramics with high green strength and similar green density are essential when joining ceramics by combined CIP and HIP processes.« less

First principles study of hydroxyapatite surface

NASA Astrophysics Data System (ADS)

Slepko, Alexander; Demkov, Alexander A.

2013-07-01

The biomineral hydroxyapatite (HA) [Ca10(PO4)6(OH)2] is the main mineral constituent of mammal bone. We report a theoretical investigation of the HA surface. We identify the low energy surface orientations and stoichiometry under a variety of chemical environments. The surface most stable in the physiologically relevant OH-rich environment is the OH-terminated (1000) surface. We calculate the work function of HA and relate it to the surface composition. For the lowest energy OH-terminated surface we find the work function of 5.1 eV, in close agreement with the experimentally reported range of 4.7 eV-5.1 eV [V. S. Bystrov, E. Paramonova, Y. Dekhtyar, A. Katashev, A. Karlov, N. Polyaka, A. V. Bystrova, A. Patmalnieks, and A. L. Kholkin, J. Phys.: Condens. Matter 23, 065302 (2011), 10.1088/0953-8984/23/6/065302].

Development and characterization of porous silver-incorporated hydroxyapatite ceramic for separation and elimination of microorganisms.

PubMed

Yang, Lei; Ning, Xiaoshan; Xiao, Qunfang; Chen, Kexin; Zhou, Heping

2007-04-01

A novel filter material for separating and eliminating microorganisms in water and gas was fabricated by incorporating silver ions into porous hydroxyapatite (HA) ceramics prepared by a starch additive technique. The porous ceramics reveal a microstructure of both large and small pores. Microorganism separating and eliminating properties of the porous silver-incorporated HA ceramics (PHA-Ag) were investigated by bacterial and viral filtration tests. The PHA-Ag demonstrated excellent separating and antibacterial effects on Escherichia coli and the mechanisms were studied. Adsorption of bacterial cells to the HA and the barricading effect of small pores contribute to the separating property of PHA-Ag, while the Ag+ ions equip the ceramics with antibacterial property. Furthermore, the PHA-Ag exhibited an observable virus-eliminating property and its probable mechanism was also discussed. (c) 2006 Wiley Periodicals, Inc.

Biodegradable magnesium-hydroxyapatite metal matrix composites.

PubMed

Witte, Frank; Feyerabend, Frank; Maier, Petra; Fischer, Jens; Störmer, Michael; Blawert, Carsten; Dietzel, Wolfgang; Hort, Norbert

2007-04-01

Recent studies indicate that there is a high demand to design magnesium alloys with adjustable corrosion rates and suitable mechanical properties. An approach to this challenge might be the application of metal matrix composite (MMC) based on magnesium alloys. In this study, a MMC made of magnesium alloy AZ91D as a matrix and hydroxyapatite (HA) particles as reinforcements have been investigated in vitro for mechanical, corrosive and cytocompatible properties. The mechanical properties of the MMC-HA were adjustable by the choice of HA particle size and distribution. Corrosion tests revealed that HA particles stabilised the corrosion rate and exhibited more uniform corrosion attack in artificial sea water and cell solutions. The phase identification showed that all samples contained hcp-Mg, Mg(17)Al(12), and HA before and after immersion. After immersion in artificial sea water CaCO3 was found on MMC-HA surfaces, while no formation of CaCO3 was found after immersion in cell solutions with and without proteins. Co-cultivation of MMC-HA with human bone derived cells (HBDC), cells of an osteoblasts lineage (MG-63) and cells of a macrophage lineage (RAW264.7) revealed that RAW264.7, MG-63 and HBDC adhere, proliferate and survive on the corroding surfaces of MMC-HA. In summary, biodegradable MMC-HA are cytocompatible biomaterials with adjustable mechanical and corrosive properties.

The effect of hydroxyapatite addition on the mechanical properties of polyvinyl alcohol/chitosan biomaterials for bone scaffolds application

NASA Astrophysics Data System (ADS)

Ramahdita, Ghiska; Puspita, Debie Maya; Albab, Muh Fadhil; Alfata, Rowi; Sofyan, Nofrijon; Yuwono, Akhmad Herman

2018-02-01

The increasing number of bone fracture incident in Indonesia from year to year needs an urgent problem solving of the limited bone substitute which can meet the necessary criteria for that purpose. Motivated by this, therefore, the current study is focusing on the optimization of material properties used as bone scaffold. A biomaterial of polyvinyl alcohol (PVA)/chitosan-hydroxyapatite (HA) composite was successfully made by wet chemistry method, followed by freeze thawing and freeze drying. For comparison purposes, the percentage of HA has been varied from 0, 25 and 40 % (wt/v). The resulting composites were characterized by Fourier transform infrared (FTIR) spectroscopy, scanning electron microscope (SEM), compressive test, and swelling behavior. The results showed that the addition of HA up to 40% (wt/v) has yielded a porous structure with an average pore size of 42.39 µm. In addition, the compressive modulus was enhanced from 14 MPa for 0% HA to 143, and 191 MPa for composites with the addition of HA from 25 to 40% (wt/v). The addition of HA has also reduced the swelling ratio from 296% for the sample without HA to 85 and 78 % for sample with addition of HA from 25 to 40 (wt/v), respectively. The obtained results show that PVA/chitosan-HA in this study is potential to be used as scaffold in bone tissue engineering.

Mechanical properties and crystallization behavior of hydroxyapatite/poly(butylenes succinate) composites.

PubMed

Guo, Wenmin; Zhang, Yihe; Zhang, Wei

2013-09-01

Biodegradable synthetic polymers have attracted much attention nowadays, and more and more researches have been done on biodegradable polymers due to their excellent mechanical properties, biocompatibility, and biodegradability. In this work, hydroxyapatite (HA) particles were melt-mixing with poly (butylenes succinate) (PBS) to prepare the material, which could be used in the biomedical industry. To develop high-performance PBS for cryogenic engineering applications, it is necessary to investigate the cryogenic mechanical properties and crystallization behavior of HA/PBS composites. Cryogenic mechanical behaviors of the composites were studied in terms of tensile and impact strength at the glass transition temperature (-30°C) and compared to their corresponding behaviors at room temperature. With the increase of HA content, the crystallization of HA/PBS composites decreased and crystallization onset temperature shifted to a lower temperature. The diameter of spherulites increased at first and decreased with a further HA content. At the same time, the crystallization rate became slow when the HA content was no more than 15wt% and increased when HA content reached 20wt%. In all, the results we obtained demonstrate that HA/PBS composites reveal a better tensile strength at -30°C in contrast to the strength at room temperature. HA particles with different amount affect the crystallization of PBS in different ways. Copyright © 2013 Wiley Periodicals, Inc.

Hydroxyapatite coating on cobalt alloys using electrophoretic deposition method for bone implant application

NASA Astrophysics Data System (ADS)

Aminatun; M, Shovita; I, Chintya K.; H, Dyah; W, Dwi

2017-05-01

Damage on bone due to osteoporosis and cancer triggered high demand for bone implant prosthesis which is a permanent implant. Thus, a prosthesis coated with hydroxyapatite (HA) is required because it is osteoconductive that can trigger the growth of osteoblast cells. The purpose of this study is to determine the optimum concentration of HA suspension in terms of the surface morphology, coating thickness, adhesion strength and corrosion rate resulting in the HA coating with the best characteristics for bone implant. Coating using electrophoretic deposition (EPD) method with concentrations of 0.02M, 0.04M, 0.06M, 0.08M, and 0.1M was performed on the voltage and time of 120V and 30 minutes respectively. The process was followed by sintering at the temperature of 900 °C for 10 minutes. The results showed that the concentration of HA suspension influences the thickness and the adhesion of layer of HA. The higher the concentration of HA-ethanol suspension the thicker the layer of HA, but its coating adhesion strength values became lower. The concentration of HA suspension of 0.04 M is the best concentration, with characteristics that meet the standards of the bone implant prosthesis. The characteristics are HA coating thickness of 199.93 ± 4.85 μm, the corrosion rate of 0.0018 mmpy and adhesion strength of 4.175 ± 0.716 MPa.

A novel route for synthesis of nanocrystalline hydroxyapatite from eggshell waste.

PubMed

Siva Rama Krishna, D; Siddharthan, A; Seshadri, S K; Sampath Kumar, T S

2007-09-01

The eggshell waste has been value engineered to a nanocrystalline hydroxyapatite (HA) by microwave processing. To highlight the advantages of eggshell as calcium precursor in the synthesis of HA (OHA), synthetic calcium hydroxide was also used to form HA (SHA) following similar procedure and were compared with a commercially available pure HA (CHA). All the HAs were characterized by X-ray powder diffraction (XRD) method, Fourier transform infrared (FT-IR) spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM) and specific surface area measurements. Nanocrystalline nature of OHA is revealed through characteristic broad peaks in XRD patterns, platelets of length 33-50 nm and width 8-14 nm in TEM micrograph and size calculations from specific surface area measurements. FT-IR spectra showed characteristic bands of HA and additionally peaks of carbonate ions. The cell parameter calculations suggest the formation of carbonated HA of B-type. The OHA exhibits superior sinterability in terms of hardness and density than both SHA and CHA may be due to larger surface area of its spherulite structure. The in vitro dissolution study shows longer stability in phosphate buffer and cell culture test using osteoblast cells establishes biocompatibility of OHA.

Electroactive Mg2+-Hydroxyapatite Nanostructured Networks against Drug-Resistant Bone Infection Strains.

PubMed

Andrés, Nancy C; Sieben, Juan M; Baldini, Mónica; Rodríguez, Carlos H; Famiglietti, Ángela; Messina, Paula V

2018-06-13

Surface colonization competition between bacteria and host cells is one of the critical factors involved in tissue/implant integration. Current biomaterials are evaluated for their ability both of withstanding favorable responses of host tissue cells and of resisting bacterial contamination. In this work, the antibacterial ability of biocompatible Mg 2+ -substituted nanostructured hydroxyapatite (HA) was investigated. The densities of Staphylococcus aureus, Pseudomonas aeruginosa, and Escherichia coli strains were significantly decreased after culture in the presence of Mg-substituted HA materials in direct correlation with Mg 2+ -Ca 2+ switch in the HA lattice. It was noticed that this decrease was accompanied by a minimal alteration of bacterial environments; therefore, the Mg 2+ -HA antibacterial effect was associated with the material surface topography and it electroactive behavior. It was observed that 2.23 wt % Mg 2+ -HA samples exhibited the best antibacterial performance; it decreased 2-fold the initial population of E. coli, P. aeruginosa, and S. aureus at the intermediate concentration (50 mg mL -1 of broth). Our results reinforce the potential of Mg-HA nanostructured materials to be used in antibacterial coatings for implantable devices and/or medicinal materials to prevent bone infection and to promote wound healing.

New Coll-HA/BT composite materials for hard tissue engineering.

PubMed

Zanfir, Andrei Vlad; Voicu, Georgeta; Busuioc, Cristina; Jinga, Sorin Ion; Albu, Madalina Georgiana; Iordache, Florin

2016-05-01

The integration of ceramic powders in composite materials for bone scaffolds can improve the osseointegration process. This work was aimed to the synthesis and characterization of new collagen-hydroxyapatite/barium titanate (Coll-HA/BT) composite materials starting from barium titanate (BT) nanopowder, hydroxyapatite (HA) nanopowder and collagen (Coll) gel. BT nanopowder was produced by combining two wet-chemical approaches, sol-gel and hydrothermal methods. The resulting materials were characterized in terms of phase composition and microstructure by X-ray diffraction, Raman spectroscopy, scanning electron microscopy and transmission electron microscopy. Moreover, the biocompatibility and bioactivity of the composite materials were assessed by in vitro tests. The synthesized BT particles exhibit an average size of around 35 nm and a spherical morphology, with a pseudo-cubic or tetragonal symmetry. The diffraction spectra of Coll-HA and Coll-HA/BT composite materials indicate a pronounced interaction between Col and the mineral phases, meaning a good mineralization of Col fibres. As well, the in vitro tests highlight excellent osteoinductive properties for all biological samples, especially for Coll-HA/BT composite materials, fact that can be attributed to the ferromagnetic properties of BT. Copyright © 2016 Elsevier B.V. All rights reserved.

Development of electrochemical folic acid sensor based on hydroxyapatite nanoparticles

NASA Astrophysics Data System (ADS)

Kanchana, P.; Sekar, C.

2015-02-01

We report the synthesis of hydroxyapatite (HA) nanoparticles (NPs) by a simple microwave irradiation method and its application as sensing element for the precise determination of folic acid (FA) by electrochemical method. The structure and composition of the HA NPs characterized using XRD, FTIR, Raman and XPS. SEM and EDX studies confirmed the formation of elongated spherical shaped HA NPs with an average particle size of about 34 nm. The HA NPs thin film on glassy carbon electrode (GCE) were deposited by drop casting method. Electrocatalytic behavior of FA in the physiological pH 7.0 was investigated by cyclic voltammetry (CV), linear sweep voltammetry (LSV) and chronoamperometry. The fabricated HA/GCE exhibited a linear calibration plot over a wide FA concentration ranging from 1.0 × 10-7 to 3.5 × 10-4 M with the detection limit of 75 nM. In addition, the HA NPs modified GCE showed good selectivity toward the determination of FA even in the presence of a 100-fold excess of ascorbic acid (AA) and 1000-fold excess of other common interferents. The fabricated biosensor exhibits good sensitivity and stability, and was successfully applied for the determination of FA in pharmaceutical samples.

Magnesium- and strontium-co-substituted hydroxyapatite: the effects of doped-ions on the structure and chemico-physical properties.

PubMed

Aina, Valentina; Lusvardi, Gigliola; Annaz, Basil; Gibson, Iain R; Imrie, Flora E; Malavasi, Gianluca; Menabue, Ledi; Cerrato, Giuseppina; Martra, Gianmario

2012-12-01

The present study is aimed at investigating the contribution of two biologically important cations, Mg(2+) and Sr(2+), when substituted into the structure of hydroxyapatite (Ca(10)(PO(4))(6)(OH)(2),HA). The substituted samples were synthesized by an aqueous precipitation method that involved the addition of Mg(2+)- and Sr(2+)-containing precursors to partially replace Ca(2+) ions in the apatite structure. Eight substituted HA samples with different concentrations of single (only Mg(2+)) or combined (Mg(2+) and Sr(2+)) substitution of cations have been investigated and the results compared with those of pure HA. The obtained materials were characterized by X-ray powder diffraction, specific surface area and porosity measurements (N(2) adsorption at 77 K), FT-IR and Raman spectroscopies and scanning electron microscopy. The results indicate that the co-substitution gives rise to the formation of HA and β-TCP structure types, with a variation of their cell parameters and of the crystallinity degree of HA with varying levels of substitution. An evaluation of the amount of substituents allows us to design and prepare BCP composite materials with a desired HA/β-TCP ratio.

Effects of Dentifrice Containing Hydroxyapatite on Dentinal Tubule Occlusion and Aqueous Hexavalent Chromium Cations Sorption: A Preliminary Study

PubMed Central

Liu, Jing; Hou, Yarong; Zhu, Manqun; Huang, Jiansheng; Xu, Pingping

2012-01-01

In order to endow environmental protection features to dentifrice, hydroxyapatite (HA) was added to ordinary dentifrice. The effects on dentinal tubule occlusion and surface mineralization were compared after brushing dentine discs with dentifrice with or without HA. The two types of dentifrice were then added to 100 µg/ml of hexavalent chromium cation (Cr6+) solution in order to evaluate their capacities of adsorbing Cr6+ from water. Our results showed that the dentifrice containing HA was significantly better than the ordinary dentifrice in occluding the dentinal tubules with a plugging rate greater than 90%. Moreover, the effect of the HA dentifrice was persistent and energy-dispersive spectrometer (EDS) revealed that the atomic percentages of calcium and phosphorus on the surface of dentine discs increased significantly. Adding HA to ordinary dentifrice significantly enhanced the ability of dentifrice to adsorb Cr6+ from water with the removal rate up to 52.36%. In addition, the sorption was stable. Our study suggests that HA can be added to ordinary dentifrice to obtain dentifrice that has both relieving dentin hypersensitivity benefits and also helps to control environmental pollution. PMID:23300511

Preparation of foam-like carbon nanotubes/hydroxyapatite composite scaffolds with superparamagnetic properties

NASA Astrophysics Data System (ADS)

Lu, X. Y.; Qiu, T.; Wang, X. F.; Zhang, M.; Gao, X. L.; Li, R. X.; Lu, X.; Weng, J.

2012-12-01

In this paper, the foam-like composite scaffolds composed of hydroxyapatite (HA) and carbon nanotubes (CNTs) were prepared by a new method, where a polymer impregnating method was used for porous HA-based scaffold and a chemical vapor deposition (CVD) method was used for the growth of CNTs from the HA-based scaffold. The process produces the CNTs/HA scaffolds that have a foam-like structure with better mechanical property, better microstructure and a high degree of interconnection. A favorable pore size with big pores of 1-2 mm and small pores of 20-300 μm for osteoconduction and bone ingrowth is presented in these scaffolds. About 2 wt% multi-walled CNTs with the diameter of 60-100 nm are observed to be in situ grown from deficient nano-HA crystallites. Magnetic measurement exhibits these scaffolds are superparamagnetic with a saturation magnetization of 1.14 emu g-1 at a room temperature, benefiting the scaffolds to take up growth factors in vivo, stem cell or other bioactive molecules easily. This new type of CNTs/HA scaffolds is expected to have a promising applications in bone tissue engineering, targeted drug delivery system and other biomedical fields.

Characterisation and sintering of nanophase hydroxyapatite synthesised by a species of Serratia

NASA Astrophysics Data System (ADS)

LSammons, R.; Thackray, A. C.; Medina Ledo, H.; Marquis, P. M.; Jones, I. P.; Yong, P.; Macaskie, L. E.

2007-12-01

The bacterium Serratia sp. NCIMB40259, which grows as a biofilm on polymeric, glass and metal substrates, produces extracellular crystals of hydroxyapatite (HA) by enzymatic cleavage of β-glycerophosphate in the presence of calcium chloride. Following growth on polyurethane foam, biomineralisation and subsequent sintering, an HA scaffold is formed whose three-dimensional architecture replicates that of the foam and the biofilm. Serratia HA was characterised using X-ray diffraction (XRD), Fourier Transform Infra-Red Spectroscopy (FTIR), energy dispersive X-ray analysis (EDX) scanning electron microscopy (SEM), transmission electron microscopy (TEM) and electron diffraction (ED). The nascent, unsintered material consisted mainly of calcium-deficient HA (CDHA) with a Ca/P ratio of 1.61+/- 0.06 and crystal size (TEM) of 50 +/- 10nm length. ED of unsintered crystals and crystals sintered at 600° C showed resolvable ring (unsintered) or dot (600° C) patterns ascribed to (0002), (1122) and (0006) planes of crystalline HA. Material sintered at 1200° C consisted of needle-like crystals of length range 54-111nm (XRD) with lattice parameters of a = 9.441 Å and c = 6.875 Å, consistent with HA.

Rheological, mechanical and degradable properties of injectable chitosan/silk fibroin/hydroxyapatite/glycerophosphate hydrogels.

PubMed

Wu, Jingjing; Liu, Jiaoyan; Shi, Yanmei; Wan, Ying

2016-12-01

Silk fibroin (SF) and hydroxyapatite (HA) were incorporated into chitosan/glycerophosphate (GP) system to prepare new types of hydrogels. The formulated chitosan/SF/GP and chitosan/SF/HA/GP solutions were found to be injectable at room temperature, and able to form into hydrogels at near-physiological temperature and pH. Rheological measurements showed that elastic modulus of certain chitosan/SF/GP and chitosan/SF/HA/GP gels could reach around 1.8 and 15kPa, respectively, and was much higher than their respective viscous modulus. Compressive measurements revealed that some chitosan/SF/GP and chitosan/SF/HA/GP gels had 8 and 20-fold modulus and strength higher than the chitosan/GP gel, respectively, confirming that compressive properties of these gels were greatly improved. Results obtained from in vivo degradation demonstrated that degradation endurance of the optimized chitosan/SF/GP and chitosan/SF/HA/GP gels was significantly enhanced as compared to the chitosan/GP gel, and the degradation rate of the gels could be regulated by the SF component alone or by the combination of SF and HA components. Copyright © 2016 Elsevier Ltd. All rights reserved.

Enhancement of aptamer immobilization using egg shell-derived nano-sized spherical hydroxyapatite for thrombin detection in neuroclinic.

PubMed

Derkus, Burak; Arslan, Yavuz Emre; Emregul, Kaan C; Emregul, Emel

2016-09-01

In the present study, we describe the sonochemical isolation of nano-sized spherical hydroxyapatite (nHA) from egg shell and application towards thrombin aptasensing. In addition to the sonochemical method, two conventional methods present in literature were carried out to perform a comparative study. Various analysis methods including Transmission Electron Microscopy (TEM), Scanning Electron Microscopy (SEM), Fourier Transform Infrared Spectroscopy (FTIR), X-Ray Diffraction (XRD), Energy-Dispersive Analysis of X-Rays (EDAX), and Thermal Gravimetric Analysis (TGA) have been applied for the characterization of nHA and its nanocomposite with marine-derived collagen isolated from Rhizostoma pulmo jellyfish. TEM micrographs revealed the sonochemically synthesized nHA nanoparticles to have a unique porous spherical shape with a diameter of approximately 60-80nm when compared to hydroxyapatite nanoparticles synthesized using the other two methods which had a typical needle shaped morphology. EDAX, XRD and FTIR results demonstrated that the obtained patterns belonged to hydroxyapatite. Electrochemical impedance spectroscopy (EIS) is the main analyzing technique of the developed thrombin aptasensor. The proposed aptasensor has a detection limit of 0.25nM thrombin. For clinical application of the developed aptasensor, thrombin levels in blood and cerebrospinal fluid (CSF) samples obtained from patients with Multiple Sclerosis, Myastenia Gravis, Epilepsy, Parkinson, polyneuropathy and healthy donors were analyzed using both the aptasensor and commercial ELISA kit. The results showed that the proposed system is a promising candidate for clinical analysis of thrombin. Copyright © 2016 Elsevier B.V. All rights reserved.

Differential osteogenic activity of osteoprogenitor cells on HA and TCP/HA scaffold of tissue engineered bone.

PubMed

Ng, Angela M H; Tan, K K; Phang, M Y; Aziyati, O; Tan, G H; Isa, M R; Aminuddin, B S; Naseem, M; Fauziah, O; Ruszymah, B H I

2008-05-01

Biomaterial, an essential component of tissue engineering, serves as a scaffold for cell attachment, proliferation, and differentiation; provides the three dimensional (3D) structure and, in some applications, the mechanical strength required for the engineered tissue. Both synthetic and naturally occurring calcium phosphate based biomaterial have been used as bone fillers or bone extenders in orthopedic and reconstructive surgeries. This study aims to evaluate two popular calcium phosphate based biomaterial i.e., hydroxyapatite (HA) and tricalcium phosphate/hydroxyapatite (TCP/HA) granules as scaffold materials in bone tissue engineering. In our strategy for constructing tissue engineered bone, human osteoprogenitor cells derived from periosteum were incorporated with human plasma-derived fibrin and seeded onto HA or TCP/HA forming 3D tissue constructs and further maintained in osteogenic medium for 4 weeks to induce osteogenic differentiation. Constructs were subsequently implanted intramuscularly in nude mice for 8 weeks after which mice were euthanized and constructs harvested for evaluation. The differential cell response to the biomaterial (HA or TCP/HA) adopted as scaffold was illustrated by the histology of undecalcified constructs and evaluation using SEM and TEM. Both HA and TCP/HA constructs showed evidence of cell proliferation, calcium deposition, and collagen bundle formation albeit lesser in the former. Our findings demonstrated that TCP/HA is superior between the two in early bone formation and hence is the scaffold material of choice in bone tissue engineering. Copyright 2007 Wiley Periodicals, Inc.

Characterization of Multiwalled Carbon Nanotube-Reinforced Hydroxyapatite Composites Consolidated by Spark Plasma Sintering

PubMed Central

Kim, Duk-Yeon; Han, Young-Hwan; Lee, Jun Hee; Kang, Inn-Kyu; Jang, Byung-Koog; Kim, Sukyoung

2014-01-01

Pure HA and 1, 3, 5, and 10 vol% multiwalled carbon nanotube- (MWNT-) reinforced hydroxyapatite (HA) were consolidated using a spark plasma sintering (SPS) technique. The relative density of pure HA increased with increasing sintering temperature, but that of the MWNT/HA composite reached almost full density at 900°C, and then decreased with further increases in sintering temperature. The relative density of the MWNT/HA composites increased with increasing MWNT content due to the excellent thermal conductivity of MWNTs. The grain size of MWNT/HA composites decreased with increasing MWNT content and increased with increasing sintering temperature. Pull-out toughening of the MWNTs of the MWNT/HA composites was observed in the fractured surface, which can be used to predict the improvement of the mechanical properties. On the other hand, the existence of undispersed or agglomerate MWNTs in the MWNT/HA composites accompanied large pores. The formation of large pores increased with increasing sintering temperature and MWNT content. The addition of MWNT in HA increased the hardness and fracture toughness by approximately 3~4 times, despite the presence of large pores produced by un-dispersed MWNTs. This provides strong evidence as to why the MWNTs are good candidates as reinforcements for strengthening the ceramic matrix. The MWNT/HA composites did not decompose during SPS sintering. The MWNT-reinforced HA composites were non-toxic and showed a good cell affinity and morphology in vitro for 1 day. PMID:24724100

Fabrication and characterization of drug-loaded nano-hydroxyapatite/polyamide 66 scaffolds modified with carbon nanotubes and silk fibroin

PubMed Central

Yao, Meng-Zhu; Huang-Fu, Ming-Yi; Liu, Hui-Na; Wang, Xia-Rong; Sheng, Xiaoxia; Gao, Jian-Qing

2016-01-01

Nano-hydroxyapatite/polyamide 66 (nHA/PA66) porous scaffolds were fabricated by a phase inversion method. Carbon nanotubes (CNTs) and silk fibroin (SF) were used to modify the surface of the nHA/PA66 scaffolds by freeze-drying and cross-linking. Dexamethasone was absorbed to the CNTs to promote the osteogenic differentiation of bone mesenchymal stem cells (BMSCs). The cell viability of BMSCs was investigated by changing the concentration of the CNT dispersion, and the most biocompatible scaffold was selected. In addition, the morphology and mechanical property of the scaffolds were investigated. The results showed that the nHA/PA66 scaffolds modified with CNTs and SF met the requirements of bone tissue engineering scaffolds. The dexamethasone-loaded CNT/SF-nHA/PA66 composite scaffold promoted the osteogenic differentiation of BMSCs, and the drug-loaded scaffolds are expected to function as effective bone tissue engineering scaffolds. PMID:27920525

Synthesis of hydroxyapatite whiskers through dissolution reprecipitation process using EDTA

NASA Astrophysics Data System (ADS)

Seo, Dong Seok; Lee, Jong Kook

2008-04-01

Hydroxyapatite (HA) has been of interest in many industrial applications, such as ion exchange, catalysis and biomaterials. Chelating agents have often been used to prepare inorganic powders in the form of sphere, rod, whisker and fiber. In this study, HA whiskers were synthesized directly from typically shaped HA powders by refluxing at 80 and 100 °C for 24 h using ethylenediamine tetraacetic acid (EDTA). 3% or 6% of hydrogen peroxide (H 2O 2) was used to promote precipitation of HA crystals. The pH of the solution was adjusted at 7 or 9 by adding ammonia solution. The higher the H 2O 2 concentration, pH value and refluxing temperature, the longer and thinner whiskers were formed. The whiskers produced at 100 °C with 6% of H 2O 2 and pH 9 had the highest aspect ratio of about 50-60 (a length of 3 μm and a width of 0.05 μm).

Experimental evidence and structural modeling of nonstoichiometric (010) surfaces coexisting in hydroxyapatite nano-crystals.

PubMed

Ospina, C A; Terra, J; Ramirez, A J; Farina, M; Ellis, D E; Rossi, A M

2012-01-01

High-resolution transmission electron microscopy (HRTEM) and ab initio quantum-mechanical calculations of electronic structure were combined to investigate the structure of the hydroxyapatite (HA) (010) surface, which plays an important role in HA interactions with biological media. HA was synthesized by in vitro precipitation at 37°C. HRTEM images revealed thin elongated rod nanoparticles with preferential growth along the [001] direction and terminations parallel to the (010) plane. The focal series reconstruction (FSR) technique was applied to develop an atomic-scale structural model of the high-resolution images. The HRTEM simulations identified the coexistence of two structurally distinct terminations for (010) surfaces: a rather flat Ca(II)-terminated surface and a zig-zag structure with open OH channels. Density functional theory (DFT) was applied in a periodic slab plane-wave pseudopotential approach to refine details of atomic coordination and bond lengths of Ca(I) and Ca(II) sites in hydrated HA (010) surfaces, starting from the HRTEM model. Copyright © 2011 Elsevier B.V. All rights reserved.

Microleakage under orthodontic bands cemented with nano-hydroxyapatite-modified glass ionomer.

PubMed

Enan, Enas T; Hammad, Shaza M

2013-11-01

To estimate the in vivo effect of nano-hydroxyapatite (HA) modification of banding glass-ionomer cement on microleakage under orthodontic bands. Eighty noncarious premolars scheduled for extraction in 20 orthodontic patients were randomly divided into four groups. Grouping was based on the ratio of nano-HA (0%, 5%, 10%, 15% by weight) added to the luting glass-ionomer cement (GIC) Ketac-Cem, which was used for cementation of prefabricated micro-etched orthodontic bands. Dye penetration method was used for microleakage evaluation at the cement-band and cement-enamel interfaces. Statistical evaluation was performed with a Kruskal-Wallis test and a Mann-Whitney U-test, and a Bonferroni-adjusted significance level was calculated. Bands cemented with conventional GIC showed the highest microleakage scores in comparison to those cemented with nano-HA-modified GIC. No significant difference was found between teeth banded with 10% and 15% modified GIC. Modification of the banding GIC with 15% nano-HA revealed a positive effect on reducing microleakage around orthodontic bands.

[Characteristics of hydroxyapatite/PMMA nanocomposites for provisional restoration and its biocompatibility with human gingival fibroblasts].

PubMed

Zhang, Jing-chao; Mo, An-chun; Li, Ji-dong; Wang, Xue-jiang; Li, Yu-bao

2014-05-01

To formulate hydroxyapatite (HA)/polymethyl methacrylate (PMMA) composites with improved cytocompatibility for provisional restoration. Nanocomposites with 20 wt%, 30 wt%, 40 wt%, and 50 wt% HA/PMMA (H/P) were developed and examined using X-ray photoelectron spectroscopy (XPS) and scanning electron microscope (SEM). Human gingival fibroblasts were cultured on those HA/PMMA discs and investigated by fluorescent staining on 24 h and MTT assay at 1 d, 3 d, 5 d and 7 d. Chemical integration of HA/PMMA interface was confirmed by XPS. Typical fusiform cells with adhesion spots were detected on 40 wt% and 50 wt% H/P discs. MTT results showed insignificant differences in cell growth between 40 wt% H/P and pure titanium (Ti, P > 0.05), while the other H/P discs showed significantly lower cell growth than pure Ti (P < 0.05). 40 wt% H/P might be a promising candidate for provisional dental implant restoration and for esthetic gingival contour.

Detachment strength of human osteoblasts cultured on hydroxyapatite with various surface roughness. Contribution of integrin subunits.

PubMed

Kokkinos, Petros A; Koutsoukos, Petros G; Deligianni, Despina D

2012-06-01

Hydroxyapatite (HA) has been widely used as a bone substitute in dental, maxillofacial and orthopaedic surgery and as osteoconductive bone substitute or precoating of pedicle screws and cages in spine surgery. The aim of the present study was to investigate the osteoblastic adhesion strength on HA substrata with different surface topography and biochemistry (pre-adsorption of fibronectin) after blocking of specific integrin subunits with monoclonal antibodies. Stoichiometric HA was prepared by precipitation followed by ageing and characterized by SEM, EDX, powder XRD, Raman spectroscopy, TGA, and specific surface area analysis. Human bone marrow derived osteoblasts were cultured on HA disc-shaped substrata which were sintered and polished resulting in two surface roughness grades. For attachment evaluation, cells were incubated with monoclonal antibodies and seeded for 2 h on the substrata. Cell detachment strength was determined using a rotating disc device. Cell detachment strength was surface roughness, fibronectin preadsorption and intergin subunit sensitive.

Influence of pretreatment on the surface characteristics of PLLA fibers and subsequent hydroxyapatite coating.

PubMed

Peng, F; Olson, J R; Shaw, M T; Wei, M

2009-01-01

A fibrous precursor for bone repair composites was made by coating poly(L-lactide) (PLLA) fibers with hydroxyapatite (HA) using a biomimetic method. To enhance the bonding between the HA coating and the PLLA fiber, PLLA fibers were etched with either sodium hydroxide or sodium hypochlorite to generate carboxyl groups on fiber surfaces. The experiments were designed to determine the influence of etching on the fiber surface morphology and chemistry as well as the subsequent HA coating on the etched fiber surfaces. It was found that the etching pretreatment increased the roughness as well as the hydrophilicity of fibers, indicating that hydrolysis of PLLA chains had taken place on fiber surfaces. The etching pretreatment also promoted HA coating formation by introducing thicker coating on the surface of fibers with a longer etching time, a higher etching concentration, or with NaOCl as the etching agent. A mechanism of surface hydrolysis and oxidation of PLLA was proposed. (c) 2008 Wiley Periodicals, Inc.

Effect of silver additive on physicochemical properties of hydroxyapatite applied to reconstructive surgery

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhuk, I. V., E-mail: zhukiv1993@mail.ru; Rasskazova, L. A., E-mail: ly-2207@mail.ru; Korotchenko, N. M., E-mail: korotch@mail.ru

The effect of silver adding to hydroxyapatite (HA) in its solubility in physiological solution and biological activity was investigated. Samples of HA containing silver (AgHA) obtained by liquid-phase method in the conditions of microwave exposure. Solubility (C{sub Ca}{sup 2+}·10{sup 3}, mol/l) of the powders AgHA was determined by chemical methods according trilonometric titration of the calcium ions in physiological solution at 25 and 37 °C. To investigate the biological activity of the samples, a series of experiments on the formation of the calcium-phosphate layer on the surface of the SBF-solution at 37 °C for 28 days. Electronic micrographs of samplesmore » taken at the end of each 7 days of the experiment, indicate the formation of calcium-phosphate layer (CPL) in the samples, the kinetics of which is shown as a function of cumulative concentrations of calcium and magnesium ions from time.« less

Affinity of the interface between hydroxyapatite (0001) and titanium (0001) surfaces: a first-principles investigation.

PubMed

Sun, Jin P; Dai, Jianhong; Song, Yan; Wang, You; Yang, Rui

2014-12-10

A basic understanding of the affinity between the hydroxyapatite (HA) and α-Ti surfaces is obtained through electronic structure calculations by first-principles method. The surface energies of HA(0001), HA (011̅0), HA (101̅1), and Ti(0001) surfaces have been calculated. The HA(0001) presents the most thermodynamically stable of HA. The HA/Ti interfaces were constructed by two kinds of interface models, the single interface (denoted as SI) and the double-interface (denoted as DI). Two methods, the full relaxation and the UBER, were applied to determine the interfacial separation and the atomic arrangement in the interfacial zone. The works of adhesion of interfaces with various stoichiometric HA surfaces were evaluated. For the HA(0001)/Ti(0001) interfaces, the work of adhesion is strongly dependent on the chemical environment of the HA surface. The values are -2.33, -1.52, and -0.80 J/m(2) for the none-, single-, and double-Ca terminated HA/Ti interfaces, respectively. The influence of atomic relaxation on the work of adhesion and interface separation is discussed. Full relaxation results include -1.99 J/m(2) work of adhesion and 0.220 nm separation between HA and Ti for the DI of 1-Ca-HA/Ti interface, while they are -1.14 J/m(2) and 0.235 nm by partial relaxation. Analysis of electronic structure reveals that charge transfer between HA and Ti slabs occurs during the formation of the HA/Ti interface. The transfer generates the Ti-O or Ti-Ca bonds across the interface and drives the HA/Ti interface system to metallic characteristic. The energetically favorable interfaces are formed when the outmost layer of HA comprises more O atoms at the interface.

Biocompatibility and Biocorrosion of Hydroxyapatite-Coated Magnesium Plate: Animal Experiment.

PubMed

Lim, Ho-Kyung; Byun, Soo-Hwan; Woo, Jae-Man; Kim, Sae-Mi; Lee, Sung-Mi; Kim, Bong-Ju; Kim, Hyoun-Ee; Lee, Jung-Woo; Kim, Soung-Min; Lee, Jong-Ho

2017-09-30

Magnesium (Mg) has the advantage of being resorbed in vivo, but its resorption rate is difficult to control. With uncontrolled resorption, Magnesium as a bone fixation material has minimal clinical value. During resorption not only is the strength rapidly weakened, but rapid formation of metabolite also occurs. In order to overcome these disadvantages, hydroxyapatite (HA) surface coating of pure magnesium plate was attempted in this study. Magnesium plates were inserted above the frontal bone of Sprague-Dawley rats in both the control group (Bare-Mg group) and the experimental group (HA-Mg group). The presence of inflammation, infection, hydrogen gas formation, wound dehiscence, and/or plate exposure was observed, blood tests were performed, and the resorption rate and tensile strength of the retrieved metal plates were measured. The HA-Mg group showed no gas formation or plate exposure until week 12. However, the Bare-Mg group showed consistent gas formation and plate exposure beginning in week 2. WBC (White Blood Cell), BUN (Blood Urea Nitrogen), Creatinine, and serum magnesium concentration levels were within normal range in both groups. AST (Aspartate Aminotransferase) and ALT (Alanine Aminotransferase) values, however, were above normal range in some animals of both groups. The HA-Mg group showed statistically significant advantage in resistance to degradation compared to the Bare-Mg group in weeks 2, 4, 6, 8, and 12. Degradation of HA-Mg plates proceeded after week 12. Coating magnesium plates with hydroxyapatite may be a viable method to maintain their strength long enough to allow bony healing and to control the resorption rate during the initial period.

Biocompatibility and Biocorrosion of Hydroxyapatite-Coated Magnesium Plate: Animal Experiment

PubMed Central

Woo, Jae-Man; Kim, Sae-Mi; Lee, Sung-Mi; Kim, Hyoun-Ee; Lee, Jung-Woo; Lee, Jong-Ho

2017-01-01

Magnesium (Mg) has the advantage of being resorbed in vivo, but its resorption rate is difficult to control. With uncontrolled resorption, Magnesium as a bone fixation material has minimal clinical value. During resorption not only is the strength rapidly weakened, but rapid formation of metabolite also occurs. In order to overcome these disadvantages, hydroxyapatite (HA) surface coating of pure magnesium plate was attempted in this study. Magnesium plates were inserted above the frontal bone of Sprague-Dawley rats in both the control group (Bare-Mg group) and the experimental group (HA-Mg group). The presence of inflammation, infection, hydrogen gas formation, wound dehiscence, and/or plate exposure was observed, blood tests were performed, and the resorption rate and tensile strength of the retrieved metal plates were measured. The HA-Mg group showed no gas formation or plate exposure until week 12. However, the Bare-Mg group showed consistent gas formation and plate exposure beginning in week 2. WBC (White Blood Cell), BUN (Blood Urea Nitrogen), Creatinine, and serum magnesium concentration levels were within normal range in both groups. AST (Aspartate Aminotransferase) and ALT (Alanine Aminotransferase) values, however, were above normal range in some animals of both groups. The HA-Mg group showed statistically significant advantage in resistance to degradation compared to the Bare-Mg group in weeks 2, 4, 6, 8, and 12. Degradation of HA-Mg plates proceeded after week 12. Coating magnesium plates with hydroxyapatite may be a viable method to maintain their strength long enough to allow bony healing and to control the resorption rate during the initial period. PMID:28973984

Synthesis, characterization and cell behavior of fluoridated hydroxyapatite

NASA Astrophysics Data System (ADS)

Qu, Haibo

Fluorine-containing hydroxyapatite (Ca5(PO4) 3(OH)1-xFx FHA), where F- partially replaces OH- in hydroxyapatite (HA), is recognized as a possible biomaterial for bone and tooth implants and gaining attention in the last several years as a possible alternative to HA. In this study, FHA powders were synthesized through a pH-cycling method. It was discovered that fluorine incorporation increased with the fluorine content in the initial solution and the number of pH cycles employed. A relatively low fluorine incorporation efficiency, ˜60%, was attained for most of the FHA samples. The short time of stay at each pH cycle and the limited number of cycles used are believed to be the main reasons of the low fluorine incorporation into the apatite structure. It was also revealed that the FHA particles produced by the pH-cycling method were inhomogeneous. They were a mixture of hydroxyapatite and F-rich apatite (or FA) particles. The mechanisms of incorporation of fluorine ions into hydroxyapatite by a pH cyclicing method were studied using TEM, XRD and fluorine measurement. Instead of forming laminated structures as reported by other research groups, a mixture of nano-sized F-rich apatite (FHA) and hydroxyapatite (HA) particles were obtained using the pH-cyclicing method. After calcination, these FHA particles were homogenized and became single phased FHA. The effect of fluorine content, preparing method, and sintering temperature on both the bulk density and biaxial flexural strength of sintered FHA was studied. Both uniaxially pressed un-milled (UPU) and cold isostatically pressed milled (IPM) FHA discs were sintered at temperatures between 1200˜400°C at an interval of 100°C. It was found that the fluorine content had a significant impact on the sintering behavior, densification, and mechanical properties of FHA discs. A close correlation between the sintered density and biaxial flexural strength of the specimens was revealed, where the biaxial flexural strength increased exponentially with the sintered density. FHA discs with various fluorine contents have been used to investigate the effect of fluorine content on osteoblastic cell behaviors. Rat osteosarcoma (ROS 17/28) cells were cultured on FHA discs for appropriate times. The osteoblastic cell behaviors were examined in terms of cell attachment, proliferation, morphology and differentiation. The fluorine content in FHA strongly affected the cell activities. More cell attachment and proliferation were observed on the fluorine-containing FHA than pure HA. Fluorine content also affected the differentiation behaviors of osteoblastic cells. Cells on fluorine-containing FHA had higher alkaline phosphatase (ALP) activity than pure HA in 2 weeks. The morphology of the cells showed that it took less time for cells to cover the surface of fluorine-containing samples than that of pure HA. These results suggested that fluorine ions had a significant impact on osteoblastic cell behaviors.

Periodontal tissue reaction to customized nano-hydroxyapatite block scaffold in one-wall intrabony defect: a histologic study in dogs

PubMed Central

Lee, Jung-Seok; Park, Weon-Yeong; Cha, Jae-Kook; Jung, Ui-Won; Kim, Chang-Sung; Lee, Yong-Keun

2012-01-01

Purpose This study evaluated histologically the tissue responses to and the effects of a customized nano-hydroxyapatite (n-HA) block bone graft on periodontal regeneration in a one-wall periodontal-defect model. Methods A customized block bone for filling in the standardized periodontal defect was fabricated from prefabricated n-HA powders and a polymeric sponge. Bilateral 4×4×5 mm (buccolingual width×mesiodistal width×depth), one-wall, critical-size intrabony periodontal defects were surgically created at the mandibular second and fourth premolars of five Beagle dogs. In each dog, one defect was filled with block-type HA and the other served as a sham-surgery control. The animals were sacrificed following an 8-week healing interval for clinical and histological evaluations. Results Although the sites that received an n-HA block showed minimal bone formation, the n-HA block was maintained within the defect with its original hexahedral shape. In addition, only a limited inflammatory reaction was observed at sites that received an n-HA block, which might have been due to the high stability of the customized block bone. Conclusions In the limitation of this study, customized n-HA block could provide a space for periodontal tissue engineering, with minimal inflammation. PMID:22586523

The Antimicrobial Properties of Zinc-Releasing Bioceramics

NASA Astrophysics Data System (ADS)

He, Xin

Up to 80% of nosocomial infections are caused by biofilm-producing bacteria such as Staphylococci and Pseudomonas aeruginosa. These types of microorganisms can become resistant to antibiotics and are difficult to eliminate. As such, there is tremendous interest in developing bioactive implant materials that can help to minimize these post- operative infections. Using water-based chemistry, we developed an economical, biodegradable and biocompatible orthopedic implant material consisting of zinc- doped hydroxyapatite (HA), which mimics the main inorganic component of the bone. Because the crystallinity of HA is typically too compact for efficient drug release, we substituted calcium ions in HA with zinc during the synthesis step to perturb the crystal structure. An added benefit is that zinc itself is a microelement of the human body with anti-inflammatory property, and we hypothesized that Zn-doped HA is an inherently antibacterial material. All HA samples were synthesized by a co-precipitation method using aqueous solutions of Zinc nitrate, Calcium Nitrate, and Ammonium Phosphate. XRD data showed that Zn was successfully incorporated into the HA. The effectiveness of Zn-doped HA against a model biofilm-forming bacterium is currently being evaluated using a wild-type strain and a streptomycin- resistant strain of Pseudomonas syringae pv. papulans (Psp) which is a plant pathogen isolated from diseased apples. Key words: Hydroxyapatite, Zinc, Citrate, Pseudomonas, Antibacterial.

The differential regulation of osteoblast and osteoclast activity by surface topography of hydroxyapatite coatings.

PubMed

Costa, Daniel O; Prowse, Paul D H; Chrones, Tom; Sims, Stephen M; Hamilton, Douglas W; Rizkalla, Amin S; Dixon, S Jeffrey

2013-10-01

The behavior of bone cells is influenced by the surface chemistry and topography of implants and scaffolds. Our purpose was to investigate how the topography of biomimetic hydroxyapatite (HA) coatings influences the attachment and differentiation of osteoblasts, and the resorptive activity of osteoclasts. Using strategies reported previously, we directly controlled the surface topography of HA coatings on polycaprolactone discs. Osteoblasts and osteoclasts were incubated on HA coatings having distinct isotropic topographies with submicrometer and micro-scale features. Osteoblast attachment and differentiation were greater on more complex, micro-rough HA surfaces (Ra ~2 μm) than on smoother topographies (Ra ~1 μm). In contrast, activity of the osteoclast marker tartrate-resistant acid phosphatase was greater on smoother than on micro-rough surfaces. Furthermore, scanning electron microscopy revealed the presence of resorption lacunae exclusively on smoother HA coatings. Inhibition of resorption on micro-rough surfaces was associated with disruption of filamentous actin sealing zones. In conclusion, HA coatings can be prepared with distinct topographies, which differentially regulate responses of osteoblasts, as well as osteoclastic activity and hence susceptibility to resorption. Thus, it may be possible to design HA coatings that induce optimal rates of bone formation and degradation specifically tailored for different applications in orthopedics and dentistry. Copyright © 2013 Elsevier Ltd. All rights reserved.

Innovative micro-textured hydroxyapatite and poly(l-lactic)-acid polymer composite film as a flexible, corrosion resistant, biocompatible, and bioactive coating for Mg implants.

PubMed

Kim, Sae-Mi; Kang, Min-Ho; Kim, Hyoun-Ee; Lim, Ho-Kyung; Byun, Soo-Hwan; Lee, Jong-Ho; Lee, Sung-Mi

2017-12-01

The utility of a novel ceramic/polymer-composite coating with a micro-textured microstructure that would significantly enhance the functions of biodegradable Mg implants is demonstrated here. To accomplish this, bioactive hydroxyapatite (HA) micro-dots can be created by immersing a Mg implant with a micro-patterned photoresist surface in an aqueous solution containing calcium and phosphate ions. The HA micro-dots can then be surrounded by a flexible poly(l-lactic)-acid (PLLA) polymer using spin coating to form a HA/PLLA micro-textured coating layer. The HA/PLLA micro-textured coating layer showed an excellent corrosion resistance when it was immersed in a simulated body fluid (SBF) solution and good biocompatibility, which was assessed by in vitro cell tests. In addition, the HA/PLLA micro-textured coating layer had high deformation ability, where no apparent changes in the coating layer were observed even after a 5% elongation, which would be unobtainable using HA and PLLA coating layers; furthermore, this allowed the mechanically-strained Mg implant with the HA/PLLA micro-textured coating layer to preserve its excellent corrosion resistance and biocompatibility in vitro. Copyright © 2017 Elsevier B.V. All rights reserved.

A further insight into the adsorption mechanism of protein on hydroxyapatite by FTIR-ATR spectrometry

NASA Astrophysics Data System (ADS)

Lin, Zhongyu; Hu, Ren; Zhou, Jianzhang; Ye, Yiwen; Xu, Zhaoxi; Lin, Changjian

2017-02-01

The adsorption mechanism of bovine serum albumin (BSA) on hydroxyapatite (HA) for different time intervals has been studied by Fourier transform infrared (FTIR)-attenuated total internal reflectance (ATR) spectrometry in this paper. The difference spectra obtained in HA and BSA frequency regions demonstrate that the binding of Pdbnd O, from the phosphate (PO43 -) of HA, to the hydrogen of methyl (- CH3), methene (- CH2) and amideII (- CNH) in the protein appears to be much faster and stronger than that of the Psbnd O group. In addition, Ca2 + must serve as a key role in the interaction of BSA with HA. The binding of Ca2 + to the oxygen of the peptide bond seems to induce a significant reconformation of polypeptide backbones from β-pleated sheet to α-helix and β-turn of helical circles. This alteration seems to have been accompanied by much hydrogen of polypeptides driven to bind PO43 - and OH- of the HA actively and much -C = O and Hsbnd Nsbnd groups of the peptide bond freed from inter-chain hydrogen bonding to react on Ca2 + and combine strongly with the HA surface. This might be well expected to promote the HA biomineralization.

Fabrication and physico-mechanical properties of thin magnetron sputter deposited silver-containing hydroxyapatite films

NASA Astrophysics Data System (ADS)

Ivanova, A. A.; Surmeneva, M. A.; Tyurin, A. I.; Pirozhkova, T. S.; Shuvarin, I. A.; Prymak, O.; Epple, M.; Chaikina, M. V.; Surmenev, R. A.

2016-01-01

As a measure of the prevention of implant associated infections, a number of strategies have been recently applied. Silver-containing materials possessing antibacterial activity as expected might have wide applications in orthopedics and dentistry. The present work focuses on the physico-chemical characterization of silver-containing hydroxyapatite (Ag-HA) coating obtained by radio frequency (RF) magnetron sputtering. Mechanochemically synthesized Ag-HA powder (Ca10⿿xAgx(PO4)6(OH)2⿿x, x = 1.5) was used as a precursor for sputtering target preparation. Morphology, composition, crystallinity, physico-mechanical features (Young's modulus and nanohardness) of the deposited Ag-HA coatings were investigated. The sputtering of the nanostructured multicomponent target at the applied process conditions allowed to deposit crystalline Ag-HA coating which was confirmed by XRD and FTIR data. The SEM results revealed the formation of the coating with the grain morphology and columnar cross-section structure. The EDX analysis confirmed that Ag-HA coating contained Ca, P, O and Ag with the Ca/P ratio of 1.6 ± 0.1. The evolution of the mechanical properties allowed to conclude that addition of silver to HA film caused increase of the coating nanohardness and elastic modulus compared with those of pure HA thin films deposited under the same deposition conditions.

Periodontal tissue reaction to customized nano-hydroxyapatite block scaffold in one-wall intrabony defect: a histologic study in dogs.

PubMed

Lee, Jung-Seok; Park, Weon-Yeong; Cha, Jae-Kook; Jung, Ui-Won; Kim, Chang-Sung; Lee, Yong-Keun; Choi, Seong-Ho

2012-04-01

This study evaluated histologically the tissue responses to and the effects of a customized nano-hydroxyapatite (n-HA) block bone graft on periodontal regeneration in a one-wall periodontal-defect model. A customized block bone for filling in the standardized periodontal defect was fabricated from prefabricated n-HA powders and a polymeric sponge. Bilateral 4×4×5 mm (buccolingual width×mesiodistal width×depth), one-wall, critical-size intrabony periodontal defects were surgically created at the mandibular second and fourth premolars of five Beagle dogs. In each dog, one defect was filled with block-type HA and the other served as a sham-surgery control. The animals were sacrificed following an 8-week healing interval for clinical and histological evaluations. Although the sites that received an n-HA block showed minimal bone formation, the n-HA block was maintained within the defect with its original hexahedral shape. In addition, only a limited inflammatory reaction was observed at sites that received an n-HA block, which might have been due to the high stability of the customized block bone. In the limitation of this study, customized n-HA block could provide a space for periodontal tissue engineering, with minimal inflammation.

Nano-scale characterization of nano-hydroxyapatite incorporated chitosan particles for bone repair.

PubMed

Gaihre, Bipin; Uswatta, Suren; Jayasuriya, Ambalangodage C

2018-05-01

In this study, injectable porous spherical particles were fabricated using chitosan (CS) biopolymer, sodium tripolyphosphate (TPP), and nano-hydroxyapatite (nHA). TPP was primarily used as an ionic crosslinker to crosslink 2% (w/v) CS droplets. 2% (w/v) nHA was used to prepare nHA incorporated particles. The surface morphological properties and nanomechanical properties such as topography, deformation, adhesion, and dissipation of CS particles with and without nHA were studied using contact mode and peakforce quantitative nanomechanical property mapping mode in atomic force microscopy. The nHA spots have higher density than CS which leads to higher forces acting on the probe tip and higher energy dissipation to lift the tip from nHA areas. The cumulative release data showed that about 87% of total BMP-2 encapsulated within the particles was released by third week of experiment period. Degradation study was conducted to understand how the particles degradation occurs in the presence of phosphate buffered saline with continues shaking in an incubator at 37° C. In addition, BMP-2 release from the 2% nHA/CS particles was studied over a three weeks period and found that BMP-2 release was governed by the simple diffusion rather than the degradation of particles. Copyright © 2018 Elsevier B.V. All rights reserved.

Control of hydroxyapatite coating by self-assembled monolayers on titanium and improvement of osteoblast adhesion.

PubMed

Shen, Juan; Qi, Yongcheng; Jin, Bo; Wang, Xiaoyan; Hu, Yamin; Jiang, Qiying

2017-01-01

Self-assembly technique was applied to introduce functional groups and form hydroxyl-, amine-, and carboxyl-terminal self-assembled monolayers (SAMs). The SAMs were grafted onto titanium substrates to obtain a molecularly smooth functional surface. Subsequent hydrothermal crystal growth formed homogeneous and crack-free crystalline hydroxyapatite (HA) coatings on these substrates. AFM and XPS were used to characterize the SAM surfaces, and XRD, SEM, and TEM were used to characterize the HA coatings. Results show that highly crystalline, dense, and oriented HA coatings can be formed on the OH-, NH 2 -, and COOH-SAM surfaces. The SAM surface with -COOH exhibited stronger nucleating ability than that with -OH and -NH 2 . The nucleation and growth processes of HA coatings were effectively controlled by varying reaction time, pH, and temperature. By using this method, highly crystalline, dense, and adherent HA coatings were obtained. In addition, in vitro cell evaluation demonstrated that HA coatings improved cell adhesion as compared with pristine titanium substrate. The proposed method is considerably effective in introducing the HA coatings on titanium surfaces for various biomedical applications and further usage in other industries. © 2015 Wiley Periodicals, Inc. J Biomed Mater Res Part B: Appl Biomater, 105B: 124-135, 2017. © 2015 Wiley Periodicals, Inc.

Nano-hydroxyapatite/β-CD/chitosan nanocomposite for potential applications in bone tissue engineering.

PubMed

Shakir, Mohammad; Jolly, Reshma; Khan, Mohd Shoeb; Rauf, Ahmar; Kazmi, Shadab

2016-12-01

Herein, we report the synthesis of a novel tri-component nanocomposite system incorporating β-cyclodextrin (β-CD) with nano-hydroxyapatite (n-HA) and chitosan (CS), (n-HA/β-CD/CS) at three different temperatures via co-precipitation method. The chemical interactions and surface morphology have been evaluated by TEM, SEM and AFM techniques revealing the agglomerated nanoparticles in CS/n-HA-HA binary system whereas the ternary systems produced needle shaped nanoparticles dispersed homogeneously at low temperature with more porous and rougher surface. The addition of β-CD in CS/n-HA at low temperature decreased the particle size and raised the thermal stability as compared to CS/n-HA. The comparative hemolytic, protein adsorption and platelet adhesion studies confirmed the better hemocompatibility of n-HA/β-CD/CS-(RT,HT,LT) nanocomposites relative to CS/n-HA. The cell viability has been evaluated in vitro using MG-63 cell line which revealed superior non toxicity of n-HA/β-CD/CS-LT nanocomposite in comparison to n-HA/β-CD/CS-(RT,HT) and CS/n-HA nanocomposites. Thus it may be concluded that the orchestrated organic/inorganic n-HA/β-CD/CS-(RT,HT,LT) nanocomposites exhibited relatively higher cell viability of human osteoblast cells, stimulated greater osteogenesis, controlled biodegradation, enhanced antibacterial activity with excellent in-vitro biomineralization and remarkable mechanical parameters as compared to CS/n-HA nanocomposite and thus may provide opportunities for potential use as an alternative biomaterial for Bone tissue engineering applications. Copyright © 2016 Elsevier B.V. All rights reserved.

The adsorptive behavior of albumin and lysozyme proteins on rod-shaped and plate-shaped hydroxyapatite.

PubMed

Ozeki, K; Hoshino, T; Aoki, H; Masuzawa, T

2013-01-01

The adsorption behavior of albumin (BSA) and lysozyme (LSZ) on rod-shaped and plate-shaped hydroxyapatite (HA) was investigated to evaluate the influence of crystal orientation and morphology on the selective protein adsorption of HA. The rod-shaped HA was prepared by hydrothermal treatment from β-tricalcium phosphate (β-TCP) in H3PO4 solution (pH 2.0 and 4.0 for HA-pH 2.0 and HA-pH 4.0). The plate-shaped HA was synthesized by hydrolysis of CaHPO4-2H2O (DCPD) in NaOH solution at 40°C and 80°C (HA-40°C and HA-80°C). The synthesized HA was characterized using scanning electron microscopy (SEM) and X-ray diffractometry (XRD). HA-pH 2.0 and HA-pH 4.0 produced rod-shaped crystals that were highly oriented to the a-face plane, whereas HA-40°C and HA-80°C showed a plate-like shape and a c-face preferred orientation. The peak intensity ratio I(300)/I(002) (a/c intensity ratio) from the XRD patterns increased in the following order: HA-80°C, HA-40°C, HA-pH 2.0 and HA-pH 4.0. It also increased as the Ca/P ratio decreased. The amount of adsorbed BSA increased in the following order: HA-pH 4.0, HA-pH 2.0, HA-40°C and HA-80°C. The amount of adsorbed LSZ on HA increased in the following order--HA-pH 2.0, HA-pH 4.0, HA-40°C and HA-80°C--with a corresponding decrease in the a/c intensity ratio. The BSA/LSA adsorption ratio increased with the a/c intensity ratio in the range of 3.3-8.9, and the BSA and LSZ were selectively adsorbed on HA, depending on the crystal shape.

Development of wear resistant NFSS-HA novel biocomposites and study of their tribological properties for orthopaedic applications.

PubMed

Younesi, M; Bahrololoom, M E; Fooladfar, H

2010-02-01

Implants made of nickel free austenitic stainless steel can reduce the toxic effect of released nickel ion and compounds from the conventional stainless steels. On the other hand, hydroxyapatite is a ceramic which has been used in orthopaedic applications due to its good osteoconductivity, biocompatibility and bioactivity. However, there is no evidence in the literature up to now on producing composites based on nickel free stainless steel and hydroxyapatite and study of their tribology. The aim of this work was to produce novel biocomposites made up of nickel free stainless steel with hydroxyapatite (prepared by heat treating bone ash) and studying their tribology under various loads in air and in Ringer's physiological solution. Different amounts of hydroxyapatite powder (10, 20, 30 and 40% Vol.) were added to this nickel free stainless steel powder to get the biocomposites. Variation of their density, hardness, wear resistance and friction with the ceramic (hydroxyapatite) content and wear load were investigated in air and in Ringer's solution. The density of the composites was decreased by increasing the volume percentage of the hydroxyapatite, while wear resistance of the composites was increased. The wear mechanism of these composites was changed by increasing the wear load and consequently the volume loss was enhanced dramatically. Furthermore, by increasing the sliding distance, the rate of volume loss was decreased slightly. The friction coefficient of the composites was also decreased by increasing the weight percentage of hydroxyapatite. Effect of the physiological Ringer's solution on wear resistance and friction coefficient of the composites was nearly negligible. The wear mechanisms of the samples were identified by studying the SEM images of the worn surfaces of the tested samples in different wear loads and HA contents. Copyright 2009 Elsevier Ltd. All rights reserved.

Improvement of the stability of hydroxyapatite through glass ceramic reinforcement.

PubMed

Ha, Na Ra; Yang, Zheng Xun; Hwang, Kyu Hong; Kim, Tae Suk; Lee, Jong Kook

2010-05-01

Hydroxyapatite has achieved significant application in orthopedic and dental implants due to its excellent biocompatibility. Sintered hydroxyapatites showed significant dissolution, however, after their immersion in water or simulated body fluid (SBF). This grain boundary dissolution, even in pure hydroxyapatites, resulted in grain separation at the surfaces, and finally, in fracture. In this study, hydroxyapatite ceramics containing apatite-wollastonite (AW) or calcium silicate (SG) glass ceramics as additives were prepared to prevent the dissolution. AW and SG glass ceramics were added at 0-7 wt% and powder-compacted uniaxially followed by firing at moisture conditions. The glass phase was incorporated into the hydroxyapatite to act as a sintering aid, followed by crystallization, to improve the mechanical properties without reducing the biocompatibility. As seen in the results of the dissolution test, a significant amount of damage was reduced even after more than 14 days. TEM and SEM showed no decomposition of HA to the secondary phase, and the fracture toughness increased, becoming even higher than that of the commercial hydroxyapatite.

Determination of the Mechanical Properties of Plasma-Sprayed Hydroxyapatite Coatings Using the Knoop Indentation Technique

NASA Astrophysics Data System (ADS)

Hasan, Md. Fahad; Wang, James; Berndt, Christopher

2015-06-01

The microhardness and elastic modulus of plasma-sprayed hydroxyapatite coatings were evaluated using Knoop indentation on the cross section and on the top surface. The effects of indentation angle, testing direction, measurement location and applied load on the microhardness and elastic modulus were investigated. The variability and distribution of the microhardness and elastic modulus data were statistically analysed using the Weibull modulus distribution. The results indicate that the dependence of microhardness and elastic modulus on the indentation angle exhibits a parabolic shape. Dependence of the microhardness values on the indentation angle follows Pythagoras's theorem. The microhardness, Weibull modulus of microhardness and Weibull modulus of elastic modulus reach their maximum at the central position (175 µm) on the cross section of the coatings. The Weibull modulus of microhardness revealed similar values throughout the thickness, and the Weibull modulus of elastic modulus shows higher values on the top surface compared to the cross section.

Biomimetic Hydroxyapatite Growth on Functionalized Surfaces of Ti-6Al-4V and Ti-Zr-Nb Alloys

NASA Astrophysics Data System (ADS)

Pylypchuk, Ie V.; Petranovskaya, A. L.; Gorbyk, P. P.; Korduban, A. M.; Markovsky, P. E.; Ivasishin, O. M.

2015-08-01

A biomimetic approach for coating titanium-containing alloys with hydroxyapatite (HA) is reported in the article. Two types of Ti-containing alloys were chosen as an object for coating: Ti-6Al-4V (recommended for orthopedic application) and a novel highly biocompatible Ti-Zr-Nb alloy, with good mechanical compatibility due to a modulus that is more close to that of human bones (E ≈ 50 GPa instead of 110 GPa in Ti-6Al-4V). Coating process was carried out in a 10×-concentrated simulated body fluid (SBF)—synthetic analog of human body plasma. The effect of oxidized and carboxylated alloy surface on formation of biomimetic hydroxyapatite has been studied. By XRD, we found influence of thermal conditions on HA crystal formation and size. SEM images and Fourier transform infrared confirmed that hydroxyapatite with different morphology, crystallinity, and Ca/P ratio formed on metallic surfaces. X-ray photoelectron spectroscopy showed that in the Ti-6AL-4V sample the observed Ca/P ratio reach 0.97, whereas in the Ti-Zr-Nb sample the observed Ca/P ratio reach 1.15.

Functionally graded bioactive coatings: From fabrication to testing

NASA Astrophysics Data System (ADS)

Foppiano, Silvia

Every year about half a million Americans undergo total joint replacement surgery of some kind. This number is expected to steadily increase in the future. About 20% of these patients will need a revision surgery because of implant failure, with a significant increase in health care cost. Current implant materials for load bearing applications must be strong enough to support the loads involved in daily activities, and bioinert, to limit reactivity in the body that may cause inflammatory and other adverse reactions. Metal alloys are typically used as materials for load bearing implants and rely on mechanical interlocking to achieve fixation which can be improved by using bone cements. To improve implant osteointegration, metal implants have been coated with a bone-like mineral: hydroxyapatite (HA). The plasma spray technique is commonly used to apply the HA coating. Such implants do not require the use of bone cement. Plasma sprayed HA coated implants are FDA approved and currently on the market, but their properties are not reproducible or reliable. Thus, coating delamination can occur. Our research group developed a novel family of bioactive glasses which were enameled onto titanium alloy using a functionally graded approach. We stratified the coating with different glass compositions to fulfill different functions. We coupled a first glass layer, with a good CTE match to the alloy, with a second layer of bioactive glass obtaining a functionally graded bioactive coating (FGC). In this thesis for the first time the cytocompatibility of novel bioactive glasses, and their functionally graded coatings on Ti6Al4V, was studied with an in vitro bone model (MC3T3-E1.4 mouse preosteblast cells). The novel bioactive glasses are cytocompatible and no compositional change is required. The fabrication process is reproducible, introduces a small (average 6 vol%) amount of crystallization, which does not significantly affect bioactivity in SBF as tested. The coatings are cytocompatible, but should be preconditioned in SBF prior to their use. Preconditioning stabilizes the coatings, eliminates possible contaminants introduced during processing and handling, and yields dissolution products capable of inducing specific gene expression (e.g. Runx-2). Future research will involve identification of such dissolution products as well as in vivo testing.

Effect of cell-seeded hydroxyapatite scaffolds on rabbit radius bone regeneration.

PubMed

Rathbone, C R; Guda, T; Singleton, B M; Oh, D S; Appleford, M R; Ong, J L; Wenke, J C

2014-05-01

Highly porous hydroxyapatite (HA) scaffolds were developed as bone graft substitutes using a template coating process, characterized, and seeded with bone marrow-derived mesenchymal stem cells (BMSCs). To test the hypothesis that cell-seeded HA scaffolds improve bone regeneration, HA scaffolds without cell seeding (HA-empty), HA scaffolds with 1.5 × 10(4) BMSCs (HA-low), and HA scaffolds with 1.5 × 10(6) BMSCs (HA-high) were implanted in a 10-mm rabbit radius segmental defect model for 4 and 8 weeks. Three different fluorochromes were administered at 2, 4, and 6 weeks after implantation to identify differences in temporal bone growth patterns. It was observed from fluorescence histomorphometry analyses that an increased rate of bone infiltration occurred from 0 to 2 weeks (p < 0.05) of implantation for the HA-high group (2.9 ± 0.5 mm) as compared with HA-empty (1.8 ± 0.8 mm) and HA-low (1.3 ± 0.2 mm) groups. No significant differences in bone formation within the scaffold or callus formation was observed between all groups after 4 weeks, with a significant increase in bone regenerated for all groups from 4 to 8 weeks (28.4% across groups). Although there was no difference in bone formation within scaffolds, callus formation was significantly higher in HA-empty scaffolds (100.9 ± 14.1 mm(3) ) when compared with HA-low (57.8 ± 7.3 mm(3) ; p ≤ 0.003) and HA-high (69.2 ± 10.4 mm(3) ; p ≤ 0.02) after 8 weeks. These data highlight the need for a better understanding of the parameters critical to the success of cell-seeded HA scaffolds for bone regeneration. Copyright © 2013 Wiley Periodicals, Inc.

Kinetics and thermodynamics studies on the BMP-2 adsorption onto hydroxyapatite surface with different multi-morphological features.

PubMed

Lu, Zhiwei; Huangfu, Changxin; Wang, Yanying; Ge, Hongwei; Yao, Yao; Zou, Ping; Wang, Guangtu; He, Hua; Rao, Hanbing

2015-01-01

The effect of the surface topography on protein adsorption process is of great significance for designing hydroxyapatite (HA) ceramic material surfaces. In this work, three different topographies of HA materials HA-sheet, HA-rod, and HA-whisker were synthesized and testified by X-ray diffraction (XRD), Fourier transform infrared (FT-IR), Brunauer-Emmett-Teller (BET) and a field emission scanning electron microscopy (FE-SEM). We have systematically investigated the adsorption kinetics and thermodynamics of bone morphogenetic proteins (BMP-2) on the three different topography surfaces of HA, respectively. The results showed that the maximum adsorption capacities of HA-sheet, HA-rod and HA-whisker were (219.96 ± 10.18), (247.13 ± 12.35), and (354.67 ± 17.73) μg · g(-1), respectively. Kinetic parameters, rate constants, equilibrium adsorption capacities and related correlation coefficients, for each kinetic model were calculated as well as discussed. It demonstrated that the adsorption of BMP-2 onto HA could be described by the pseudo second-order equation. Adsorption of BMP-2 onto HA followed the Langmuir isotherm. It confirmed that compared with other samples HA-whisker had more adsorption sites for its high specific surface area which could provide more opportunities for protein molecules. The adsorption processes were endothermic (ΔH > 0), spontaneous (ΔG < 0) and entropy increasing (ΔS > 0). A possible adsorption mechanism has been proposed. In addition, the BMP-2 could be adsorbed to the surface which existed slight conformational changes by FT-IR. Copyright © 2015 Elsevier B.V. All rights reserved.

Nanostructured hydroxyapatite/poly(lactic-co-glycolic acid) composite coating for controlling magnesium degradation in simulated body fluid.

PubMed

Johnson, Ian; Akari, Khalid; Liu, Huinan

2013-09-20

Biodegradable magnesium (Mg) and its alloys have many attractive properties (e.g. comparable mechanical properties to cortical bone) for orthopedic implant applications, but they degrade too rapidly in the human body to meet clinical requirements. Nanostructured hydroxyapatite (nHA)/poly(lactic-co-glycolic acid) (PLGA) composite coatings provide synergistic properties for controlling degradation of Mg-based substrates and improving bone-implant integration. In this study, nHA/PLGA composites were spin coated onto Mg-based substrates and the results showed that the nHA/PLGA coatings retained nano-scale features with nHA dispersed in PLGA matrix. In comparison with non-coated Mg, the nHA/PLGA composite coated Mg increased the corrosion potential and decreased the corrosion current in revised simulated body fluid (rSBF). After 24 h of immersion in rSBF, increased calcium phosphate (CaP) deposition and formation of Mg-substituted CaP rosettes were observed on the surface of the nHA/PLGA coated Mg, indicating greater bioactivity. In contrast, no significant CaP was deposited on the PLGA coated Mg. Since both PLGA coating and nHA/PLGA coating showed some degree of delamination from Mg-based substrates during extended immersion in rSBF, the coating processing and properties should be further optimized in order to take full advantage of biodegradable Mg and nHA/PLGA nanocomposites for orthopedic applications.

The Effect of Titanium Dioxide (TiO2) Nanoparticles on Hydroxyapatite (HA)/TiO2 Composite Coating Fabricated by Electrophoretic Deposition (EPD)

NASA Astrophysics Data System (ADS)

Amirnejad, M.; Afshar, A.; Salehi, S.

2018-05-01

Composite coatings of Hydroxyapatite (HA) with ceramics, polymers and metals are used to modify the surface structure of implants. In this research, HA/TiO2 composite coating was fabricated by electrophoretic deposition (EPD) on 316 stainless steel substrate. HA/TiO2 composite coatings with 5, 10 and 20 wt.% of TiO2, deposited at 40 V and 90 s as an optimum condition. The samples coated at this condition led to an adherent, continuous and crack-free coating. The influence of TiO2 content was studied by performing different characterization methods such as scanning electron microscopy (SEM), energy dispersive x-ray spectroscopy (EDS), corrosion resistance in simulated body fluid (SBF), coating's dissolution rate in physiological solution and bond strength to the substrate. The results showed that the higher amount of TiO2 in the composite coating led to increase in bond strength of coating to stainless steel substrate from 3 MPa for HA coating to 5.5 MPa for HA-20 wt.% TiO2 composite coating. In addition, it caused to reduction of corrosion current density of samples in the SBF solution from 18.92 μA/cm2 for HA coating to 6.35 μA/cm2 for HA-20 wt.% TiO2 composite coating.

Synthesis, characterization and biological evaluation of strontium/magnesium-co-substituted hydroxyapatite.

PubMed

Geng, Zhen; Wang, Renfeng; Li, Zhaoyang; Cui, Zhenduo; Zhu, Shengli; Liang, Yanqin; Liu, Yunde; Huijing, Bao; Li, Xue; Huo, Qianyu; Liu, Zhili; Yang, Xianjin

2016-07-01

The present study aims to investigate the contribution of two biologically important cations, Mg(2+) and Sr(2+), when co-substituted into the structure of hydroxyapatite (Ca10(PO4)6(OH)2, HA). The substituted samples were synthesized by a hydrothermal method that involved the addition of Mg(2+) and Sr(2+) containing precursors to partially replace Ca(2+) in the apatite structure. Four co-substituted HA samples with different concentrations of Mg(2+) and Sr(2+) ((Mg + Sr)/(Mg + Sr + Ca) = 30%) were investigated, and they were compared with pure HA. Experimental results showed that only a limited amount of Mg (Mg/(Mg + Ca + Sr) < 14%) could successfully substitute for Ca in HA. In addition, Mg substitution resulted in reduced crystallinity, thermal stability and lattice parameters of HA. In contrast, Sr could fully substitute for Ca. Furthermore, the addition of Sr increased the lattice parameters of HA. Here, we obtained the cation leach liquor by immersing the prepared samples in a culture medium for cell experiments. The in vitro study showed that 10Mg20Sr promoted better MG63 cell attachment, proliferation and differentiation than HA. Thus, the presence of an appropriate proportion of Mg and Sr could play a significant role in the increased biocompatibility of HA. © The Author(s) 2016.

The Effect of Titanium Dioxide (TiO2) Nanoparticles on Hydroxyapatite (HA)/TiO2 Composite Coating Fabricated by Electrophoretic Deposition (EPD)

NASA Astrophysics Data System (ADS)

Amirnejad, M.; Afshar, A.; Salehi, S.

2018-04-01

Composite coatings of Hydroxyapatite (HA) with ceramics, polymers and metals are used to modify the surface structure of implants. In this research, HA/TiO2 composite coating was fabricated by electrophoretic deposition (EPD) on 316 stainless steel substrate. HA/TiO2 composite coatings with 5, 10 and 20 wt.% of TiO2, deposited at 40 V and 90 s as an optimum condition. The samples coated at this condition led to an adherent, continuous and crack-free coating. The influence of TiO2 content was studied by performing different characterization methods such as scanning electron microscopy (SEM), energy dispersive x-ray spectroscopy (EDS), corrosion resistance in simulated body fluid (SBF), coating's dissolution rate in physiological solution and bond strength to the substrate. The results showed that the higher amount of TiO2 in the composite coating led to increase in bond strength of coating to stainless steel substrate from 3 MPa for HA coating to 5.5 MPa for HA-20 wt.% TiO2 composite coating. In addition, it caused to reduction of corrosion current density of samples in the SBF solution from 18.92 μA/cm2 for HA coating to 6.35 μA/cm2 for HA-20 wt.% TiO2 composite coating.

Preparation and mechanical properties of carbon fiber reinforced hydroxyapatite/polylactide biocomposites.

PubMed

Shen, Lie; Yang, Hui; Ying, Jia; Qiao, Fei; Peng, Mao

2009-11-01

A novel biocomposite of carbon fiber (CF) reinforced hydroxyapatite (HA)/polylactide (PLA) was prepared by hot pressing a prepreg which consisting of PLA, HA and CF. The prepreg was manufactured by solvent impregnation process. Polymer resin PLA dissolved with chloroform was mixed with HA. After reinforcement CF bundle was impregnated in the mixture, the solvent was dried completely and subsequently hot-pressed uniaxially under a pressure of 40 MPa at 170 degrees C for 20 min. A study was carried out to investigate change in mechanical properties of CF/HA/PLA composites before and after degradation in vitro. The composites have excellent mechanical properties. A peak showed in flexural strength, flexural modulus and shear strength aspects, reaching up 430 MPa, 22 GPa, 212 MPa, respectively, as the HA content increased. Degraded in vitro for 3 months, the flexural strength and flexural modulus of the CF/HA/PLA fell 13.2% and 5.4%, respectively, while the shear strength of the CF/HA/PLA composites remains at the 190 MPa level. The SEM photos showed that there were gaps between the PLA matrix and CF after degradation. Water uptake increased to 5%, but the mass loss rate was only 1.6%. The pH values of the PBS dropped less than 0.1. That's because the alkaline of HA neutralize the acid degrades from PLA, which can prevent the body from the acidity harm.

Mesenchymal stem cell-based repair of articular cartilage with polyglycolic acid-hydroxyapatite biphasic scaffold.

PubMed

Zhou, X Z; Leung, V Y; Dong, Q R; Cheung, K M; Chan, D; Lu, W W

2008-06-01

This study investigates the capacity of a composite scaffold composed of polyglycolic acid-hydroxyapatite (PGA-HA) and autologous mesenchymal stem cells (MSCs) to promote repair of osteochondral defects. MSCs from culture-expanded rabbits were seeded onto a PGA and HA scaffold. After a 72-hour co-culture period, the cell-adhered PGA and HA were joined together, forming an MSCs-PGA-HA composite. Full-thickness cartilage defects in the intercondylar fossa of the femur were then implanted with the MSC-PGA-HA composite, the PGA-HA scaffold only, or they were left empty (n=20). Animals were sacrificed 16 or 32 weeks after surgery and the gross appearance of the defects was evaluated. The specimens were examined histologically for morphologic features, and stained immunohistochemically for type 2 collagen. Specimens of the MSCs-PGA-HA composite implantation group demonstrated hyaline cartilage and a complete subchondral bone formation. At 16 weeks post-implantation, significant integration of the newly formed tissue with surrounding normal cartilage and subchondral bone was observed when compared to the two control groups. At 32 weeks, no sign of progressive degeneration of the newly formed tissue was found. A significant difference in histological grading score was found compared with the control groups. The novel MSCs-seeded, PGA-HA biphasic graft facilitated both articular cartilage and subchondral bone regeneration in an animal model and might serve as a new approach for clinical applications.

Nanostructured hydroxyapatite/poly(lactic-co-glycolic acid) composite coating for controlling magnesium degradation in simulated body fluid

NASA Astrophysics Data System (ADS)

Johnson, Ian; Akari, Khalid; Liu, Huinan

2013-09-01

Biodegradable magnesium (Mg) and its alloys have many attractive properties (e.g. comparable mechanical properties to cortical bone) for orthopedic implant applications, but they degrade too rapidly in the human body to meet clinical requirements. Nanostructured hydroxyapatite (nHA)/poly(lactic-co-glycolic acid) (PLGA) composite coatings provide synergistic properties for controlling degradation of Mg-based substrates and improving bone-implant integration. In this study, nHA/PLGA composites were spin coated onto Mg-based substrates and the results showed that the nHA/PLGA coatings retained nano-scale features with nHA dispersed in PLGA matrix. In comparison with non-coated Mg, the nHA/PLGA composite coated Mg increased the corrosion potential and decreased the corrosion current in revised simulated body fluid (rSBF). After 24 h of immersion in rSBF, increased calcium phosphate (CaP) deposition and formation of Mg-substituted CaP rosettes were observed on the surface of the nHA/PLGA coated Mg, indicating greater bioactivity. In contrast, no significant CaP was deposited on the PLGA coated Mg. Since both PLGA coating and nHA/PLGA coating showed some degree of delamination from Mg-based substrates during extended immersion in rSBF, the coating processing and properties should be further optimized in order to take full advantage of biodegradable Mg and nHA/PLGA nanocomposites for orthopedic applications.

Foliar spray banding characteristics

Treesearch

A.R. Womac; C.W. Smith; Joseph E. Mulrooney

2004-01-01

Foliar spray banding was explored as a means of reducing peticide use compared to broadcast applications. Barious geometric spray patterns and delivery angles of foliar spray bands were investigated to increase spray deposits in a crop row at a constant spray rate of 94 L/ha. Wind-free laboratory results indicated that a banded application using three 65° hollow-cone...

The effect of nanobioceramic reinforcement on mechanical and biological properties of Co-base alloy/hydroxyapatite nanocomposite.

PubMed

Bahrami, M; Fathi, M H; Ahmadian, M

2015-03-01

The goal of the present research was to fabricate, characterize, and evaluate mechanical and biological properties of Co-base alloy composites with different amounts of hydroxyapatite (HA) nanopowder reinforcement. The powder of Co-Cr-Mo alloy was mixed with different amounts of HA by ball milling and it was then cold pressed and sintered. X-ray diffraction (XRD) and scanning electron microscopy (SEM) techniques were used. Microhardness measurement and compressive tests were also carried out. Bioactivity behavior was evaluated in simulated body fluid (SBF). A significant decrease in modulus elasticity and an increase in microhardness of the sintered composites were observed. Apatite formation on the surface of the composites showed that it could successfully convert bioinert Co-Cr-Mo alloy to bioactive type by adding 10, 15, and 20wt.% HA which have lower modulus elasticity and higher microhardness. Copyright © 2014 Elsevier B.V. All rights reserved.

Hydroxyapatite/poly(epsilon-caprolactone) double coating on magnesium for enhanced corrosion resistance and coating flexibility.

PubMed

Jo, Ji-Hoon; Li, Yuanlong; Kim, Sae-Mi; Kim, Hyoun-Ee; Koh, Young-Hag

2013-11-01

Hydroxyapatite was deposited on pure magnesium (Mg) with a flexible poly(ε-caprolactone) interlayer to reduce the corrosion rate of Mg and enhance coating flexibility. The poly(ε-caprolactone) interlayer was uniformly coated on Mg by a spraying method, followed by hydroxyapatite deposition on the poly(ε-caprolactone) using an aerosol deposition method. In scanning electron microscopy observations, inorganic/organic composite-like structure was observed between the hydroxyapatite and poly(ε-caprolactone) layers, resulting from the collisions of hydroxyapatite particles into the poly(ε-caprolactone) matrix at the initial stage of the aerosol deposition. The corrosion resistance of the coated Mg was examined using potentiodynamic polarization tests. The hydroxyapatite/poly(ε-caprolactone) double coating remarkably improved the corrosion resistance of Mg in Hank's solution. In the in vitro cell tests, the coated Mg showed better cell adhesion compared with the bare Mg due to the reduced corrosion rate and enhanced biocompatibility. The stability and flexibility of hydroxyapatite/poly(ε-caprolactone) double coating was investigated by scanning electron microscopy inspections after the coated Mg was deformed. The hydroxyapatite coating on the poly(ε-caprolactone) interlayer revealed enhanced coating stability and flexibility without cracking or delamination during bending and stretching compared with the hydroxyapatite single coating. These results demonstrated that the hydroxyapatite/poly(ε-caprolactone) double coating significantly improved the surface corrosion resistance of Mg and enhanced coating flexibility for use of Mg as a biodegradable implant.

Ultrasound-assisted fabrication of a biocompatible magnetic hydroxyapatite.

PubMed

Zhou, Gang; Song, Wei; Hou, Yongzhao; Li, Qing; Deng, Xuliang; Fan, Yubo

2014-10-01

This work describes the fabrication and characterization of a biocompatible magnetic hydroxyapatite (HA) using an ultrasound-assisted co-precipitation method. X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), and transmission electron microscopy (TEM) were used to characterize the structure and chemical composition of the produced samples. The M-H loops of synthesized materials were traced using a vibrating sample magnetometer (VSM) and the biocompatibility was evaluated by cell culture and MTT (3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide) assay. Furthermore, in vivo histopathological examinations were used to evaluate the potential toxicological effects of Fe₃O₄-HA composites on kidney of SD rats injected intraperitoneally with Fe₃O₄-HA particles. The results showed that magnetic iron oxide particles first replace OH ions of HA, which are parallel to the c axis, and then enter the HA crystal lattice which produces changes in the crystal surface of HA. Chemical bond interaction was observed between PO₄³⁻ groups of HA and iron ions of Fe₃O₄. The saturation magnetization (MS ) of Fe₃O₄-HA composites was 46.36 emu/g obtained from VSM data. Cell culture and MTT assays indicated that HA could affect the growth and proliferation of HEK-293 cells. This Fe₃O₄-HA composite produced no negative effects on cell morphology, viability, and proliferation and exhibited remarkable biocompatibility. Moreover, no inflammatory cell infiltration was observed in kidney histopathology slices. Therefore, this study succeeds to develop a Fe₃O₄-HA composite as a prospective biomagnetic material for future applications. © 2013 Wiley Periodicals, Inc.

Production of biologically safe and mechanically improved reduced graphene oxide/hydroxyapatite composites

NASA Astrophysics Data System (ADS)

Elif, Öztürk; Belma, Özbek; İlkay, Şenel

2017-01-01

As research trends included the improvement of the mechanical properties of hydroxyapatite (HA) for biological applications, HA was reinforced with different concentrations of reduced graphene oxide (RGO) in HA. In this context, graphene oxide was synthesized using the chemical exfoliation method and reduced using an environmentally safe and green method. As a green method, RGO was obtained using Melissa officinalis (melisa) extract and used as a second phase combination to the HA structure. RGO-HA composites with different concentrations of RGO in HA (0.25, 0.5, 1.0, 2.0% wt.) were prepared using the liquid precipitation method. Then they were pelleted and sintered. Characterization studies were carried out using UV-vis, Fourier transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), zetasizer (ZS), x-ray powder diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM) images. The mechanical properties of the composites were analyzed using a universal testing machine. Compared to pure HA, the compressive strength values of composites were increased significantly with the increase in RGO content. The optimum increase was observed for the RGO-HA (1%) composite, which was 3.2 times higher than the pure HA sample. Therefore, the RGO-HA (1%) composite was chosen as the best composition, and its cytotoxic and proliferative effects were examined using a minimum essential media elution test and a 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide assay. The results showed that RGO-HA (1%) composites are biocompatible and even though they are proliferative at concentrations lower than 25%.

Synthesis and structural characterization of nano-hydroxyapatite biomaterials prepared by microwave processing

NASA Astrophysics Data System (ADS)

Ramli, Rosmamuhamadani; Arawi, Ainaa Zafirah Omar; Talari, Mahesh Kumar; Mahat, Mohd Muzamir; Jais, Umi Sarah

2012-07-01

Synthetic hydroxyapatite, (HA, Ca10(PO4)6(OH)2), is an attractive and widely utilized bio-ceramic material for orthopedic and dental implants because of its close resemblance of native tooth and bone crystal structure. Synthetic HA exhibits excellent osteoconductive properties. Osteoconductivity means the ability to provide the appropriate scaffold or template for bone formation. Calcium phosphate biomaterials [(HA), tri-calcium phosphate (TCP) and biphasic calcium phosphate (HA/TCP)] with appropriate three-dimensional geometry are able to bind and concentrate endogenous bone morphogenetic proteins in circulation, and may become osteoinductive and can be effective carriers of bone cell seeds. This HA can be used in bio-implants as well as drug delivery application due to the unique properties of HA. Biomaterials synthesized from the natural species like mussel shells have additional benefits such as high purity, less expensive and high bio compatibility. In this project, HA-nanoparticles of different crystallite size were prepared by microwave synthesis of precursors. High purity CaO was extracted from the natural mussel shells for the synthesis of nano HA. Dried nano HA powders were analyzed using X-Ray Diffraction (XRD) technique for the determination of crystal structure and impurity content. Scanning Electron Microscopic (SEM) investigation was employed for the morphological investigation of nano HA powders. From the results obtained, it was concluded that by altering the irradiation time, nano HA powders of different crystallite sizes and morphologies could be produced. Crystallite sizes calculated from the XRD patterns are found to be in the range of 10-55 nm depending on the irradiation time.

Syntheses of near-net-shaped monolithic hydroxyapatite and hydroxyapatite-ASTM F75 composites by the oxidation of solid metal-bearing precursors

NASA Astrophysics Data System (ADS)

Saw, Eaden

A novel powder-metallurgical route was used to fabricate near net-shaped hydroxyapatite, Ca10(PO4)6(OH)2 (HA) and HA+Co-C-Mo composite bodies. Ca and beta-Ca2P 2O7 with Ca/P ˜ 1.67 was intimately mixed by high-energy mechanical alloying, formed into desired shapes by pressing and machining, and then converted into HA with a series of heat treatments: a 600°C annealing in dry O2 completely oxidized calcium within 3 h, and a subsequent annealing at ≤1150°C in moist O2 yielded phase-pure HA. The reduction in solid volume associated with the oxidation of calcium (Vm[CaO] < Vm[Ca]) was offset by the increase in solid volume associated with the conversion of CaO and Ca2P2O7 into HA. Thus, the overall dimensional changes upon transformation of Ca+beta-Ca2P 2O7 precursors into HA can be relatively small. A mixture of Co-Cr-Mo powder with the precursor prepared from Ca and beta-Ca 2P2O7, targeted to yield a 75 to 25 volume ratio of Co-Cr-Mo to stoichiometric HA were prepared with the same method but different annealing cycles: annealing at 1150°C in de-oxygenized, flowing Ar resulted in partial densification of the composite bodies, and subsequent annealing at 850°C in a moist O2 atmosphere yielded a composite of Co-Cr-Mo alloy with phase-pure HA. The overall dimensional changes upon transformation of Ca+beta-Ca2P2O7+CO-Cr-Mo precursors into HA/Co-Cr-Mo composite were relatively small. In this thesis, the phase and microstructural evolution at various stages of transformation to monolithic HA and to HA/Co-Cr-Mo alloy composites are discussed. Planar reaction couples and powder compacts of CaO-TCP were prepared to study the kinetics for HA formation from CaO+TCP. Pt strips were used in the planar reaction couples as inert markers. These reaction couples were heated at 1150°C for various times in moist O2. The results of powder compact analyses fits Carter's model, which indicated that the rate of HA conversion from CaO and TCP is limited by solid state diffusion of Ca 2+ and/or OH- through the HA layer.

Effect of micro-nano-hybrid structured hydroxyapatite bioceramics on osteogenic and cementogenic differentiation of human periodontal ligament stem cell via Wnt signaling pathway.

PubMed

Mao, Lixia; Liu, Jiaqiang; Zhao, Jinglei; Chang, Jiang; Xia, Lunguo; Jiang, Lingyong; Wang, Xiuhui; Lin, Kaili; Fang, Bing

2015-01-01

The surface structure of bioceramic scaffolds is crucial for its bioactivity and osteoinductive ability, and in recent years, human periodontal ligament stem cells have been certified to possess high osteogenic and cementogenic differential ability. In the present study, hydroxyapatite (HA) bioceramics with micro-nano-hybrid surface (mnHA [the hybrid of nanorods and microrods]) were fabricated via hydrothermal reaction of the α-tricalcium phosphate granules as precursors in aqueous solution, and the effects of mnHA on the attachment, proliferation, osteogenic and cementogenic differentiations of human periodontal ligament stem cells as well as the related mechanisms were systematically investigated. The results showed that mnHA bioceramics could promote cell adhesion, proliferation, alkaline phosphatase (ALP) activity, and expression of osteogenic/cementogenic-related markers including runt-related transcription factor 2 (Runx2), ALP, osteocalcin (OCN), cementum attachment protein (CAP), and cementum protein (CEMP) as compared to the HA bioceramics with flat and dense surface. Moreover, mnHA bioceramics stimulated gene expression of low-density lipoprotein receptor-related protein 5 (LRP5) and β-catenin, which are the key genes of canonical Wnt signaling. Moreover, the stimulatory effect on ALP activity and osteogenic and cementogenic gene expression, including that of ALP, OCN, CAP, CEMP, and Runx2 of mnHA bioceramics could be repressed by canonical Wnt signaling inhibitor dickkopf1 (Dkk1). The results suggested that the HA bioceramics with mnHA could act as promising grafts for periodontal tissue regeneration.

Preparation and characterization of chitosan-natural nano hydroxyapatite-fucoidan nanocomposites for bone tissue engineering.

PubMed

Lowe, Baboucarr; Venkatesan, Jayachandran; Anil, Sukumaran; Shim, Min Suk; Kim, Se-Kwon

2016-12-01

Solid three dimensional (3D) composite scaffolds for bone tissue engineering were prepared using the freeze-drying method. The scaffolds were composed of chitosan, natural nano-hydroxyapatite (nHA) and fucoidan in the following combinations: chitosan, chitosan-fucoidan, chitosan-nHA, and chitosan-nHA-fucoidan. Fourier transform infrared spectroscopy (FT-IR), thermal gravimetric analysis (TGA), X-ray diffraction analysis (XRD), scanning electron microscopy (SEM), and optical microscopy (OM) were used to determine the physiochemical constituents and the morphology of the scaffolds. The addition of nHA into the chitosan-fucoidan composite scaffold reduced the water uptake and water retention. FT-IR analysis confirmed the presence of a phosphate group in the chitosan-nHA-fucoidan scaffold. This group is present because of the presence of nHA (isolated via alkaline hydrolysis from salmon fish bones). Microscopic results indicated that the dispersion of nHA and fucoidan in the chitosan matrix was uniform with a pore size of 10-400μm. The composite demonstrated a suitable micro architecture for cell growth and nutrient supplementation. This compatibility was further elucidated in vitro using periosteum-derived mesenchymal stem cells (PMSCs). The cells demonstrated high biocompatibility and excellent mineralization for the chitosan-nHA-fucoidan scaffold. We believe that a chitosan-nHA-fucoidan composite is a promising biomaterial for the scaffold that can be used for bone tissue regeneration. Copyright © 2016 Elsevier B.V. All rights reserved.

A biological method for in-situ synthesis of hydroxyapatite-coated magnetite nanoparticles using Enterobacter aerogenes: Characterization and acute toxicity assessments.

PubMed

Ahmadzadeh, Elham; Talebnia Rowshan, Farid; Hosseini, Morteza

2017-04-01

Hydroxyapatite (HA)-coated magnetite nanoparticles (MNPs) are being widely investigated for various applications in medical engineering and wastewater treatment. In this work, the MNPs were thoroughly coated by bacterial synthesized HA nanoparticles during biomineralization process using Enterobacter aerogenes. The resulting bacterial-induced precipitate was then calcined at 600°C and investigated with respect to structural characteristics, particle size and magnetic strength by XRD, FT-IR, SEM, EDS, TEM and VSM analyses. The effects of MNPs and HA-coated MNPs (HA-MNPs) on the viability of human MCF-7 cell lines were also investigated via mitochondrial activity test (MTT) and lactate dehydrogenase (LDH) assays. The powder characterization results showed appropriate structural properties for HA-MNPs samples. The particles diameter size of the MNPs and HA-MNPs were in the range of 3-25nm and 20-80nm, respectively. The biologically-synthesized HA-MNPs formed a stable suspension in water while keeping their magnetic property. The saturation magnetization (Ms) of HA-MNPs was measured at ~10emug -1 which was in good agreement with the structural composition of this sample. Finally, the results of the cell lines viability indicated that coating of toxic MNPs via biomineralization was a promising approach in order to synthesize bio-compatible magnetic nanoparticles with suitable physical and chemical structural characteristics. The toxicity level of MNPs was reduced by 10 fold when coated by bacterial-synthesized HA. Copyright © 2016 Elsevier B.V. All rights reserved.

Influence of Silver-hydroxyapatite Nanocomposite Coating on Biofilm Formation of Joint Prosthesis and Its Mechanism.

PubMed

Zhao, L; Ashraf, M A

2015-12-01

The main reason for biomaterial related refractory infections is biofilm formation caused by bacterial adhesion on the surface of materials. Silver-hydroxyapatite (Ag/HA) nanocomposite coating can inhibit the formation of biofilm, but its mechanism is not clear. In order to clarify the mechanism, the amounts of biofilm on the Ag/HA composite coating and HA coating were determined, the release rates of silver nanoparticles in simulated body fluid (SBF) were detected by atomic absorption spectrometry, and the expression values of atlE , fbe , sap , iapB genes of Staphylococcus aureus were studied when they grew on Ag/HA composite coating and HA coating. The amount of the biofilm on the Ag/HA composite coating was significantly less than that on the HA coating, and the bacterial adhesion was decreased. The silver nanoparticles were released continuously in SBF and the release rate decreased gradually with time. The expression values of atlE , fbe and sap were high in the initial stage of adhesion and the expression value of iapB was high in the colonies-gathering stage in the control group, but they were all significantly inhibited in the presence of Ag. These results indicated that the main antibacterial effect of Ag/HA composite coating was achieved by the release of silver nanoparticles. The addition of Ag inhibited the expression of genes related to biofilm formation, which in turn inhibited the formation of biofilms. This provided theoretical support for the clinical application of Ag/HA composite coating.

Doped biocompatible layers prepared by laser

NASA Astrophysics Data System (ADS)

Jelínek, M.; Weiserová, M.; Kocourek, T.; Jurek, K.; Strnad, J.

2010-03-01

The contribution deals with KrF laser synthesis and study of doped biocompatible materials with focus on diamond-like carbon (DLC) and hydroxyapatite (HA). Overview of materials used for dopation is given. Experimental results of study of HA layers doped with silver are presented. Films properties were characterized using profilometer, SEM, WDX, XRD and optical transmission. Content of silver in layers moved from 0.06 to 13.7 at %. The antibacterial properties of HA, silver and doped HA layers were studied in vivo using Escherichia coli cells.

Hyper-elastic modeling and mechanical behavior investigation of porous poly-D-L-lactide/nano-hydroxyapatite scaffold material.

PubMed

Han, Quan Feng; Wang, Ze Wu; Tang, Chak Yin; Chen, Ling; Tsui, Chi Pong; Law, Wing Cheung

2017-07-01

Poly-D-L-lactide/nano-hydroxyapatite (PDLLA/nano-HA) can be used as the biological scaffold material in bone tissue engineering as it can be readily made into a porous composite material with excellent performance. However, constitutive modeling for the mechanical response of porous PDLLA/nano-HA under various stress conditions has been very limited so far. In this work, four types of fundamental compressible hyper-elastic constitutive models were introduced for constitutive modeling and investigation of mechanical behaviors of porous PDLLA/nano-HA. Moreover, the unitary expressions of Cauchy stress tensor have been derived for the PDLLA/nano-HA under uniaxial compression (or stretch), biaxial compression (or stretch), pure shear and simple shear load by using the theory of continuum mechanics. The theoretical results determined from the approach based on the Ogden compressible hyper-elastic constitutive model were in good agreement with the experimental data from the uniaxial compression tests. Furthermore, this approach can also be used to predict the mechanical behaviors of the porous PDLLA/nano-HA material under the biaxial compression (or stretch), pure shear and simple shear. Copyright © 2017 Elsevier Ltd. All rights reserved.

Electrophoretic deposition of silicon substituted hydroxyapatite coatings from n-butanol-chloroform mixture.

PubMed

Xiao, Xiu Feng; Liu, Rong Fang; Tang, Xiao Lian

2008-01-01

Silicon Substituted Hydroxyapatite (Si-HA) coatings were prepared on titanium substrates by electrophoretic deposition (EPD). The stability of Si-HA suspension in n-butanol and chloroform mixture has been studied by electricity conductivity and sedimentation test. The microstructure, shear strength and bioactivity in vitro has been tested. The stability of Si-HA suspension containing n-butanol and chloroform mixture as medium is better than that of pure n-butanol as medium. The good adhesion of the particles with the substrate and good cohesion between the particles were obtained in n-butanol and chloroform mixture. Adding triethanolamine (TEA) as additive into the suspension is in favor of the formation of uniform and compact Si-HA coatings on the titanium substrates by EPD. The shear strength of the coatings can reach 20.43 MPa after sintering at 700 degrees C for 2 h, when the volume ratio of n-butanol: chloroform is 2:1 and the concentration of TEA is 15 ml/L. Titanium substrates etched in H(2)O(2)/NH(3) solution help to improve the shear strength of the coatings. After immersion in simulated body fluid for 7 days, Si-HA coatings have the ability to induce the bone-like apatite formation.

Distributed vasculogenesis from modular agarose-hydroxyapatite-fibrinogen microbeads.

PubMed

Rioja, Ana Y; Daley, Ethan L H; Habif, Julia C; Putnam, Andrew J; Stegemann, Jan P

2017-06-01

Critical limb ischemia impairs circulation to the extremities, causing pain, disrupted wound healing, and potential tissue necrosis. Therapeutic angiogenesis seeks to repair the damaged microvasculature directly to restore blood flow. In this study, we developed modular, micro-scale constructs designed to possess robust handling qualities, allow in vitro pre-culture, and promote microvasculature formation. The microbead matrix consisted of an agarose (AG) base to prevent aggregation, combined with cell-adhesive components of fibrinogen (FGN) and/or hydroxyapatite (HA). Microbeads encapsulating a co-culture of human umbilical vein endothelial cells (HUVEC) and fibroblasts were prepared and characterized. Microbeads were generally 80-100µm in diameter, and the size increased with the addition of FGN and HA. Addition of HA increased the yield of microbeads, as well as the homogeneity of distribution of FGN within the matrix. Cell viability was high in all microbead types. When cell-seeded microbeads were embedded in fibrin hydrogels, HUVEC sprouting and inosculation between neighboring microbeads were observed over seven days. Pre-culture of microbeads for an additional seven days prior to embedding in fibrin resulted in significantly greater HUVEC network length in AG+HA+FGN microbeads, as compared to AG, AG+HA or AG+FGN microbeads. Importantly, composite microbeads resulted in more even and widespread endothelial network formation, relative to control microbeads consisting of pure fibrin. These results demonstrate that AG+HA+FGN microbeads support HUVEC sprouting both within and between adjacent microbeads, and can promote distributed vascularization of an external matrix. Such modular microtissues may have utility in treating ischemic tissue by rapidly re-establishing a microvascular network. Critical limb ischemia (CLI) is a chronic disease that can lead to tissue necrosis, amputation, and death. Cell-based therapies are being explored to restore blood flow and prevent the complications of CLI. In this study, we developed small, non-aggregating agarose-hydroxyapatite-fibrinogen microbeads that contained endothelial cells and fibroblasts. Microbeads were easy to handle and culture, and endothelial sprouts formed within and between microbeads. Our data demonstrates that the composition of the microbead matrix altered the degree of endothelial sprouting, and that the addition of hydroxyapatite and fibrinogen resulted in more distributed sprouting compared to pure fibrin microbeads. The microbead format and control of the matrix formulation may therefore be useful in developing revascularization strategies for the treatment of ischemic disease. Copyright © 2017 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Hydroxyapatite formation on graphene oxide modified with amino acids: arginine versus glutamic acid

PubMed Central

Tavafoghi, M.; Brodusch, N.; Gauvin, R.; Cerruti, M.

2016-01-01

Hydroxyapatite (HA, Ca5(PO4)3OH) is the main inorganic component of hard tissues, such as bone and dentine. HA nucleation involves a set of negatively charged phosphorylated proteins known as non-collagenous proteins (NCPs). These proteins attract Ca2+ and PO43− ions and increase the local supersaturation to a level required for HA precipitation. Polar and charged amino acids (AAs) are highly expressed in NCPs, and seem to be responsible for the mineralizing effect of NCPs; however, the individual effect of these AAs on HA mineralization is still unclear. In this work, we investigate the effect of a negatively charged (Glu) and positively charged (Arg) AA bound to carboxylated graphene oxide (CGO) on HA mineralization in simulated body fluids (SBF). Our results show that Arg induces HA precipitation faster and in larger amounts than Glu. We attribute this to the higher stability of the complexes formed between Arg and Ca2+ and PO43− ions, and also to the fact that Arg exposes both carboxyl and amino groups on the surface. These can electrostatically attract both Ca2+ and PO43− ions, thus increasing local supersaturation more than Glu, which exposes carboxyl groups only. PMID:26791001

New nanostructural biomaterials based on active silicate systems and hydroxyapatite: characterization and genotoxicity in human peripheral blood lymphocytes.

PubMed

Opačić-Galić, V; Petrović, V; Zivković, S; Jokanović, V; Nikolić, B; Knežević-Vukčević, J; Mitić-Ćulafić, D

2013-06-01

To characterize and investigate the genotoxic effect of a new endodontic cement based on dicalcium- and tricalcium-silicate (CS) with hydroxyapatite (HA) on human lymphocytes. Hydrothermal treatment was applied for synthesis of CS and HA. The final mixture HA-CS, with potential to be used in endodontic practice, is composed of CS (34%) and HA (66%). Human lymphocytes were incubated with HA, HA-CS and CS for 1 h, at 37 °C and 5% CO2. Cell viability was determined using the trypan blue exclusion assay. To evaluate the level of DNA damage comet assay (single cell gel electrophoresis) was performed. For the statistical analysis anova and Duncan's Post Hoc Test were used. The SEM analysis indicated that CS consisted mostly of agglomerates of several micrometers in size, built up from smaller particles, with dimensions between 117 and 477 nm. This is promising because dimensions of agglomerates are not comparable with channels inside the cell membranes, whereas their nano-elements provide evident activity, important for faster setting of these mixtures compared to MTA. Values of DNA damage obtained in the comet assay indicated low genotoxic risk of the new endodontic materials. The significantly improved setting characteristics and low genotoxic risk of the new material support further research. © 2012 International Endodontic Journal.

Hydroxyapatite formation on graphene oxide modified with amino acids: arginine versus glutamic acid.

PubMed

Tavafoghi, M; Brodusch, N; Gauvin, R; Cerruti, M

2016-01-01

Hydroxyapatite (HA, Ca5(PO4)3OH) is the main inorganic component of hard tissues, such as bone and dentine. HA nucleation involves a set of negatively charged phosphorylated proteins known as non-collagenous proteins (NCPs). These proteins attract Ca(2+) and PO4(3-) ions and increase the local supersaturation to a level required for HA precipitation. Polar and charged amino acids (AAs) are highly expressed in NCPs, and seem to be responsible for the mineralizing effect of NCPs; however, the individual effect of these AAs on HA mineralization is still unclear. In this work, we investigate the effect of a negatively charged (Glu) and positively charged (Arg) AA bound to carboxylated graphene oxide (CGO) on HA mineralization in simulated body fluids (SBF). Our results show that Arg induces HA precipitation faster and in larger amounts than Glu. We attribute this to the higher stability of the complexes formed between Arg and Ca(2+) and PO4(3-) ions, and also to the fact that Arg exposes both carboxyl and amino groups on the surface. These can electrostatically attract both Ca(2+) and PO4(3-) ions, thus increasing local supersaturation more than Glu, which exposes carboxyl groups only. © 2016 The Author(s).

Nano-Ag-loaded hydroxyapatite coatings on titanium surfaces by electrochemical deposition

PubMed Central

Lu, Xiong; Zhang, Bailin; Wang, Yingbo; Zhou, Xianli; Weng, Jie; Qu, Shuxin; Feng, Bo; Watari, Fumio; Ding, Yonghui; Leng, Yang

2011-01-01

Hydroxyapatite (HA) coatings on titanium (Ti) substrates have attracted much attention owing to the combination of good mechanical properties of Ti and superior biocompatibility of HA. Incorporating silver (Ag) into HA coatings is an effective method to impart the coatings with antibacterial properties. However, the uniform distribution of Ag is still a challenge and Ag particles in the coatings are easy to agglomerate, which in turn affects the applications of the coatings. In this study, we employed pulsed electrochemical deposition to co-deposit HA and Ag simultaneously, which realized the uniform distribution of Ag particles in the coatings. This method was based on the use of a well-designed electrolyte containing Ag ions, calcium ions and l-cysteine, in which cysteine acted as the coordination agent to stabilize Ag ions. The antibacterial and cell culture tests were used to evaluate the antibacterial properties and biocompatibility of HA/Ag composite coatings, respectively. The results indicated the as-prepared coatings had good antibacterial properties and biocompatibility. However, an appropriate silver content should be chosen to balance the biocompatibility and antibacterial properties. Heat treatments promoted the adhesive strength and enhanced the biocompatibility without sacrificing the antibacterial properties of the HA/Ag coatings. In summary, this study provided an alternative method to prepare bioactive surfaces with bactericidal ability for biomedical devices. PMID:20880853

Development of electrochemical folic acid sensor based on hydroxyapatite nanoparticles.

PubMed

Kanchana, P; Sekar, C

2015-02-25

We report the synthesis of hydroxyapatite (HA) nanoparticles (NPs) by a simple microwave irradiation method and its application as sensing element for the precise determination of folic acid (FA) by electrochemical method. The structure and composition of the HA NPs characterized using XRD, FTIR, Raman and XPS. SEM and EDX studies confirmed the formation of elongated spherical shaped HA NPs with an average particle size of about 34 nm. The HA NPs thin film on glassy carbon electrode (GCE) were deposited by drop casting method. Electrocatalytic behavior of FA in the physiological pH 7.0 was investigated by cyclic voltammetry (CV), linear sweep voltammetry (LSV) and chronoamperometry. The fabricated HA/GCE exhibited a linear calibration plot over a wide FA concentration ranging from 1.0×10(-7) to 3.5×10(-4) M with the detection limit of 75 nM. In addition, the HA NPs modified GCE showed good selectivity toward the determination of FA even in the presence of a 100-fold excess of ascorbic acid (AA) and 1000-fold excess of other common interferents. The fabricated biosensor exhibits good sensitivity and stability, and was successfully applied for the determination of FA in pharmaceutical samples. Copyright © 2014 Elsevier B.V. All rights reserved.

Electrochemical corrosion and bioactivity of Ti-Nb-Sn-hydroxyapatite composites fabricated by pulse current activated sintering.

PubMed

Xiaopeng, Wang; Fantao, Kong; Biqing, Han; Yuyong, Chen

2017-11-01

Ti-Nb-Sn-hydroxyapatite (HA) composites were prepared by mechanical alloying for different times (unmilled, 4, 8 and 12h), followed by pulse current activated sintering. The effects of the milling time on the electrochemical corrosion resistance and bioactivity of the sintered Ti-35Nb-2.5Sn-15HA composites were investigated. Potentiodynamic polarization test results indicated that the sintered Ti-35Nb-2.5Sn-15HA composites exhibited higher corrosion resistance with increasing milling time. The corrosion potential and current of the Ti-35Nb-2.5Sn-15HA composite sintered by 12h milled powders were - 0.261V and 0.18μA/cm 2 , respectively, and this sintered composite showed a stable and wide passivation region. The hemolysis rate of the sintered Ti-35Nb-2.5Sn-15HA composites reduced with increasing milling time and the lowest hemolytic rate of the composites was 0.87%. In addition, the in vitro cell culture results indicated that the composite sintered by 12h milled powders had good biocompatibility. These results indicate the significant potential of Ti-35Nb-2.5Sn/xHA composites for biomedical implant applications. Copyright © 2017 Elsevier Ltd. All rights reserved.

Better early osteogenesis of electroconductive hydroxyapatite-calcium titanate composites in a rabbit animal model.

PubMed

Mallik, Prafulla Kumar; Basu, Bikramjit

2014-03-01

In view of the fact that bone healing can be enhanced due to external electric field application, it is important to assess the influence of the implant conductivity on the bone regeneration in vivo. To address this issue, this study reports the in vivo biocompatibility property of multistage spark plasma sintered hydroxyapatite (HA)-80 wt % calcium titanate (CaTiO3 ) composites and monolithic HA, which have widely different conductivity property (14 orders of magnitude difference). The ability of bone regeneration was assessed by implantation in cylindrical femoral bone defects of rabbit animal model for varying time period of 1, 4, and 12 weeks. The overall assessment of the histology results suggests that the progressive healing of bone defects around HA-80 wt % CaTiO3 is associated with a better efficacy with respect to (w.r.t) early stage neobone formation, which is histomorphometrically around 140% higher than monolithic HA. Overall, this study demonstrates that the in vivo biocompatibility property of HA-80 wt % CaTiO3 with respect to local effects after 12 weeks of implantation is not compromised both qualitatively and quantitatively, and a comparison with control implant (HA) points toward the critical role of electrical conductivity on better early stage bone regeneration. Copyright © 2013 Wiley Periodicals, Inc.

Ion-substituted calcium phosphate coatings deposited by plasma-assisted techniques: A review.

PubMed

Graziani, Gabriela; Bianchi, Michele; Sassoni, Enrico; Russo, Alessandro; Marcacci, Maurilio

2017-05-01

One of the main critical aspects behind the failure or success of an implant resides in its ability to fast bond with the surrounding bone. To boost osseointegration, the ideal implant material should exhibit composition and structure similar to those of biological apatite. To this aim, the most common approach is to coat the implant surface with a coating of hydroxyapatite (HA), resembling the main component of mineralized tissues. However, bone apatite is a non-stoichiometric, multi-substituted poorly-crystalline apatite, containing significant amounts of foreign ions, with high biological relevance. Ion-substituted HAs can be deposited by so called "wet methods", which are however poorly reproducible and hardly industrially feasible; at the same time bioactive coatings realized by plasma assisted method, interesting for industrial applications, are generally made of stoichiometric (i.e. un-substituted) HA. In this work, the literature concerning plasma-assisted deposition methods used to deposit ion-substituted HA was reviewed and the last advances in this field discussed. The ions taken into exam are those present in mineralized tissues and possibly having biological relevance. Notably, literature about this topic is scarce, especially relating to in vivo animal and clinical trials; further on, available studies evaluate the performance of substituted coatings from different points of view (mechanical properties, bone growth, coating dissolution, etc.) which hinders a proper evaluation of the real efficacy of ion-doped HA in promoting bone regeneration, compared to stoichiometric HA. Moreover, results obtained for plasma sprayed coatings (which is the only method currently employed for deposition at the industrial scale) were collected and compared to those of novel plasma-assisted techniques, that are expected to overcome its limitations. Data so far available on the topic were discussed to highlight advantages, limitations and possible perspectives of these procedures. Copyright © 2016 Elsevier B.V. All rights reserved.

Comparison between PCL/hydroxyapatite (HA) and PCL/halloysite nanotube (HNT) composite scaffolds prepared by co-extrusion and gas foaming.

PubMed

Jing, Xin; Mi, Hao-Yang; Turng, Lih-Sheng

2017-03-01

In this work, three-dimensional poly(caprolactone) (PCL) tissue engineering scaffolds were prepared by co-extrusion and gas foaming. Biocompatible hydroxyapatite (HA) and halloysite nanotubes (HNT) were added to the polymer matrix to enhance the mechanical properties and bioactivity of the composite scaffolds. The effects of HA and HNT on the rheological behavior, microstructure, and mechanical properties of the composite scaffolds were systematically compared. It was found that the HNT improved viscosity more significantly than HA, and reduced the pore size of scaffolds, while the mechanical performance of PCL/HNT scaffolds was higher than PCL/HA scaffolds with the same filler content. Human mesenchymal stem cells (hMSCs) were used as the cell model to compare the biological properties of two composite scaffolds. The results demonstrated that cells could survive on all scaffolds, and showed a more flourishing living state on the composite scaffolds. The cell differentiation for 5% HA and 1% HNT scaffolds were significantly higher than other scaffolds, while the differentiation of 5% HNT scaffolds was lower than that of 1% HNT scaffolds mainly because of the reduced pore size and pore interconnectivity. Therefore, this study suggested that, with proper filler content and control of microstructure through processing, HNT could be a suitable substitute for HA for bone tissue engineering to reduce the cost and improve mechanical performance. Copyright © 2016. Published by Elsevier B.V.

In Vitro and In Vivo Evaluations of Nano-Hydroxyapatite/Polyamide 66/Glass Fibre (n-HA/PA66/GF) as a Novel Bioactive Bone Screw

PubMed Central

Su, Bao; Peng, Xiaohua; Jiang, Dianming; Wu, Jun; Qiao, Bo; Li, Weichao; Qi, Xiaotong

2013-01-01

In this study, we prepared nano-hydroxyapatite/polyamide 66/glass fibre (n-HA/PA66/GF) bioactive bone screws. The microstructure, morphology and coating of the screws were characterised, and the adhesion, proliferation and viability of MC3T3-E1 cells on n-HA/PA66/GF scaffolds were determined using scanning electron microscope, CCK-8 assays and cellular immunofluorescence analysis. The results confirmed that n-HA/PA66/GF scaffolds were biocompatible and had no negative effect on MC3T3-E1 cells in vitro. To investigate the in vivo biocompatibility, internal fixation properties and osteogenesis of the bioactive screws, both n-HA/PA66/GF screws and metallic screws were used to repair intercondylar femur fractures in dogs. General photography, CT examination, micro-CT examination, histological staining and biomechanical assays were performed at 4, 8, 12 and 24 weeks after operation. The n-HA/PA66/GF screws exhibited good biocompatibility, high mechanical strength and extensive osteogenesis in the host bone. Moreover, 24 weeks after implantation, the maximum push-out load of the bioactive screws was greater than that of the metallic screws. As shown by their good cytocompatibility, excellent biomechanical strength and fast formation and ingrowth of new bone, n-HA/PA66/GF screws are thus suitable for orthopaedic clinical applications. PMID:23861888

The Osteogenesis of Bone Marrow Stem Cells on mPEG-PCL-mPEG/Hydroxyapatite Composite Scaffold via Solid Freeform Fabrication

PubMed Central

Liao, Han-Tsung; Jiang, Cho-Pei

2014-01-01

The study described a novel bone tissue scaffold fabricated by computer-aided, air pressure-aided deposition system to control the macro- and microstructure precisely. The porcine bone marrow stem cells (PBMSCs) seeded on either mPEG-PCL-mPEG (PCL) or mPEG-PCL-mPEG/hydroxyapatite (PCL/HA) composite scaffold were cultured under osteogenic medium to test the ability of osteogenesis in vitro. The experimental outcomes indicated that both scaffolds possessed adequate pore size, porosity, and hydrophilicity for the attachment and proliferation of PBMSCs and the PBMSCs expressed upregulated genes of osteogensis and angiogenesis in similar manner on both scaffolds. The major differences between these two types of the scaffolds were the addition of HA leading to higher hardness of PCL/HA scaffold, cell proliferation, and VEGF gene expression in PCL/HA scaffold. However, the in vivo bone forming efficacy between PBMSCs seeded PCL and PCL/HA scaffold was different from the in vitro results. The outcome indicated that the PCL/HA scaffold which had bone-mimetic environment due to the addition of HA resulted in better bone regeneration and mechanical strength than those of PCL scaffold. Therefore, providing a bone-mimetic scaffold is another crucial factor for bone tissue engineering in addition to the biocompatibility, 3D architecture with high porosity, and interpored connection. PMID:24868523

Osteoinductive silk fibroin/titanium dioxide/hydroxyapatite hybrid scaffold for bone tissue engineering.

PubMed

Kim, Jung-Ho; Kim, Dong-Kyu; Lee, Ok Joo; Ju, Hyung Woo; Lee, Jung Min; Moon, Bo Mi; Park, Hyun Jung; Kim, Dong Wook; Lee, Jun Ho; Park, Chan Hum

2016-01-01

The present study demonstrated the fabrication that incorporation of titanium isopropoxide (TiO2) and hydroxyapatite (HA) nanoparticles into the silk fibroin (SF) scaffolds. In this process, we prepared TiO2 nanoparticles using sol-gel synthesis and the porous structure was developed by salt-leaching process. Homogeneous distribution of TiO2 and HA nanoparticles were confirmed by images of VP-FE-SEM and those equipped with energy dispersive X-ray spectrometer. Structural characteristics of the porous SF/TiO2/HA hybrid scaffold were also determined using FTIR analysis and X-ray diffractometer. In this study, the porous SF/TiO2/HA hybrid scaffold showed similar porosity, enhanced mechanical property, but decreased water binding abilities, compared with the porous SF scaffold. For evaluation of the osteogenic differentiation of rat bone marrow mesenchymal stem cells, alkaline phosphatase activity and osteogenic gene expression were employed. Our results revealed that the porous SF/TiO2/HA hybrid scaffold had improved osteoinductivity compared with the porous SF scaffold. These results suggest that the osteogenic property as well as mechanical property of the porous SF/TiO2/HA hybrid scaffold could be better than the porous SF scaffold. Therefore, the porous SF/TiO2/HA hybrid scaffold may be a good promising biomaterial for bone tissue engineering application. Copyright © 2015 Elsevier B.V. All rights reserved.

Antibacterial activation of hydroxyapatite (HA) with controlled porosity by different antibiotics.

PubMed

Chai, F; Hornez, J-C; Blanchemain, N; Neut, C; Descamps, M; Hildebrand, H F

2007-11-01

In order to prevent the increasing frequency of per-operative infections, bioceramics can be loaded with anti-bacterial agents, which will release with respect to their chemical characteristics. A novel hydroxyapatite (HA) was elaborated with specific internal porosities for using as a bone-bioactive antibiotic (ATB) carrier material. UV spectrophotometry and bacteria inhibition tests were performed for testing the ATB adsorption and the microbiological effectiveness after loading with different antibiotics. The impregnation time, ATB impregnating concentration, impregnation condition and other factors, which might influence the ATB loading effect, were studied by exposure to different releasing solvents and different pathogenic bacteria: Staphylococcus aureus, Staphylococcus epidermidis and Escherichia coli. It clearly showed that the facility of ATB loading on this porous HA is even possible just under simple non-vacuum impregnation conditions in a not-so-long impregnating interval. The results also showed that, for all three types of ATB (vancomycin, ciprofloxacin and gentamicin), adsorbed amount on the micro-porous HA were hugely higher than that on dense HA. The micro-porosity of test HA had also significantly prolonged the release time of antibiotics even under mimic physiological conditions. Furthermore, it also has primarily proved by a pilot test that the antibacterial efficiency of crude micro-porous HA could be further significantly improved by other methods of functionalization such as cold plasma technique.

Effect of spray angle and spray volume on deposition of a medium droplet spray with air support in ivy pot plants.

PubMed

Foqué, Dieter; Pieters, Jan G; Nuyttens, David

2014-03-01

Spray boom systems, an alternative to the predominantly-used spray guns, have the potential to considerably improve crop protection management in glasshouses. Based on earlier experiments, the further optimization of the deposits of a medium spray quality extended range flat fan nozzle type using easy adjustable spray boom settings was examined. Using mineral chelate tracers and water sensitive papers, the spray results were monitored at three plant levels, on the upper side and the underside of the leaves, and on some off-target collectors. In addition, the deposition datasets of all tree experiments were compared. The data showed that the most efficient spray distribution with the medium spray quality flat fan nozzles was found with a 30° forward angled spray combined with air support and an application rate of 1000 L ha(-1) . This technique resulted in a more uniform deposition in the dense canopy and increased spray deposition on the lower side of the leaves compared with the a standard spray boom application. Applying 1000 L ha(-1) in two subsequent runs instead of one did not seem to show any added value. Spray deposition can be improved hugely simply by changing some spray boom settings like nozzle type, angling the spray, using air support and adjusting the spray volume to the crop. © 2013 Society of Chemical Industry.

The role of amino acids in hydroxyapatite mineralization

PubMed Central

2016-01-01

Polar and charged amino acids (AAs) are heavily expressed in non-collagenous proteins (NCPs), and are involved in hydroxyapatite (HA) mineralization in bone. Here, we review what is known on the effect of single AAs on HA precipitation. Negatively charged AAs, such as aspartic acid, glutamic acid (Glu) and phosphoserine are largely expressed in NCPs and play a critical role in controlling HA nucleation and growth. Positively charged ones such as arginine (Arg) or lysine (Lys) are heavily involved in HA nucleation within extracellular matrix proteins such as collagen. Glu, Arg and Lys intake can also increase bone mineral density by stimulating growth hormone production. In vitro studies suggest that the role of AAs in controlling HA precipitation is affected by their mobility. While dissolved AAs are able to inhibit HA precipitation and growth by chelating Ca2+ and PO43− ions or binding to nuclei of calcium phosphate and preventing their further growth, AAs bound to surfaces can promote HA precipitation by attracting Ca2+ and PO43− ions and increasing the local supersaturation. Overall, the effect of AAs on HA precipitation is worth being investigated more, especially under conditions closer to the physiological ones, where the presence of other factors such as collagen, mineralization inhibitors, and cells heavily influences HA precipitation. A deeper understanding of the role of AAs in HA mineralization will increase our fundamental knowledge related to bone formation, and could lead to new therapies to improve bone regeneration in damaged tissues or cure pathological diseases caused by excessive mineralization in tissues such as cartilage, blood vessels and cardiac valves. PMID:27707904

Surface characteristics of a novel hydroxyapatite-coated dental implant

PubMed Central

Jung, Ui-Won; Hwang, Ji-Wan; Choi, Da-Yae; Hu, Kyung-Seok; Kwon, Mi-Kyung; Choi, Seong-Ho

2012-01-01

Purpose This study evaluated the surface characteristics and bond strength produced using a novel technique for coating hydroxyapatite (HA) onto titanium implants. Methods HA was coated on the titanium implant surface using a super-high-speed (SHS) blasting method with highly purified HA. The coating was performed at a low temperature, unlike conventional HA coating methods. Coating thickness was measured. The novel HA-coated disc was fabricated. X-ray diffraction analysis was performed directly on the disc to evaluate crystallinity. Four novel HA-coated discs and four resorbable blast medium (RBM) discs were prepared. Their surface roughnesses and areas were measured. Five puretitanium, RBM-treated, and novel HA-coated discs were prepared. Contact angle was measured. Two-way analysis of variance and the post-hoc Scheffe's test were used to analyze differences between the groups, with those with a probability of P<0.05 considered to be statistically significant. To evaluate exfoliation of the coating layer, 7 sites on the mandibles from 7 mongrel dogs were used. Other sites were used for another research project. In total, seven novel HA-coated implants were placed 2 months after extraction of premolars according to the manufacturer's instructions. The dogs were sacrificed 8 weeks after implant surgery. Implants were removed using a ratchet driver. The surface of the retrieved implants was evaluated microscopically. Results A uniform HA coating layer was formed on the titanium implants with no deformation of the RBM titanium surface microtexture when an SHS blasting method was used. Conclusions These HA-coated implants exhibited increased roughness, crystallinity, and wettability when compared with RBM implants. PMID:22586524

Hydroxyapatite implants with designed internal architecture.

PubMed

Chu, T M; Halloran, J W; Hollister, S J; Feinberg, S E

2001-06-01

Porous hydroxyapatite (HA) has been used as a bone graft material in the clinics for decades. Traditionally, the pores in these HAs are either obtained from the coralline exoskeletal patterns or from the embedded organic particles in the starting HA powder. Both processes offer very limited control on the pore structure. A new method for manufacturing porous HA with designed pore channels has been developed. This method is essentially a lost-mold technique with negative molds made with Stereolithography and a highly loaded curable HA suspension as the ceramic carrier. Implants with designed channels and connection patterns were first generated from a Computer-Aided-Design (CAD) software and Computer Tomography (CT) data. The negative images of the designs were used to build the molds on a stereolithography apparatus with epoxy resins. A 40 vol% HA suspension in propoxylated neopentyl glycol diacrylate (PNPGDA) and iso-bornyl acrylate (IBA) was formulated. HA suspension was cast into the epoxy molds and cured into solid at 85 degrees C. The molds and acrylate binders were removed by pyrolysis, followed by HA green body sintering. With this method, implants with six different channel designs were built successfully and the designed channels were reproduced in the sintered HA implants. The channels created in the sintered HA implants were between 366 microm and 968 microm in diameter with standard deviations of 50 microm or less. The porosity created by the channels were between 26% and 52%. The results show that HA implants with designed connection pattern and well controlled channel size can be built with the technique developed in this study. Copyright 2001 Kluwer Academic Publishers

Preparation of poly(lactic acid)/sintered hydroxyapatite composite biomaterial by supercritical CO2.

PubMed

Zhang, Yumin; Wang, Jianru; Ma, Yanmiao; Han, Bo; Niu, Xiaojun; Liu, Jianchun; Gao, Lan; Wang, Jue; Zhai, Xiaoyan; Chu, Kaibo; Yang, Liwang

2018-01-01

Based on a kind of sintered hydroxyapatite (HA) with a good cytocompatibility, a series of polylactic acid (PLA) and PLA/HA with the various PLA:HA weight ratio (5:5, 4:6, 3:7, 2:8, 1:9) were fabricated by supercritical CO2. The physical and chemical properties were evaluated by pH, degradation, water absorption, porosity, density, mechanical property, and cytotoxicity respectively. With the increase of HA content, the pH value and porosity increased gradually, while weight loss rate and the density showed a gradual downward trend. Existence of HA can drastically improve the hydroscopicity of PLA scaffolds. The compression strength values slightly increased (p>0.05) from 39.96 MPa of PLA to 45.00 MPa of PLA/HA with the ratio of 7:3, subsequently, the values decreased (p<0.05) from 43.29 MPa (8:2) to 19.00 MPa (9:1). While the modulus of elasticity decreased (p<0.05) from 5.89 to 1.84 GPa with increasing HA content. The PLA/HA (8:2) promoted cell proliferation more significantly than any of other groups (p<0.05). Based on the results, the overall properties of porous scaffolds are the optimal when the weight ratio of PLA/HA is 8:2. Its pH, porosity, density, compression strength, and elasticity modulus are 7.39, 83.0%, 0.60g/cm-3, 34.1 MPa and 2.63 GPa, respectively. SEM observation presented a homogeneous distribution of HA in PLA matrix and a foam-like structure comprising interconnected pores.

Effect of Hydroxyapatite on the Mechanical Properties and Corrosion Behavior of Mg-Zn-Y Alloy

PubMed Central

Chiu, Chun; Lu, Chih-Te; Chen, Shih-Hsun; Ou, Keng-Liang

2017-01-01

Mg-Zn-Y alloys with a long period stacking ordered (LPSO) phase are potential candidates for biodegradable implants; however, an unfavorable degradation rate has limited their applications. Hydroxyapatite (HA) has been shown to enhance the corrosion resistance of Mg alloys. In this study, Mg97Zn1Y2-0.5 wt% HA composite was synthesized and solution treated at 500 °C for 10 h. The corrosion behavior of the composite was studied by electrochemical and immersion tests, while the mechanical properties were investigated by a tensile test. Addition of HA particles improves the corrosion resistance of Mg97Zn1Y2 alloy without sacrificing tensile strength. The improved corrosion resistance is due to the formation of a compact Ca-P surface layer and a decrease of the volume fraction of the LPSO phase, both resulting from the addition of HA. After solution-treatment, the corrosion resistance of the composite decreases. This is due to the formation of a more extended LPSO phase, which weakens its role as a corrosion barrier in protecting the Mg matrix. PMID:28773216

Hydroxyapatite coating on PEEK implants: biomechanical and histological study in a rabbit model

PubMed Central

Durham, John W.; Montelongo, Sergio A.; Ong, Joo L.; Guda, Teja; Allen, Matthew J.; Rabiei, Afsaneh

2016-01-01

A bioactive two-layer coating consisting of hydroxyapatite (HA) and yttria-stabilized zirconia (YSZ) was investigated on cylindrical polyether ether ketone (PEEK) implants using ion beam assisted deposition (IBAD). Post-deposition heat treatments via variable frequency microwave annealing with and without subsequent autoclaving were used to crystallize the as-deposited amorphous HA layer. Microstructural analysis, performed by TEM and EDS, showed that these methods were capable of crystallizing HA coating on PEEK. The in vivo response to cylindrical PEEK samples with and without coating was studied by implanting uncoated PEEK and coated PEEK implants in the lateral femoral condyle of 18 rabbits. Animals were studied in two groups 9 for observation at 6 or 18 weeks post surgery. MicroCT analysis, histology, and mechanical pull-out tests were performed to determine the effect of the coating on osseointegration. The heat-treated HA/YSZ coatings showed improved implant fixation as well as higher bone regeneration and bone-implant contact area compared to uncoated PEEK. The study offers a novel method to coat PEEK implants with improved osseointegration. PMID:27524073

Structural evolution and growth mechanisms of RF-magnetron sputter-deposited hydroxyapatite thin films on the basis of unified principles

NASA Astrophysics Data System (ADS)

Ivanova, Anna A.; Surmeneva, Maria A.; Surmenev, Roman A.; Depla, Diederik

2017-12-01

The structural features of RF-magnetron sputter-deposited hydroxyapatite (HA) coatings are investigated in order to reveal the effect of the working gas composition and the sample position of the substrate relative to the target erosion zone. The film properties were observed to change as a result of bombardment with energetic ions. XRD analysis of the coated substrates indicates that with the increase of the ion-to-atom ratio, the fiber texture changes from a mixed (11 2 bar 2) + (0002) over (0002) orientation, finally reaching a (30 3 bar 0) out-of-plane orientation at high ion-to-atom ratios. TEM reveals that the microstructure of the HA coating consists of columnar grains and differs with the coating texture. The contribution of Ji/Ja to the development of microstructure and texture of the HA coating is schematically represented and discussed. The obtained results may contribute substantially to the progress of research into the development of HA coatings with tailored properties, and these coatings may be applied on the surfaces of metal implants used in bone surgery.

Electrophoretic-deposited novel ternary silk fibroin/graphene oxide/hydroxyapatite nanocomposite coatings on titanium substrate for orthopedic applications

NASA Astrophysics Data System (ADS)

Li, Ming; Xiong, Pan; Mo, Maosong; Cheng, Yan; Zheng, Yufeng

2016-09-01

The combination of graphene oxide (GO) with robust mechanical property, silk fibroin (SF) with fascinating biological effects and hydroxyapatite (HA) with superior osteogenic activity is a competitive approach to make novel coatings for orthopedic applications. Herein, the feasibility of depositing ternary SF/GO/HA nanocomposite coatings on Ti substrate was firstly verified by exploiting electrophoretic nanotechnology, with SF being used as both a charging additive and a dispersion agent. The surface morphology, microstructure and composition, in vitro hemocompatibility and in vitro cytocompatibility of the resulting coatings were investigated by SEM, Raman, FTIR spectra and biocompatibility tests. Results demonstrated that GO, HA and SF could be co-deposited with a uniform, smooth thin-film morphology. The hemolysis rate analysis and the platelet adhesion test indicated good blood compatibility of the coatings. The human osteosarcoma MG63 cells displayed well adhesion and proliferation behaviors on the prepared coatings, with enhanced ALP activities. The present study suggested that SF/GO/HA nanocomposite coatings could be a promising candidate for the surface functionalization of biomaterials, especially as orthopedic implant coating.

Effect of Heat Treatment Temperature on Chemical Compositions of Extracted Hydroxyapatite from Bovine Bone Ash

NASA Astrophysics Data System (ADS)

Younesi, M.; Javadpour, S.; Bahrololoom, M. E.

2011-11-01

This article presents the effect of heat treating temperature on chemical composition of hydroxyapatite (HA) that was produced by burning bovine bone, and then heat treating the obtained bone ash at different temperatures in range of 600-1100 °C in air. Bone ash and the resulting white powder from heat treating were characterized by Fourier transformed infrared spectroscopy (FT-IR) and x-ray diffractometry (XRD). The FT-IR spectra confirmed that heat treating of bone ash at temperature of 800 °C removed the total of organic substances. x-ray diffraction analysis showed that the white powder was HA and HA was the only crystalline phase indicated in heat treating product. x-ray fluorescence analyses revealed that calcium and phosphorous were the main elements and magnesium and sodium were minor impurities of produced powder at 800 °C. The results of the energy dispersive x-ray analysis showed that Ca/P ratio in produced HA varies in range of 1.46-2.01. The resulting material was found to be thermally stable up to 1100 °C.

Porous hydroxyapatite/gelatine scaffolds with ice-designed channel-like porosity for biomedical applications.

PubMed

Landi, Elena; Valentini, Federica; Tampieri, Anna

2008-11-01

A cryogenic process, including freeze-casting and drying has been performed to obtain hydroxyapatite (HA) scaffolds (approx. diameter 10 mm, height 20 mm) with completely lamellar morphology due to preferentially aligned channel-like pores. Changing the process parameters that influence the cold transmission efficiency from the bottom to the top of the poured HA slurry, lamellar ice crystals with different thickness grew throughout the samples. After sintering, scaffolds with porosity features nearly resembling the ice ones were obtained. The interconnection of pores and the ability of the scaffolds to be rapidly penetrated by synthetic body fluid has been proven. Biohybrid HA/gel composites were prepared, infiltrating HA lamellar scaffolds (45-55 vol.% of porosity) with a 10wt.% solution of gelatine. Colouring genipine was used to cross-link gelatine and clearly show the distribution of the protein in the composite. The compressive mechanical properties of lamellar scaffolds improved with the addition of gelatine: the strength increased up to 5-6 times, while the elastic modulus and strain approximately doubled. The effectiveness of the cross-linkage has been preliminarily verified following scaffold degradation in synthetic body fluid.

First principles study of biomineral hydroxyapatite

NASA Astrophysics Data System (ADS)

Slepko, Alexander

2010-03-01

Hydroxyapatite (HA) [Ca10(PO4)6(OH)2] is one of the most abundant materials in mammal bone. It crystallizes within the spaces between the tropocollagen chains and strengthens the bone tissue. The mineral content of human bone increases with age reaching a maximum value from which it starts to decrease leading to diseases such as osteomalacia. Therefore, an emergent application of this study is bone repair and the production of synthetic bone. Despite its importance, little is known about the growth of HA crystallites in bones. Nor is it well understood how the HA attaches to protein chains and interacts with the surrounding aqueous solution. Using density functional theory (DFT) we calculate the theoretical ground state structure, electronic and vibration properties of hexagonal HA. We find several low energy structures and analyze the energy barriers for spontaneous phase transitions. We calculate the phonon density of states and study the surface energetics for different orientations. We identify the surfaces with highest reactivity using the frontier orbital approach and analyze interactions between these surfaces and water molecules/amino acids.

Hydroxyapatite coating on PEEK implants: Biomechanical and histological study in a rabbit model.

PubMed

Durham, John W; Montelongo, Sergio A; Ong, Joo L; Guda, Teja; Allen, Matthew J; Rabiei, Afsaneh

2016-11-01

A bioactive two-layer coating consisting of hydroxyapatite (HA) and yttria-stabilized zirconia (YSZ) was investigated on cylindrical polyetheretherketone (PEEK) implants using ion beam assisted deposition (IBAD). Post-deposition heat treatments via variable frequency microwave annealing with and without subsequent autoclaving were used to crystallize the as-deposited amorphous HA layer. Microstructural analysis, performed by TEM and EDS, showed that these methods were capable of crystallizing HA coating on PEEK. The in vivo response to cylindrical PEEK samples with and without coating was studied by implanting uncoated PEEK and coated PEEK implants in the lateral femoral condyle of 18 rabbits. Animals were studied in two groups of 9 for observation at 6 or 18weeks post surgery. Micro-CT analysis, histology, and mechanical pull-out tests were performed to determine the effect of the coating on osseointegration. The heat-treated HA/YSZ coatings showed improved implant fixation as well as higher bone regeneration and bone-implant contact area compared to uncoated PEEK. The study offers a novel method to coat PEEK implants with improved osseointegration. Copyright © 2016 Elsevier B.V. All rights reserved.

Development and Characterization of Biphasic Hydroxyapatite/β-TCP Cements.

PubMed

Gallinetti, Sara; Canal, Cristina; Ginebra, Maria-Pau; Ferreira, J

2014-04-01

Biphasic calcium phosphate bioceramics composed of hydroxyapatite (HA) and β-tricalcium phosphate (β-TCP) have relevant properties as synthetic bone grafts, such as tunable resorption, bioactivity, and intrinsic osteoinduction. However, they have some limitations associated to their condition of high-temperature ceramics. In this work self-setting Biphasic Calcium Phosphate Cements (BCPCs) with different HA/β-TCP ratios were obtained from self-setting α-TCP/β-TCP pastes. The strategy used allowed synthesizing BCPCs with modulated composition, compressive strength, and specific surface area. Due to its higher solubility, α-TCP was fully hydrolyzed to a calcium-deficient HA (CDHA), whereas β-TCP remained unreacted and completely embedded in the CDHA matrix. Increasing amounts of the non-reacting β-TCP phase resulted in a linear decrease of the compressive strength, in association to the decreasing amount of precipitated HA crystals, which are responsible for the mechanical consolidation of apatitic cements. Ca 2+ release and degradation in acidic medium was similar in all the BCPCs within the timeframe studied, although differences might be expected in longer term studies once β-TCP, the more soluble phase was exposed to the surrounding media.

EDTA assisted synthesis of hydroxyapatite nanoparticles for electrochemical sensing of uric acid.

PubMed

Kanchana, P; Sekar, C

2014-09-01

Hydroxyapatite nanoparticles have been synthesized using EDTA as organic modifier by a simple microwave irradiation method and its application for the selective determination of uric acid (UA) has been demonstrated. Electrochemical behavior of uric acid at HA nanoparticle modified glassy carbon electrode (E-HA/GCE) has been investigated by electrochemical impedance spectroscopy (EIS), cyclic voltammetry (CV), linear sweep voltammetry (LSV) and amperometry. The E-HA modified electrode exhibits efficient electrochemical activity towards uric acid sensing without requiring enzyme or electron mediator. Amperometry studies revealed that the fabricated electrode has excellent sensitivity for uric acid with the lowest detection limit of 142 nM over a wide concentration range from 1 × 10(-7) to 3 × 10(-5)M. Moreover, the studied E-HA modified GC electrode exhibits a good reproducibility and long-term stability and an admirable selectivity towards the determination of UA even in the presence of potential interferents. The analytical performance of this sensor was evaluated for the detection of uric acid in human urine and blood serum samples. Copyright © 2014. Published by Elsevier B.V.

Fabrication, ultra-structure characterization and in vitro studies of RF magnetron sputter deposited nano-hydroxyapatite thin films for biomedical applications

NASA Astrophysics Data System (ADS)

Surmeneva, Maria A.; Surmenev, Roman A.; Nikonova, Yulia A.; Selezneva, Irina I.; Ivanova, Anna A.; Putlyaev, Valery I.; Prymak, Oleg; Epple, Matthias

2014-10-01

A series of nanostructured low-crystalline hydroxyapatite (HA) coatings averaging 170, 250, and 440 nm in thickness were deposited onto previously etched titanium substrates through radio-frequency (RF) magnetron sputtering. The HA coatings were analyzed using infrared spectroscopy (FTIR), X-ray diffraction (XRD), and scanning and transmission electron microscopy (SEM and TEM). Cross sections of the thin specimens were prepared by FIB to study the microstructure of the coatings by TEM. The deposition process formed nano-scale grains, generating an amorphous layer at the substrate/coating interface and inducing the growth of a columnar grain structure perpendicular to the substrate surface. A microstructural analysis of the film confirmed that the grain size and crystallinity increased when increasing the deposition time. The nanostructured HA coatings were not cytotoxic, as proven by in vitro assays using primary dental pulp stem cells and mouse fibroblast NCTC clone L929 cells. Low-crystallinity HA coatings with different thicknesses stimulated cells to attach, proliferate and form mineralized nodules on the surface better than uncoated titanium substrates.

Study on clinical application of nano-hydroxyapatite bone in bone defect repair.

PubMed

Zhu, Weimin; Wang, Daping; Xiong, Jianyi; Liu, Jianquan; You, Wei; Huang, Jianghong; Duan, Li; Chen, Jielin; Zeng, Yanjun

2015-01-01

To study the clinical effect of bone defect treated with nano-hydroxyapatite(Nano-HA) artificial bone. From September 2009 to June 2012, 27 cases of bone defect were analyzed retrospectively. The position of bone defect included humerus, radius, ulna, femur, tibia and calcaneus. The range of bone defect was from 0.3 × 1.0 cm to 3 × 6.5 cm. Among them, there were 22 cases with fractures and 5 cases with tumors. All patients were treated with Nano-HA artificial bone. The ability of bone defect repair was evaluated by X-ray exams performed preoperatively and postoperatively. HSS scores were adopted for final evaluation at the latest follow-up. The patients were followed up from 11 to 26 months (average of 18.5 months). No general side effects occurred. X-ray photo showed an integrity interface between Nano-HA and bone. Primary healing was obtained in all cases without any complication. The Nano-HA artificial bone had a good biocompatibility and could be an ideal artificial bone in the reconstruction of bone defect.

In situ synthesis of bilayered gradient poly(vinyl alcohol)/hydroxyapatite composite hydrogel by directional freezing-thawing and electrophoresis method.

PubMed

Su, Cui; Su, Yunlan; Li, Zhiyong; Haq, Muhammad Abdul; Zhou, Yong; Wang, Dujin

2017-08-01

Bilayered poly(vinyl alcohol) (PVA)/hydroxyapatite (HA) composite hydrogels with anisotropic and gradient mechanical properties were prepared by the combination of directional freezing-thawing (DFT) and electrophoresis method. Firstly, PVA hydrogels with aligned channel structure were prepared by the DFT method. Then, HA nanoparticles were in situ synthesized within the PVA hydrogels via electrophoresis. By controlling the time of the electrophoresis process, a bilayered gradient hydrogel containing HA particles in only half of the gel region was obtained. The PVA/HA composite hydrogel exhibited gradient mechanical strength depending on the distance to the cathode. The gradient initial tensile modulus ranging from 0.18MPa to 0.27MPa and the gradient initial compressive modulus from 0.33MPa to 0.51MPa were achieved. The binding strength of the two regions was relatively high and no apparent internal stress or defect was observed at the boundary. The two regions of the bilayered hydrogel also showed different osteoblast cell adhesion properties. Copyright © 2017 Elsevier B.V. All rights reserved.

The importance of amino acid interactions in the crystallization of hydroxyapatite

PubMed Central

Jahromi, M. Tavafoghi; Yao, G.; Cerruti, M.

2013-01-01

Non-collagenous proteins (NCPs) inhibit hydroxyapatite (HA; Ca5(PO4)3OH) formation in living organisms by binding to nascent nuclei of HA and preventing their further growth. Polar and charged amino acids (AAs) are highly expressed in NCPs, and the negatively charged ones, such as glutamic acid (Glu) and phosphoserine (P-Ser) seem to be mainly responsible for the inhibitory effect of NCPs. Despite the recognized importance of these AAs on the behaviour of NCPs, their specific effect on HA crystallization is still unclear, and controversial results have been reported concerning the efficacy of HA inhibition of positively versus negatively charged AAs. We focused on a positively charged (arginine, Arg) and a negatively charged (Glu) AA, and their combination in the same solution. We studied their inhibitory effect on HA nucleation and growth at physiological temperature and pH and we determined the mechanism by which they can affect HA crystallization. Our results showed a strong inhibitory effect of Arg on HA nucleation; however, Glu was more effective in inhibiting HA crystal growth during the growth stage. The combination of Glu and Arg was less effective in controlling HA nucleation, but it inhibited HA crystal growth. We attributed these differences to the stability of complexes formed between AAs and calcium and phosphate ions at the nucleation stage, and in bonding strength of AAs to HA crystal faces during the growth stage. The AAs also influenced the morphology of synthesized HA. Presence of either Arg or Glu resulted in the formation of spherulites consisting of preferentially oriented nanoplatelets orientation. This was attributed to kinetic factors favoring growth front nucleation (GFN) mechanism. PMID:23269851

Ridge Preservation After Maxillary Third Molar Extraction Using 30% Porosity PLGA/HA/β-TCP Scaffolds With and Without Simvastatin: A Pilot Randomized Controlled Clinical Trial.

PubMed

Noronha Oliveira, Miguel; Rau, Levy Hermes; Marodin, Aline; Corrêa, Márcio; Corrêa, Letícia Ruhland; Aragones, Aguedo; Magini, Ricardo de Souza

2017-12-01

To evaluate clinically and radiographically, in humans, the healing of maxillary third molars postextraction sockets after application of different ridge preservation techniques 3 months after tooth extraction. Twenty-six sockets (13 patients) were randomly assigned to 4 treatment modalities: deproteinized bovine bone mineral with 10% collagen (DBBM-C), poly(D,L-lactide-co-glycolide) with hydroxyapatite/β-TCP scaffold (PLGA/HA), PLGA/HA/β-TCP with 2.0% simvastatin scaffold (PLGA/HA/S), and spontaneous healing (control). Clinical complications were assessed, and cone-beam computed tomographies were taken in 5 patients 3 months after surgeries. For statistical purposes, the Fisher exact test was used (P < 0.05). After 3 months, 6 of 9 grafts from the PLGA/HA group were lost (P < 0.05). PLGA/HA/S' loss was only 2 of 8 (P > 0.05), but no loss was observed in the DBBM-C group. Pain was present in 3 of 8 sites that lost the graft (37.5%) (P > 0.05) and infection in 1 of 8 (12.5%) (P > 0.05), with these only occurring in the PLGA/HA group. Poly (D, L-lactide-co-glycolide) with hydroxyapatite/β-TCP (PLGA/HA/β-TCP) scaffolds, with and without simvastatin, failed to obtain the initial expected results and presented more complications. Scaffolds with simvastatin showed to be superior, with less clinical complications than scaffolds without simvastatin.

Hydroxyapatite coating affects the Wnt signaling pathway during peri-implant healing in vivo.

PubMed

Thorfve, A; Lindahl, C; Xia, W; Igawa, K; Lindahl, A; Thomsen, P; Palmquist, A; Tengvall, P

2014-03-01

Owing to its bio- and osteoconductivity, hydroxyapatite (HA) is a widely used implant material, but its osteogenic properties are only partly evaluated in vitro and in vivo. The present study focused on bone healing adjacent to HA-coated titanium (Ti) implants, with or without incorporated lithium ions (Li(+)). Special attention was given to the Wnt signaling pathway. The implants were inserted into rat tibia for 7 or 28 days and analyzed ex vivo, mainly by histomorphometry and quantitative real-time polymerase chain reaction (qPCR). HA-coated implants showed, irrespective of Li(+) content, bone-implant contact (BIC) and removal torque values significantly higher than those of reference Ti. Further, the expression of OCN, CTSK, COL1A1, LRP5/6 and WISP1 was significantly higher in implant-adherent cells of HA-coated implants, with or without Li(+). Significantly higher β-catenin expression and significantly lower COL2A1 expression were observed in peri-implant bone cells from HA with 14 ng cm(-2) released Li(+). Interestingly, Ti implants showed a significantly larger bone area (BA) in the threads than HA with 39 ng cm(-2) released Li(+), but had a lower BIC than any HA-coated implant. This study shows that HA, with or without Li(+), is a strong activator of the Wnt signaling pathway, and may to some degree explain its high bone induction capacity. Copyright © 2013 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Hydroxyapatite-coated magnesium implants with improved in vitro and in vivo biocorrosion, biocompatibility, and bone response.

PubMed

Kim, Sae-Mi; Jo, Ji-Hoon; Lee, Sung-Mi; Kang, Min-Ho; Kim, Hyoun-Ee; Estrin, Yuri; Lee, Jong-Ho; Lee, Jung-Woo; Koh, Young-Hag

2014-02-01

Magnesium and its alloys are candidate materials for biodegradable implants; however, excessively rapid corrosion behavior restricts their practical uses in biological systems. For such applications, surface modification is essential, and the use of anticorrosion coatings is considered as a promising avenue. In this study, we coated Mg with hydroxyapatite (HA) in an aqueous solution containing calcium and phosphate sources to improve its in vitro and in vivo biocorrosion resistance, biocompatibility and bone response. A layer of needle-shaped HA crystals was created uniformly on the Mg substrate even when the Mg sample had a complex shape of a screw. In addition, a dense HA-stratum between this layer and the Mg substrate was formed. This HA-coating layer remarkably reduced the corrosion rate of the Mg tested in a simulated body fluid. Moreover, the biological response, including cell attachment, proliferation and differentiation, of the HA-coated samples was enhanced considerably compared to samples without a coating layer. The preliminary in vivo experiments also showed that the biocorrosion of the Mg implant was significantly retarded by HA coating, which resulted in good mechanical stability. In addition, in the case of the HA-coated implants, biodegradation was mitigated, particularly over the first 6 weeks of implantation. This considerably promoted bone growth at the interface between the implant and bone. These results confirmed that HA-coated Mg is a promising material for biomedical implant applications. © 2013 Wiley Periodicals, Inc.

Biocompatibility assessment of graphene oxide-hydroxyapatite coating applied on TiO2 nanotubes by ultrasound-assisted pulse electrodeposition.

PubMed

Fathyunes, Leila; Khalil-Allafi, Jafar; Sheykholeslami, Seyed Omid Reza; Moosavifar, Maryam

2018-06-01

In this study, the ultrasound-assisted pulse electrodeposition was introduced to fabricate the graphene oxide (GO)-hydroxyapatite (HA) coating on TiO 2 nanotubes. The results of the X-ray diffraction (XRD), Fourier Transform Infrared spectroscope (FTIR), Transmission Electron Microscope (TEM) and micro-Raman spectroscopy showed the successful synthesis of GO. The Scanning Electron Microscope (SEM) images revealed that in the presence of ultrasonic waves and GO sheets a more compact HA-based coating with refined microstructure could be formed on the pretreated titanium. The results of micro-Raman analysis confirmed the successful incorporation of the reinforcement filler of GO into the coating electrodeposited by the ultrasound-assisted method. The FTIR analysis showed that the GO-HA coating was consisted predominantly of the B-type carbonated HA (CHA) phase. The pretreatment of the substrate and incorporation of the GO sheets into the HA coating had a significant effect on improving the bonding strength at the coating-substrate interface. Moreover, the results of the fibroblast cell culture and 3‑(4,5‑dimethylthiazolyl‑2)‑2, 5‑diphenyltetrazolium bromide (MTT) assay after 2 days demonstrated a higher percentage of cell activity for the GO-HA coated sample. Finally, the 7-day exposure to simulated body fluid (SBF) showed a faster rate of apatite precipitation on the GO-HA coating, as compared to the HA coating and pretreated titanium. Copyright © 2018 Elsevier B.V. All rights reserved.

The efficacy of porous hydroxyapatite bone chip as an extender of local bone graft in posterior lumbar interbody fusion.

PubMed

Kim, Hyoungmin; Lee, Choon-Ki; Yeom, Jin-Sup; Lee, Jae-Hyup; Lee, Ki-Ho; Chang, Bong-Soon

2012-07-01

To evaluate whether a synthetic bone chip made of porous hydroxyapatite can effectively extend local decompressed bone graft in instrumented posterior lumbar interbody fusion (PLIF). 130 patients, 165 segments, who had undergone PLIF with cages and instrumentation for single or double level due to degenerative conditions, were investigated retrospectively by independent blinded observer. According to the material of graft, patients were divided into three groups. HA group (19 patients, 25 segments): with hydroxyapatite bone chip in addition to autologous local decompressed bone, IBG group (25 patients, 28 segments): with autologous iliac crest bone graft in addition to local decompressed bone and LB group (86 patients, 112 segments): with local decompressed bone only. Radiologic and clinical outcome were compared among groups and postoperative complications, transfusion, time and cost of operation and duration of hospitalization were also investigated. Radiologic fusion rate and clinical outcome were not different. Economic cost, transfusion and hospital stay were also similar. But operation time was significantly longer in IBG group than in other groups. There were no lasting complications associated with HA and LB group with contrast to five cases with persisting donor site pain in IBG group. Porous hydroxyapatite bone chip is a useful bone graft extender in PLIF when used in conjunction with local decompressed bone.

Synthesis, bioactivity and zeta potential investigations of chlorine and fluorine substituted hydroxyapatite.

PubMed

Fahami, Abbas; Beall, Gary W; Betancourt, Tania

2016-02-01

Chlorine and fluorine substituted hydroxyapatites (HA-Cl-F) with different degrees of ion replacement were successfully prepared by the one step mechanochemical activation method. X-ray diffraction (XRD) and FT-IR spectra indicated that substitution of these anions in milled powders resulted in the formation of pure hydroxyapatite phase except for the small observed change in the lattice parameters and unit cell volumes of the resultant hydroxyapatite. Microscopic observations showed that the milled product had a cluster-like structure made up of polygonal and spherical particles with an average particle size of approximately ranged from 20±5 to 70±5nm. The zeta potential of milled samples was performed at three different pH (5, 7.4, and 9). The obtained zeta potential values were negative for all three pH values. Negative zeta potential was described to favor osseointegration, apatite nucleation, and bone regeneration. The bioactivity of samples was investigated on sintered pellets soaked in simulated body fluid (SBF) solution and apatite crystals formed on the surface of the pellets after being incubated for 14days. Zeta potential analysis and bioactivity experiment suggested that HA-Cl-F will lead to the formation of new apatite particles and therefore be a potential implant material. Copyright © 2015 Elsevier B.V. All rights reserved.

Fractionated-combustion analysis of carbonate-containing phases in composite materials of the hydroxyapatite-calcium carbonate system

NASA Astrophysics Data System (ADS)

Goldberg, M. A.; Shibaeva, T. V.; Smirnov, V. V.; Kutsev, S. V.; Barinov, S. M.; Grigorovich, K. V.

2012-12-01

Materials in the hydroxyapatite (HA)-calcium carbonate (CC) system were synthesized by a precipitation method from aqueous solutions. According to the data of X-ray phase analysis and IR spectroscopy, the powders consisted of CC and AB-type carbonate-substituted HA (CHA). In order to determine the content of carbonate-containing phases in materials, the temperature-temporal mode of fractionated-combustion analysis of carbon was developed. The quantitative phase ratios and the degree of substitution of carbonate groups in CHA were determined. It was shown that the degree of substitution of carbonate groups in CHA increased from 2.47 to 5.31 wt % as the CC content increased from 13.50 to 88.33 wt %.

Fracture modes under uniaxial compression in hydroxyapatite scaffolds fabricated by robocasting.

PubMed

Miranda, Pedro; Pajares, Antonia; Saiz, Eduardo; Tomsia, Antoni P; Guiberteau, Fernando

2007-12-01

The fracture modes of hydroxyapatite (HA) scaffolds fabricated by direct-write assembly (robocasting) are analyzed in this work. Concentrated HA inks with suitable viscoelastic properties were developed to enable the fabrication of prototype structures consisting of a 3-D square mesh of interpenetrating rods. The fracture behavior of these model scaffolds under compressive stresses is determined from in situ uniaxial tests performed in two different directions: perpendicular to the rods and along one of the rod directions. The results are analyzed in terms of the stress field calculated by finite element modeling (FEM). This analysis provides valuable insight into the mechanical behavior of scaffolds for bone tissue engineering applications fabricated by robocasting. Copyright 2007 Wiley Periodicals, Inc.