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Sample records for hydroxyapatite ha microspheres

  1. Modified composite microspheres of hydroxyapatite and poly(lactide-co-glycolide) as an injectable scaffold

    NASA Astrophysics Data System (ADS)

    Hu, Xixue; Shen, Hong; Yang, Fei; Liang, Xinjie; Wang, Shenguo; Wu, Decheng

    2014-02-01

    The compound of hydroxyapatite-poly(lactide-co-glycolide) (HA-PLGA) was prepared by ionic bond between HA and PLGA. HA-PLGA was more stable than the simple physical blend of hydroxyapatite and poly(lactide-co-glycolide) (HA/PLGA). The surface of HA-PLGA microsphere fabricated by an emulsion-solvent evaporation method was rougher than that of HA/PLGA microspheres. Moreover, surface HA content of HA-PLGA microspheres was more than that of HA/PLGA microspheres. In vitro mouse OCT-1 osteoblast-like cell culture results showed that the HA-PLGA microspheres clearly promoted osteoblast attachment, proliferation and alkaline phosphatase activity. It was considered that surface rich HA component and rough surface of HA-PLGA microsphere enhanced cell growth and differentiation. The good cell affinity of the HA-PLGA microspheres indicated that they could be used as an injectable scaffold for bone tissue engineering.

  2. 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. PMID:26478351

  3. Hollow and porous hydroxyapatite microspheres prepared with an O/W emulsion by spray freezing method.

    PubMed

    Xiao, Qiyao; Zhou, Kechao; Chen, Chao; Jiang, Mingxiang; Zhang, Yan; Luo, Hang; Zhang, Dou

    2016-12-01

    Microspheres with hollow and/or porous structures have been widely used in various applications. A new method of spraying and freezing emulsions was developed to prepare hollow HA (hydroxyapatite) microspheres with interconnected pores by using PVA (polyvinyl alcohol) as emulsifiers and binders. The relationships between viscosity and shear time or rates were tested and the dispersing stability of oil in water (O/W) emulsions was characterized with comparison to suspensions without the addition of oil phase. The effects of solid loadings of HA and the volume ratio between oil and water on the morphologies of microspheres were investigated. Hollow HA microspheres with particle diameter of ~20μm and pore size of ~0.6μm were successfully obtained by spray freezing method. Besides, drying and sintering processes were crucial to the formation of hollow and porous structures, respectively. The gentamicin loading and releasing of HA porous microspheres with different hollow volumes were tested. PMID:27612804

  4. 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 6μm, a specific surface area of 40m(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 16nm. 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 200μm, 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 15days 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. PMID:27040244

  5. Porous hydroxyapatite and gelatin/hydroxyapatite microspheres obtained by calcium phosphate cement emulsion.

    PubMed

    Perez, Roman A; Del Valle, Sergio; Altankov, George; Ginebra, Maria-Pau

    2011-04-01

    Hydroxyapatite and hybrid gelatine/hydroxyapatite microspheres were obtained through a water in oil emulsion of a calcium phosphate cement (CPC). The setting reaction of the CPC, in this case the hydrolysis of α-tricalcium phosphate, was responsible for the consolidation of the microspheres. After the setting reaction, the microspheres consisted of an entangled network of hydroxyapatite crystals, with a high porosity and pore sizes ranging between 0.5 and 5 μm. The size of the microspheres was tailored by controlling the viscosity of the hydrophobic phase, the rotation speed, and the initial powder size of the CPC. The incorporation of gelatin increased the sphericity of the microspheres, as well as their size and size dispersion. To assess the feasibility of using the microspheres as cell microcarriers, Saos-2 cells were cultured on the microspheres. Fluorescent staining, SEM studies, and LDH quantification showed that the microspheres were able to sustain cell growth. Cell adhesion and proliferation was significantly improved in the hybrid gelatin/hydroxyapatite microspheres as compared to the hydroxyapatite ones. PMID:21290594

  6. Hollow hydroxyapatite microspheres as a device for controlled delivery of proteins.

    PubMed

    Fu, Hailuo; Rahaman, Mohamed N; Day, Delbert E; Brown, Roger F

    2011-03-01

    Hollow hydroxyapatite (HA) microspheres were prepared by reacting solid microspheres of Li(2)O-CaO-B(2)O(3) glass (106-150 μm) in K(2)HPO(4) solution, and evaluated as a controlled delivery device for a model protein, bovine serum albumin (BSA). Reaction of the glass microspheres for 2 days in 0.02 M K(2)HPO(4) solution (pH = 9) at 37°C resulted in the formation of biocompatible HA microspheres with a hollow core diameter equal to 0.6 the external diameter, high surface area (~100 m(2)/g), and a mesoporous shell wall (pore size ≈ 13 nm). After loading with a solution of BSA in phosphate-buffered saline (PBS) (5 mg BSA/ml), the release kinetics of BSA from the HA microspheres into a PBS medium were measured using a micro bicinchoninic acid (BCA) protein assay. Release of BSA initially increased linearly with time, but almost ceased after 24-48 h. Modification of the BSA release kinetics was achieved by modifying the microstructure of the as-prepared HA microspheres using a controlled heat treatment (1-24 h at 600-900°C). Sustained release of BSA was achieved over 7-14 days from HA microspheres heated for 5 h at 600°C. The amount of BSA released at a given time was dependent on the concentration of BSA initially loaded into the HA microspheres. These hollow HA microspheres could provide a novel inorganic device for controlled local delivery of proteins and drugs. PMID:21290170

  7. Preparation and characterization of gelatin-hydroxyapatite composite microspheres for hard tissue repair.

    PubMed

    Chao, Shao Ching; Wang, Ming-Jia; Pai, Nai-Su; Yen, Shiow-Kang

    2015-12-01

    Gelatin-hydroxyapatite composite microspheres composed of 21% gelatin (G) and 79% hydroxyapatite (HA) with uniform morphology and controllable size were synthesized from a mixed solution of Ca(NO3)2, NH4H2PO4 and gelatin by a wet-chemical method. Material analyses such as X-ray diffraction (XRD), scanning/transmission electron microscopy examination (SEM/TEM) and inductively coupled plasma-mass spectroscopy (ICP-MS) were used to characterize G-HA microspheres by analyzing their crystalline phase, microstructure, morphology and composition. HA crystals precipitate along G fibers to form nano-rods with diameters of 6-10nm and tangle into porous microspheres after blending. The cell culture indicates that G-HA composite microspheres without any toxicity could enhance the proliferation and differentiation of osteoblast-like cells. In a rat calvarial defect model, G-HA bioactive scaffolds were compared with fibrin glue (F) and Osteoset® Bone Graft Substitute (OS) for their capacity of regenerating bone. Four weeks post-implantation, new bone, mineralization, and expanded blood vessel area were found in G-HA scaffolds, indicating greater osteoconductivity and bioactivity than F and OS. PMID:26354246

  8. Preparation of Hydroxyapatite Coating on the Surface of Hollow Glass Microspheres Using a Biomimetic Process

    NASA Astrophysics Data System (ADS)

    Jiao, Yan; Yang, Hai-Ying; Zhang, Ying-Long; Duan, Rong-Shuai; Lu, Yu-Peng

    2014-07-01

    Microcarrier culture technology has attached more attention, especially for scale-up cell culture in the filed of tissue engineering. The present work introduces a microcarrier with hydroxyapatite (HA) on hollow glass microsphere. Hollow glass microspheres with a main composition of SiO2 (55-65 wt.%), Al2O3 (26-35 wt.%), were pretreated by NaOH, on which hydroxyapatite coating was deposited by biomimetic process. The phase composition and morphology were characterized by X-ray diffractometer (XRD), Fourier transform infrared (FTIR) spectroscope, field emission scanning electron microscope (FE-SEM) and high resolution transmission electron microscope (HRTEM), respectively. The results showed that after immersion for 15 days in 1.5 SBF, the uniform and dense HA coating was formed and it has porous surface and low crystallinity.

  9. Synthesis, characterization and osteoconductivity properties of bone fillers based on alendronate-loaded poly(ε-caprolactone)/hydroxyapatite microspheres.

    PubMed

    Chen, Jianhong; Luo, Yun; Hong, Liangqing; Ling, You; Pang, Jun; Fang, Youqiang; Wei, Kun; Gao, Xin

    2011-03-01

    A superior drug controlled release system capable of achieving efficient osteogenesis is in imperative demand because of limited bone substitute tissue for the treatment of bone defect. In the present study, we investigated the potential of using poly(ε-caprolactone)-hydroxyapatite (PCL-HA) composite microspheres as an injectable bone repair vehicle by controlled release of alendronate (AL), a medicine that belongs to the bisphosphonates family. The PCL/HA-AL microspheres were prepared with solid/oil/water emulsion technique, which included two processes: (1) AL was loaded on the hydroxyapatite nanoparticles; (2) the HA-AL complex was built in the PCL matrix. The spherical PCL/HA-AL microspheres were characterized with its significantly improved encapsulation efficiency of hydrophilic AL and better sustained release. Human bone mesenchymal stem cells (hMSCs) were cultured on the surface of these microspheres and exhibited high proliferative profile. Specifically, in osteogenic medium, hMSCs on the surface of PCL/HA-AL microspheres displayed superior osteogenic differentiation which was verified by alkaline phosphatase activity assay. In conclusion, by presenting strong osteogenic commitment of hMSCs in vitro, the PCL/HA-AL microspheres have the potential to be used as an injectable vehicle for local therapy of bone defect. PMID:21318627

  10. Hydroxyapatite/polyurethane scaffold incorporated with drug-loaded ethyl cellulose microspheres for bone regeneration.

    PubMed

    Liu, Haohuai; Zhang, Li; Shi, Pujiang; Zou, Qin; Zuo, Yi; Li, Yubao

    2010-10-01

    The purpose of this study is to explore and develop biodegradable scaffold for bone regeneration or tissue engineering with the capacity of controlled drug delivery. Ceftazidime as a model drug was encapsulated in ethyl cellulose (EC) microspheres, which were subsequently incorporated in a hydroxyapatite/polyurethane (HA/PU) composite scaffold to generate an antibiotic drug delivery system. HA/PU scaffolds had an interconnected pore network with an average porosity of about 83%. The presence of microspheres in the composite scaffolds was confirmed by scanning electron microscopy. The drug-loaded EC microspheres were uniformly distributed in the HA/PU scaffold matrix and showed no significant effect on the pore structure of the scaffold. Incorporation of microspheres into scaffolds significantly reduced the initial burst release, and the system exhibited a sustained release of the model drug for up to 60 days. Moreover, the scaffold with drug-loaded microspheres was proved to be an effective drug delivery system with good cytocompatibility and antibacterial properties. The novel drug-loaded microsphere/scaffold composites developed in this study are promising to serve as vehicles for controlled drug delivery in bone regeneration or bone tissue engineering. PMID:20665683

  11. Strontium-substituted, luminescent and mesoporous hydroxyapatite microspheres for sustained drug release.

    PubMed

    Jiang, Fei; Wang, De-Ping; Ye, Song; Zhao, Xin

    2014-02-01

    The multifunctional strontium (Sr)-substituted hydroxyapatite microsphere was prepared via hydrothermal method, in which the luminescent and controlled drug release functions can be realized. The structure and morphology of the as-prepared microspheres were studied by using XRD, FTIR, SEM, TEM, HR-TEM, BET method. The optical properties was investigated by using photoluminescence (PL) and XPS measurement. Then, the as-prepared multifunctional microspheres were performed as a drug delivery carrier using vancomycin as a model drug. The experimental results show that the composition, morphology, luminescent properties and drug storage/release behaviour were obviously influenced by the amount of Sr. The microspheres with Sr(2+)/(Ca(2+) + Sr(2+)) = 0.3 of Sr substitution showed the maximum specific surface area, best pore structure and strongest PL intensity. All the samples presented remarkable sustained drug release kinetics. In addition, the PL intensity of SrHA in the drug delivery system increased with the cumulative release time (amount) of vancomycin, which would make the drug release might be possibly tracked by the change of the luminescent intensity. Our study indicated a potential prospect that the fabricated multifunctional SrHA mesoporous microspheres might be applied in the field of bone regeneration and drug delivery. PMID:24402509

  12. Spheroidized Hydroxyapatite (HA) Powders Plasma Spraying of Combustion Flame

    NASA Astrophysics Data System (ADS)

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

    1998-06-01

    Tailoring powder characteristics to suit the plasma spray process can alleviate difficulties associated with the preparation of hydroxyapatite (HA) coatings. Commercial HA feedstock normally exhibit an angular morphology and a wide particle size range that present difficulties in powder transport from the powder hopper to the plasma spray gun and in nonuniform melting of the powders in the plasma flame. Hence, combustion flame spheroidized hydroxyapatite (SHA) was used as the feedstock for plasma spraying. Spherical particles within a narrow particle size range are found to be more effective for the plasma spray processes. Results show coatings generated from spheroidized HA powders have unique surface and microstructure characteristics. Scanning electron microscope (SEM) observation of the coating surface revealed well-formed splats that spread and flatten into disc configurations with no disintegration, reflecting adequate melting of the HA in the plasma and subsequent deposition consistency. The surface topography is generally flat with good overlapping of subsequent spreading droplets. Porosity in the form of macropores is substantially reduced. The cross-section microstructure reveals a dense coating comprised of randomly stacked lamellae. The tensile bond strengths of the SHA coatings, phase composition, and characteristics of the coatings generated with different particle sizes (125 to 75 µm, 45 to 75 µm, 20 to 45 µm, and 5 to 20 µm) showed that a high bond strength of ˜16 MPa can be obtained with SHA in the size range from 20 to 45 µm. This can be improved further by a postspray treatment by hot isostatic pressing (HIP). However, larger particle size ranges exhibited higher degrees of crystallinity and relatively higher HA content among the various calcium phosphate phases found in the coatings.

  13. 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.

  14. Preparation of hollow hydroxyapatite microspheres by the conversion of borate glass at near room temperature

    SciTech Connect

    Yao, Aihua; Ai, Fanrong; Liu, Xin; Wang, Deping; Huang, Wenhai; Xu, Wei

    2010-01-15

    Hollow hydroxyapatite microspheres, consisting of a hollow core and a porous shell, were prepared by converting Li{sub 2}O-CaO-B{sub 2}O{sub 3} glass microspheres in dilute phosphate solution at 37 {sup o}C. The results confirmed that Li{sub 2}O-CaO-B{sub 2}O{sub 3} glass was transformed to hydroxyapatite without changing the external shape and dimension of the original glass object. Scanning electron microscopy images showed the shell wall of the microsphere was built from hydroxyapatite particles, and these particles spontaneously align with one another to form a porous sphere with an interior cavity. Increase in phosphate concentration resulted in an increase in the reaction rate, which in turn had an effect on shell wall structure of the hollow hydroxyapatite microsphere. For the Li{sub 2}O-CaO-B{sub 2}O{sub 3} glass microspheres reacted in low-concentration K{sub 2}HPO{sub 4} solution, lower reaction rate and a multilayered microstructure were observed. On the other hand, the glass microspheres reacted in higher phosphate solution converted more rapidly and produced a single hydroxyapatite layer. Furthermore, the mechanism of forming hydroxyapatite hollow microsphere was described.

  15. Hollow hydroxyapatite microspheres: a novel bioactive and osteoconductive carrier for controlled release of bone morphogenetic protein-2 in bone regeneration

    PubMed Central

    Xiao, Wei; Fu, Hailuo; Rahaman, Mohamed N.; Liu, Yonxing; Bal, B. Sonny

    2013-01-01

    The regeneration of large bone defects is a common and significant clinical problem. Limitations associated with existing treatments such as autologous bone grafts and allografts have increased the need for synthetic bone graft substitutes. The objective of this study was to evaluate the capacity of novel hollow hydroxyapatite (HA) microspheres to serve as a carrier for controlled release of bone morphogenetic-2 (BMP2) in bone regeneration. Hollow HA microspheres (106–150 μm) with a high surface area (>100 m2/g) and a mesoporous shell wall (pore size 10–20 nm) were created using a glass conversion technique. The release of BMP2 from the microspheres into a medium composed of diluted fetal bovine serum in vitro was slow, but it occurred continuously for over 2 weeks. When implanted in rat calvarial defects for 3 or 6 weeks, the microspheres loaded with BMP2 (1 μg/defect) showed a significantly better capacity to regenerate bone than those without BMP2. The amount of new bone in the defects implanted with the BMP2-loaded microspheres was 40% and 43%, respectively, at 3 and 6 weeks, compared to 13% and 17%, respectively, for the microspheres without BMP2. Coating the BMP2-loaded microspheres with a biodegradable polymer, poly(lactic-co-glycolic acid), reduced the amount of BMP2 released in vitro and, above a certain coating thickness, significantly reduced bone regeneration in vivo. The results indicate that these hollow HA microspheres could provide a bioactive and osteoconductive carrier for growth factors in bone regeneration. PMID:23747325

  16. Structure design and fabrication of porous hydroxyapatite microspheres for cell delivery

    NASA Astrophysics Data System (ADS)

    Li, Ruijing; Chen, Kexin; Li, Geng; Han, Guoxiang; Yu, Sheng; Yao, Juming; Cai, Yurong

    2016-09-01

    Porous microspheres fabricated from bioceramics have great potential for cell delivery in injectable tissue engineering application. The size and structure of pores in the microspheres are important for the effective protection and transportation of cells. In this study, porous hydroxyapatite microspheres are fabricated through the water-in-oil emulsion method followed by a calcination treatment at the high temperature. Both self-made resorcinol-formaldehyde (RF) composite spheres and camphene are used as pore-forming agents to produce big pores corresponding to the size of RF spheres and connected channel among big pores in hydroxyapatite matrix. The properties of the microspheres are characterized using X-ray diffraction, thermogravimetry analysis, universal material machine, field emission scanning electron microscopy. Cell assays are carried out to evaluate the cellular compatibility of the microspheres. The results showed that the hydroxyapatite microspheres with controllable pore structure and high porosity could be fabricated by this method, which have better strength to resist the compressive force. The microspheres are conducive to support adhesion, proliferation and differentiation of MC3T3-E1 cells. The results indicate that the obtained porous hydroxyapatite microspheres can be a permeable microenvironment for cell delivery in injectable tissue engineering.

  17. BMP2-loaded hollow hydroxyapatite microspheres exhibit enhanced osteoinduction and osteogenicity in large bone defects

    PubMed Central

    Xiong, Long; Zeng, Jianhua; Yao, Aihua; Tu, Qiquan; Li, Jingtang; Yan, Liang; Tang, Zhiming

    2015-01-01

    The regeneration of large bone defects is an osteoinductive, osteoconductive, and osteogenic process that often requires a bone graft for support. Limitations associated with naturally autogenic or allogenic bone grafts have demonstrated the need for synthetic substitutes. The present study investigates the feasibility of using novel hollow hydroxyapatite microspheres as an osteoconductive matrix and a carrier for controlled local delivery of bone morphogenetic protein 2 (BMP2), a potent osteogenic inducer of bone regeneration. Hollow hydroxyapatite microspheres (100±25 μm) with a core (60±18 μm) and a mesoporous shell (180±42 m2/g surface area) were prepared by a glass conversion technique and loaded with recombinant human BMP2 (1 μg/mg). There was a gentle burst release of BMP2 from microspheres into the surrounding phosphate-buffered saline in vitro within the initial 48 hours, and continued at a low rate for over 40 days. In comparison with hollow hydroxyapatite microspheres without BMP2 or soluble BMP2 without a carrier, BMP2-loaded hollow hydroxyapatite microspheres had a significantly enhanced capacity to reconstitute radial bone defects in rabbit, as shown by increased serum alkaline phosphatase; quick and complete new bone formation within 12 weeks; and great biomechanical flexural strength. These results indicate that BMP2-loaded hollow hydroxyapatite microspheres could be a potential new option for bone graft substitutes in bone regeneration. PMID:25609957

  18. Controlled degradation pattern of hydroxyapatite/calcium carbonate composite microspheres.

    PubMed

    Yang, Ning; Zhong, Qiwei; Zhou, Ying; Kundu, Subhas C; Yao, Juming; Cai, Yurong

    2016-06-01

    Hydroxyapatite (HAP) is widely used in clinic due to its good biocompatibility and osteoconductivity except for its slow degradation speed. In the present study, spherical calcium carbonate (CaCO3 ) is fabricated in the presence of silk protein sericin, which is transmuted into HAP microsphere in phosphate solution with the assistance of microwave irradiation. The effect of reaction conditions on the conversion of CaCO3 is investigated including reaction time, chemical composition of phosphate solution, and microwave power to get a series of HAP/CaCO3 composites. The degradation property of the composites is evaluated in vitro. Results show the degradation speed of the composite with higher HAP content is slower. The degradation rate of the composite could be changed effectively by modulating the proportion of HAP and CaCO3 . This work provides a feasible method for the preparation of spherical HAP/CaCO3 composite with controllable degradability. The composite thus obtained may be an ideal material for bone tissue engineering application. Microsc. Res. Tech. 79:518-524, 2016. © 2016 Wiley Periodicals, Inc. PMID:27037606

  19. Evaluation of bone regeneration in implants composed of hollow HA microspheres loaded with TGF– 1 in a rat calvarial defect model

    PubMed Central

    Fu, Hailuo; Rahaman, Mohamed N.; Brown, Roger F.; Day, Delbert E.

    2012-01-01

    Implants that serve simultaneously as an osteoconductive matrix and as a device for local growth factor delivery may be required for optimal bone regeneration in some applications. In the present study, hollow hydroxyapatite (HA) microspheres (106–150 μm) in the form of three-dimensional (3D) scaffolds or individual (loose) microspheres were created using a glass conversion process. The capacity of the implants, with or without transforming growth factor- 1 (TGF- 1), to regenerate bone in a rat calvarial defect model was compared. The 3D scaffolds supported the proliferation and alkaline phosphatase activity of osteogenic MLO-A5 cells in vitro, showing their cytocompatibility. Release of TGF- 1 from the 3D scaffolds into phosphate-buffered saline ceased after 2–3 days when 30% of the growth factor was released. Bone regeneration in the 3D scaffolds and the individual microspheres increased with time from 6 to 12 weeks, but it was significantly higher (23%) in the individual microspheres than in the 3D scaffolds (15%) after 12 weeks. Loading with TGF-β1 (5 μg/defect) enhanced bone regeneration in the 3D scaffolds and individual microspheres after 6 weeks, but had little effect after 12 weeks. 3D scaffolds and individual microspheres with larger HA diameter (150–250 μm) showed better ability to regenerate bone. Based on these results, implants composed of hollow HA microspheres show promising potential as an osteoconductive matrix for local growth factor delivery in bone regeneration. PMID:23168225

  20. Fabrication of inorganic hydroxyapatite nanoparticles and organic biomolecules-dual encapsulated alginate microspheres.

    PubMed

    Wang, Yu-Pu; Liao, Yu-Te; Liu, Chia-Hung; Yu, Jiashing; Chen, Jung-Chih; Wu, Kevin C-W

    2015-01-01

    Inorganic hydroxyapatite nanoparticles (HANPs) and two kinds of organic biomolecules (i.e., fluorescent dye rhodamine 6G and protein lysozyme) were coencapsulated into alginate microspheres through an air dynamical atomization with optimized operation conditions. The synthesized microspheres have several advantages: HANP provides osteoconductivity and mechanical strength, rhodamine 6G (R6G) and lysozyme act as model drugs, and alginate provides excellent biocompatibility and carboxylate functionality. The results of fluorescent microscopic images indicated the successful dual encapsulation of HANPs and lysozyme inside the alginate microspheres. Furthermore, the results of 3- (4,5-cimethylthiazol-2-yl)-2,5-diphenyl tetrazolium bromide assay showed that the fabricated alginate microspheres could be uptaken by HepG2 without apparent cytotoxicity. The dual encapsulated alginate microspheres fabricated in this study show great potential in many biomedical applications. PMID:25939572

  1. 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. PMID:25791461

  2. [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. PMID:25219247

  3. 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.

  4. Novel synthesis strategy for composite hydrogel of collagen/hydroxyapatite-microsphere originating from conversion of CaCO3 templates

    NASA Astrophysics Data System (ADS)

    Wei, Qingrong; Lu, Jian; Wang, Qiaoying; Fan, Hongsong; Zhang, Xingdong

    2015-03-01

    Inspired by coralline-derived hydroxyapatite, we designed a methodological route to synthesize carbonated-hydroxyapatite microspheres from the conversion of CaCO3 spherulite templates within a collagen matrix under mild conditions and thus constructed the composite hydrogel of collagen/hydroxyapatite-microspheres. Fourier transform infrared spectroscopy (FTIR) and x-ray diffraction (XRD) were employed to confirm the successful generation of the carbonated hydroxyapatite phase originating from CaCO3, and the ratios of calcium to phosphate were tracked over time. Variations in the weight portion of the components in the hybrid gels before and after the phase transformation of the CaCO3 templates were identified via thermogravimetric analysis (TGA). Scanning electron microscopy (SEM) shows these composite hydrogels have a unique multiscale microstructure consisting of a collagen nanofibril network and hydroxyapatite microspheres. The relationship between the hydroxyapatite nanocrystals and the collagen fibrils was revealed by transmission electron microscopy (TEM) in detail, and the selected area electron diffraction (SAED) pattern further confirmed the results of the XRD analyses which show the typical low crystallinity of the generated hydroxyapatite. This smart synthesis strategy achieved the simultaneous construction of microscale hydroxyapatite particles and collagen fibrillar hydrogel, and appears to provide a novel route to explore an advanced functional hydrogel materials with promising potentials for applications in bone tissue engineering and reconstruction medicine.

  5. Effects of Nano-hydroxyapatite/Poly(DL-lactic-co-glycolic acid) Microsphere-Based Composite Scaffolds on Repair of Bone Defects: Evaluating the Role of Nano-hydroxyapatite Content.

    PubMed

    He, Shu; Lin, Kai-Feng; Sun, Zhen; Song, Yue; Zhao, Yi-Nan; Wang, Zheng; Bi, Long; Liu, Jian

    2016-07-01

    The aim of the current study was to prepare microsphere-based composite scaffolds made of nano-hydroxyapatite (nHA)/poly (DL-lactic-co-glycolic acid) (PLGA) at different ratios and evaluate the effects of nHA on the characteristics of scaffolds for tissue engineering application. First, microsphere-based composite scaffolds made of two ratios of nHA/PLGA (nHA/PLGA = 20/80 and nHA/PLGA = 50/50) were prepared. Then, the effects of nHA on the wettability, mechanical strength, and degradation of scaffolds were investigated. Second, the biocompatibility and osteoinductivity were evaluated and compared by co-culture of scaffolds with bone marrow stromal stem cells (BMSCs). The results showed that the adhesion, proliferation, and osteogenic differentiation of BMSCs with nHA/PLGA (50/50) were better than those with nHA/PLGA (20/80). Finally, we implanted the scaffolds into femur bone defects in a rabbit model, then the capacity of guiding bone regeneration as well as the in vivo degradation were observed by micro-CT and histological examinations. After 4 weeks' implantation, there was no significant difference on the repair of bone defects. However, after 8 and 12 weeks' implantation, the nHA/PLGA (20/80) exhibited better bone formation than nHA/PLGA (50/50). These results suggested that a proper concentration of nHA in the nHA/PLGA composite should be taken into account when the composite scaffolds were prepared, which plays an important role in the biocompatibility, degradation rate and osteoconductivity. PMID:27378617

  6. In Vivo Osteogenic Potential of Biomimetic Hydroxyapatite/Collagen Microspheres: Comparison with Injectable Cement Pastes

    PubMed Central

    Manzanares, Maria-Cristina; Ginebra, Maria-Pau; Franch, Jordi

    2015-01-01

    The osteogenic capacity of biomimetic calcium deficient hydroxyapatite microspheres with and without collagen obtained by emulsification of a calcium phosphate cement paste has been evaluated in an in vivo model, and compared with an injectable calcium phosphate cement with the same composition. The materials were implanted into a 5 mm defect in the femur condyle of rabbits, and bone formation was assessed after 1 and 3 months. The histological analysis revealed that the cements presented cellular activity only in the margins of the material, whereas each one of the individual microspheres was covered with osteogenic cells. Consequently, bone ingrowth was enhanced by the microspheres, with a tenfold increase compared to the cement, which was associated to the higher accessibility for the cells provided by the macroporous network between the microspheres, and the larger surface area available for osteoconduction. No significant differences were found in terms of bone formation associated with the presence of collagen in the materials, although a more extensive erosion of the collagen-containing microspheres was observed. PMID:26132468

  7. Sr-containing hydroxyapatite: morphologies of HA crystals and bioactivity on osteoblast cells.

    PubMed

    Aina, Valentina; Bergandi, Loredana; Lusvardi, Gigliola; Malavasi, Gianluca; Imrie, Flora E; Gibson, Iain R; Cerrato, Giuseppina; Ghigo, Dario

    2013-04-01

    A series of Sr-substituted hydroxyapatites (HA), of general formula Ca(10-x)Srx(PO4)6(OH)2, where x=2 and 4, were synthesized by solid state methods and characterized extensively. The reactivity of these materials in cell culture medium was evaluated, and the behavior towards MG-63 osteoblast cells (in terms of cytotoxicity and proliferation assays) was studied. Future in vivo studies will give further insights into the behavior of the materials. A paper by Lagergren et al. (1975), concerning Sr-substituted HA prepared by a solid state method, reports that the presence of Sr in the apatite composition strongly influences the apatite diffraction patterns. Zeglinsky et al. (2012) investigated Sr-substituted HA by ab initio methods and Rietveld analyses and reported changes in the HA unit cell volume and shape due to the Sr addition. To further clarify the role played by the addition of Sr on the physico-chemical properties of these materials we prepared Sr-substituted HA compositions by a solid state method, using different reagents, thermal treatments and a multi-technique approach. Our results indicated that the introduction of Sr at the levels considered here does influence the structure of HA. There is also evidence of a decrease in the crystallinity degree of the materials upon Sr addition. The introduction of increasing amounts of Sr into the HA composition causes a decrease in the specific surface area and an enrichment of Sr-apatite phase at the surface of the samples. Bioactivity tests show that the presence of Sr causes changes in particle size and/or morphology during soaking in MEM solution; on the contrary the morphology of pure HA does not change after 14 days of reaction. The presence of Sr, as Sr-substituted HA and SrCl2, in cultures of human MG-63 osteoblasts did not produce any cytotoxic effect. In fact, Sr-substituted HA increased the proliferation of osteoblast cells and enhanced cell differentiation: Sr in HA has a positive effect on MG-63 cells

  8. Microsphere-based scaffolds encapsulating tricalcium phosphate and hydroxyapatite for bone regeneration.

    PubMed

    Gupta, Vineet; Lyne, Dina V; Barragan, Marilyn; Berkland, Cory J; Detamore, Michael S

    2016-07-01

    Bioceramic mixtures of tricalcium phosphate (TCP) and hydroxyapatite (HAp) are widely used for bone regeneration because of their excellent cytocompatibility, osteoconduction, and osteoinduction. Therefore, we hypothesized that incorporation of a mixture of TCP and HAp in microsphere-based scaffolds would enhance osteogenesis of rat bone marrow stromal cells (rBMSCs) compared to a positive control of scaffolds with encapsulated bone-morphogenic protein-2 (BMP-2). Poly(D,L-lactic-co-glycolic acid) (PLGA) microsphere-based scaffolds encapsulating TCP and HAp mixtures in two different ratios (7:3 and 1:1) were fabricated with the same net ceramic content (30 wt%) to evaluate how incorporation of these ceramic mixtures would affect the osteogenesis in rBMSCs. Encapsulation of TCP/HAp mixtures impacted microsphere morphologies and the compressive moduli of the scaffolds. Additionally, TCP/HAp mixtures enhanced the end-point secretion of extracellular matrix components relevant to bone tissue compared to the "blank" (PLGA-only) microsphere-based scaffolds as evidenced by the biochemical, gene expression, histology, and immunohistochemical characterization. Moreover, the TCP/HAp mixture groups even surpassed the BMP-2 positive control group in some instances in terms of matrix synthesis and gene expression. Lastly, gene expression data suggested that the rBMSCs responded differently to different TCP/HAp ratios presented to them. Altogether, it can be concluded that TCP/HAp mixtures stimulated the differentiation of rBMSCs toward an osteoblastic phenotype, and therefore may be beneficial in gradient microsphere-based scaffolds for osteochondral regeneration. PMID:27272903

  9. Modification and cytocompatibility of biocomposited porous PLLA/HA-microspheres scaffolds.

    PubMed

    Xiao, Guiyong; Yin, Han; Xu, Wenhua; Lu, Yupeng

    2016-10-01

    Poly(L-lactic acid) and hydroxyapatie (PLLA/HA) composite scaffolds have good properties and suit to use as bone tissue engineering. In this work, hollow HA microspheres (HAM) with poor crystallinity were fabricated by a flame-drying method. The HAM has the potential to be used to release drugs or proteins in addition to improve osteoconductivity. Different ratios of PLLA/HAM were used to prepare porous composite scaffolds using the thermally induced phase separation technique. The HAMs were randomly incorporated into the PLLA porous scaffolds. As the HAMs ratio was increased, the porous composite scaffolds changed from ladder-like into isotropic structure. In addition, the compressive strength of PLLA/HAMs composite scaffolds improved first and declined with the increasing of HAMs ratio in the scaffolds. In vitro experiment showed that PLLA/HAMs composite scaffolds improved the attachment, migration, and differentiation of osteoblastic cells. These results demonstrated that the PLLA/HAMs composite scaffolds were superior to plain PLLA scaffold for bone tissue engineering. PMID:27398630

  10. Hydrothermal fabrication of porous hollow hydroxyapatite microspheres for a drug delivery system.

    PubMed

    Lai, Wen; Chen, Cen; Ren, Xiaoyuan; Lee, In-Seop; Jiang, Guohua; Kong, Xiangdong

    2016-05-01

    Porous hollow hydroxyapatite microspheres (PHHMs) are the promising biomaterials, owing to their excellent biocompatibility, biodegradability and bioactivity. PHHMs have been used as drug controlled carriers due to their advantages such as large drug loading capacity, nanochannels for drug loading and release and high specific surface area. In this study, PHHMs were prepared successfully in Na2HPO4 solution by an anion-exchange process using vaterite CaCO3 through a hydrothermal method. The previous vaterite CaCO3 was synthesized by a polymer-templated method in the poly(styrene sulfonic acid) sodium salt (PSS) aqueous solutions. The PHHMs have a size distribution from 0.8 to 2.0 μm, with an average pore size of about 24.3 nm. The wall of PHHMs is constructed with building units of hydroxyapatite nanofibers with an average length of 300 nm and an average width of 20 nm. The PHHMs displayed a high drug loading capacity and pH-responsive sustained-controlled drug release behavior when we used doxorubicin hydrochloride (DOX) as a loading drug. Moreover, the controlled drug release system showed a high ability to kill cancer cells and less damage to normal cells. These results indicated that PHHMs are promising for applications in various biomedical fields such as drug delivery system and oncotherapy. PMID:26952411

  11. In vitro study of hydroxyapatite/polycaprolactone (HA/PCL) nanocomposite synthesized by an in situ sol-gel process.

    PubMed

    Rezaei, A; Mohammadi, M R

    2013-01-01

    Hydroxyapatite (HA) is the most substantial mineral constituent of a bone which has been extensively used in medicine as implantable materials, owing to its good biocompatibility, bioactivity high osteoconductive, and/or osteoinductive properties. Nevertheless, its mechanical property is not utmost appropriate for a bone substitution. Therefore, a composite consist of HA and a biodegradable polymer is usually prepared to generate an apt bone scaffold. In the present work polycaprolactone (PCL), a newly remarkable biocompatible and biodegradable polymer, was employed as a matrix and hydroxyapatite nanoparticles were used as a reinforcement element of the composite. HA/PCL nanocomposites were synthesized by a new in situ sol-gel process using calcium hydroxide and phosphoric acid precursors in the presence of Tetrahydrofuran (THF) as a solvent. Chemical and physical characteristics of the nanocomposite were studied by X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM) and Fourier transform infrared (FTIR) analyses. The results indicated that pure HA nanoparticles were well-incorporated and homogenously dispersed in the PCL matrix. It was found that the mechanical property of PCL was improved by addition of 20wt.% HA nanoparticles. Furthermore, the biological property of nanocomposites was investigated under in vitro condition. For this purpose, HA/PCL scaffolds were prepared through a salt leaching process and immersed in a saturated simulated body fluid (SBF) after 3 and 7days. It was found that a uniform layer of biomimetic HA could be deposited on the surface of HA/PCL scaffolds. Therefore, the prepared HA/PCL scaffolds showed good potential for bone tissue engineering and could be used for many clinical applications in orthopedic and maxillofacial surgery. PMID:25428086

  12. Physicochemical and mechanical properties of freeze cast hydroxyapatite-gelatin scaffolds with dexamethasone loaded PLGA microspheres for hard tissue engineering applications.

    PubMed

    Ghorbani, Farnaz; Nojehdehian, Hanieh; Zamanian, Ali

    2016-12-01

    Hydroxyapatite (HA)-gelatin scaffolds incorporated with dexamethasone-loaded polylactic-co-glycolic acid (PLGA) microspheres were synthesized by freeze casting technique. Scanning electron microscopy (SEM) micrographs demonstrated a unidirectional microstructure and a decrease in the pore size as a function of temperature gradient. Higher amounts of HA resulted in a decrease in the pore size. According to the results, at lower cooling rates, the formation of a lamellar structure decreased the mechanical strength, but at the same time, enhanced the swelling ratio, biodegradation rate and drug release level. On the other hand, higher weight ratios of HA increased the compressive strength, and reduced the swelling ratio, biodegradation rate and drug release level. The results obtained by furrier transform infrared spectroscopy (FTIR) and bioactivity analysis illustrated that the interactions of the materials support the apatite formation in the simulated body fluid (SBF) solution. Based on the obtained results, the synthesized composite scaffolds have the necessary mechanical and physicochemical features to support the regeneration of defects and to maintain their stability during the neo-tissue formation. PMID:27612706

  13. Hydroxyapatite (HA)/poly-L-lactic acid (PLLA) dual coating on magnesium alloy under deformation for biomedical applications.

    PubMed

    Diez, Mathilde; Kang, Min-Ho; Kim, Sae-Mi; Kim, Hyoun-Ee; Song, Juha

    2016-02-01

    The introduction of a protective coating layer to highly corrosive magnesium (Mg) has been proposed as one of the common approaches for improved corrosion resistance of Mg-based implants as load-bearing biomedical applications. However, only few studies have focused on the mechanical stability of the coated Mg under practical conditions where significant deformation of the load-bearing implants is induced during the surgical operation or under physiological environments. Therefore, in this study, we developed a dual coating system composed of an interlayer hydroxyapatite (HA) and a top layer poly-L-lactic acid (PLLA) to improve the coating stability under deformation of Mg alloy (WE43) substrate. The HA interlayer was directly formed on the Mg alloy surface, followed by dip-coating of PLLA. As the interlayer, HA improved the adhesion of PLLA by modulating nano- and microscale roughness, in addition to its inherently good bonding strength to Mg. The flexible and deformable top coating PLLA layer mitigated crack propagation in the HA layer under deformation. Thus, the dual coating layer provided good protection to the underlying WE43 from corrosion regardless of deformation. The enhanced corrosion behavior of dual-coated WE43 exhibited better mechanical and biological performance compared to the non-coated or single-coated WE43. Therefore, this dual coating layer on Mg is expected to accelerate Mg-based applications in biomedical devices. PMID:26704551

  14. Preparation and bioevaluation of 166Ho labelled hydroxyapatite (HA) particles for radiosynovectomy.

    PubMed

    Unni, P R; Chaudhari, P R; Venkatesh, Meera; Ramamoorthy, N; Pillai, M R A

    2002-02-01

    The preparation of 166Ho labeled hydroxy apatite (HA) particles for radiosynovectomy applications is described in this paper. 166Ho was prepared by the irradiation of Ho2O3 at a flux of 1.8 x 10(13) neutrons/cm2/s for about 7 days. The irradiation resulted in the production of approximately 17 GBq of 166Ho activity at the end of six hours post end of bombardment and the corresponding specific activity was approximately 3-4 GBq/mg of Ho. The irradiated target was dissolved in 0.1 N HCl solution. Radionuclidic purity was ascertained by high resolution gamma ray spectrometry. HA particles were synthesized and characterized by X-ray diffractometry. Labeling studies were carried out with and without citric acid as a transchelating agent. Radiochemical yield and purity of the 166Ho-HA particles were ascertained by paper chromatography and by paper electrophoresis techniques. Labeling yield of >98% could be achieved at pH 7, with 40 mg of HA particles and 8.6 microg of Ho. 166Ho-HA particles prepared were stable for 72 h. Bio-evaluation of the 166Ho -HA particles were carried out by injecting approximately 74 MBq dose in 200 microL (approximately 8 mg of 166Ho-HA particles) directly into the arthritis induced knee joints as well as into the healthy knee joints of white New Zealand rabbits. Images of the injected joints of the animals recorded using a gamma camera at regular intervals showed good retention. Blood samples were collected from the animals and activity assayed in a scintillation detector. Experiments were also carried out under identical conditions in normal rabbits. In both the cases, it was observed that there was no significant extra articular leakage of the injected activity over the study period of 96 h post injection. PMID:11823125

  15. Hydroxyapatite (HA) coating appears to be of benefit for implant durability of tibial components in primary total knee arthroplasty

    PubMed Central

    2011-01-01

    Background It is unclear whether there is a clinical benefit to adding hydroxyapatite (HA) coatings to total knee implants, especially with the tibial component, where failure of the implant more often occurs. A systematic review of the literature was undertaken to identify all prospective randomized trials for determining whether the overall clinical results (as a function of durability, function, and adverse events) favored HA-coated tibial components. Methods A comprehensive literature search was performed for the years 1990 to September 16, 2010. We restricted our search to randomized controlled trials involving participants receiving either an HA-coated tibia or other forms of tibial fixation. The primary outcome measures evaluated were durability, function, and acute adverse events. Results Data from 926 evaluable primary total knee implants in 14 studies were analyzed. Using an RSA definition for durability, HA-coated tibial components (porous or press-fit) without screw fixation were less likely to be unstable at 2 years than porous and cemented metal-backed tibial components (RR = 0.58, 95% CI: 0.34–0.98; p = 0.04, I2 = 39%, M-H random effects model). There was no significant difference in durability, as measured from revision and evaluated at 2 and 8–10 years, between groups. Also, functional status using different validated measures showed no significant difference at 2 and 5 years, no matter what measure was used. Lastly, there was no significant difference in adverse events. Limitations included small numbers of evaluable patients (≤ 50) in 7 of the 14 trials identified, and a lack of “hard” evidence of durability with need for replacement (i.e. frank failure, pain, or loss of functionality). Interpretation In patients > 65 years of age, an HA-coated tibial implant may provide better durability than other forms of tibial fixation. Larger trials should be undertaken comparing the long-term durability, function, and adverse events of HA

  16. Microspheres

    NASA Technical Reports Server (NTRS)

    1990-01-01

    Vital information on a person's physical condition can be obtained by identifying and counting the population of T-cells and B-cells, lymphocytes of the same shape and size that help the immune system protect the body from the invasion of disease. The late Dr. Alan Rembaum developed a method for identifying the cells. The method involved tagging the T-cells and B-cells with microspheres of different fluorescent color. Microspheres, which have fluorescent dye embedded in them, are chemically treated so that they can link with antibodies. With the help of a complex antibody/antigen reaction, the microspheres bind themselves to specific 'targets,' in this case the T-cells or B-cells. Each group of cells can then be analyzed by a photoelectronic instrument at different wavelengths emitted by the fluorescent dyes. Same concept was applied to the separation of cancer cells from normal cells. Microspheres were also used to conduct many other research projects. Under a patent license Magsphere, Inc. is producing a wide spectrum of microspheres on a large scale and selling them worldwide for various applications.

  17. 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.

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

    PubMed Central

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

    2016-01-01

    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. PMID:26956660

  19. Enhancement of Cell-Based Therapeutic Angiogenesis Using a Novel Type of Injectable Scaffolds of Hydroxyapatite-Polymer Nanocomposite Microspheres

    PubMed Central

    Koyama, Hidenori; Okada, Masahiro; Tanaka, Shinji; Shoji, Tetsuo; Emoto, Masanori; Furuzono, Tsutomu; Nishizawa, Yoshiki; Inaba, Masaaki

    2012-01-01

    Background Clinical trials demonstrate the effectiveness of cell-based therapeutic angiogenesis in patients with severe ischemic diseases; however, their success remains limited. Maintaining transplanted cells in place are expected to augment the cell-based therapeutic angiogenesis. We have reported that nano-hydroxyapatite (HAp) coating on medical devices shows marked cell adhesiveness. Using this nanotechnology, HAp-coated poly(l-lactic acid) (PLLA) microspheres, named nano-scaffold (NS), were generated as a non-biological, biodegradable and injectable cell scaffold. We investigate the effectiveness of NS on cell-based therapeutic angiogenesis. Methods and Results Bone marrow mononuclear cells (BMNC) and NS or control PLLA microspheres (LA) were intramuscularly co-implanted into mice ischemic hindlimbs. When BMNC derived from enhanced green fluorescent protein (EGFP)-transgenic mice were injected into ischemic muscle, the muscle GFP level in NS+BMNC group was approximate fivefold higher than that in BMNC or LA+BMNC groups seven days after operation. Kaplan-Meier analysis demonstrated that NS+BMNC markedly prevented hindlimb necrosis (P<0.05 vs. BMNC or LA+BMNC). NS+BMNC revealed much higher induction of angiogenesis in ischemic tissues and collateral blood flow confirmed by three-dimensional computed tomography angiography than those of BMNC or LA+BMNC groups. NS-enhanced therapeutic angiogenesis and arteriogenesis showed good correlations with increased intramuscular levels of vascular endothelial growth factor and fibroblast growth factor-2. NS co-implantation also prevented apoptotic cell death of transplanted cells, resulting in prolonged cell retention. Conclusion A novel and feasible injectable cell scaffold potentiates cell-based therapeutic angiogenesis, which could be extremely useful for the treatment of severe ischemic disorders. PMID:22529991

  20. In vitro degradation and cytocompatibility of dicalcium phosphate dihydrate cements prepared using the monocalcium phosphate monohydrate/hydroxyapatite system reveals rapid conversion to HA as a key mechanism.

    PubMed

    Alge, Daniel L; Goebel, W Scott; Chu, Tien-Min Gabriel

    2012-04-01

    We previously showed that dicalcium phosphate dihydrate (DCPD) cements can be prepared using monocalcium phosphate monohydrate (MCPM) and hydroxyapatite (HA). In this study, we have characterized the degradation properties and biocompatibility of these novel cements. To study the degradation properties, cements were prepared using MCPM:HA molar ratios of 4:1, 2:1, 2:3, and 2:5. Degradation was evaluated in vitro by static soaking in PBS, and changes in pH, mass, compressive strength, and composition were monitored. Conversion of DCPD to HA was noted in the 4:1 group, which initially consisted of pure DCPD. However, the 2:1 group, which initially consisted of DCPD and an intermediate amount of unreacted HA, underwent rapid conversion to HA associated with significantly greater pH drop and mass loss as well as a complete loss of mechanical integrity. On the basis of these results, we directly compared the cytocompatibility of 2:1 MCPM:HA cements to DCPD cements prepared with an equivalent percent molar excess of β-tricalcium phosphate (β-TCP) using an in vitro cell viability assay. Viability of cells co-cultured with 2:1 MCPM:HA cements was significantly reduced after just 48 h, while viability of cells cultured with the β-TCP-based cements was no different from control cells. In conclusion, this study demonstrates that conversion to HA plays an important role in the degradation of DCPD cements prepared with the MCPM/HA system, affecting both physical properties and cytocompatibility. These results could have important clinical implications for MCPM/HA cements. PMID:22323239

  1. 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

  2. Analyzing the behavior of a porous nano-hydroxyapatite/polyamide 66 (n-HA/PA66) composite for healing of bone defects.

    PubMed

    Xiong, Yan; Ren, Cheng; Zhang, Bin; Yang, Hongsheng; Lang, Yun; Min, Li; Zhang, Wenli; Pei, Fuxing; Yan, Yonggang; Li, Hong; Mo, Anchun; Tu, Chongqi; Duan, Hong

    2014-01-01

    The aim of this study was to analyze the behavior of the porous nano-hydroxyapatite/polyamide 66 (n-HA/PA66) composite grafted for bone defect repair through a series of biological safety experiments, animal experiments, and a more than 5-year long clinical follow-up. The biological safety experiments, carried out in accordance with the Chinese Guo Biao and Tolerancing (GB/T)16886 and GB/T16175, revealed that porous n-HA/PA66 composite had no cytotoxicity, no sensitization effect, no pyrogenic reaction, and that its hemolysis rate was 0.59% (less than 5%). Rabbit models of tibia defects with grafted porous n-HA/PA66 composite were established. After 2 weeks, the experiment showed that osteogenesis was detected in the porous n-HA/PA66 composite; the density of new bone formation was similar to the surrounding host bone at 12 weeks. After 26 weeks, the artificial bone rebuilt to lamellar bone completely. In the clinical study, a retrospective review was carried out for 21 patients who underwent serial radiographic assessment after treatment with porous n-HA/PA66 composite grafts following bone tumor resection. All wounds healed to grade A. No postoperative infections, delayed deep infection, nonspecific inflammation, rejection, or fractures were encountered. At a mean follow-up of 5.3 years, the mean Musculoskeletal Tumor Society's (MSTS) 93 score was 29.3 points (range: 28-30 points) and mean radiopaque density ratio was 0.77±0.10. The radiologic analysis showed that porous n-HA/PA66 composite had been completely incorporated with the host bone about 1.5 years later. In conclusion, this study indicated that the porous n-HA/PA66 composite had biological safety, and good biocompatibility, osteoinduction, and osseointegration. Thus, the porous n-HA/PA66 composite is an ideal artificial bone substitute and worthy of promotion in the field. PMID:24531621

  3. Carboxylated Agarose (CA)-Silk Fibroin (SF) Dual Confluent Matrices Containing Oriented Hydroxyapatite (HA) Crystals: Biomimetic Organic/Inorganic Composites for Tibia Repair.

    PubMed

    Hu, Jing-Xiao; Ran, Jia-Bing; Chen, Si; Jiang, Pei; Shen, Xin-Yu; Tong, Hua

    2016-07-11

    By in situ combining the dual cross-linking matrices of the carboxylated agarose (CA) and the silk fibroin (SF) with the hydroxyapatite (HA) crystals, the CA-SF/HA composites with optimal physicochemical and biological properties were obtained, which were designed to meet the clinical needs of load-bearing bone repair. With the synergistic modulation of the dual organic matrices, the HA nanoparticles presented sheet and rod morphologies due to the preferred orientation, which successfully simulated the biomineralization in nature. The chemical reactivity of the native agarose (NA) was significantly enhanced via carboxylation, and the CA exhibited higher thermal stability than the NA. In the presence of SF, the composites showed optimal mechanical properties that could meet the standard of bone repair. The degradation of the composites in the presence of CA and SF was significantly delayed such that the degradation rate of the implant could satisfy the growth rate of the newly formed bone tissue. The in vitro tests confirmed that the CA-SF/HA composite scaffolds enabled the MG63 cells to proliferate and differentiate well, and the CA/HA composite presented greater capability of promoting the cell behaviors than the NA/HA composite. After 24 days of implantation, newly formed bone was observed at the tibia defect site and around the implant. Extensive osteogenesis was presented in the rats treated with the CA-SF/HA composites. In general, the CA-SF/HA composites prepared in this work had the great potential to be applied for repairing large bone defects. PMID:27314146

  4. Degradation pattern of porous CaCO3 and hydroxyapatite microspheres in vitro and in vivo for potential application in bone tissue engineering.

    PubMed

    Zhong, Qiwei; Li, Wenhua; Su, Xiuping; Li, Geng; Zhou, Ying; Kundu, Subhas C; Yao, Juming; Cai, Yurong

    2016-07-01

    Despite superior clinical handling, excellent biocompatibility, biodegradation property of calcium phosphate needs to be improved to coincide with the rate of new bone formation. In this study, spherical CaCO3 are fabricated in the presence of the silk sericin and then transformed into porous hydroxyapatite (HAP) microspheres via hydrothermal method. The degradation behavior of obtained CaCO3, HAP and their mixture is first investigated in vitro. The result demonstrates that the weight loss of HAP microspheres are almost 24.3% after immersing in pH 7.40 Tris-HCl buffer solution for 12 weeks, which is far slower than that of spherical CaCO3 (97.5%). The degradation speed of the mixtures depends on the proportion of CaCO3 and HAP. The mixture with higher content of CaCO3 possesses a quicker degradation speed. The obtained CaCO3 and HAP microspheres are injected into subcutaneous tissue of ICR mice with the assistance of sodium alginate. The result in vivo also shows an obvious difference of degradation speed between the obtained CaCO3 and HAP microspheres, implying it is feasible to modulate the degradation property of the mixture through changing the proportion of CaCO3 and HAP The good cytocompatibility of the two kinds of microspheres is proved and a mild inflammation response is observed only at early stage of implantation. The job offers a simple method to modify the degradation properties of biomaterial for potential use in bone tissue engineering. PMID:26998866

  5. Facile fabrication of poly(L-lactic acid) microsphere-incorporated calcium alginate/hydroxyapatite porous scaffolds based on Pickering emulsion templates.

    PubMed

    Hu, Yang; Ma, Shanshan; Yang, Zhuohong; Zhou, Wuyi; Du, Zhengshan; Huang, Jian; Yi, Huan; Wang, Chaoyang

    2016-04-01

    In this study, we develop a facile one-pot approach to the fabrication of poly(L-lactic acid) (PLLA) microsphere-incorporated calcium alginate (ALG-Ca)/hydroxyapatite (HAp) porous scaffolds based on HAp nanoparticle-stabilized oil-in-water Pickering emulsion templates, which contain alginate in the aqueous phase and PLLA in the oil phase. The emulsion aqueous phase is solidified by in situ gelation of alginate with Ca(2+) released from HAp by decreasing pH with slow hydrolysis of d-gluconic acid δ-lactone (GDL) to produce emulsion droplet-incorporated gels, followed by freeze-drying to form porous scaffolds containing microspheres. The pore structure of porous scaffolds can be adjusted by varying the HAp or GDL concentration. The compressive tests show that the increase of HAp or GDL concentration is beneficial to improve the compressive property of porous scaffolds, while the excessive HAp can lead to the decrease in compressive property. Moreover, the swelling behavior studies display that the swelling ratios of porous scaffolds reduce with increasing HAp or GDL concentration. Furthermore, hydrophobic drug ibuprofen (IBU) and hydrophilic drug bovine serum albumin (BSA) are loaded into the microspheres and scaffold matrix, respectively. In vitro drug release results indicate that BSA has a rapid release while IBU has a sustained release in the dual drug-loaded scaffolds. In vitro cell culture experiments verify that mouse bone mesenchymal stem cells can proliferate on the porous scaffolds well, indicating the good biocompatibility of porous scaffolds. All these results demonstrate that the PLLA microsphere-incorporated ALG-Ca/HAp porous scaffolds have a promising potential for tissue engineering and drug delivery applications. PMID:26774574

  6. Computer-aided design and manufacturing and rapid prototyped nanoscale hydroxyapatite/polyamide (n-HA/PA) construction for condylar defect caused by mandibular angle ostectomy.

    PubMed

    Li, Jihua; Hsu, Yuchun; Luo, En; Khadka, Ashish; Hu, Jing

    2011-08-01

    The fracture or defect of the mandibular condyle is one of the serious complications during angle-reduction ostectomy. Reconstruction of such defects also is a daunting task. The case report describes a method based on computer-aided design/computer-aided manufacturing (CAD/CAM) and rapid prototyping nanoscale hydroxyapatite/polyamide (n-HA/PA) for individual design, fabrication, and implantation of a mandibular condyle. A 27-year-old woman with a square-shaped face who had previously undergone mandibular angle reduction reported with malocclusion, deviated mouth, collapse of the right side of the face, and masticatory problems. The reason for the problems was the unintended removal of the condyle during the ostectomy procedure. Using computed tomography (CT) data, a biomimetic n-HA/PA scaffold, and CAD/CAM for rapid prototyping by three-dimensional (3D) printing, a perfect-fitting condylar implant was fabricated. A surgical guide system also was developed to reproduce the procedures accurately so a perfect fit could be obtained during surgery. The patient ultimately regained reasonable jaw contour and appearance, as well as appreciable temporomandibular joint (TMJ) function. PMID:20972567

  7. Bioactive apatite incorporated alginate microspheres with sustained drug-delivery for bone regeneration application.

    PubMed

    Li, Haibin; Jiang, Fei; Ye, Song; Wu, Yingying; Zhu, Kaiping; Wang, Deping

    2016-05-01

    The strontium-substituted hydroxyapatite microspheres (SrHA) incorporated alginate composite microspheres (SrHA/Alginate) were prepared via adding SrHA/alginate suspension dropwise into calcium chloride solution, in which the gel beads were formed by means of crosslinking reaction. The structure, morphology and in vitro bioactivity of the composite microspheres were studied by using XRD, SEM and EDS methods. The biological behaviors were characterized and analyzed through inductively coupled plasma optical emission spectroscopy (ICP-OES), CCK-8, confocal laser microscope and ALP activity evaluations. The experimental results indicated that the synthetic SrHA/Alginate showed similar morphology to the well-known alginate microspheres (Alginate) and both of them possessed a great in vitro bioactivity. Compared with the control Alginate, the SrHA/Alginate enhanced MC3T3-E1 cell proliferation and ALP activity by releasing osteoinductive and osteogenic Sr ions. Furthermore, vancomycin was used as a model drug to investigate the drug release behaviors of the SrHA/Alginate, Alginate and SrHA. The results suggested that the SrHA/Alginate had a highest drug-loading efficiency and best controlled drug release properties. Additionally, the SrHA/Alginate was demonstrated to be pH-sensitive as well. The increase of the pH value in phosphate buffer solution (PBS) accelerated the vancomycin release. Accordingly, the multifunctional SrHA/Alginate can be applied in the field of bioactive drug carriers and bone filling materials. PMID:26952484

  8. Porous nano-hydroxyapatite/collagen scaffold containing drug-loaded ADM-PLGA microspheres for bone cancer treatment.

    PubMed

    Rong, Zi-Jie; Yang, Lian-Jun; Cai, Bao-Ta; Zhu, Li-Xin; Cao, Yan-Lin; Wu, Guo-Feng; Zhang, Zan-Jie

    2016-05-01

    To develop adriamycin (ADM)-encapsulated poly(lactic-co-glycolic acid) (PLGA) nanoparticles in a porous nano-hydroxyapatite/collagen scaffold (ADM-PLGA-NHAC). To provide novel strategies for future treatment of osteosarcoma, the properties of the scaffold, including its in vitro extended-release properties, the inhibition effects of ADM-PLGA-NHAC on the osteosarcoma MG63 cells, and its bone repair capacity, were investigated in vivo and in vitro. The PLGA copolymer was utilized as a drug carrier to deliver ADM-PLGA nanoparticles (ADM-PLGA-NP). Porous nano-hydroxyapatite and collagen were used to materials to produce the porous nano-hydroxyapatite/collagen scaffold (NHAC), into which the ADM-PLGA-NP was loaded. The performance of the drug-carrying scaffold was assessed using multiple techniques, including scanning electron microscopy and in vitro extended release. The antineoplastic activities of scaffold extracts on the human osteosarcoma MG63 cell line were evaluated in vitro using the cell counting kit-8 (CCK8) method and live-dead cell staining. The bone repair ability of the scaffold was assessed based on the establishment of a femoral condyle defect model in rabbits. ADM-PLGA-NHAC and NHAC were implanted into the rat muscle bag for immune response experiments. A tumor-bearing nude mice model was created, and the TUNEL and HE staining results were observed under optical microscopy to evaluate the antineoplastic activity and toxic side effects of the scaffold. The composite scaffold demonstrated extraordinary extended-release properties, and its extracts also exhibited significant inhibition of the growth of osteosarcoma MG63 cells. In the bone repair experiment, no significant difference was observed between ADM-PLGA-NHAC and NHAC by itself. In the immune response experiments, ADM-PLGA-NHAC exhibited remarkable biocompatibility. The in vivo antitumor experiment revealed that the implantation of ADM-PLGA-NHAC in the tumor resulted in a improved antineoplastic

  9. Treatment of Staphylococcus aureus-induced chronic osteomyelitis with bone-like hydroxyapatite/poly amino acid loaded with rifapentine microspheres

    PubMed Central

    Yan, Ling; Jiang, Dian-Ming; Cao, Zhi-Dong; Wu, Jun; Wang, Xin; Wang, Zheng-Long; Li, Ya-Jun; Yi, Yong-Fen

    2015-01-01

    Purpose The purpose of this study was to investigate the curative effect of bone-like hydroxyapatite/poly amino acid (BHA/PAA) as a carrier for poly(lactic-co-glycolic acid)-coated rifapentine microsphere (RPM) in the treatment of rabbit chronic osteomyelitis induced by Staphylococcus aureus. Methods RPM was prepared through an oil-in-water emulsion solvent evaporation method, and RPM was combined with BHA/PAA to obtain drug-loaded, slow-releasing materials. Twenty-six New Zealand white rabbits were induced to establish the animal model of chronic osteomyelitis. After debridement, the animals were randomly divided into three groups (n=8): the experimental group (with RPM-loaded BHA/PAA), the control group (with BHA/PAA), and the blank group. The RPM-loaded BHA/PAA was evaluated for antibacterial activity, dynamics of drug release, and osteogenic ability through in vitro and in vivo experiments. Results In vitro, RPM-loaded BHA/PAA released the antibiotics slowly, inhibiting the bacterial growth of S. aureus for up to 5 weeks. In vivo, at week 4, the bacterial colony count was significantly lower in the experimental group than in the control and blank groups (P<0.01). At week 12, the chronic osteomyelitis was cured and the bone defect was repaired in the experimental group, whereas the infection and bone defect persisted in the control and blank groups. Conclusion In vitro and in vivo experiments demonstrated that RPM-loaded BHA/PAA effectively cured S. aureus-induced chronic osteomyelitis. Therefore, BHA/PAA has potential value as a slow-releasing material in clinical setting. Further investigation is needed to determine the optimal dosage for loading rifapentine. PMID:26213463

  10. Histomorphometric evaluation of strontium-containing nanostructured hydroxyapatite as bone substitute in sheep.

    PubMed

    Machado, Callinca Paolla Gomes; Sartoretto, Suelen Cristina; Alves, Adriana Terezinha Neves Novellino; Lima, Inayá Barbosa Correa; Rossi, Alexandre Malta; Granjeiro, José Mauro; Calasans-Maia, Mônica Diuana

    2016-01-01

    The aim of this study is to evaluate the biocompatibility and osteoconductivity in surgical defects of sheep tibias filled with 1% strontium-containing nanostructured hydroxyapatite microspheres (SrHA), stoichiometric hydroxyapatite without strontium microspheres (HA), or blood clots. Santa Ines sheep were subjected to three perforations on the medial side of the left tibia. The biomaterials were characterized by X-ray Diffraction (XRD) and Fourier Transform Infrared (FTIR) before implantation and by X-Ray Microfluorescence (µFRX) and Scanning Electron Microscopy (SEM) after sheep tibias implantation. Surgical defects were filled with blood clots (control), SrHA (Group 1) or HA (Group 2). After 30 days, 5-µm bone blocks were obtained for histological evaluation, and the blocks obtained from 1 animal were embedded in methylmethacrylate for undecalcified sections. Mononuclear inflammatory infiltrate remained mild in all experimental groups. Giant cells were observed surrounding biomaterials particles of both groups and areas of bone formation were detected in close contact with biomaterials. All groups showed newly formed bone from the periphery to the center of the defects, which the control, HA and SrHA presented 36.4% (± 21.8), 31.2% (± 14.7) and 26.2% (± 12.9) of newly formed bone density, respectively, not presenting statistical differences. In addition, the connective tissue density did not show any significant between groups. The SrHA showing a higher volume density of biomaterial (51.2 ± 14.1) present in the defect compared to HA (32.6 ± 8.5) after 30 days (p = 0.03). Microspheres containing 1% SrHA or HA can be considered biocompatible, have osteoconductive properties and may be useful biomaterials for clinical applications. PMID:27191738

  11. Optical and biological properties of transparent nanocrystalline hydroxyapatite obtained through spark plasma sintering.

    PubMed

    Li, Zhong; Thompson, Brianna C; Dong, Zhili; Khor, Khiam Aik

    2016-12-01

    Transparent bioceramics have attracted a large amount of research interest as they facilitate direct observation of biointerfacial reactions. Thus far, attempts to achieve transparent hydroxyapatite have been focused on augmenting the sintering pressure and/or extending the sintering duration. This study aims at fabricating transparent HA using a direct and fast spark plasma sintering process with appropriate starting powder and moderate sintering pressure. Three types of raw powder, namely micro-spheres, nano-rods and nano-spheres, were sintered to investigate the optical and biological properties of the compacted pellets. It was found that in terms of transparency, the micro-sphere pellet sintered at 1000°C stood out with an in-line transmittance as high as 84% achieved at 1300nm for a 2mm thick sample. In addition, pellets fabricated from micro-spheres demonstrated the highest cell viability in in vitro biological tests with L929 cells. Living cells cultured on a transparent micro-sphere pellet could be directly and clearly observed by light microscopy. It is thus concluded that the micro-sphere powder is the most desirable raw material to manufacture transparent hydroxyapatite because it could enable dense pellets with notably high transparency and outstanding in vitro biocompatibility to be readily obtained. PMID:27612791

  12. 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

    2015-08-01

    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. PMID:26066071

  13. Scanning Small- and Wide-Angle X-ray Scattering Microscopy Selectively Probes HA Content in Gelatin/Hydroxyapatite Scaffolds for Osteochondral Defect Repair.

    PubMed

    Altamura, Davide; Pastore, Stella G; Raucci, Maria G; Siliqi, Dritan; De Pascalis, Fabio; Nacucchi, Michele; Ambrosio, Luigi; Giannini, Cinzia

    2016-04-01

    This study is aimed at investigating the structure of a scaffold made of bovine gelatin and hydroxyapatite for bone tissue engineering purposes. In particular, the detailed characterization of such a material has a great relevance because of its application in the healing process of the osteochondral defect that consists of a damage of cartilage and injury of the adjacent subchondral bone, significantly compromising millions of patient's quality of life. Two different techniques exploiting X-ray radiation, with table-top setups, are used: microtomography (micro-CT) and microdiffraction. Micro-CT characterizes the microstructure in the three dimensions at the micrometer scale spatial resolution, whereas microdiffraction provides combined structural/morphological information at the atomic and nanoscale, in two dimensional microscopy images with a hundred micrometer spatial resolution. The combination of these two techniques allowed an appropriate structural characterization for the purpose of validating the engineering approach used for the realization of the hydroxyapatite gradient across the scaffold, with properties close to the natural model. PMID:27020229

  14. Polymeric microspheres

    DOEpatents

    Walt, David R.; Mandal, Tarun K.; Fleming, Michael S.

    2004-04-13

    The invention features core-shell microsphere compositions, hollow polymeric microspheres, and methods for making the microspheres. The microspheres are characterized as having a polymeric shell with consistent shell thickness.

  15. 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

  16. Production and characterization of HA and SiHA coatings.

    PubMed

    Tang, Qian; Brooks, Roger; Rushton, Neil; Best, Serena

    2010-01-01

    Plasma sprayed hydroxyapatite (HA) coatings on metallic prostheses have been used clinically in dentistry and orthopedics since the mid 1980s. The coating properties are dependent on the spraying parameters. Since silicon-substituted hydroxyapatite (SiHA) has been shown to offer improved bioactivity over phase pure HA, SiHA coatings have the potential for enhanced performance in clinical application. In this study, phase pure HA and 0.8 wt% SiHA powders were synthesized with similar particle size distribution and morphology. The powders were plasma sprayed onto Ti-6Al-4V substrates at 37 kW and 40 kW plasma gun input power respectively. Four kinds of samples were prepared, HAC 37, HAC 40, SiHAC 37 and SiHAC 40. Materials characterization showed that the coatings were of relatively high phase purity. In vitro cell culture demonstrated that human osteoblast cells grew well on all samples, with the highest cell growth observed on SiHA coatings produced under the lower plasma gun input power. PMID:19672562

  17. Osteogenic effect of controlled released rhBMP-2 in 3D printed porous hydroxyapatite scaffold.

    PubMed

    Wang, Hai; Wu, Gui; Zhang, Jing; Zhou, Kui; Yin, Bo; Su, Xinlin; Qiu, Guixing; Yang, Guang; Zhang, Xianglin; Zhou, Gang; Wu, Zhihong

    2016-05-01

    Recently, 3D printing as effective technology has been highlighted in the biomedical field. Previously, a porous hydroxyapatite (HA) scaffold with the biocompatibility and osteoconductivity has been developed by this method. However, its osteoinductivity is limited. The main purpose of this study was to improve it by the introduction of recombinant human bone morphogenetic protein-2 (rhBMP-2). This scaffold was developed by coating rhBMP-2-delivery microspheres with collagen. These synthesized scaffolds were characterized by Scanning Electron Microscopy (SEM), a delivery test in vitro, cell culture, and the experiments in vivo by a Micro-computed tomography (μCT) scan and histological evaluation of VanGieson staining. SEM results indicated the surface of scaffolds were more fit for the adhesion of hMSCs to coat collagen/rhBMP-2 microspheres. Biphasic release of rhBMP-2 could continue for more than 21 days, and keep its osteoinductivity to induce osteogenic differentiation of hMSCs in vitro. In addition, the experiments in vivo showed that the scaffold had a good bone regeneration capacity. These findings demonstrate that the HA/Collagen/Chitosan Microspheres system can simultaneously achieve localized long-term controlled release of rhBMP-2 and bone regeneration, which provides a promising route for improving the treatment of bone defects. PMID:26896655

  18. Crystallization of modified hydroxyapatite on titanium implants

    NASA Astrophysics Data System (ADS)

    Golovanova, O. A.; Izmailov, R. R.; Ghyngazov, S. A.; Zaits, A. V.

    2016-02-01

    Carbonated-hydroxyapatite (CHA) and Si-hydroxyapatite (Si-HA) precipitation have been synthesized from the model bioliquid solutions (synovial fluid and SBF). It is found that all the samples synthesized from the model solutions are single-phase and represent hydroxyapatite. The crystallization of the modified hydroxyapatite on alloys of different composition, roughness and subjected to different treatment techniques was investigated. Irradiation of the titanium substrates with the deposited biomimetic coating can facilitate further growth of the crystal and regeneration of the surface.

  19. Microsphere-based selective laser sintering for building macroporous bone scaffolds with controlled microstructure and excellent biocompatibility.

    PubMed

    Du, Yingying; Liu, Haoming; Shuang, Jiaqi; Wang, Jianglin; Ma, Jun; Zhang, Shengmin

    2015-11-01

    Fabrication of bulk biomaterials with controlled structures and excellent properties is increasingly important in tissue engineering, but remains a major challenge in the current stage. Herein we used selective laser sintering (SLS) to construct a series of three-dimensional (3D) bone scaffolds with uniform multi-scaled porosity, moderate mechanical properties as well as good biocompatibility. As starting architectural units for SLS, the pure microspheres of polycaprolactone (PCL) and the composite microspheres of PCL and hydroxyapatite (HA) were firstly synthesized via a modified solvent evaporation method, respectively. Our findings showed that the as-prepared microspheres exhibited the uniform size and monodispersity. Moreover, the microsphere-based 3D scaffolds generated by SLS technique showed a multi-scaled porous structure, and adequate mechanical features. Both in vitro and in vivo evaluations further demonstrated that the resultant SLS-derived scaffolds can not only manipulate multiple stem cell behaviors including promoting cell adhesion, supporting cell proliferation and inducing cell differentiation in vitro, but also showed an excellent histocompatibility and induced the vascularization of newly formed tissue in vivo. Consequently, our current study suggests a feasible and effective protocol for fabricating new biomimetic bone biomaterials via SLS technique, also paves a new way for other bulk biomaterials. PMID:26241919

  20. Hydroxyapatite in Physiological Environment

    NASA Astrophysics Data System (ADS)

    Slepko, Alexander; Demkov, Alexander A.

    2011-03-01

    A carbonated form of hydroxyapatite (HA) [ Ca 10 (PO4)6 (OH)2 ] is one of the most abundant materials in mammal bone. It crystallizes within the spaces between tropocollagen protein chains in an aqueous solution and strengthens the bone tissue. An emerging application of synthetic HA is bone repair and replacement. Bulk electronic and chemical properties of HA were studied theoretically recently. However, the absorption of H2 O molecules and amino acids of the tropocollagen chains at HA surfaces remains an area of active research. Using density functional theory we analyze the electronic properties and surface energetics of HA for different orientations and terminations and generate a theoretical surface phase diagram of HA. The reactivity of these surface models is analyzed using the frontier orbital approach. We find two dominant surfaces which are most stable over the widest chemical range. However, we expect them to show little surface reactivity. Using a HA slab with a highly reactive surface we build atomistic models of HA covered with up to one monolayer of water and analyze interactions between this surface and the water molecules.

  1. Dissolution studies of hydroxyapatite and glass-reinforced hydroxyapatite ceramics

    SciTech Connect

    Queiroz, A.C.; Santos, J.D.; Monteiro, F.J.; Prado da Silva, M.H

    2003-03-15

    In the continuous agitation assays, glass-reinforced hydroxyapatite (GR-HA) was shown to form a calcium phosphate (CaP) layer, but hydroxyapatite (HA) only formed dispersed precipitates. The formation of this layer was first detected on the GR-HA with a 7.5% glass addition (7.5 GR-HA) after only 3 days of immersion in simulated body fluid (SBF). The time required for layer formation decreased as the amount of glass added to the HA increased. The dissolution rate of the materials followed a similar pattern, i.e. the dissolution rate for GR-HA was higher than for HA, and increased with the addition of glass. The immersion of 7.5 GR-HA in water showed almost linear dissolution kinetics over the immersion periods (3, 7, 15, 30 and 60 days). The concentration of calcium ions in solution and the scanning electron microscopy (SEM) analysis of the 7.5 GR-HA specimens immersed in water and in SBF revealed a clear competition between the material dissolution and the precipitation of a CaP phase. Fourier transformed infrared spectroscopy with alternated total reflectance (FTIR-ATR) analysis indicated that the CaP phase that formed during longer immersion times (30 and 60 days) could be a carbonate-substituted CaP precipitate. As expected from previous work, the GR-HA behavior in terms of its in vitro bioactivity is higher than HA because a homogeneous CaP layer is formed and the precipitation occurs faster. From the dissolution test and in accordance with the chemical composition of the samples, GR-HA was more soluble than HA.

  2. Polyacrolein microspheres

    NASA Technical Reports Server (NTRS)

    Rembaum, Alan (Inventor)

    1986-01-01

    Microspheres of acrolein homopolymers and copolymer with hydrophillic comonomers such as methacrylic acid and/or hydroxyethylmethacrylate are prepared by cobalt gamma irradiation of dilute aqueous solutions of the monomers in presence of suspending agents, especially alkyl sulfates such as sodium dodecyl sulfate. Amine or hydroxyl modification is achieved by forming adducts with diamines or alkanol amines. Carboxyl modification is effected by oxidation with peroxides. Pharmaceuticals or other aldehyde reactive materials can be coupled to the microspheres. The microspheres directly form antibody adducts without agglomeration.

  3. Polyacrolein microspheres

    NASA Technical Reports Server (NTRS)

    Rembaum, Alan (Inventor)

    1983-01-01

    Microspheres of acrolein homopolymers and co-polymer with hydrophillic comonomers such as methacrylic acid and/or hydroxyethylmethacrylate are prepared by cobalt gamma irradiation of dilute aqueous solutions of the monomers in presence of suspending agents, especially alkyl sulfates such as sodium dodecyl sulfate. Amine or hydroxyl modification is achieved by forming adducts with diamines or alkanol amines. Carboxyl modification is effected by oxidation with peroxides. Pharmaceuticals or other aldehyde reactive materials can be coupled to the microspheres. The microspheres directly form antibody adducts without agglomeration.

  4. Polyacrolein microspheres

    NASA Technical Reports Server (NTRS)

    Rembaum, Alan (Inventor)

    1987-01-01

    Microspheres of acrolein homopolymers and copolymer with hydrophillic comonomers such as methacrylic acid and/or hydroxyethylmethacrylate are prepared by cobalt gamma irradiation of dilute aqueous solutions of the monomers in presence of suspending agents, especially alkyl sulfates such as sodium dodecyl sulfate. Amine or hydroxyl modification is achieved by forming adducts with diamines or alkanol amines. Carboxyl modification is effected by oxidation with peroxides. Pharmaceuticals or other aldehyde reactive materials can be coupled to the microspheres. The microspheres directly form antibody adducts without agglomeration.

  5. 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

  6. 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.

  7. Mechanical properties of hydroxyapatite/mica composite.

    PubMed

    Nordström, E G; Herø, H; Jørgensen, R B

    1994-01-01

    Bend specimens of the inorganic synthetic materials hydroxyapatite (HA) and a composite of hydroxyapatite/muscovite mica have been prepared and tested mechanically. Sintering followed by hot isostatic pressing (HIP) without encapsulation gave an increased strength for HA alone, but no significant increase in strength compared with sintering alone for HA/mica composites. The bend strength of the HA/mica composite was inferior to that of HA alone, the reason being inadequate bonding between HA and mica. HIP in glass capsules and an increased cold compaction pressure tended to improve the bend strength of the composite. Corrosion in tris for 7 d did not affect the bend strength of the investigated materials significantly. PMID:7950878

  8. Magnesium incorporation into hydroxyapatite.

    PubMed

    Laurencin, Danielle; Almora-Barrios, Neyvis; de Leeuw, Nora H; Gervais, Christel; Bonhomme, Christian; Mauri, Francesco; Chrzanowski, Wojciech; Knowles, Jonathan C; Newport, Robert J; Wong, Alan; Gan, Zhehong; Smith, Mark E

    2011-03-01

    The incorporation of Mg in hydroxyapatite (HA) was investigated using multinuclear solid state NMR, X-ray absorption spectroscopy (XAS) and computational modeling. High magnetic field (43)Ca solid state NMR and Ca K-edge XAS studies of a ∼10% Mg-substituted HA were performed, bringing direct evidence of the preferential substitution of Mg in the Ca(II) position. (1)H and (31)P solid state NMR show that the environment of the anions is disordered in this substituted apatite phase. Both Density Functional Theory (DFT) and interatomic potential computations of Mg-substituted HA structures are in agreement with these observations. Indeed, the incorporation of low levels of Mg in the Ca(II) site is found to be more favourable energetically, and the NMR parameters calculated from these optimized structures are consistent with the experimental data. Calculations provide direct insight in the structural modifications of the HA lattice, due to the strong contraction of the M⋯O distances around Mg. Finally, extensive interatomic potential calculations also suggest that a local clustering of Mg within the HA lattice is likely to occur. Such structural characterizations of Mg environments in apatites will favour a better understanding of the biological role of this cation. PMID:21144581

  9. Chemical characterization of silicon-substituted hydroxyapatite.

    PubMed

    Gibson, I R; Best, S M; Bonfield, W

    1999-03-15

    Bioceramic specimens have been prepared by incorporating a small amount of silicon (0.4 wt %) into the structure of hydroxyapatite [Ca10(PO4)6(OH)2, HA] via an aqueous precipitation reaction to produce a silicon-substituted hydroxyapatite (Si-HA). The results of chemical analysis confirmed the proposed substitution of the silicon (or silicate) ion for the phosphorus (or phosphate) ion in hydroxyapatite. The Si-HA was produced by first preparing a silicon-substituted apatite (Si-Ap) by a precipitation process. A single-phase Si-HA was obtained by heating/calcining the as-prepared Si-Ap to temperatures above 700 degrees C; no secondary phases, such as tricalcium phosphate (TCP), tetracalcium phosphate (TeCP), or calcium oxide (CaO), were observed by X-ray diffraction analysis. Although the X-ray diffraction patterns of Si-HA and stoichiometric HA appeared to be identical, refinement of the diffraction data revealed some small structural differences between the two materials. The silicon substitution in the HA lattice resulted in a small decrease in the a axis and an increase in the c axis of the unit cell. This substitution also caused a decrease in the number of hydroxyl (OH) groups in the unit cell, which was expected from the proposed substitution mechanism. The incorporation of silicon in the HA lattice resulted in an increase in the distortion of the PO4 tetrahedra, indicated by an increase in the distortion index. Analysis of the Si-HA by Fourier transform infrared (FTIR) spectroscopy indicated that although the amount of silicon incorporated into the HA lattice was small, silicon substitution appeared to affect the FTIR spectra of HA, in particular the P-O vibrational bands. The results demonstrate that phase-pure silicon-substituted hydroxyapatite may be prepared using a simple precipitation technique. PMID:10397946

  10. Cements from nanocrystalline hydroxyapatite.

    PubMed

    Barralet, J E; Lilley, K J; Grover, L M; Farrar, D F; Ansell, C; Gbureck, U

    2004-04-01

    Calcium phosphate cements are used as bone substitute materials because they may be moulded to fill a void or defect in bone and are osteoconductive. Although apatite cements are stronger than brushite cements, they are potentially less resorbable in vivo. Brushite cements are three-component systems whereby phosphate ions and water react with a soluble calcium phosphate to form brushite (CaHPO4 x 2H2O). Previously reported brushite cement formulations set following the mixture of a calcium phosphate, such as beta-tricalcium phosphate (beta-TCP), with an acidic component such as H3PO4 or monocalcium phosphate monohydrate (MCPM). Due to its low solubility, hydroxyapatite (HA) is yet to be reported as a reactive component in calcium phosphate cement systems. Here we report a new cement system setting to form a matrix consisting predominantly of brushite following the mixture of phosphoric acid with nanocrystalline HA. As a result of the relative ease with which ionic substitutions may be made in apatite this route may offer a novel way to control cement composition or setting characteristics. Since kinetic solubility is dependent on particle size and precipitation temperature is known to affect precipitated HA crystal size, the phase composition and mechanical properties of cements made from HA precipitated at temperatures between 4 and 60 degrees C were investigated. PMID:15332608

  11. Osteogenesis and Trophic Factor Secretion are Influenced by the Composition of Hydroxyapatite/Poly(Lactide-Co-Glycolide) Composite Scaffolds

    PubMed Central

    He, Jiawei; Genetos, Damian C.

    2010-01-01

    The use of composite biomaterials for bone repair capitalizes on the beneficial aspects of individual materials while tailoring the mechanical properties of the composite. We hypothesized that substrate composition would modulate the osteogenic response and secretion of potent trophic factors by human mesenchymal stem cells (hMSCs). Composite scaffolds were prepared by combining nanosized hydroxyapatite (HA) and microspheres formed of poly(lactic-co-glycolic acid) (PLG) at varying ratios between 0:1 and 5:1. Scaffolds were seeded with hMSCs for culture in osteogenic conditions or subcutaneous implantation into nude rats. Compressive moduli increased with HA content in a near-linear fashion. The osteogenic differentiation of hMSCs increased in a dose-dependent manner as determined by alkaline phosphatase activity and osteopontin secretion after 4 weeks of culture. Further, endogenous secretion of vascular endothelial growth factor was sustained at significantly higher levels over 28 days for hMSCs seeded in 2.5:1 and 5:1 HA:PLG scaffolds. Eight weeks after implantation, scaffolds with higher HA:PLG ratios exhibited greater vascularization and more mineralized tissue. These data demonstrate that the mechanical properties, osteogenic differentiation, as well as the timing and duration of trophic factor secretion by hMSCs can be tailored through controlling the composition of the polymer–bioceramic composite. PMID:19642853

  12. Femur bone repair in ovariectomized rats under the local action of alendronate, hydroxyapatite and the association of alendronate and hydroxyapatite

    PubMed Central

    Canettieri, Antonio Carlos Victor; Colombo, Carlos Eduardo Dias; Chin, Chung Man; Faig-Leite, Horácio

    2009-01-01

    An evaluation was made of the local action of alendronate sodium (A), hydroxyapatite (HA) and the association of both substances (A + HA), in different molar concentrations, on the femur bone repair of ovariectomized rats. Ninety-eight animals were divided into seven groups: control (C), starch (S), alendronate 1 mol (A1), alendronate 2 mols (A2), hydroxyapatite 1 mol (HA1), hydroxyapatite 2 mols (HA2) and the association of alendronate + hydroxyapatite (A + HA). Rats weighing about 250 g were ovariectomized and 2.5-mm diameter bone defects were made on the left femur 30 days later. Each experimental group had defects filled with appropriate material, except for group C (control). The animals were killed 7 and 21 days after surgery. Histological, histomorphometric and statistical analyses of bone neoformation in the bone defect site were performed. From the histological standpoint, the major differences occurred after 21 days. All specimens in groups C, S, HA1 and HA2 presented linear closure of the bone defect, and most animals in groups A1, A2 and A + HA showed no bone neoformation in the central area of the defect. No statistically significant difference was found among the experimental groups after 7 days; after 21 days, group HA2 presented the highest amount of neoformed bone. There was no significant difference among groups A1, A2 and A + HA in the two study periods. It was concluded that alendronate, either isolated or in association with hydroxyapatite, had an adverse effect on bone repair in this experimental model. Moreover, the hydroxyapatite used here proved to be biocompatible and osteoconductive, with group HA2 showing the best results. PMID:19765106

  13. Microradiographic microsphere manipulator

    DOEpatents

    Singleton, Russell M.

    1980-01-01

    A method and apparatus for radiographic characterization of small hollow spherical members (microspheres), constructed of either optically transparent or opaque materials. The apparatus involves a microsphere manipulator which holds a batch of microspheres between two parallel thin plastic films for contact microradiographic characterization or projection microradiography thereof. One plastic film is translated to relative to and parallel to the other to roll the microspheres through any desired angle to allow different views of the microspheres.

  14. Microradiographic microsphere manipulator

    DOEpatents

    Singleton, R.M.

    A method and apparatus is disclosed for radiographic characterization of small hollow spherical members (microspheres), constructed of either optically transparent or opaque materials. The apparatus involves a microsphere manipulator which holds a batch of microspheres between two parallel thin plastic films for contact microradiographic characterization or projection microradiography thereof. One plastic film is translated relative to and parallel to the other to roll the microspheres through any desired angle to allow different views of the microspheres.

  15. Dissolution of human teeth-derived hydroxyapatite.

    PubMed

    Seo, Dong Seok; Lee, Jong Kook

    2008-01-01

    We have been interested in human teeth which consist of hydroxyapatite (HA), but do not degrade for a long time. In order to overcome dissolution and mechanical degradation of man-made HA, biologically derived hydroxyapatite (BHA) ceramics were prepared from human teeth and their dissolving behavior was investigated in distilled water for 3-14 days and compared with an artificial HA made of synthetic HA powder. BHA ceramics were prepared by calcining freshly extracted human teeth at 900 degrees C and followed by sintering at 1200 degrees C for 2 h. All detectable peaks in the artificial HA are identical to HA lattice planes, whereas BHA consisted of a mixture of HA and beta-tricalcium phosphate (TCP). Although the artificial HA was expected to be stable in water, the surface dissolution initiated at grain boundaries followed by generated many separated grains and their associated pores. On the other hand, BHA showed that definite grains considered as beta-TCP were predominantly dissolved and the grains were separated from the matrix leaving pores. In the mean time, the rest region, mainly consisting of HA, did not show any evidence of dissolution. It indicates that BHA showed rather stable grain boundaries and lack of excessive dissolution in liquid environment. PMID:17943445

  16. Metabolic microspheres

    NASA Astrophysics Data System (ADS)

    Fox, Sidney W.

    1980-08-01

    A systematic review of catalytic activities in thermal proteinoids and microspheres aggregated therefrom yields some new inferences on the origins and evolution of metabolism. Experiments suggest that, instead of being inert, protocells were already biochemically and cytophysically competent. The emergence and refinement of metabolism ab initio is thus partly traced conceptually. When the principle of molecular self-instruction, as of amino acids in peptide synthesis, is taken into account as a concomitant of natural selection, an expanded theory of organismic evolution, including saltations, emerges.

  17. Hybrid microspheres

    NASA Technical Reports Server (NTRS)

    Rembaum, Alan (Inventor); Yen, Richard C. K. (Inventor)

    1985-01-01

    Substrates, particularly inert synthetic organic resin beads (10) or sheet (12) such as polystyrene are coated with a covalently bound layer (24) of polyacrolein by irradiation a solution (14) of acrolein or other aldehyde with high intensity radiation. Individual microspheres (22) are formed which attach to the surface to form the aldehyde containing layer (24). The aldehyde groups can be converted to other functional groups by reaction with materials such as hydroxylamine. Adducts of proteins such as antibodies or enzymes can be formed by direct reaction with the surface aldehyde groups.

  18. Monoclonal antibody purification with hydroxyapatite.

    PubMed

    Gagnon, Pete

    2009-06-01

    Hydroxyapatite (HA) has been used for IgG purification since its introduction in the 1950s. Applications expanded to include IgA and IgM in the 1980s, along with elucidation of its primary binding mechanisms and the development of ceramic HA media. With the advent of recombinant monoclonal antibodies, HA was demonstrated to be effective for removal of antibody aggregates, as well as host cell proteins and leached protein A. HA's inherent abilities have been enhanced by the development of elution strategies that permit differential control of its primary binding mechanisms: calcium metal affinity and phosphoryl cation exchange. These strategies support reduction of antibody aggregate content from greater than 60% to less than 0.1%, in conjunction with enhanced removal of DNA, endotoxin, and virus. HA also has a history of discriminating various immunological constructs on the basis of differences in their variable regions, or discriminating Fab fragments from Fc contaminants in papain digests of purified monoclonal IgG. Continuing development of novel elution strategies, alternative forms of HA, and application of robotic high throughput screening systems promise to expand HA's utility in the field. PMID:19491046

  19. Preparation of irregular mesoporous hydroxyapatite

    SciTech Connect

    Wang Hualin Zhai Linfeng; Li Yanhong; Shi Tiejun

    2008-06-03

    An irregular mesoporous hydroxyapatite (meso-HA), Ca{sub 10}(PO{sub 4}){sub 6}(OH){sub 2}, is successfully prepared from Ca(NO{sub 3}){sub 2}.4H{sub 2}O and NH{sub 4}H{sub 2}PO{sub 4} using surfactant cetyltrimethyl ammonium bromide (CTAB) as template. Fourier transform infrared spectroscopy (FTIR) and differential scanning calorimetry (DSC) results reveal that the positive head of CTAB is assembled on the surface precipitated HA and much NH{sub 4}{sup +} is enclosed in precipitated HA before calcination. Field scanning electron microscope (FSEM) reveals that there exist many interconnected pores throughout the HA reticular skeleton. Nitrogen adsorption-desorption experiment exhibits a mesoporous material type IV curve, and pore size distribution calculated from the desorption branch of the isotherms based on Barrett-Joyner-Halenda (BJH) model shows that most pores throughout the HA reticular skeleton are sized at about 40 nm, but the pores are not uniform on the whole, owning to decomposition of the 'organic' CTAB templating structures and ammonium salt enclosed in the precipitated HA. The specific surface area of irregular meso-HA is calculated to be 37.6 m{sup 2}/g according to the Brunauer-Emmett-Teller (BET) equation. Moreover, after polylactic acid/meso-HA (PLA/meso-HA) composites degraded 12 weeks in normal saline at 37 deg. C, the interconnected pores throughout the HA skeleton were enlarged and sized in micron degree, which resemble trabecular bone structure very much.

  20. Fabrication and characterization of needle-like nano-HA and HA/MWNT composites.

    PubMed

    Meng, Y H; Tang, Chak Yin; Tsui, Chi Pong; Chen, Da Zhu

    2008-01-01

    Hydroxyapatite (HA) ceramic has been used in tissue engineering and orthopedics for its good biocompatibility and osteoconductivity. However, its clinical applications are usually limited by the low strength and brittleness. The objective of this research was to develop a new kind of HA composites in which multi-wall carbon nanotubes (MWNTs) were introduced to the HA ceramic matrix to improve the mechanical properties of the resulting composites. A simple chemical wet method was applied to synthesize the HA ceramic particles with the aid of surfactant and ultrasonication technique at normal atmospheric pressure. The morphology and microstructure of the synthesized HA were characterized by XRD and TEM as a function of treatment time. The results showed that the synthesized HA particles are needle-like with a length of 80-160 nm along the (211) direction and an aspect ratio of 5-15. MWNTs were treated with a mixture of nitric acid and sulfuric acid. The HA/MWNT composites were prepared by solution blending. The composites were sintered using a hot-press method. The mechanical properties of the HA/MWNT composites with different volume percentages of MWNTs were examined. The fracture toughness and flexural strength were improved by 50% and 28% separately when the volume percentage of MWNTs reached 7%. PMID:17577639

  1. Pitch carbon microsphere composite

    NASA Technical Reports Server (NTRS)

    Price, H. L.; Nelson, J. B.

    1977-01-01

    Petroleum pitch carbon microspheres were prepared by flash heating emulsified pitch and carbonizing the resulting microspheres in an inert atmosphere. Microsphere composites were obtained from a mixture of microspheres and tetraester precursor pyrrone powder. Scanning electron micrographs of the composite showed that it was an aggregate of microspheres bonded together by the pyrrone at the sphere contact points, with voids in and among the microspheres. Physical, thermal, and sorption properties of the composite are described. Composite applications could include use as a honeycomb filler in elevated-temperature load-bearing sandwich boards or in patient-treatment tables for radiation treatment of tumors.

  2. Influence of Barium Hexaferrite on Magnetic Properties of Hydroxyapatite Ceramics.

    PubMed

    Jarupoom, P; Jaita, P

    2015-11-01

    Hydroxyapatite (HA) powders was derived from natural bovine bone by sequence of thermal processes. The barium hexaferrite (BF) find magnetic powders were added into HA powders in ratio of 1-3 vol.%. The HA-BF ceramics were prepared by a solid state reaction method and sintered at 1250 degrees C for 2 h. Effects of BF additive on structural, physical and magnetic properties of HA ceramics were investigated. X-ray diffraction revealed that all HA-BF samples showed a main phase of high purity hydroxyapatite [Ca10(PO4)6(OH)2] with calcium and phosphate molar ratio of 1.67. The addition of BF into HA inhibited grain growth and caused an improvement of mechanical properties. The M-H hysteresis loops also showed an improvement in magnetic behavior for higher content of BF. Moreover, in vitro bioactivity test indicated that the 2-3 vol.% sample may be suitable for biological applications. PMID:26726671

  3. Characterisation of Suspension Precipitated Nanocrystalline Hydroxyapatite Powders

    NASA Astrophysics Data System (ADS)

    Mallik, P. K.; Swain, P. K.; Patnaik, S. C.

    2016-02-01

    Hydroxyapatite (HA) is a well-known biomaterial for coating on femoral implants, filling of dental cavity and scaffold for tissue replacement. Hydroxyapatite possess limited load bearing capacity due to their brittleness. In this paper, the synthesis of nanocrystalline hydroxyapatite powders was prepared by dissolving calcium oxide in phosphoric acid, followed by addition of ammonia liquor in a beaker. The prepared solution was stirred by using magnetic stirrer operated at temperature of 80°C for an hour. This leads to the formation of hydroxyapatite precipitate. The precipitate was dried in oven for overnight at 100°C. The dried agglomerated precipitate was calcined at 800°C in conventional furnace for an hour. The influence of calcium oxide concentration and pH on the resulting precipitates was studied using BET, XRD and SEM. As result, a well-defined sub-rounded morphology of powders size of ∼41 nm was obtained with a salt concentration of 0.02 M. Finally, it can be concluded that small changes in the reaction conditions led to large changes in final size, shape and degree of aggregation of the hydroxyapatite particles.

  4. microsphere assemblies

    NASA Astrophysics Data System (ADS)

    Peña-Flores, Jesús I.; Palomec-Garfias, Abraham F.; Márquez-Beltrán, César; Sánchez-Mora, Enrique; Gómez-Barojas, Estela; Pérez-Rodríguez, Felipe

    2014-09-01

    The effect of Fe ion concentration on the morphological, structural, and optical properties of TiO2 films supported on silica (SiO2) opals has been studied. TiO2:Fe2O3 films were prepared by the sol-gel method in combination with a vertical dip coating procedure; precursor solutions of Ti and Fe were deposited on a monolayer of SiO2 opals previously deposited on a glass substrate by the same procedure. After the dip coating process has been carried out, the samples were thermally treated to obtain the TiO2:Fe2O3/SiO2 composites at the Fe ion concentrations of 1, 3, and 5 wt%. Scanning electron microscopy (SEM) micrographs show the formation of colloidal silica microspheres of about 50 nm diameter autoensembled in a hexagonal close-packed fashion. Although the X-ray diffractograms show no significant effect of Fe ion concentration on the crystal structure of TiO2, the μ-Raman and reflectance spectra do show that the intensity of a phonon vibration mode and the energy bandgap of TiO2 decrease as the Fe+3 ion concentration increases.

  5. 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...

  6. Adhesion behaviors of Escherichia coli on hydroxyapatite.

    PubMed

    Kamitakahara, Masanobu; Takahashi, Shohei; Yokoi, Taishi; Inoue, Chihiro; Ioku, Koji

    2016-04-01

    Optimum design of support materials for microorganisms is required for the construction of bioreactors. However, the effects of support materials on microorganisms are still unclear. In this study, we investigated the adhesion behavior of Escherichia coli (E. coli) on hydroxyapatite (HA), polyurethane (PU), poly(vinyl chloride) (PVC), and carbon (Carbon) to obtain basic knowledge for the design of support materials. The total metabolic activity and number of E. coli adhering on the samples followed the order of HA ≈ Carbon>PVC>PU. On the other hand, the water contact angle of the pellet surfaces followed the order of HAHA surface might be one of the suitable characters for the adhesion of E. coli. The results implied that HA has a potential as a support material for microorganisms used in bioreactors. PMID:26838837

  7. Development of model hydroxyapatite bone scaffolds with multiscale porosity for potential load bearing applications

    NASA Astrophysics Data System (ADS)

    Dellinger, Jennifer Gwynne

    2005-11-01

    Model hydroxyapatite (HA) bone scaffolds consisting of a latticed pattern of rods were fabricated by a solid freeform fabrication (SFF) technique based on the robotic deposition of colloidal pastes. An optimal HA paste formulation for this method was developed. Local porosity, i.e. microporosity (1--30 mum) and sintering porosity (less than 1 mum), were produced by including polymer microsphere porogens in the HA pastes and by controlling the sintering of the scaffolds. Scaffolds with and without local porosity were evaluated with and without in vitro accelerated degradation. Percent weight loss of the scaffolds and calcium and phosphorus concentrations in solution increased with degradation time. After degradation, compressive strength and modulus decreased significantly for scaffolds with local porosity, but did not change significantly for scaffolds without local porosity. The compressive strength and modulus of scaffolds without local porosity were comparable to human cortical bone and were significantly greater than the scaffolds with local porosity. Micropores in HA disks caused surface pits that increased the surface roughness as compared to non-microporous HA disks. Mouse mesenchymal stem cells extended their cell processes into these microporous pits on HA disks in vitro. ALP expression was prolonged, cell attachment strength increased, and ECM production appeared greater on microporous HA disks compared to non-microporous HA disks and tissue culture treated polystyrene controls. Scaffolds with and without microporosity were implanted in goats bones. Microporous scaffolds with rhBMP-2 increased the percent of the scaffold filled with bone tissue compared to microporous scaffolds without rhBMP-2. Lamellar bone inside scaffolds was aligned near the rods junctions whereas lamellar bone was aligned in a more random configuration away from the rod junctions. Microporous scaffolds stained darkly with toluidine blue beneath areas of contact with new bone. This

  8. Preparation of bioactive porous HA/PCL composite scaffolds

    NASA Astrophysics Data System (ADS)

    Zhao, J.; Guo, L. Y.; Yang, X. B.; Weng, J.

    2008-12-01

    Porous hydroxyapatite (HA) bioceramic scaffold has been widely attracted the attention to act as a three-dimensional (3D) template for cell adhesion, proliferation, differentiation and thus promoting bone and cartilage regeneration because of its osteoinduction. However, the porous bioceramic scaffold is fragile so that it is not suitable to be applied in clinic for bone repair or replacement. Therefore, it is significant to improve the mechanical property of porous HA bioceramics while the interconnected structure is maintained for tissue ingrowth in vivo. In the present research, a porous composite scaffold composed of HA scaffold and polycaprolactone (PCL) lining was fabricated by the method of polymer impregnating to produce HA scaffold coated with PCL lining. Subsequently, the composite scaffolds were deposited with biomimetic coating for improving the bioactivity. The HA/PCL composite scaffolds with improved mechanical property and bioactivity is expected to be a promising bone substitute in tissue engineering applications.

  9. Surface-induced changes in the conformation and glucan production of glucosyltransferase adsorbed on saliva-coated hydroxyapatite.

    PubMed

    Fears, Kenan P; Gonzalez-Begne, Mireya; Love, Corey T; Day, Delbert E; Koo, Hyun

    2015-04-28

    Glucosyltransferases (Gtfs) from S. mutans play critical roles in the development of virulent oral biofilms associated with dental caries disease. Gtfs adsorbed to the tooth surface produce glucans that promote local microbial colonization and provide an insoluble exopolysaccharides (EPS) matrix that facilitates biofilm initiation. Moreover, agents that inhibit the enzymatic activity of Gtfs in solution often have reduced or no effects on surface-adsorbed Gtfs. This study elucidated the mechanisms responsible for the differences in functionality that GtfB exhibits in solution vs surface-adsorbed. Upon adsorption to planar fused-quartz substrates, GtfB displayed a 37% loss of helices and 36% increase of β-sheets, as determined by circular dichroism (CD) spectroscopy, and surface-induced conformational changes were more severe on substrates modified with CH3- and NH2-terminated self-assembled monolayers. GtfB also underwent substantial conformation changes when adsorbing to hydroxyapatite (HA) microspheres, likely due to electrostatic interactions between negatively charged GtfB and positively charged HA crystal faces. Conformational changes were lessened when HA surfaces were coated with saliva (sHA) prior to GtfB adsorption. Furthermore, GtfB remained highly active on sHA, as determined by in situ attenuated total reflectance Fourier transform infrared (ATR-FTIR) spectroscopy, producing glucans that were structurally different than GtfB in solution and known to increase the accumulation and virulence of biofilms. Our data provide the first insight into the structural underpinnings governing Gtf conformation and enzymatic function that occur on tooth surfaces in vivo, which may lead to designing potent new inhibitors and improved strategies to combat the formation of pathogenic oral biofilms. PMID:25867796

  10. In situ deposition of hydroxyapatite on graphene nanosheets

    SciTech Connect

    Neelgund, Gururaj M.; Oki, Aderemi; Luo, Zhiping

    2013-02-15

    Graphical abstract: A facile chemical precipitation method is reported for effective in situ deposition of hydroxyapatite on graphene nanosheets. Prior to grafting of hydroxyapatite, chemically modified graphene nanosheets were obtained by the reduction of graphene oxide in presence of ethylenediamine. Display Omitted Highlights: ► It is a facile and effective method for deposition of HA on GR nanosheets. ► It avoids the use of harmful reducing agents like hydrazine, NaBH{sub 4} etc. ► GR nanosheets were produced using bio-compatible, ethylenediamine. ► The graphitic structure of synthesized GR nanosheets was high ordered. ► The ratio of Ca to P in HA was 1.64, which is close to ratio in natural bone. -- Abstract: Graphene nanosheets were effectively functionalized by in situ deposition of hydroxyapatite through a facile chemical precipitation method. Prior to grafting of hydroxyapatite, chemically modified graphene nanosheets were obtained by the reduction of graphene oxide in presence of ethylenediamine. The resulting hydroxyapatite functionalized graphene nanosheets were characterized by attenuated total reflection IR spectroscopy, X-ray diffraction, field emission scanning electron microscopy, transmission electron microscopy, X-ray energy dispersive spectroscopy, Raman spectroscopy and thermogravimetric analysis. These characterization techniques revealed the successful grafting of hydroxyapatite over well exfoliated graphene nanosheets without destroying their structure.

  11. Characterization of New PEEK/HA Composites with 3D HA Network Fabricated by Extrusion Freeforming.

    PubMed

    Vaezi, Mohammad; Black, Cameron; Gibbs, David M R; Oreffo, Richard O C; Brady, Mark; Moshrefi-Torbati, Mohamed; Yang, Shoufeng

    2016-01-01

    Addition of bioactive materials such as calcium phosphates or Bioglass, and incorporation of porosity into polyetheretherketone (PEEK) has been identified as an effective approach to improve bone-implant interfaces and osseointegration of PEEK-based devices. In this paper, a novel production technique based on the extrusion freeforming method is proposed that yields a bioactive PEEK/hydroxyapatite (PEEK/HA) composite with a unique configuration in which the bioactive phase (i.e., HA) distribution is computer-controlled within a PEEK matrix. The 100% interconnectivity of the HA network in the biocomposite confers an advantage over alternative forms of other microstructural configurations. Moreover, the technique can be employed to produce porous PEEK structures with controlled pore size and distribution, facilitating greater cellular infiltration and biological integration of PEEK composites within patient tissue. The results of unconfined, uniaxial compressive tests on these new PEEK/HA biocomposites with 40% HA under both static and cyclic mode were promising, showing the composites possess yield and compressive strength within the range of human cortical bone suitable for load bearing applications. In addition, preliminary evidence supporting initial biological safety of the new technique developed is demonstrated in this paper. Sufficient cell attachment, sustained viability in contact with the sample over a seven-day period, evidence of cell bridging and matrix deposition all confirmed excellent biocompatibility. PMID:27240326

  12. 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.

  13. Metallic coating of microspheres

    SciTech Connect

    Meyer, S.F.

    1980-08-15

    Extremely smooth, uniform metal coatings of micrometer thicknesses on microscopic glass spheres (microspheres) are often needed as targets for inertial confinement fusion (ICF) experiments. The first part of this paper reviews those methods used successfully to provide metal coated microspheres for ICF targets, including magnetron sputtering, electro- and electroless plating, and chemical vapor pyrolysis. The second part of this paper discusses some of the critical aspects of magnetron sputter coating of microspheres, including substrate requirements, the sticking of microspheres during coating (preventing a uniform coating), and the difficulties in growing the desired dense, smooth, uniform microstructure on continuously moving spherical substrates.

  14. 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. PMID:25485944

  15. Effect of protein on the dissolution of HA coatings.

    PubMed

    Bender, S A; Bumgardner, J D; Roach; Bessho, K; Ong, J L

    2000-02-01

    The dissolution behavior of hydroxyapatite (HA) in the presence and absence of protein needs to be investigated in order to fully understand the initial cellular response to HA surfaces. In this study, HA coatings were characterized using X-ray diffraction, X-ray photoelectron spectroscopy, and Fourier transform infrared spectroscopy (FTIR) prior to protein study. Fibronectin and albumin adsorption study were also performed. Calcium and phosphorus released in the presence and absence of albumin were measured. pH of the solution was measured daily. From the materials characterization, it was observed that the coatings exhibit a HA-type structure, with traces of sodium on the surface. FTIR indicated the possible presence of carbonates on the coatings. From the adsorption study, the amount of albumin adsorbed (0.052+/-0.005 microg/mm2) was statistically higher than the amount of fibronectin adsorbed on HA surfaces (0.035+/-0.002 microg/mm2). Flame atomic absorption indicated a significantly higher calcium ions released initially for HA coatings incubated with proteins as compared to coatings in the absence of proteins. However, after 7 days incubation, no significant difference in calcium ions release was observed between the HA coatings in the presence and absence of proteins. Phosphorus dissolution on HA coatings was not significantly affected by the presence of proteins. Thus, it was suggested from this study that the initial dissolution properties of calcium ions from HA coatings was dependent on the media. PMID:10646947

  16. Effect of Thickness of HA-Coating on Microporous Silk Scaffolds Using Alternate Soaking Technology

    PubMed Central

    Zhu, Rui; Xue, Yingsen; Hao, Zhangying; Xie, Zhenghong; Fan, Xiangli; Fan, Hongbin

    2014-01-01

    Hydroxyapatite (HA) can be coated on various materials surface and has the function of osteogenicity. Microporous silk scaffold has excellent biocompatibility. In this study, alternate soaking technology was used to coat HA on microporous silk scaffolds. However, the cell proliferation was found to decrease with the increasing thickness (cycles of soaking) of HA-coating. This study aims to determine the best thickness (cycles of soaking) of HA-coating on microporous silk scaffolds. The SEM observation showed that group with one cycle of alternate soaking (1C-HA) has the most optimal porosity like non-HA-modified microporous silk scaffolds. The proliferation of osteoblasts has no significant difference between noncoated HA (N-HA) and 1C-HA groups, which are both significantly higher than those in two cycles of soaking (2C-HA) and three cycles of soaking (3C-HA) groups. The transcription levels of specific genes (runx2 and osteonectin) in osteoblasts of 1C-HA group were significantly higher than those of N-HA group. Moreover, the levels showed no significant difference among 1C-HA, 2C-HA, and 3C-HA groups. In conclusion, microporous silk scaffold with 1 cycle of HA-coating can combine the biocompatibility of silk and osteogenicity of HA. PMID:25093176

  17. Characterization of processed tooth hydroxyapatite for potential biomedical implant applications.

    PubMed

    Oktar, F N; Kesenci, K; Pişkin, E

    1999-07-01

    In this study hydroxyapatite (HA) (100-150 microns) derived from freshly-extracted human teeth in laboratory conditions was investigated. Scanning electron microscope (SEM), energy dispersive x-ray spectroscopy (EDXS), wet chemical, ion chromatographic peak method (ICP), atomic absorption, x-ray diffraction and infra-red (IR) were performed separately for HA obtained from dentine and enamel. This naturally derived HA did not differ from synthetic ones. Its production was simple when compared with other methods. Processed tooth HA could safely be used in animal subjects prior to human studies as a graft material after biocompatibility studies fully conducted. PMID:10427420

  18. 188Re-labeled hydroxyapatite particles for radiation synovectomy.

    PubMed

    Kothari, K; Suresh, S; Sarma, H D; Meera, V; Pillai, M R A

    2003-04-01

    A new procedure for labeling hydroxyapatite (HA) particles with 188Re for radiation synovectomy is described and standardized. The particles were labeled with 188Re in high yields (99%) in acidic medium. HA particle size remained unaffected by reaction conditions as checked by laser diffraction particle analyzer. 188Re-HA was found to be stable retaining 99% radiochemical purity after 4 days when stored in ascorbic acid solution (10mg/ml, pH 5). Intra-articular injection in rats revealed approximately 98% retention of 188Re-HA in the knee after 48-h pi. PMID:12672625

  19. Production of hollow aerogel microspheres

    SciTech Connect

    Upadhye, R.S.; Henning, S.A.

    1990-12-31

    A method is described for making hollow aerogel microspheres of 800--1200{mu} diameter and 100--300{mu} wall thickness by forming hollow alcogel microspheres during the sol/gel process in a catalytic atmosphere and capturing them on a foam surface containing catalyst. Supercritical drying of the formed hollow alcogel microspheres yields hollow aerogel microspheres which are suitable for ICF targets.

  20. Production of hollow aerogel microspheres

    DOEpatents

    Upadhye, Ravindra S.; Henning, Sten A.

    1993-01-01

    A method is described for making hollow aerogel microspheres of 800-1200 .mu. diameter and 100-300 .mu. wall thickness by forming hollow alcogel microspheres during the sol/gel process in a catalytic atmosphere and capturing them on a foam surface containing catalyst. Supercritical drying of the formed hollow alcogel microspheres yields hollow aerogel microspheres which are suitable for ICF targets.

  1. Metabolism of proteinoid microspheres

    NASA Technical Reports Server (NTRS)

    Nakashima, T.; Fox, S. W. (Principal Investigator)

    1987-01-01

    The literature of metabolism in proteinoids and proteinoid microspheres is reviewed and criticized from a biochemical and experimental point of view. Closely related literature is also reviewed in order to understand the function of proteinoids and proteinoid microspheres. Proteinoids or proteinoid microspheres have many activities. Esterolysis, decarboxylation, amination, deamination, and oxidoreduction are catabolic enzyme activities. The formation of ATP, peptides or oligonucleotides is synthetic enzyme activities. Additional activities are hormonal and inhibitory. Selective formation of peptides is an activity of nucleoproteinoid microspheres; these are a model for ribosomes. Mechanisms of peptide and oligonucleotide syntheses from amino acids and nucleotide triphosphate by proteinoid microspheres are tentatively proposed as an integrative consequence of reviewing the literature.

  2. Metabolism of proteinoid microspheres

    NASA Technical Reports Server (NTRS)

    Nakashima, T.; Fox, S. W. (Principal Investigator)

    1987-01-01

    The literature of metabolism in proteinoids and proteinoid microspheres is reviewed and criticized from a biochemical and experimental point of view. Closely related literature is also reviewed in order to understand the function of proteinoids and proteinoid microspheres. Proteinoids or proteinoid microspheres have many activities. Esterolyis, decarboxylation, amination, deamination, and oxidoreduction are catabolic enzyme activities. The formation of ATP, peptides or oligonucleotides is synthetic enzyme activities. Additional activities are hormonal and inhibitory. Selective formation of peptides is an activity of nucleoproteinoid microspheres; these are a model for ribosomes. Mechanisms of peptide and oligonucleotide syntheses from amino acids and nucleotide triphosphate by proteinoid microspheres are tentatively proposed as an integrative consequence of reviewing the literature.

  3. Growth of one-dimensional single-crystalline hydroxyapatite nanorods

    NASA Astrophysics Data System (ADS)

    Ren, Fuzeng; Ding, Yonghui; Ge, Xiang; Lu, Xiong; Wang, Kefeng; Leng, Yang

    2012-06-01

    A facile, effective and template/surfactant-free hydrothermal route in the presence of sodium bicarbonate was developed to synthesize highly uniform single-crystalline hydroxyapatite (HA) nanorods with the lengths of several hundred nanometers and aspect ratio up to ˜20. One dimensional (1-D) growth and aspect ratio could be controlled by hydrothermal reaction time and temperature. The longitudinal axis, also the growth direction of the nanorods, is parallel to the [001] direction of HA hexagonal crystal structure.

  4. 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. PMID:25109458

  5. Controlled, sustained release of proteins via an injectable, mineral-coated microsphere delivery vehicle

    NASA Astrophysics Data System (ADS)

    Franklin-Ford, Travelle

    Hydroxyapatite interfaces have demonstrated strong protein binding and protein selection from a passing solution and can serve as a biocompatible carrier for controlled protein delivery. Hydroxyapatite is a major component of long bones and tooth enamel and is the most stable of all calcium phosphate isoforms in aqueous solutions at physiologic pH, providing a sensitive chromatographic mechanism for separating proteins. Here we describe an approach to create a synthetic hydroxyapatite coating through a biomimetic, heterogeneous nucleation from a modified simulated body fluid--supersaturated with calcium and phosphate ions on the surface of injectable polymer microspheres. We are able to bind and release bioactive growth factors into a variety of in vitro and in vivo conditions, demonstrating the functionality and advantage of the biomaterial. Creating a hydroxyapatite layer on the Poly(D,L-lactide-co-glycolide) (PLG) microsphere surface, avails the microsphere interior for another application that will not compete with protein binding and release. Encapsulating an imaging agent within the aqueous phase of the emulsion provides a visual reference for the injectable therapy upon microsphere fabrication. Another advantage of this system is that the mineral coating and subsequent protein binding is not compromised by the encapsulated imaging agent. This dual function delivery vehicle is not only advantageous for spatial tracking therapeutic applications, but also determining the longevity of the delivery vehicle once injected. In the broader sense, providing a mechanism to image and track our temporally controlled, sustained delivery system gives more evidence to support the effects of released protein on in vivo responses (bioactivity) and locate microspheres within different biological systems.

  6. Biomechanical analysis of hydroxyapatite cement cranioplasty.

    PubMed

    Matic, Damir B; Manson, Paul N

    2004-05-01

    A recent review of the authors' experience with hydroxyapatite (HA) cement cranioplasties revealed a high infection rate. During removal of these implants, all were loose and fractured. Forty percent of these patients had a history of minor trauma at the site of cranioplasty before experiencing infection. Minor trauma may fracture HA cranioplasties and result in infection. The purpose of this study is to determine the force to fracture full- and partial-thickness cranial defects reconstructed with HA cement and to compare peak loads of differing HA cement cranioplasty techniques. Standardized craniotomy defects were created in five fresh cadaver heads. Full-thickness defects were reconstructed with either rigid or flexible titanium mesh and then covered with HA cement. Partial-thickness defects were reconstructed with HA alone. After setting, a uniaxial impact was delivered to each of the defects. Peak loads were recorded, and defects were examined for evidence of fracture.Predictable fractures of the HA cranioplasties occurred at 1200 N in all full-thickness defects reconstructed with mesh and a thin layer of HA. Implant loosening and chipping was similar to what was seen clinically in the authors' patients with infections. Full-thickness defects in which titanium mesh was shaped like a cup and filled with a thick layer of HA resist fracture at 1200 N. Partial-thickness defects reconstructed with HA alone also do not fracture at this peak load. Patient selection, defect characteristics, and reconstructive techniques are factors that need to be considered before using HA cement for cranioplasty purposes. PMID:15111799

  7. Electrospinning of Hyaluronic acid (HA) and HA/Gelatin Blends

    NASA Astrophysics Data System (ADS)

    He, Aihua; Li, Junxing; Han, Charles; Fang, Dufei; Hsiao, Benjamin; Chu, Benjamin

    2007-03-01

    It was found that the processability of HA solution with high viscosity had been improved greatly by using a DMF-water solvent mixture or/and by adding gelatin(GE) into the HA solution. Nano-fibrous membranes with different average fiber diameters and different HA/GE compositions could be obtained. Measurements on viscosity indicated that the HA solution in DMF-water mixed solvent still showed high viscosity. The decrease in surface tension contributed to the fiber formation of HA and HA/GE by electrospinning. Therefore, this study not only provided a novel and simpler way to electrospin the natural polyanion HA solution, but also provided the fundamental physical insight and solution to this spinning difficulty. The HA-GE nanofibrous membranes at different HA/GE compositions are expected to be useful in the biomedical field as novel scaffolds for many applications.

  8. Osteoclasts in the interface with electrospun hydroxyapatite.

    PubMed

    Pasuri, Jenni; Holopainen, Jani; Kokkonen, Hanna; Persson, Maria; Kauppinen, Kyösti; Lehenkari, Petri; Santala, Eero; Ritala, Mikko; Tuukkanen, Juha

    2015-11-01

    Electrospinning is a method to produce lightweight, resorbable and bioinspired scaffolds for tissue engineering. Here we investigated the influence of electrospun hydroxyapatite fibers (HA) on macrophages and osteoclasts. A mouse macrophage cell line (RAW 264.7) and human bone marrow derived primary osteoclasts (hOC) were cultured with electrospun HA fibers embedded in Matrigel. Cell morphology and the secretion of pro-inflammatory cytokines (IL-6 and TNF-α) were analyzed using macrophages. Both fluorescent microscopy and scanning electron microscopy indicated that the cell morphology differed on the various materials (HA fibers on Matrigel, pure Matrigel and a glass control). Control macrophages were activated with bacterial lipopolysaccharide (LPS) but electrospun HA did not provoke an inflammatory response. Cytokine secretion detected with enzyme-linked immunosorbent assay (ELISA) also supported this observation. LPS, but not HA fibers, stimulated TNF-α and IL-6 secretion by macrophages at the 2 day time point. After 4 days in culture there was an increasing trend in cytokine secretion in the HA fiber samples. Human bone marrow myeloid precursor cells were able to fuse and differentiate on the fibrous mineral scaffold to form functional multinuclear osteoclasts that were able to resorb the HA nanofibers. This indicates that osteoclasts do not necessarily need a continuous bone surface but osteoclast ruffled border membranes can form a resorption interface with a fibrous mineral scaffold. PMID:26342323

  9. First principles study of hydroxyapatite surface.

    PubMed

    Slepko, Alexander; Demkov, Alexander A

    2013-07-28

    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)]. PMID:23902010

  10. 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.

  11. Nanostructured nickel-free austenitic stainless steel/hydroxyapatite composites.

    PubMed

    Tulinski, Maciej; Jurczyk, Mieczyslaw

    2012-11-01

    In this work Ni-free austenitic stainless steels with nanostructure and their nanocomposites with hydroxyapatite are presented and characterized by means of X-ray diffraction and optical profiling. The samples were synthesized by mechanical alloying, heat treatment and nitriding of elemental microcrystalline powders with addition of hydroxyapatite (HA). In our work we wanted to introduce into stainless steel hydroxyapatite ceramics that have been intensively studied for bone repair and replacement applications. Such applications were chosen because of their high biocompatibility and ability to bond to bone. Since nickel-free austenitic stainless steels seem to have better mechanical properties, corrosion resistance and biocompatibility compared to 316L stainless steels, it is possible that composite made of this steel and HA could improve properties, as well. Mechanical alloying and nitriding are very effective technologies to improve the corrosion resistance of stainless steel. Similar process in case of nanocomposites of stainless steel with hydroxyapatite helps achieve even better mechanical properties and corrosion resistance. Hence nanocrystalline nickel-free stainless steels and nickel-free stainless steel/hydroxyapatite nanocomposites could be promising bionanomaterials for use as a hard tissue replacement implants, e.g., orthopedic implants. In such application, the surface roughness and more specifically the surface topography influences the proliferation of cells (e.g., osteoblasts). PMID:23421285

  12. 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. PMID:24268261

  13. Microsphere Insulation Panels

    NASA Technical Reports Server (NTRS)

    Mohling, R.; Allen, M.; Baumgartner, R.

    2006-01-01

    Microsphere insulation panels (MIPs) have been developed as lightweight, longlasting replacements for the foam and vacuum-jacketed systems heretofore used for thermally insulating cryogenic vessels and transfer ducts. The microsphere core material of a typical MIP consists of hollow glass bubbles, which have a combination of advantageous mechanical, chemical, and thermal-insulation properties heretofore available only separately in different materials. In particular, a core filling of glass microspheres has high crush strength and low density, is noncombustible, and performs well in soft vacuum.

  14. Dissolution of synthetic and bovine bone-derived hydroxyapatites fabricated by hot-pressing

    NASA Astrophysics Data System (ADS)

    Kim, Young Gook; Seo, Dong Seok; Lee, Jong Kook

    2008-11-01

    Dissolving behavior of hydroxyapatite (HA) ceramics prepared from bovine bone (BHA) was investigated and compared with synthetic HA. BHA power was obtained by calcining at 800 °C for 1 h to remove organics and then attritor-milling for 24 h. Synthetic HA and BHA powders were prepared by hot-pressing at 1000 °C for 0.5 h under the pressure of 30 MPa in Ar atmosphere. Sintered densities of the synthetic HA and the BHA were about 96% and 95%, respectively. The BHA consisted of mainly HA and small amount of magnesium oxide. Immersion test revealed that there was no clear evidence of dissolution for the BHA, whereas extensive dissolution on the surface of the synthetic HA occurred in buffered water. Accordingly, dense hydroxyapatite from bovine bone was more stable than synthetic HA in liquid environment.

  15. Organic aerogel microspheres

    DOEpatents

    Mayer, Steven T.; Kong, Fung-Ming; Pekala, Richard W.; Kaschmitter, James L.

    1999-01-01

    Organic aerogel microspheres which can be used in capacitors, batteries, thermal insulation, adsorption/filtration media, and chromatographic packings, having diameters ranging from about 1 micron to about 3 mm. The microspheres can be pyrolyzed to form carbon aerogel microspheres. This method involves stirring the aqueous organic phase in mineral oil at elevated temperature until the dispersed organic phase polymerizes and forms nonsticky gel spheres. The size of the microspheres depends on the collision rate of the liquid droplets and the reaction rate of the monomers from which the aqueous solution is formed. The collision rate is governed by the volume ratio of the aqueous solution to the mineral oil and the shear rate, while the reaction rate is governed by the chemical formulation and the curing temperature.

  16. Organic aerogel microspheres

    DOEpatents

    Mayer, S.T.; Kong, F.M.; Pekala, R.W.; Kaschmitter, J.L.

    1999-06-01

    Organic aerogel microspheres are disclosed which can be used in capacitors, batteries, thermal insulation, adsorption/filtration media, and chromatographic packings, having diameters ranging from about 1 micron to about 3 mm. The microspheres can be pyrolyzed to form carbon aerogel microspheres. This method involves stirring the aqueous organic phase in mineral oil at elevated temperature until the dispersed organic phase polymerizes and forms nonstick gel spheres. The size of the microspheres depends on the collision rate of the liquid droplets and the reaction rate of the monomers from which the aqueous solution is formed. The collision rate is governed by the volume ratio of the aqueous solution to the mineral oil and the shear rate, while the reaction rate is governed by the chemical formulation and the curing temperature.

  17. 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.

  18. Risedronate/zinc-hydroxyapatite based nanomedicine for osteoporosis.

    PubMed

    Khajuria, Deepak Kumar; Disha, Choudhary; Vasireddi, Ramakrishna; Razdan, Rema; Mahapatra, D Roy

    2016-06-01

    Targeting of superior osteogenic drugs to bone is an ideal approach for treatment of osteoporosis. Here, we investigated the potential of using risedronate/zinc-hydroxyapatite (ZnHA) nanoparticles based formulation in a rat model of experimental osteoporosis. Risedronate, a targeting moiety that has a strong affinity for bone, was loaded to ZnHA nanoparticles by adsorption method. Prepared risedronate/ZnHA drug formulation was characterized by field-emission scanning electron microscopy, X-ray diffraction analysis and fourier transform infrared spectroscopy. In vivo performance of the prepared risedronate/ZnHA nanoparticles was tested in an experimental model of postmenopausal osteoporosis. Therapy with risedronate/ZnHA drug formulation prevented increase in serum levels of bone-specific alkaline phosphatase and tartrate-resistant acid phosphatase 5b better than risedronate/HA or risedronate. With respect to improvement in the mechanical strength of the femoral mid-shaft and correction of increase in urine calcium and creatinine levels, the therapy with risedronate/ZnHA drug formulation was more effective than risedronate/HA or risedronate therapy. Moreover, risedronate/ZnHA drug therapy preserved the cortical and trabecular bone microarchitecture better than risedronate/HA or risedronate therapy. Furthermore, risedronate/ZnHA drug formulation showed higher values of calcium/phosphorous ratio and zinc content. The results strongly implicate that risedronate/ZnHA drug formulation has a therapeutic advantage over risedronate or risedronate/HA therapy for the treatment of osteoporosis. PMID:27040198

  19. Citric acid-based hydroxyapatite composite scaffolds enhance calvarial regeneration.

    PubMed

    Sun, Dawei; Chen, Yuhui; Tran, Richard T; Xu, Song; Xie, Denghui; Jia, Chunhong; Wang, Yuchen; Guo, Ying; Zhang, Zhongmin; Guo, Jinshan; Yang, Jian; Jin, Dadi; Bai, Xiaochun

    2014-01-01

    Citric acid-based polymer/hydroxyapatite composites (CABP-HAs) are a novel class of biomimetic composites that have recently attracted significant attention in tissue engineering. The objective of this study was to compare the efficacy of using two different CABP-HAs, poly (1,8-octanediol citrate)-click-HA (POC-Click-HA) and crosslinked urethane-doped polyester-HA (CUPE-HA) as an alternative to autologous tissue grafts in the repair of skeletal defects. CABP-HA disc-shaped scaffolds (65 wt.-% HA with 70% porosity) were used as bare implants without the addition of growth factors or cells to renovate 4 mm diameter rat calvarial defects (n = 72, n = 18 per group). Defects were either left empty (negative control group), or treated with CUPE-HA scaffolds, POC-Click-HA scaffolds, or autologous bone grafts (AB group). Radiological and histological data showed a significant enhancement of osteogenesis in defects treated with CUPE-HA scaffolds when compared to POC-Click-HA scaffolds. Both, POC-Click-HA and CUPE-HA scaffolds, resulted in enhanced bone mineral density, trabecular thickness, and angiogenesis when compared to the control groups at 1, 3, and 6 months post-trauma. These results show the potential of CABP-HA bare implants as biocompatible, osteogenic, and off-shelf-available options in the repair of orthopedic defects. PMID:25372769

  20. Surface modification for titanium implants by hydroxyapatite nanocomposite

    PubMed Central

    Family, Roxana; Solati-Hashjin, Mehran; Namjoy Nik, Shahram; Nemati, Ali

    2012-01-01

    Background: Titanium (Ti) implants are commonly coated with hydroxyapatite (HA). However, HA has some disadvantages such as brittleness, low tensile strength and fracture toughness. It is desirable to combine the excellent mechanical properties of ZrO2 and the chemical inertness of Al2O3 with respect to the purpose of this project which was coating Ti implants with HA-ZrO2-Al2O3 to modify the surface of these implants by adding ZrO2 and Al2O3 to HA. The purpose of this study was to evaluate the efficacy of hydroxyapatite coating nonocomposite. Methods: From September 2009 to January2011, functionally graded HA-Al2O3-ZrO2 and HA coatings were applied on Ti samples. HA-Al2O3-ZrO2 and HA sols were orderly dip coated on the substrates and calcined. Scanning electron microscopy and EDS were used to estimate the particle size of the surfaces and for morphological analysis. The morphology of non-coated HA-coated HA-Al2O3-ZrO2 (composite-coated) and double-layer composite coated samples were compared with one other. Mechanical test (heat & quench) was also done for comparing single-phase (HA), composite and double-layer composite samples. Results: The morphology of HA-Al2O3-ZrO2 coating is more homogenous than HA-coated and uncoated samples. Furthermore, single-layer coating is more homogenous than double-layer coating. EDS analysis was done on HA-coated sample and showed that the Ca/P ratio in the film was similar to the theoretical value 1.67 in HA. Conclusion: Surface modification of Ti implants can be done by coating them with single-layer of HA-Al2O3-ZrO2. Single-layer hydroxyapatite-alumina-zirconia coated sample has the most homogenous morphology on the surface. PMID:24009915

  1. Hydroxyapatite-binding peptides for bone growth and inhibition

    DOEpatents

    Bertozzi, Carolyn R.; Song, Jie; Lee, Seung-Wuk

    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.

  2. 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.

  3. Electrokinetic properties of hydroxyapatite under flotation conditions.

    PubMed

    Vucinić, Dusica R; Radulović, Dragan S; Deusić, Slaven D

    2010-03-01

    The effect of calcite supernatant, calcium, and carbonate ions on the hydroxyapatite (HA) zeta potential without and in the presence of sodium oleate (1x10(-4) mol L(-1)) was examined within the pH range from 4 to 12. The interpretation of results was based on the HA surface and oleate solution chemistry, and on some floatability tests. HA, with different positive and negative surface sites formed depending on its solubility and pH, had a negative zeta potential over the whole pH range. This mineral is not naturally floatable (flotation recovery, 5%HA surface centers [triple bond]Ca(+), [triple bond]HPO(4)Ca(+), and [triple bond]OH(2)(+), increasing the negative zeta potential of the mineral. Within the pH range from 7 to 9, the dominant oleate species Ol(-) ion and ion-molecule complex, H(Ol)(2)(-), adsorbed on HA by head groups toward the solid and associated due to chain-chain interaction in hemimicelles, made the HA surface with zeta potential about -22/-23 mV, and more floatable (R=80-100%) than in 49.3. The HA surface is less negatively charged in calcite supernatant than in water from pH 6.6 to 9.2 due to the adsorption on HA negative surface active centers ([triple bond]HPO(4)(-) and [triple bond]PO(4)(2-)) of the Ca(2+), and CaOH(+) ions (present in the calcite supernatant), producing more surface sites [triple bond]HPO(4)Ca(+), [triple bond]PO(4)Ca, [triple bond]HPO(4)CaOH, and [triple bond]PO(4)(-) CaOH, and new centers [triple bond]HPO(4)CaHCO(3) and [triple bond]PO(4)(-) CaHCO(3). In the presence of 1x10(-3) mol L(-1) CaCl(2), the HA sample has positive zeta potential, the same as calcite from the same deposit, up to IEP at pH 11.25. Carbonate ions (1x10(-3) mol L(-1) Na(2)CO(3)) do not affect the HA zeta potential. However, a possible process can be the ion-exchange reaction between

  4. Hydroxyapatite with environmental applications

    SciTech Connect

    Popa, C. L.; Ciobanu, C. S.; Predoi, D.; Petre, C. C.; Jiga, G.; Motelica-Heino, M.; Iconaru, S. L.

    2014-05-15

    The aim of this study was to synthetize new nanoparticles based on methyltrimethoxysilane coated hydroxyapatite (MTHAp) for lead removal in aqueous solutions. The morphological and compositional analysis of MTHAp was investigated by scanning electron microscopy (SEM) equipped with an energy dispersive X-ray spectrometer (EDS). Removal experiments of Pb{sup 2+} ions were carried out in aqueous solutions with controlled concentration of Pb{sup 2+} and at fixed pH of 5. After the removal experiment of Pb{sup 2+} ions from solutions, porous hydroxyapatite nanoparticles were transformed into PbMTHAp-5 via the adsorption of Pb{sup 2+} ions followed by a cation exchange reaction. Our results demonstrate that the porous hydroxyapatite nanoparticles can be used as an adsorbent for removing Pb{sup 2+} ions from aqueous solution.

  5. Preparation and characterization of PHBV microsphere/45S5 bioactive glass composite scaffolds with vancomycin releasing function.

    PubMed

    Li, Wei; Ding, Yaping; Rai, Ranjana; Roether, Judith A; Schubert, Dirk W; Boccaccini, Aldo R

    2014-08-01

    PHBV microsphere/45S5 bioactive glass (BG) composite scaffolds with drug release function were developed for bone tissue engineering. BG-based glass-ceramic scaffolds with high porosity (94%) and interconnected pore structure prepared by foam replication method were coated with PHBV microspheres (nominal diameter=3.5 μm) produced by water-in-oil-in-water double emulsion solvent evaporation method. A homogeneous microsphere coating throughout the porous structure of scaffolds was obtained by a simple dip coating method, using the slurry of PHBV microspheres in hexane. Compressive strength tests showed that the microsphere coating slightly improved the mechanical properties of the scaffolds. It was confirmed that the microsphere coating did not inhibit the bioactivity of the scaffolds in SBF. Hydroxyapatite crystals homogeneously grew not only on the struts of the scaffolds but also on the surface of microspheres within 7 days of immersion in SBF. Vancomycin was successfully encapsulated into the PHBV microspheres. The encapsulated vancomycin was released with a dual release profile involving a relatively low initial burst release (21%) and a sustained release (1 month), which is favorable compared to the high initial burst release (77%) and short release period (4 days) measured on uncoated scaffolds. The developed bioactive composite scaffold with drug delivery function has thus the potential to be used advantageously in bone tissue engineering. PMID:24907766

  6. 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. PMID:26478384

  7. Method for sizing hollow microspheres

    DOEpatents

    Farnum, E.H.; Fries, R.J.

    1975-10-29

    Hollow Microspheres may be effectively sized by placing them beneath a screen stack completely immersed in an ultrasonic bath containing a liquid having a density at which the microspheres float and ultrasonically agitating the bath.

  8. 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

  9. The influence of collagen support and ionic species on the morphology of collagen/hydroxyapatite composite materials

    SciTech Connect

    Ficai, Anton; Andronescu, Ecaterina; Voicu, Georgeta; Ghitulica, Cristina; Ficai, Denisa

    2010-04-15

    The purpose of this investigation is to study the influence of collagenous supports and ionic species on the precipitation of hydroxyapatite (HA) from aqueous solutions. To this end, we obtained hydroxyapatite by co-precipitation from a solution of calcium hydroxide and sodium dihydrogenophosphate. The formation of HA was studied by energy dispersive X-ray spectroscopy (EDS), X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR). The results of this study indicate that the morphology of hydroxyapatite is highly influenced by the support material and the ionic species present. The obtained materials were studied by scanning electron microscopy (SEM).

  10. Study of thermal effects of silicate-containing hydroxyapatites

    NASA Astrophysics Data System (ADS)

    Golovanova, O. A.; Zaits, A. V.; Berdinskaya, N. V.; Mylnikova, T. S.

    2016-02-01

    The possibility of modifications of hydroxyapatite silicate ions, from the extracellular fluid prototype solution under near-physiological conditions has been studied. Formation of silicon-structured hydroxyapatite with different extent of substitution of phosphate groups in the silicate group has been established through chemical and X-ray diffraction analyses, FTIR spectroscopy and optical microscopy. The results obtained are in agreement and suggest the possibility of substitution of phosphate groups for silicate groups in the hydroxyapatite structure when introducing different sources of silica, tetraethoxysilane and sodium silicate, in the reaction mixture. Growth in the amount of silicon in Si-HA results in the increase in the thermal stability of the samples. The greatest mass loss occurs at temperatures in the range of 25-400 0C that is caused by the removal of the crystallization and adsorption water and volatile impurities. It is shown that the modified apatites are of imperfect structure and crystallize in a nanocrystalline state.

  11. Investigations on hydroxyapatite powder obtained by wet precipitation

    NASA Astrophysics Data System (ADS)

    Poinescu, Aurora Anca; Ion, Rodica Mariana; van Staden, Raluca-Ioana; van Staden, Jacobus Frederick; Ghiurea, Marius

    2010-11-01

    It is well-known that hydroxyapatite have multiple applications in tissue engineering due to compositional similarities with bone tissue. In this work, hydroxyapatite powders obtained by modified chemical precipitation route, has been investigated by AMF and SEM analysis grain size, X-ray diffraction and infra-red spectroscopy. The particle size of hydroxyapatite was observed to be very fine, uniform, around 50 -60 nm. SEM observation of the HA coatings showed the presence of nano-sized needles, with a significant level of agglomeration. The infrared analysis show the characteristic peaks of absorbed water, hydroxyl, phosphate and carbonate species. The XRD pattern clearly indicated the crystallites responsible for the Bragg reflection of the (002) and (003) planes are useful for size determination by Sherrer relationship (around 68 nm).

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

    PubMed

    Kolmas, Joanna; Groszyk, Ewa; Piotrowska, Urszula

    2015-12-01

    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. PMID:26138453

  13. 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

  14. Osteogenic Properties of PBLG-g-HA/PLLA Nanocomposites

    PubMed Central

    Liao, Lan; Yang, Shuang; Miron, Richard J.; Wei, Junchao; Zhang, Yufeng; Zhang, Meng

    2014-01-01

    New development of biomaterial scaffolds remains a prominent issue for the regeneration of lost or fractured bone. Of these scaffolds, a number of bioactive polymers have been synthesized and fabricated for diverse biological roles. Although recent evidence has demonstrated that composite scaffolds such as HA/PLLA have improved properties when compared to either HA or PLLA alone, recent investigations have demonstrated that the phase compatibility between HA and PLLA layers is weak preventing optimal enhancement of the mechanical properties and making the composites prone to breakdown. In the present study, poly (γ-benzyl-L-glutamate) modified hydroxyapatite/(poly (L-lactic acid)) (PBLG-g-HA/PLLA) composite scaffolds were fabricated with improved phase compatibility and tested for their osteogenic properties in 18 Wistar female rats by analyzing new bone formation in 3 mm bilateral femur defects in vivo. At time points, 2, 4 and 8 weeks post surgery, bone formation was evaluated by µ-CT and histological analysis by comparing 4 treatment groups; 1) blank defect, 2) PLLA, 3) HA/PLLA and 4) PBLG-g-HA/PLLA scaffolds. The in vivo analysis demonstrated that new bone formation was much more prominent in HA/PLLA and PBLG-g-HA/PLLA groups as depicted by µ-CT, H&E staining and immunohistochemistry for collagen I. TRAP staining was also utilized to determine the influence of osteoclast cell number and staining intensity to the various scaffolds. No significant differences in either staining intensity or osteoclast numbers between all treatment modalities was observed, however blank defects did contain a higher number of osteoclast-like cells. The results from the present study illustrate the potential of PBLG-g-HA/PLLA scaffolds for bone tissue engineering applications by demonstrating favorable osteogenic properties. PMID:25184285

  15. 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. PMID:22968925

  16. 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. PMID:27264723

  17. 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

  18. Effect of sintered silicate-substituted hydroxyapatite on remodelling processes at the bone-implant interface.

    PubMed

    Porter, Alexandra E; Patel, Nelesh; Skepper, Jeremy N; Best, Serena M; Bonfield, William

    2004-07-01

    Phase pure, sintered granules of hydroxyapatite (HA) and silicon-substituted hydroxyapatite (Si-HA) were implanted for 6 and 12 weeks in an ovine model. Samples containing the bone-implant interface were prepared for ultramicrotomy and transmission electron microscopy (TEM) using an anhydrous sample preparation procedure. The results demonstrate that the morphology of apatite deposits and the sequence of events at the interfaces of bone with pure HA and with Si-HA implants, were different. Organised collagen fibrils were first found at the bone/Si-HA interface after 6 weeks, whereas they were found only after 12 weeks around the pure HA implant. Many more nodular aggregates comprised of plate-like apatite crystallites were observed in the vicinity of Si-HA than around the pure HA after 12 weeks in vivo. These findings suggest that the incorporation of silicate ions into HA promotes processes of bone remodelling at the bone/HA interface. TEM observations suggested that the trabecular bone weaves over the Si-HA and that the collagen fibrils form a mechanical interlock with the Si-HA ceramic implants. High-resolution lattice imaging illustrated apatite crystallites contiguous with the Si-HA ceramic and revealed a direct relationship between the bone mineral and the Si-HA ceramic. PMID:14980425

  19. Comparison of the Weibull characteristics of hydroxyapatite and strontium doped hydroxyapatite.

    PubMed

    Yatongchai, Chokchai; Wren, Anthony W; Curran, Declan J; Hornez, Jean-Christophe; Mark R, Towler

    2013-05-01

    The effects of two strontium (Sr) additions, 5% and 10% of the total calcium (Ca) content, on the phase assemblage and Weibull statistics of hydroxyapatite (HA) are investigated and compared to those of undoped HA. Sintering was carried out in the range of 900-1200 °C in steps of 1000 °C in a conventional furnace. Sr content had little effect on the mean particulate size. Decomposition of the HA phase occurred with Sr incorporation, while β-TCP stabilization was shown to occur with 10% Sr additions. Porosity in both sets of doped samples was at a comparable level to porosity in the undoped HA samples, however the 5% Sr-HA samples displayed the greatest reduction in porosity with increasing temperature while the porosity of the 10% Sr-HA samples remain relatively constant over the full sintering temperature range. The undoped HA samples displayed the greatest Weibull strengths and the porosity was determined to be the major controlling factor. However, with the introduction of decompositional phases in the Sr-HA samples, the dependence of strength on porosity is reduced and the phase assemblage becomes the more dominant factor for Weibull strength. The Weibull modulus is relatively independent of the porosity in the undoped HA samples. The 5% Sr-HA samples experience a slight increase in Weibull modulus with porosity, indicating a possible relationship between the parameters. However the 10% Sr-HA samples show the highest Weibull modulus with a value of approximately 15 across all sintering temperatures. It is postulated that this is due to the increased amount of surface and lattice diffusion that these samples undergo, which effectively smooths out flaws in the microstructure, due to a saturation of Sr content occurring in grain boundary movement. PMID:23524073

  20. Synthesis and characterization of strontium-doped hydroxyapatite powder via sol-gel method.

    PubMed

    Mardziah, C M; Sopyan, I; Hamdi, M; Ramesh, S

    2008-07-01

    Improvement of the mechanical properties of hydroxyapatite (HA) can be achieved by the incorporation of metal. In addition, incorporation of strontium ion into HA crystal structures has been proved effective to enhance biochemical properties of bone implant. In this research, strontium-doped HA powder was developed via a sol-gel method to produce extraordinarily fine strontium-doped HA (Sr-doped HA) powder. XRD measurement had shown that the powder contained hydroxyapatite phase only for all doping concentration except for 2%, showing that Sr atoms have suppressed the appearance of beta-TCP as the secondary phase. Morphological evaluation by FESEM measurement shows that the particles of the Sr-doped HA agglomerates are globular in shape with an average size of 1-2 microm in diameter while the primary particles have a diameter of 30-150 nm in average. PMID:19024993

  1. Silicate-doped hydroxyapatite and its promotive effect on bone mineralization

    NASA Astrophysics Data System (ADS)

    Qiu, Zhi-Ye; Noh, In-Sup; Zhang, Sheng-Min

    2013-03-01

    Bone defect is one of the most common diseases in clinic. Existing therapeutic approaches have encountered many problems, such as lack of autogenous allogeneic bone and immunological rejection to allogeneic implant. Synthetic hydroxyapatite (HA) provided solutions for bone repair, since the HA is the main inorganic component of animals' bone. However, HA has good biocompatibility, but does not possess osteogenic capability, which is of significance for modern bone repair materials. Si is an essential trace element in bone tissue, and it has been demonstrated to be able to promote bone formation. Therefore, silicate-doped hydroxyapatite (Si-HA) may serve as a promising material for bone repair, and promote bone regeneration in the repair. The current review discusses development of Si-HA, focusing on its preparation and characterization, in vitro and in vivo evaluations of the material, positive effect of Si-HA on promoting bone formation in clinical applications, and molecular mechanism investigation of such promotive effect.

  2. Iron(III) and manganese(II) substituted hydroxyapatite nanoparticles: Characterization and cytotoxicity analysis

    NASA Astrophysics Data System (ADS)

    Li, Yan; Teck Nam, Chai; Ooi, Chui Ping

    2009-09-01

    Calcium hydroxyapatite (HA) is the main inorganic component of natural bones and can bond to bone directly in vivo. Thus HA is widely used as coating material on bone implants due to its good osteoconductivity and osteoinductivity. Metal ions doped HA have been used as catalyst or absorbents since the ion exchange method has introduced new properties in HA which are inherent to the metal ions. For example, Mn2+ ions have the potential to increase cell adhesion while Fe3+ ions have magnetic properties. Here, Fe(III) substituted hydroxyapatite (Fe-HA) and Mn(II) substituted hydroxyapatite (Mn-HA) were produced by wet chemical method coupled with ion exchange mechanism. Compared with pure HA, the colour of both Fe-HA and Mn-HA nanoparticles changed from white to brown and pink respectively. The intensity of the colours increased with increasing substitution concentrations. XRD patterns showed that all samples were single phased HA while the FTIR spectra revealed all samples possessed the characteristic phosphate and hydroxyl adsorption bands of HA. However, undesired adsorption bands of carbonate substitution (B-type carbonated HA) and H2O were also detected, which was reasonable since the wet chemical method was used in the synthesis of these nanoparticles. FESEM images showed all samples were elongated spheroids with small size distribution and of around 70 nm, regardless of metal ion substitution concentrations. EDX spectra showed the presence of Fe and Mn and ICP-AES results revealed all metal ion substituted HA were non-stoichiometric (Ca/P atomic ratio deviates from 1.67). Fe-HA nanoparticles were paramagnetic and the magnetic susceptibility increased with the increase of Fe content. Based on the extraction assay for cytotoxicity test, both Fe-HA and Mn-HA displayed non-cytotoxicity to osteoblast.

  3. Additive manufactured Ti6Al4V scaffolds with the RF- magnetron sputter deposited hydroxyapatite coating

    NASA Astrophysics Data System (ADS)

    Chudinova, E.; Surmeneva, M.; Koptioug, A.; Scoglund, P.; Surmenev, R.

    2016-01-01

    Present paper reports on the results of surface modification of the additively manufactured porous Ti6Al4V scaffolds. Radio frequency (RF) magnetron sputtering was used to modify the surface of the alloy via deposition of the biocompatible hydroxyapatite (HA) coating. The surface morphology, chemical and phase composition of the HA-coated alloy were studied. It was revealed that RF magnetron sputtering allows preparing a homogeneous HA coating onto the entire surface of scaffolds.

  4. 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.

  5. Rod-shaped and substituted hydroxyapatite nanoparticles stimulating type 1 and 2 cytokine secretion.

    PubMed

    Wang, Xiupeng; Li, Xia; Ito, Atsuo; Watanabe, Yohei; Sogo, Yu; Hirose, Motohiro; Ohno, Tadao; Tsuji, Noriko M

    2016-03-01

    A Th1 immune response is required for modern vaccines as the most commonly used alum adjuvant has weak capacity for inducing Th1 immune response. Herein, rod-shaped hydroxyapatite (HA), magnesium-substituted HA (MgHA) and zinc-substituted HA (ZnHA) nanoparticles with irregular nanopores were synthesized and used as immunoadjuvants. Magnesium and zinc substitution in HA showed no influence on morphology, particle size, zeta potential and surface area of the nanoparticles. The rod-shaped MgHA and ZnHA nanoparticles promoted the cellular uptake of a molecular immunopotentiator, stimulated both type 1 and 2 cytokine secretion in vitro that relate to Th1 and Th2 immunity of bone marrow dentritic cells, respectively. The MgHA and ZnHA nanoparticles may be useful as immunoadjuvants for human. PMID:26700228

  6. Method for preparing hollow metal oxide microsphere

    DOEpatents

    Schmitt, C.R.

    1974-02-12

    Hollow refractory metal oxide microspheres are prepared by impregnating resinous microspheres with a metallic compound, drying the impregnated microspheres, heating the microspheres slowly to carbonize the resin, and igniting the microspheres to remove the carbon and to produce the metal oxide. Zirconium oxide is given as an example. (Official Gazette)

  7. Hydroxyapatite whisker-reinforced polyetherketoneketone bone ingrowth scaffolds.

    PubMed

    Converse, Gabriel L; Conrad, Timothy L; Merrill, Christina H; Roeder, Ryan K

    2010-03-01

    Hydroxyapatite (HA) whisker-reinforced polyetherketoneketone (PEKK) bone ingrowth scaffolds were prepared and characterized. High levels of porosity (75-90%) and HA whisker reinforcement (0-40 vol.%) were attained using a powder processing approach to mix the HA whiskers, PEKK powder and a NaCl porogen, followed by compression molding at 350-375 degrees Celsius and particle leaching to remove the porogen. The scaffold architecture and microstructure exhibited characteristics known to be favorable for osteointegration. Scaffold porosity was interconnected with a mean pore size in the range 200-300 microm as measured by micro-computed tomography. HA whiskers were embedded within and exposed on the surface of scaffold struts, producing a microscale surface topography, shown by von Kossa staining and scanning electron microscopy. Therefore, HA whisker-reinforced PEKK bone ingrowth scaffolds may be advantageous for orthopedic implant fixation, including interbody spinal fusion. PMID:19665061

  8. Nanocrystalline Hydroxyapatite/Si Coating by Mechanical Alloying Technique

    PubMed Central

    Hannora, Ahmed E.; Mukasyan, Alexander S.; Mansurov, Zulkhair A.

    2012-01-01

    A novel approach for depositing hydroxyapatite (HA) films on titanium substrates by using mechanical alloying (MA) technique has been developed. However, it was shown that one-hour heat treatment at 800°C of such mechanically coated HA layer leads to partial transformation of desired HA phase to beta-tri-calcium phosphate (β-TCP) phase. It appears that the grain boundary and interface defects formed during MA promote this transformation. It was discovered that doping HA by silicon results in hindering this phase transformation process. The Si-doped HA does not show phase transition to β-TCP or decomposition after heat treatment even at 900°C. PMID:22312324

  9. Synthesis of sodium caseinate-calcium carbonate microspheres and their mineralization to bone-like apatite

    NASA Astrophysics Data System (ADS)

    Xu, Zhewu; Liang, Guobin; Jin, Lin; Wang, Zhenling; Xing, Chao; Jiange, Qing; Zhang, Zhiguang

    2014-06-01

    Phosphoproteins can induce and stabilize calcium carbonate (CaCO3) vaterite, which has desirable features for high reactivity. The purpose of this study was to synthesize bioactive CaCO3 microspheres for bone regeneration. Sodium caseinate (NaCas)-containing CaCO3 microspheres, with the crystal phase of vaterite, were synthesized by fast precipitation in an aqueous solution of CaCl2, Na2CO3, and 2 mg/mL of NaCas. The uniform microspheres exhibited rougher surfaces and lower negative charges than CaCO3 particles without NaCas addition. Fourier-transform infrared spectroscopy (FT-IR) of the microspheres showed characteristic peaks or bands corresponding to phosphate and hydroxyl groups. Thermogravimetric analysis (TGA) curves exhibited approximately 5% weight loss below 600 °C due to the decomposition of NaCas. Scanning electron microscope (SEM) images showed lath-like hydroxyapatite (HAp) on the surface after soaking in simulated body fluid (SBF) at 37 °C for 5 and 10 days. Energy dispersive X-ray spectrometry (EDS) revealed that the agglomerates were composed of Ca, C, O, P, Na, and Mg elements, and the Ca/P ratios ranged from 1.53 to 1.56. X-ray diffraction (XRD) patterns exhibited peaks characteristic of hydroxyapatite. The results of this study demonstrated that the addition of NaCas induced the formation of vaterite microspheres which possesses an enhanced apatite formation after soaking in SBF at 37 °C for 5 and 10 days. These NaCas-CaCO3 microspheres may be a potential biomaterial for bone regeneration.

  10. Electrohydrodynamic coating of metal with nano-sized hydroxyapatite.

    PubMed

    Li, Xiang; Huang, Jie; Ahmad, Zeeshan; Edirisinghe, Mohan

    2007-01-01

    Electrohydrodynamic spray deposition of a hydroxyapatite (HA) suspension consisting of nano-particles has been used to create a hydroxyapatite coating comprising of nanostructured surface topography. Preliminary coating experiments were carried out on an Al substrate and 30 s was found to be the most appropriate coating time. HA coating on titanium for this duration was found to be well-bonded to the substrate after heat-treatment. A thickness of 2 mum was achieved in 30 s and formation of a bone-like apatite on the surface was detected after incubation of the heat-treated coated Ti in simulated body fluid. Therefore, we have uncovered a new procedure by which nano-biomaterials can be deposited on real orthopedic substrates to prepare bioactive thin coatings in a simple and easy manner. PMID:18032815

  11. Effect of Water-Glass Coating on HA and HA-TCP Samples for MSCs Adhesion, Proliferation, and Differentiation.

    PubMed

    Bajpai, Indu; Kim, Duk Yeon; Kyong-Jin, Jung; Song, In-Hwan; Kim, Sukyoung

    2016-01-01

    Ca-P and silicon based materials have become very popular as bone tissue engineering materials. In this study, water-glass (also known as sodium silicate glass) was coated on sintered hydroxyapatite (HA) and HA-TCP (TCP stands for tricalcium phosphate) samples and subsequently heat-treated at 600°C for 2 hrs. X-rays diffraction showed the presence of β- and α-TCP phases along with HA in the HA-TCP samples. Samples without coating, with water-glass coating, and heat-treated after water-glass coating were used to observe the adhesion and proliferation response of bone marrow derived-mesenchymal stem cells (MSCs). Cell culture was carried out for 4 hrs, 1 day, and 7 days. Interestingly, all samples showed similar response for cell adhesion and proliferation up to 7-day culture but fibronectin, E-cadherin, and osteogenic differentiation related genes (osteocalcin and osteopontin) were significantly induced in heat-treated water-glass coated HA-TCP samples. A water-glass coating on Ca-P samples was not found to influence the cell proliferation response significantly but activated some extracellular matrix genes and induced osteogenic differentiation in the MSCs. PMID:27429988

  12. Effect of Water-Glass Coating on HA and HA-TCP Samples for MSCs Adhesion, Proliferation, and Differentiation

    PubMed Central

    Bajpai, Indu; Kim, Duk Yeon; Kyong-Jin, Jung; Song, In-Hwan

    2016-01-01

    Ca-P and silicon based materials have become very popular as bone tissue engineering materials. In this study, water-glass (also known as sodium silicate glass) was coated on sintered hydroxyapatite (HA) and HA-TCP (TCP stands for tricalcium phosphate) samples and subsequently heat-treated at 600°C for 2 hrs. X-rays diffraction showed the presence of β- and α-TCP phases along with HA in the HA-TCP samples. Samples without coating, with water-glass coating, and heat-treated after water-glass coating were used to observe the adhesion and proliferation response of bone marrow derived-mesenchymal stem cells (MSCs). Cell culture was carried out for 4 hrs, 1 day, and 7 days. Interestingly, all samples showed similar response for cell adhesion and proliferation up to 7-day culture but fibronectin, E-cadherin, and osteogenic differentiation related genes (osteocalcin and osteopontin) were significantly induced in heat-treated water-glass coated HA-TCP samples. A water-glass coating on Ca-P samples was not found to influence the cell proliferation response significantly but activated some extracellular matrix genes and induced osteogenic differentiation in the MSCs. PMID:27429988

  13. Preparation of Porous Hydroxyapatite Tablets and Porous Hydroxyapatite Coatings for Orthopaedic Use

    NASA Astrophysics Data System (ADS)

    Méndez-González, M.

    2004-09-01

    Porous hydroxyapatite tablets and coatings on metal substrates were obtained by the addition of polymeric additives and liofilization. Both tablets and coatings were characterized by scanning electron microscopy and x-ray diffraction. Coatings obtained by plasma spraying also exhibited interconnected porous of 100 μm while coatings obtained by laser ablation did not show any porosity. The diffraction patterns of the deposited HA were similar to that of the powder obtained by the precipitation method suggesting that no significant changes occurred during the coating procedure.

  14. Concentrated hydroxyapatite inks for direct-write assembly of 3-D periodic scaffolds.

    PubMed

    Michna, Sarah; Wu, Willie; Lewis, Jennifer A

    2005-10-01

    Hydroxyapatite (HA) scaffolds with a 3-D periodic architecture and multiscale porosity have been fabricated by direct-write assembly. Concentrated HA inks with tailored viscoelastic properties were developed to enable the construction of complex 3-D architectures comprised of self-supporting cylindrical rods in a layer-by-layer patterning sequence. By controlling their lattice constant and sintering conditions, 3-D periodic HA scaffolds were produced with a bimodal pore size distribution. Mercury intrusion porosimetry (MIP) was used to determine the characteristic pore size and volume associated with the interconnected pore channels between HA rods and the finer pores within the partially sintered HA rods. PMID:15878368

  15. Polyvinyl pyridine microspheres

    NASA Technical Reports Server (NTRS)

    Rembaum, Alan (Inventor); Gupta, Amitava (Inventor); Volksen, Willi (Inventor)

    1980-01-01

    Microspheres are produced by cobalt gamma radiation initiated polymerization of a dilute aqueous vinyl pyridine solution. Addition of cross-linking agent provides higher surface area beads. Addition of monomers such as hydroxyethylmethacrylate acrylamide or methacrylamide increases hydrophilic properties and surface area of the beads. High surface area catalytic supports are formed in the presence of controlled pore glass substrate.

  16. Doped zinc oxide microspheres

    DOEpatents

    Arnold, Jr., Wesley D.; Bond, Walter D.; Lauf, Robert J.

    1993-01-01

    A new composition and method of making same for a doped zinc oxide microsphere and articles made therefrom for use in an electrical surge arrestor which has increased solid content, uniform grain size and is in the form of a gel.

  17. Doped zinc oxide microspheres

    DOEpatents

    Arnold, W.D. Jr.; Bond, W.D.; Lauf, R.J.

    1993-12-14

    A new composition and method of making same for a doped zinc oxide microsphere and articles made therefrom for use in an electrical surge arrestor which has increased solid content, uniform grain size and is in the form of a gel. 4 figures.

  18. Fusion microsphere targets

    SciTech Connect

    Koo, J.C.

    1980-07-28

    It was shown that a microsphere within the structure limitations is hydrodynamically stable. To insure its perfect formation, the initial chemical compositions must have a blowing capability, more important, the resultant liquid compositions must also have sufficient surface tension and low viscosity.

  19. Microsphere insulation systems

    NASA Technical Reports Server (NTRS)

    Allen, Mark S. (Inventor); Willen, Gary S. (Inventor); Mohling, Robert A. (Inventor)

    2005-01-01

    A new insulation system is provided that contains microspheres. This insulation system can be used to provide insulated panels and clamshells, and to insulate annular spaces around objects used to transfer, store, or transport cryogens and other temperature-sensitive materials. This insulation system provides better performance with reduced maintenance than current insulation systems.

  20. Polyvinyl pyridine microspheres

    NASA Technical Reports Server (NTRS)

    Rembaum, Alan (Inventor); Gupta, Amitava (Inventor); Volksen, Willi (Inventor)

    1979-01-01

    Microspheres are produced by cobalt gamma radiation initiated polymerization of a dilute aqueous vinyl pyridine solution. Addition of cross-linking agent provides higher surface area beads. Addition of monomers such as hydroxyethylmethacrylate acrylamide or methacrylamide increases hydrophilic properties and surface area of the beads. High surface area catalytic supports are formed in the presence of controlled pore glass substrate.

  1. Effect of Hydrothermal Treatment on Sinterability of Hydroxyapatite

    SciTech Connect

    Kawagoe, D.; Fujimori, H.; Goto, S.; Yamasaki, N.; Ioku, K.

    2006-05-15

    Calcium hydroxyapatite, Ca10(PO4)6(OH)2:HA, is the inorganic principle component of natural bones and teeth. It has been already suggested that the amount of OH ion in the crystal structure of HA is closely related to the biocompatibility. The amount of OH ion in current HA, however, has not been controlled. In order to prepare more functional HA ceramics, the amount of OH ion must be controlled. In this study, HA ceramics with different OH amount were prepared from fine HA crystals by spark plasma sintering (SPS). Fine powder of HA was treated hydrothermally at 200 deg. C for 24 h with pH 10 NH3 aqueous solution. The samples were pressed uniaxialy under 60 MPa, and then they were SPS at 800 deg. C, 900 deg. C and 1000 deg. C for 10 min with the heating rate of 25 deg. C{center_dot}min-1. No phases other than HA were revealed by XRD for the starting samples after hydrothermal treatment and samples after sintering by SPS at 800 deg. C, 900 deg. C and 1000 deg. C for 10 min. The quantity of OH ion in HA ceramics sintered by SPS was decreased with increasing temperature of sintering. Transparent HA ceramics were prepared by SPS at 900 deg. C and 1000 deg. C.

  2. Characterization of porous hydroxyapatite.

    PubMed

    Hing, K A; Best, S M; Bonfield, W

    1999-03-01

    Hydroxyapatite has been considered for use in the repair of osseous defects for the last 20 years. Recent developments have led to interest in the potential of porous hydroxyapatite as a synthetic bone graft. However, despite considerable activity in this field, regarding assessment of the biological response to such materials, the basic materials characterization is often inadequate. This paper documents the characterization of the chemical composition, mechanical integrity, macro- and microstructure of a porous hydroxyapatite, Endobon (E. Merck GmbH), intended for the bone-graft market. Specimens possesed a range of apparent densities from 0.35 to 1.44 g cm(-3). Chemical analysis demonstrated that the natural apatite precursor of Endobon was not converted to pure hydroxyapatite, but retained many of the ionic substituents found in bone mineral, notably carbonate, sodium and magnesium ions. Investigation of the microstructure illustrated that the struts of the material were not fully dense, but had retained some traces of the network of osteocyte lacunae. Macrostructural analysis demonstrated the complex inter-relationship between the structural features of an open pore structure. Both pore size and connectivity were found to be inversely dependent on apparent density. Furthermore, measurement of pore aspect ratio and orientation demonstrated a relationship between apparent density and the degree of macrostructural anisotropy within the specimens, while, it was also noted that pore connectivity was sensitive to anisotropy. Compression testing demonstrated the effect of apparent density and macrostructural anisotropy on the mechanical properties. An increase in apparent density from 0.38 to 1.25 g cm(-3) resulted in increases in ultimate compressive stress and compressive modulus of 1 to 11 MPa and 0.2 to 3.1 GPa, respectively. Furthermore, anisotropic high density (> 0.9 g cm(-3)) specimens were found to possess lower compressive moduli than isotropic specimens

  3. Synthesis of dense nano cobalt-hydroxyapatite by modified electroless deposition technique

    NASA Astrophysics Data System (ADS)

    Mohd Zaheruddin, K.; Rahmat, A.; Shamsul, J. B.; Mohd Nazree, B. D.; Aimi Noorliyana, H.

    2016-07-01

    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 3 % wt Co and gradually decreased at higher Co content.

  4. 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

  5. Electrospun fibrous scaffold of hydroxyapatite/poly (ε-caprolactone) for bone regeneration.

    PubMed

    Li, Lingli; Li, Guang; Jiang, Jianming; Liu, Xiaona; Luo, Li; Nan, Kaihui

    2012-02-01

    Development of fibrous scaffold of hydroxyapatite/biopolymer nanocomposite offers great potential in the field of bone regeneration and tissue engineering. Hydroxyapatite (HA)/poly (ε-caprolactone) (PCL) fibrous scaffolds were successfully prepared by electrospinning dopes containing HA and PCL in this work. It was found that pre-treating HA with γ-glycioxypropyltrimethoxysilane (A-187) was effective in improving HA dispersion both in solutions and in a PCL matrix. Mechanical properties of the scaffolds were greatly enhanced by the filling of A187-HA. The bioactivity of PCL was remarkably improved by the addition of HA and A187-HA. Fibroblasts and osteoblasts were seeded on scaffolds to evaluate the effect of A-187 on biocompatibility of HA/PCL composites. Based on this study, good dispersion of HA in PCL matrix was granted by pretreatment of HA with A-187 and A187-HA/PCL fibrous scaffolds were obtained by electrospinning. These results demonstrated that the scaffolds may possess improved mechanical performance and good bioactivity due to A187-HA incorporation. PMID:22143907

  6. Dual functional selenium-substituted hydroxyapatite.

    PubMed

    Wang, Yanhua; Ma, Jun; Zhou, Lei; Chen, Jin; Liu, Yonghui; Qiu, Zhiye; Zhang, Shengmin

    2012-06-01

    Hydroxyapatite (HA) doped with trace elements has attracted much attention recently owing to its excellent biological functions. Herein, we use a facile co-precipitation method to incorporate selenium into HA by adding sodium selenite during synthesis. The obtained selenium-substituted HA products are needle-like nanoparticles which have  size and crystallinity that are similar to those of the pure HA nanoparticles (HANs) when the selenium content is low. HANs are found to have the ability to induce the apoptosis of osteosarcoma cells, and the anti-tumour effects are enhanced after incorporation of selenium. Meanwhile, the nanoparticles can also support the growth of bone marrow stem cells. Furthermore, the flow cytometric results indicate that the apoptosis induction of osteosarcoma cells is caused by the increased reactive oxygen species and decreased mitochondrial membrane potential. These results show that the selenium-substituted HANs are potentially promising bone graft materials in osteosarcoma treatment due to their dual functions of supporting normal cell growth and inducing tumour cell apoptosis. PMID:23741613

  7. 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.

  8. Synergistic interaction of platelet derived growth factor (PDGF) with the surface of PLLA/Col/HA and PLLA/HA scaffolds produces rapid osteogenic differentiation.

    PubMed

    Raghavendran, Hanumantha Rao Balaji; Mohan, Saktiswaren; Genasan, Krishnamurithy; Murali, Malliga Raman; Naveen, Sangeetha Vasudevaraj; Talebian, Sepehr; McKean, Robert; Kamarul, Tunku

    2016-03-01

    Scaffolds with structural features similar to the extracellular matrix stimulate rapid osteogenic differentiation in favorable microenvironment and with growth factor supplementation. In this study, the osteogenic potential of electrospun poly-l-lactide/hydroxyapatite/collagen (PLLA/Col/HA, PLLA/HA and PLLA/Col) scaffolds were tested in vitro with the supplementation of platelet derived growth factor-BB (PDGF-BB). Cell attachment and topography, mineralization, extracellular matrix protein localization, and gene expression of the human mesenchymal stromal cells were compared between the fibrous scaffolds PLLA/Col/HA, PLLA/Col, and PLLA/HA. The levels of osteocalcin, calcium, and mineralization were significantly greater in the PLLA/Col/HA and PLLA/HA compared with PLLA/Col. High expression of fibronectin, intracellular adhesion molecule, cadherin, and collagen 1 (Col1) suggests that PLLA/Col/HA and PLLA/HA scaffolds had superior osteoinductivity than PLLA/Col. Additionally, osteopontin, osteocalcin, osterix, Runt-related transcription factor 2 (Runx2), and bone morphogenic protein (BMP2) expression were higher in PLLA/Col/HA and PLLA/HA compared with PLLA/Col. In comparison with PLLA/Col, the PLLA/Col/HA and PLLA/HA scaffolds presented a significant upregulation of the genes Runx2, Col 1, Integrin, osteonectin (ON), bone gamma-carboxyglutamic acid-containing protein (BGALP), osteopontin (OPN), and BMP2. The upregulation of these genes was further increased with PDGF-BB supplementation. These results show that PDGF-BB acts synergistically with PLLA/Col/HA and PLLA/HA to enhance the osteogenic differentiation potential. Therefore, this combination can be used for the rapid expansion of bone marrow stromal cells into bone-forming cells for tissue engineering. PMID:26700235

  9. Porous microsphere and its applications

    PubMed Central

    Cai, Yunpeng; Chen, Yinghui; Hong, Xiaoyun; Liu, Zhenguo; Yuan, Weien

    2013-01-01

    Porous microspheres have drawn great attention in the last two decades for their potential applications in many fields, such as carriers for drugs, absorption and desorption of substances, pulmonary drug delivery, and tissue regeneration. The application of porous microspheres has become a feasible way to address existing problems. In this essay, we give a brief introduction of the porous microsphere, its characteristics, preparation methods, applications, and a brief summary of existing problems and research tendencies. PMID:23515359

  10. 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. PMID:26956413

  11. Hydroxyapatite-titanium bulk composites for bone tissue engineering applications.

    PubMed

    Kumar, Alok; Biswas, Krishanu; Basu, Bikramjit

    2015-02-01

    The research work on bulk hydroxyapatite (HA)-based composites are driven by the need to develop biomaterials with better mechanical properties without compromising its bioactivity and biocompatibility properties. Despite several years of research, the mechanical properties of the HA-based composites still need to be enhanced to match the properties of natural cortical bone. In this regard, the scope of this review on the HA-based bulk biomaterials is limited to the processing and the mechanical as well as biocompatibility properties for bone tissue engineering applications of a model system that is hydroxyapatite-titanium (HA-Ti) bulk composites. It will be discussed in this review how HA-Ti based bulk composites can be processed to have better fracture toughness and strength without compromising biocompatibility. The advantages of the functionally gradient materials to integrate the mechanical and biocompatibility properties is a promising approach in hard tissue engineering and has been emphasized here in reference to the limited literature reports. On the biomaterials fabrication aspect, the recent results are discussed to demonstrate that advanced manufacturing techniques, like spark plasma sintering can be adopted as a processing route to restrict the sintering reactions, while enhancing the mechanical properties. Various toughening mechanisms related to careful tailoring of microstructure are discussed. The in vitro cytocompatibilty, cell fate processes as well as in vivo biocompatibility results are also reviewed and the use of flow cytometry to quantify in vitro cell fate processes is being emphasized. PMID:24737723

  12. Effect of hydroxyapatite-based biomaterials on human osteoblast phenotype.

    PubMed

    Trombelli, L; Penolazzi, L; Torreggiani, E; Farina, R; Lambertini, E; Vecchiatini, R; Piva, R

    2010-03-01

    The present study evaluated human primary osteoblasts and two different osteoblast-like cell lines behaviour when cultured in presence of different hydroxyapatite-based (HA) biomaterials (SINTlife-FIN-CERAMICA S.p.a., Faenza, Italy; Bio-Oss, Geistlich Biomaterials, Woulhusen, Switzerland; Biostite-GABA Vebas, San Giuliano Milanese, MI, Italy), focusing attention on the effect of HA/Biostite in terms of modulation of osteoblastic differentiation. Analysis were about adhesion, proliferation and mineralization activity. Runt-related transcription factor 2 (Runx2), Estrogen Receptor alpha (ERalfa) expression and alkaline phosphatase activity (ALP) were measured as osteoblastic differentiation markers. Determination of viable cells was done with MTT colorimetric assay. Scanning electron microscopy (SEM) analysis was performed on biomaterial-treated cells. All hydroxyapatite-based biomaterials didn't affect cells morphology and viability, whereas only presence of HA/Biostite improved cells adhesion, growth and differentiation. Adhesion and spreading of the primary cells on HA/Biostite were the same showed by two different osteoblast-like cell lines. These results have important implications for both tissue-engineered bone grafts and enhancement of HA implants performance, to develop new teeth's supporting structure therapies and replacement. PMID:20357737

  13. Post-translational modification of osteopontin: Effects on in vitro hydroxyapatite formation and growth

    SciTech Connect

    Boskey, Adele L.; Christensen, Brian; Taleb, Hayat; Sorensen, Esben S.

    2012-03-09

    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-length 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.

  14. Influence of manganese doping into HA powders on the properties of its dense bodies.

    PubMed

    Natasha, A N; Sopyan, I; Mel, M; Ramesh, S

    2008-07-01

    The effect of Manganese (Mn) addition on the Vickers hardness and relative density of nanocrystalline hydroxyapatite (HA) dense bodies were studied. The starting Mn doped HA powders was synthesized via sol-gel method with Mn concentration varies from 2 mol% up to 15 mol% Mn. The Mn doped HA disc samples were prepared by uniaxial pressing at 200MPa and subsequently sintered at 1300 degrees C. Characterization was carried out where appropriate to determine the phases present, bulk density, Vickers hardness of the various content of Mn doped HA dense bodies. The addition of Mn was observed to influence the color appearance of the powders and dense bodies as well. Higher Mn concentration resulted in dark grey powders. It was also found that the hardness and relative density of the material increased as the Mn content increased and influenced by the crystallinity of the prepared Mn doped HA powders. PMID:19024996

  15. 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.

  16. Strontium-substituted hydroxyapatite coatings deposited via a co-deposition sputter technique.

    PubMed

    Boyd, A R; Rutledge, L; Randolph, L D; Meenan, B J

    2015-01-01

    The bioactivity of hydroxyapatite (HA) coatings can be modified by the addition of different ions, such as silicon (Si), lithium (Li), magnesium (Mg), zinc (Zn) or strontium (Sr) into the HA lattice. Of the ions listed here, strontium substituted hydroxyapatite (SrHA) coatings have received a lot of interest recently as Sr has been shown to promote osteoblast proliferation and differentiation, and reduce osteoclast activity. In this study, SrHA coatings were deposited onto titanium substrates using radio frequency (RF) magnetron co-sputtering (and compared to those surfaces deposited from HA alone). FTIR, XPS, XRD, and SEM techniques were used to analyse the different coatings produced, whereby different combinations of pure HA and 13% Sr-substituted HA targets were investigated. The results highlight that Sr could be successfully incorporated into the HA lattice to form SrHA coatings. It was observed that as the number of SrHA sputtering targets in the study were increased (increasing Sr content), the deposition rate decreased. It was also shown that as the Sr content of the coatings increased, so did the degree of preferred 002 orientation of the coating (along with obvious changes in the surface morphology). This study has shown that RF magnetron sputtering (specifically co-sputtering), offers an appropriate methodology to control the surface properties of Sr-substituted HA, such as the crystallinity, stoichiometry, phase purity and surface morphology. PMID:25491990

  17. Preparation and Comprehensive Characterization of a Calcium Hydroxyapatite Reference Material

    PubMed Central

    Markovic, Milenko; Fowler, Bruce O.; Tung, Ming S.

    2004-01-01

    Numerous biological and chemical studies involve the use of calcium hydroxyapatite (HA), Ca10(PO4)6(OH)2. In this study detailed physicochemical characterization of HA, prepared from an aqueous solution, was carried out employing different methods and techniques: chemical and thermal analyses, x-ray diffraction, infrared and Raman spectroscopies, scanning and transmission microscopies, and Brunauer, Emmett, and Teller (BET) surface-area method. The contents of calcium (Ca2+), phosphate (PO43−), hydroxide (OH−), hydrogenphosphate (HPO42−), water (H2O), carbonate (CO32−), and trace constituents, the Ca/P molar ratio, crystal size and morphology, surface area, unit-cell parameters, crystallinity, and solubility of this HA were determined. This highly pure, homogeneous, and highly crystalline HA is certified as a National Institute of Standards and Technology (NIST) standard reference material, SRM 2910. PMID:27366634

  18. Functional magnetic microspheres

    NASA Technical Reports Server (NTRS)

    Yen, Shiao-Ping S. (Inventor); Rembaum, Alan (Inventor); Landel, Robert F. (Inventor)

    1981-01-01

    Functional magnetic particles are formed by dissolving a mucopolysaccharide such as chitosan in acidified aqueous solution containing a mixture of ferrous chloride and ferric chloride. As the pH of the solution is raised magnetite is formed in situ in the solution by raising the pH. The dissolved chitosan is a polyelectrolyte and forms micelles surrounding the granules at pH of 8-9. The chitosan precipitates on the granules to form microspheres containing the magnetic granules. On addition of the microspheres to waste aqueous streams containing dissolved ions, the hydroxyl and amine functionality of the chitosan forms chelates binding heavy metal cations such as lead, copper, and mercury and the chelates in turn bind anions such as nitrate, fluoride, phosphate and borate.

  19. Characterisations of collagen-silver-hydroxyapatite nanocomposites

    NASA Astrophysics Data System (ADS)

    Ciobanu, C. S.; Popa, C. L.; Petre, C. C.; Jiga, G.; Trusca, R.; Predoi, D.

    2016-05-01

    The XRD analysis were performed to confirm the formation of hydroxyapatite structure in collagen-silver-hydroxyapatite nanocomposites. The molecular interaction in collagen-hydroxyapatite nanocomposites was highlighted by Fourier transform infrared spectroscopy (FTIR) analysis. The SEM showed a nanostructure of collagen-silverhydroxyapatite nanocomposites composed of nano needle-like particles in a veil with collagen texture. The presence of vibrational groups characteristics to the hydroxyapatite structure in collagen-silver-hydroxyapatite (AgHApColl) nanocomposites was investigated by FTIR.

  20. Trading polymeric microspheres: exchanging DNA molecules via microsphere interaction.

    PubMed

    Morimoto, Nobuyuki; Muramatsu, Kanna; Nomura, Shin-ichiro M; Suzuki, Makoto

    2015-04-01

    A new class of artificial molecular transport system is constructed by polymeric microspheres. The microspheres are prepared by self-assembly of poly(ethylene glycol)-block-poly(3-dimethyl(methacryloyloxyethyl)ammonium propane sulfonate), PEG-b-PDMAPS, by intermolecular dipole-dipole interaction of sulfobetaine side chains in water. Below the upper critical solution temperature (UCST) of PEG-b-PDMAPS, the microspheres (∼1μm) interact with other microspheres by partial and transit fusion. In order to apply the interaction between microspheres, a 3'-TAMRA-labeled single-stranded DNA oligomer (ssDNA) is encapsulated into a PEG-b-PDMAPS microsphere by thermal treatment. The exchange of ssDNA between microspheres is confirmed by fluorescence resonance energy transfer (FRET) quenching derived from double-stranded formation with complementary 5'-BHQ-2-labeled ssDNA encapsulated in PEG-b-PDMAPS microspheres. The exchange rate of ssDNA is controllable by tuning the composition of the polymer. The contact-dependent transport of molecules can be applied in the areas of microreactors, sensor devices, etc. PMID:25731098

  1. Osteoblast response to hydroxyapatite doped with divalent and trivalent cations.

    PubMed

    Webster, Thomas J; Massa-Schlueter, Elizabeth A; Smith, Jennifer L; Slamovich, Elliot B

    2004-05-01

    The present in vitro study doped hydroxyapatite (HA) with various metal cations (Mg(2+), Zn(2+), La(3+), Y(3+), In(3+), and Bi(3+)) in an attempt to enhance properties of HA pertinent to orthopedic and dental applications. X-ray diffraction material characterization indicated that the metal cations may have substituted for calcium in the HA crystal structure and that all of the doped HA formulations were single-phase and crystalline. Scanning electron microscopy analysis revealed a variety of grain sizes, depending on the dopant utilized. Energy-dispersive spectroscopy confirmed that the dopants added during synthesis were present and that all of the HA formulations synthesized were within the defined range of HA phase in the CaO-P(2)O(5)-H(2)O system. Lastly, Bi-doped HA had a slower dissolution rate than either undoped HA or HA doped with other cations when exposed to simulated physiological conditions for 21 days. In terms of cell function, results provided the first evidence that osteoblasts, bone-forming cells, adhered and differentiated (as measured by alkaline phosphatase synthesis) in response to HA doped with trivalent cations (specifically, La(3+), Y(3+), In(3+), Bi(3+)) at earlier time points than either HA doped with divalent cations (Mg(2+), Zn(2+)) or undoped HA. Of the dopants examined, Bi(3+) most enhanced osteoblast long-term calcium-containing mineral deposition. For these reasons, this study revealed for the first time the potential benefits of doping HA with Bi(3+) according to criteria critical for bone prosthetic clinical success. PMID:14741626

  2. Biological reactivity of zirconia-hydroxyapatite composites.

    PubMed

    Silva, Viviane V; Lameiras, Fernando S; Lobato, Zélia I P

    2002-01-01

    Materials and devices intended for end-use applications as implants and medical devices must be evaluated to determine their biocompatibility potential in contact with physiological systems. The use of standard practices of biological testing provides a reasonable level of confidence concerning the response of a living organism to a given material or device, as well as guidance in selecting the proper procedures to be carried out for the screening of new or modified materials. This article presents results from cytotoxicity assays of cell culture, skin irritation, and acute toxicity by systemic and intracutaneous injections for powders, ceramic bodies, and extract liquids of hydroxyapatite (HA), calcia partially stabilized zirconia (ZO), and two types of zirconia-hydroxyapatite composites (Z4H6 and Z6H4) with potential for future use as orthopedic and dental implants. They indicate that these materials present potential for this type of application because they meet the requirements of the standard practices recommended for evaluating the biological reactivity of ATCC cell cultures (CCL1 NCTC clone 929 of mouse connective tissue and CCL 81 of monkey connective tissue) and animals (rabbit and mouse) with direct or indirect patient contact, or by the injection of specific extracts prepared from the material under test. In addition, studies involving short-term intramuscular and long-term implantation assays to estimate the reaction of living tissue to the composites studied, and investigations on long-term effects that these materials can cause on the cellular metabolism, are already in progress. PMID:12209904

  3. Mechanical properties and in vitro response of strontium-containing hydroxyapatite/polyetheretherketone composites.

    PubMed

    Wong, K L; Wong, C T; Liu, W C; Pan, H B; Fong, M K; Lam, W M; Cheung, W L; Tang, W M; Chiu, K Y; Luk, K D K; Lu, W W

    2009-08-01

    Strontium-containing hydroxyapatite/polyetheretherketone (Sr-HA/PEEK) composites were developed as alternative materials for load-bearing orthopaedic applications. The amount of strontium-containing hydroxyapatite (Sr-HA) incorporated into polyetheretherketone (PEEK) polymer matrix ranged from 15 to 30 vol% and the composites were successfully fabricated by compression molding technique. This study presents the mechanical properties and in vitro human osteoblast-like cell (MG-63) response of the composite material developed. The bending modulus and strength of Sr-HA/PEEK composites were tailored to mimic human cortical bone. PEEK reinforced with 25 and 30 vol% Sr-HA exhibited bending modulus of 9.6 and 10.6 GPa, respectively; alternatively, the bending strengths of the composites were 93.8 and 89.1 MPa, respectively. Based on the qualitative comparison of apatite formation in SBF and quantitative measurement of MG-63-mediated mineralization in vitro, the Sr-HA/PEEK composite was proven to outperform HA/PEEK in providing bioactivity. However, no difference was found in the trend of cell proliferation and alkaline phosphatase activity between different composites. Strontium, in the form of strontium-containing hydroxyapatite (Sr-HA), was confirmed to enhance bioactivity in the PEEK composites. PMID:19427032

  4. 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.

  5. Deposition of titanium nitride and hydroxyapatite-based biocompatible composite by reactive plasma spraying

    NASA Astrophysics Data System (ADS)

    Roşu, Radu Alexandru; Şerban, Viorel-Aurel; Bucur, Alexandra Ioana; Dragoş, Uţu

    2012-02-01

    Titanium nitride is a bioceramic material successfully used for covering medical implants due to the high hardness meaning good wear resistance. Hydroxyapatite is a bioactive ceramic that contributes to the restoration of bone tissue, which together with titanium nitride may contribute to obtaining a superior composite in terms of mechanical and bone tissue interaction matters. The paper presents the experimental results in obtaining composite layers of titanium nitride and hydroxyapatite by reactive plasma spraying in ambient atmosphere. X-ray diffraction analysis shows that in both cases of powders mixtures used (10% HA + 90% Ti; 25% HA + 75% Ti), hydroxyapatite decomposition occurred; in variant 1 the decomposition is higher compared with the second variant. Microstructure of the deposited layers was investigated using scanning electron microscope, the surfaces presenting a lamellar morphology without defects such as cracks or microcracks. Surface roughness values obtained vary as function of the spraying distance, presenting higher values at lower thermal spraying distances.

  6. Chemical characterization of some substituted hydroxyapatites

    PubMed Central

    2011-01-01

    Synthetic multi-substituted hydroxyapatite nano powders containing silicon and or carbonate prepared by a wet chemical method. The process parameters are set up to allow the simultaneous substitution of carbonate and silicon ions in the place of phosphorus. The chemical and structural characterizations of the prepared powders are determined with the aid of; XRF, ICP, XRD and FTIR. The results show that, the ion substitution in the crystal lattice of HA caused a change in the unit cell dimensions and affected the degree of crystallization of the produced powders. The apatite formation abilityy of the prepared discs from the synthesized powders is determined by immersing in SBF solution for different periods. The degree of ion release was determined in the obtained solutions. The examined surface of the immersed discs under SEM and analyzed by CDS showed a more dense HA layer than those of un-substituted ones. The HA with the substituted silicon and carbonate ions, showed the highest solubility with greater rate of ion release, compared with carbonate-free powder. All prepared powders took sodium ion from the SBF solution during immersion, which was not recorded before. PMID:22122971

  7. Synthesis of nano-hydroxyapatite and its rapid mediated surface functionalization by silane coupling agent.

    PubMed

    Rehman, Sarish; Khan, Kishwar; Mujahid, Mohammad; Nosheen, Shaneela

    2016-01-01

    In this work, hydroxyapatite (HA) nanorods were synthesized by simple one step wet precipitation method followed by their rapid surface functionalization via aminopropyltriethoxysilane (APTS) to give modified (HA-APTS) product. Functionalized hydroxyapatite (HA-APTS) holds amino groups on their surface that can be further functionalized with other bioactive molecules. The extent of functionalization of HA was studied under three different processing conditions; at room temperature, at 80 °C and under microwave condition (600 W). Three different temperatures have been use for the purpose of comparison between the functionalized products so that we can judge that whether there is any effect of temperature on the final products. In the last we conclude that temperature has no effect. So microwave condition is best to carried out the functionalization in just 5 min. PMID:26478359

  8. Synthesis and characterization of hydroxyapatite from fish bone waste

    NASA Astrophysics Data System (ADS)

    Marliana, Ana; Fitriani, Eka; Ramadhan, Fauzan; Suhandono, Steven; Yuliani, Keti; Windarti, Tri

    2015-12-01

    Waste fish bones is a problem stemming from activities in the field of fisheries and it has not been used optimally. Fish bones contain calcium as natural source that used to synthesize hydroxyapatite (HA). In this research, HA synthesized from waste fish bones as local wisdom in Semarang. The goal are to produce HA with cheaper production costs and to reduce the environmental problems caused by waste bones. The novelty of this study was using of local fish bone as a source of calcium and simple method of synthesis. Synthesis process of HA can be done through a maceration process with firing temperatures of 1000°C or followed by a sol-gel method with firing at 550°C. The results are analyzed using FTIR (Fourier Transform Infrared), XRD (X-Ray Diffraction) and SEM-EDX (Scanning Electron Microscopy-Energy Dispersive X-Ray). FTIR spectra showed absorption of phosphate and OH group belonging to HA as evidenced by the results of XRD. The average grain size by maceration and synthesized results are not significant different, which is about 69 nm. The ratio of Ca/P of HA by maceration result is 0.89, then increase after continued in the sol-gel process to 1.41. Morphology of HA by maceration results are regular and uniform particle growth, while the morphology of HA after the sol-gel process are irregular and agglomerated.

  9. Nanocomposite bone scaffolds based on biodegradable polymers and hydroxyapatite.

    PubMed

    Becker, Johannes; Lu, Lichun; Runge, M Brett; Zeng, Heng; Yaszemski, Michael J; Dadsetan, Mahrokh

    2015-08-01

    In tissue engineering, development of an osteoconductive construct that integrates with host tissue remains a challenge. In this work, the effect of bone-like minerals on maturation of pre-osteoblast cells was investigated using polymer-mineral scaffolds composed of poly(propylene fumarate)-co-poly(caprolactone) (PPF-co-PCL) and nano-sized hydroxyapatite (HA). The HA of varying concentrations was added to an injectable formulation of PPF-co-PCL and the change in thermal and mechanical properties of the scaffolds was evaluated. No change in onset of degradation temperature was observed due to the addition of HA, however compressive and tensile moduli of copolymer changed significantly when HA amounts were increased in composite formulation. The change in mechanical properties of copolymer was found to correlate well to HA concentration in the constructs. Electron microscopy revealed mineral nucleation and a change in surface morphology and the presence of calcium and phosphate on surfaces was confirmed using energy dispersive X-ray analysis. To characterize the effect of mineral on attachment and maturation of pre-osteoblasts, W20-17 cells were seeded on HA/copolymer composites. We demonstrated that cells attached more to the surface of HA containing copolymers and their proliferation rate was significantly increased. Thus, these findings suggest that HA/PPF-co-PCL composite scaffolds are capable of inducing maturation of pre-osteoblasts and have the potential for use as scaffold in bone tissue engineering. PMID:25504776

  10. Biomedical nanocomposites of hydroxyapatite/polycaprolactone obtained by surfactant mediation.

    PubMed

    Kim, Hae-Won

    2007-10-01

    The composite approach to combining bioactive ceramic and degradable polymer is a promising strategy in the development of bone regenerative matrices. Moreover, in the fabrication of composites, the nanoscale organization of each component should improve the level of structural integration as well as the resultant mechanical and biological properties. The aim of this study was to develop a novel nanocomposite system consisting of hydroxyapatite (HA) and poly(epsilon-caprolactone) (PCL), wherein the HA nanoparticles were uniformly dispersed within the PCL matrix. The strategy was based on applying an amphiphilic surfactant, oleic acid in this case, between the HA and PCL. Oleic acid, which belongs to the fatty acid family and is generally noncytotoxic at the levels used in this study, is believed to mediate the interaction between the hydrophilic HA and hydrophobic PCL. With the mediation of oleic acid, the HA nanoparticles were distributed uniformly within the PCL matrix on the nanoscale (distributed particle size of less than 1 microm), which is in marked contrast to the conventionally mixed HA-PCL composite, in which the HA particles were severely agglomerated. The developed nanocomposite had significantly higher mechanical strength than did the conventional composite and the pure PCL. Moreover, the osteoblastic cells showed a better proliferation behavior on the nanocomposite than on the conventional composite. This HA-PCL nanocomposite mediated by oleic acid is expected to be useful in the bone regeneration field. Moreover, this methodology is applicable to the nanocomposite processing of other biomedical materials. PMID:17390319

  11. Synthesis and characterization of hydroxyapatite from fish bone waste

    SciTech Connect

    Marliana, Ana Fitriani, Eka; Ramadhan, Fauzan; Suhandono, Steven; Yuliani, Keti; Windarti, Tri

    2015-12-29

    Waste fish bones is a problem stemming from activities in the field of fisheries and it has not been used optimally. Fish bones contain calcium as natural source that used to synthesize hydroxyapatite (HA). In this research, HA synthesized from waste fish bones as local wisdom in Semarang. The goal are to produce HA with cheaper production costs and to reduce the environmental problems caused by waste bones. The novelty of this study was using of local fish bone as a source of calcium and simple method of synthesis. Synthesis process of HA can be done through a maceration process with firing temperatures of 1000°C or followed by a sol-gel method with firing at 550°C. The results are analyzed using FTIR (Fourier Transform Infrared), XRD (X-Ray Diffraction) and SEM-EDX (Scanning Electron Microscopy-Energy Dispersive X-Ray). FTIR spectra showed absorption of phosphate and OH group belonging to HA as evidenced by the results of XRD. The average grain size by maceration and synthesized results are not significant different, which is about 69 nm. The ratio of Ca/P of HA by maceration result is 0.89, then increase after continued in the sol-gel process to 1.41. Morphology of HA by maceration results are regular and uniform particle growth, while the morphology of HA after the sol-gel process are irregular and agglomerated.

  12. Luminescence studies of rare-earth doped and Co-doped hydroxyapatite

    NASA Astrophysics Data System (ADS)

    Vasugi, G.; Thamizhavel, A.; Girija, E. K.

    2012-06-01

    Rare-earth doped and co-doped hydroxyapatite (Eu: HA, Eu-Y: HA) were prepared by wet precipitation method by using CTAB as the organic modifier. The synthesized samples were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), Scanning electron microscopy (SEM) and Photoluminescence spectra (PL). Upon excitation at 350 nm the samples Eu: HA and Eu-Y: HA shows the emission band in the visible region, which makes it suitable for potential application such as bio-imaging.

  13. Deposition of hydroxyapatite thin films by Nd:YAG laser ablation: a microstructural study

    SciTech Connect

    Nistor, L.C.; Ghica, C.; Teodorescu, V.S.; Nistor, S.V. . E-mail: snistor@alpha1.infim.ro; Dinescu, M.; Matei, D.; Frangis, N.; Vouroutzis, N.; Liutas, C.

    2004-11-02

    Hydroxyapatite (HA) thin films has been successfully deposited by Nd:YAG laser ablation at {lambda} = 532 nm. The morphology and microstructure of the deposited layers was studied by scanning electron microscopy (SEM), transmission electron microscopy (TEM) and high resolution electron microscopy (HREM). Polycrystalline HA films were directly obtained with the substrate at 300 deg. C and without introducing water vapors in the deposition chamber. Electron paramagnetic resonance (EPR) measurements show that the oxygen stoichiometry in the HA films is also maintained. Depositions performed at {lambda} = 335 nm laser wavelength and 300 deg. C substrate temperature resulted in polycrystalline layers of mixed composition of HA and tricalciumphosphate (TCP)

  14. Metal containing polymeric functional microspheres

    NASA Technical Reports Server (NTRS)

    Yen, Shiao-Ping S. (Inventor); Rembaum, Alan (Inventor); Molday, Robert S. (Inventor)

    1979-01-01

    Polymeric functional microspheres containing metal or metal compounds are formed by addition polymerization of a covalently bondable olefinic monomer such as hydroxyethylmethacrylate in the presence of finely divided metal or metal oxide particles, such as iron, gold, platinum or magnetite, which are embedded in the resulting microspheres. The microspheres can be covalently bonded to chemotherapeutic agents, antibodies, or other proteins providing a means for labeling or separating labeled cells. Labeled cells or microspheres can be concentrated at a specific body location such as in the vicinity of a malignant tumor by applying a magnetic field to the location and then introducing the magnetically attractable microspheres or cells into the circulatory system of the subject. Labeled cells can be separated from a cell mixture by applying a predetermined magnetic field to a tube in which the mixture is flowing. After collection of the labeled cells, the magnetic field is discontinued and the labeled sub-cell population recovered.

  15. Immunofluorescence detection methods using microspheres

    NASA Astrophysics Data System (ADS)

    Szurdoki, Ferenc; Michael, Karri L.; Agrawal, Divya; Taylor, Laura C.; Schultz, Sandra L.; Walt, David R.

    1999-01-01

    Microsphere-based immunoassays were devised for compounds of agricultural and biomedical interest (e.g., digoxin, theophylline, and zearalenone). Commercially available microspheres with surface functional groups for chemical derivatization were used as solid carriers. After immobilizing the target substances, the surface of the haptenized microspheres was blocked by a protein to reduce aspecific binding. Competitive immunoassays were performed using the functionalized microspheres and antibodies labeled with horseradish peroxidase. Immunofluorescence signal amplification was achieved by enzyme-catalyzed reporter deposition (CARD). An epifluorescence microscope, a CCD camera interfaced with a computer, and microscopy image analysis software were employed for quantitative detection of fluorescent light emitted from individual microspheres. Integration of several such immunoassays and application of an optical encoding method enabled multianalyte determination. These immunoassays can also be utilized in an immunosensor array format. This immunoarray format could facilitate miniaturization and automation of multianalyte immunoassays.

  16. Real-Time Protein and Cell Binding Measurements on Hydroxyapatite Coatings.

    PubMed

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

    2016-01-01

    Although a lot of in vitro and in vivo assays have been performed during the last few decades years for hydroxyapatite bioactive coatings, there is a lack of exploitation of real-time in vitro interaction measurements. In the present work, real-time interactions for a plasma sprayed hydroxyapatite coating were measured by a Multi-Parametric Surface Plasmon Resonance (MP-SPR), and the results were compared with standard traditional cell viability in vitro assays. MP-SPR is proven to be suitable not only for measurement of molecule-molecule interactions but also molecule-material interaction measurements and cell interaction. Although SPR is extensively utilized in interaction studies, recent research of protein or cell adsorption on hydroxyapatite coatings for prostheses applications was not found. The as-sprayed hydroxyapatite coating resulted in 62.4% of crystalline phase and an average thickness of 24 ± 6 μm. The MP-SPR was used to measure lysozyme protein and human mesenchymal stem cells interaction to the hydroxyapatite coating. A comparison between the standard gold sensor and Hydroxyapatite (HA)-plasma coated sensor denoted a clearly favourable cell attachment on HA coated sensor as a significantly higher signal of cell binding was detected. Moreover, traditional cell viability and proliferation tests showed increased activity with culture time indicating that cells were proliferating on HA coating. Cells show homogeneous distribution and proliferation along the HA surface between one and seven days with no significant mortality. Cells were flattened and spread on rough surfaces from the first day, with increasing cytoplasmatic extensions during the culture time. PMID:27618911

  17. Bioactive glass/hydroxyapatite composites: mechanical properties and biological evaluation.

    PubMed

    Bellucci, Devis; Sola, Antonella; Anesi, Alexandre; Salvatori, Roberta; Chiarini, Luigi; Cannillo, Valeria

    2015-06-01

    Bioactive glass/hydroxyapatite composites for bone tissue repair and regeneration have been produced and discussed. The use of a recently developed glass, namely BG_Ca/Mix, with its low tendency to crystallize, allowed one to sinter the samples at a relatively low temperature thus avoiding several adverse effects usually reported in the literature, such as extensive crystallization of the glassy phase, hydroxyapatite (HA) decomposition and reaction between HA and glass. The mechanical properties of the composites with 80wt.% BG_Ca/Mix and 20wt.% HA are sensibly higher than those of Bioglass® 45S5 reference samples due to the presence of HA (mechanically stronger than the 45S5 glass) and to the thermal behaviour of the BG_Ca/Mix, which is able to favour the sintering process of the composites. Biocompatibility tests, performed with murine fibroblasts BALB/3T3 and osteocites MLO-Y4 throughout a multi-parametrical approach, allow one to look with optimism to the produced composites, since both the samples themselves and their extracts do not induce negative effects in cell viability and do not cause inhibition in cell growth. PMID:25842126

  18. Titanium--hydroxyapatite porous structures for endosseous applications.

    PubMed

    Popa, C; Simon, V; Vida-Simiti, I; Batin, G; Candea, V; Simon, S

    2005-12-01

    Materials for uncemented endosseous implants have to assure an as short as possible osseointegration time. Thus, a material with both surface bioactivity and a porous outer structure can become a preferred choice for this type of applications. This paper presents a class of titanium-base PM composites, reinforced with particulate hydroxyapatite. Raw materials were titanium powder, obtained through hydriding--milling--dehydriding, with the grain size of 63-100 microm, and sol-gel hydroxyapatite (HA) powder, produced by the reaction between Ca(NO3)2 x 4H2O and (NH4)2HPO4. Blends with 5 to 50% HA were prepared and pressed in a rigid die, producing single composition or gradual composition samples. The applied pressure was of 400, 500 or 600 MPa. Sintering was performed in vacuum, at 1160 ( composite function)C. All samples, although well sintered, displayed swelling during sintering, due to diffusion into the matrix. The increase in volume is more severe for higher amounts of HA in the green compacts and for higher applied compaction pressure. Compacts with a gradual increase of the HA content are recommended from the functional and mechanical point of view, but the increase should be slow, not to produce interlayer cracks. The outer surface shows interconnected pores, suitable for the ingrowth of vital new bone. PMID:16362217

  19. In vivo response to HA-polyhydroxybutyrate/polyhydroxyvalerate composite.

    PubMed

    Luklinska, Z B; Schluckwerder, H

    2003-08-01

    This study examined the morphological and compositional structure of bone-implant interfaces after in vivo implantation into the tibias of rabbits. The implants were composed of biodegradable polyhydroxybutyrate/polyhydroxyvalerate copolymer reinforced with synthetic hydroxyapatite (HA) particles. Optical and scanning electron microscopy techniques were used, including energy-dispersive X-ray analysis. The interface was found to be morphologically, biologically and chemically active throughout the period of study. There was a strong tendency to rebuild the bone structure at the interface after implantation, independent of the composition of the implant, but direct bone bonding with the implant depended on the bioactive nature of the interface, as represented by the HA particles. At all implantation times, lamellar bone formed at the interface and replaced degrading polymer matrix, while engulfing HA filler particles. In regions about 50-100 from the interface, the bone region displayed an osteon organization. Osteoblasts and osteocytes were identified throughout the interface region. The thickness of the newly formed bone significantly increased over the period of the experiment from about 130 microm at 1 month to about 770 microm at 6 months. Materials that behave in this manner may be useful in some bone replacement therapies. PMID:12887706

  20. The influence of hydroxyapatite particles on osteoclast cell activities.

    PubMed

    Sun, J S; Lin, F H; Hung, T Y; Tsuang, Y H; Chang, W H; Liu, H C

    1999-06-15

    Aseptic loosening after total joint arthroplasty is a major problem in orthopedic surgery. Small particles from material wear have been reported as the main cause of implant failure. For this reason, investigation into possible wear particles from the materials used in the implant may lead to longevity after arthroplasty. Hydroxyapatite (HA) has been extensively investigated and reported as an excellent biomaterial with excellent biocompatibility. In this study, we used an in vitro osteoblast/osteoclast model to test the biocompatibility of various-sized HA particles. Primary osteoclasts/osteoblasts were co-cultured with different-sized HA particles (0.5-3.0 microm, 37-53 microm, 177-205 microm, and 420-841 microm) for 3 h, 1 day, 3 days, and 7 days. Cellular responses to the HA particles were evaluated by changes in cell counts and the secretion of transforming growth factor (TGF-beta1), alkaline phosphatase (ALP), tumor necrosis factor (TNF-alpha), prostaglandin (PGE2), and lactate dehydrogenase (LDH) in the supernatant of the culture media. The results showed that osteoblasts/osteoclasts co-cultured with HA particles smaller than 53 microm undergo the most significant changes. Cellular counts significantly decreased, and the changes were more obvious in the osteoblast population. There also was a significant decrease in TGF-beta1 concentration and a significant increase in PGE2 and LDH concentration, but there were no changes in the TNF-alpha or ALP titer. It can be concluded that larger HA particles may be quite compatible with bone cells while smaller-sized HA particles can both activate the osteoclasts and decrease the cell population of the osteoblasts. Justification for the additional expense incurred with the use of hydroxyapatite in primary total hip arthroplasty should be further evaluated. PMID:10321703

  1. Omnifit-HA stem in total hip arthroplasty. A 2- to 5-year followup.

    PubMed

    D'Lima, D D; Walker, R H; Colwell, C W

    1999-06-01

    Outcomes of the first 60 noncemented Omnifit-HA total hip arthroplasties in 56 patients were studied prospectively for 2 to 5 years. The femoral prosthesis had a proximal third circumferential hydroxyapatite coated surface treatment. The acetabular component was a hemispheric modular, porous, nonhydroxyapatite press fit cup, supplemented with screw fixation. One cup was revised for recurrent dislocation, with no femoral revisions. The mean Harris hip score was 54 (range, 20-76) before surgery and 96 (range, 83-100) at final followup, with all patients having an excellent or good outcome. Mild thigh pain occurred in 6% of hips. Subsidence occurred in 9% of hips (range, 1-2.8 mm); in all cases, subsidence was nonprogressive after 1 year. Stable bone ingrowth fixation was evident at the hydroxyapatite coated portion in 100%. A sclerotic reactive line adjacent to the nonhydroxyapatite portion of the stem occurred in 81% but was not adjacent to the hydroxyapatite coated portion of any stem. Endosteal condensation occurred in 90% and correlated with a higher Harris hip score (mean score, 96 with, 91 without). Endosteal lysis adjacent to or distal to the hydroxyapatite coating did not occur. Lytic lesions at the calcar occurred in 19% and correlated with a greater linear acetabular polyethylene wear rate (mean, 0.30 mm/year with lytic lesions, 0.17 mm/year without). This noncemented stem with proximal third hydroxyapatite coating showed excellent short term clinical and radiographic outcome. Absence of distal endosteal lysis, along with correlation of calcar erosion to polyethylene wear, suggests that early circumferential bony ingrowth afforded by hydroxyapatite coating prevents distal endosteal access to polyethylene debris at short term followup. PMID:10379318

  2. Osteoblast response to the surface of amino acid-functionalized hydroxyapatite.

    PubMed

    Lee, Wing-Hin; Loo, Ching-Yee; Chrzanowski, Wojciech; Rohanizadeh, Ramin

    2015-06-01

    Interactions between proteins and the surface of biomaterials are crucial for the biological function and success of materials implanted in the human body. In this study, hydroxyapatite (HA) with negative and positive surface charges were fabricated by functionalizing the HA surface with acidic or basic amino acids. The influence of HA surface charge on protein adsorption and cell activities was studied. The crystallinity, morphology, and surface charge of amino acid-functionalized HA (AA-HA) particles and the stability of amino acids on the HA surface were determined. Both AA-HA and unmodified HA were studied for their capacity to adsorb proteins present in biological medium. The results showed that the presence of glutamic acid; Glu (acidic amino acids) and arginine; Arg (basic amino acids) on the HA surface resulted in higher protein adsorption owing to stronger electrostatic attraction between the HA particles and the proteins in medium. Functionalizing HA with Glu and Arg significantly promoted osteoblast adhesion on the surface of treated HA. No significant differences in cell proliferation between negatively and positively charged HA was observed. Significantly higher alkaline phosphatase (ALP) activity of osteoblasts on both charged surfaces was seen as compared to the unmodified HA. The study demonstrated that immobilization of amino acids (Glu and Arg) on the surface of HA promoted osteoblast proliferation and ALP activity. PMID:25346517

  3. 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. PMID:26952486

  4. Characterization of Sr-substituted hydroxyapatite thin film by sputtering technique from mixture targets of hydroxyapatite and strontium apatite.

    PubMed

    Ozeki, K; Goto, T; Aoki, H; Masuzawa, T

    2014-01-01

    Sr-substituted hydroxyapatite thin films were prepared by sputtering technique from mixture targets of hydroxyapatite (HA) and strontium apatite (SrAp). The HA and SrAp powders were mixed at 0-100% Sr/(Sr+Ca) target ratios. The coated films were recrystallized by a hydrothermal treatment to reduce film dissolution. The films were then characterized by X-ray diffractometry (XRD), scanning electron microscopy (SEM) and inductively coupled plasma atomic emission spectrometry (ICP). The osteocompatiblity of the films was also evaluated by the size of the bone formation area in osteoblast cells.In the XRD patterns, peaks shifted to lower 2θ values with increasing Sr/(Sr+Ca) target ratios, which indicated Sr incorporation into the HA lattice. In the SEM observation of the hydrothermally treated films, the surface was covered with globular particles, and the size of the globular particles increased from Sr0 to Sr40, and then the size decreased from Sr60 to Sr100. The ICP analysis showed that the Sr/(Sr+Ca) film ratios were almost the same as the target ratios. In the cell culture, the bone formation area on the Sr-substituted HA films increased with increasing Sr concentration, and saturated at Sr60. PMID:24642972

  5. 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. PMID:26083784

  6. A study on improving mechanical properties of porous HA tissue engineering scaffolds by hot isostatic pressing.

    PubMed

    Zhao, Jing; Xiao, Suguang; Lu, Xiong; Wang, Jianxin; Weng, Jie

    2006-12-01

    Various interconnected porous hydroxyapatite (HA) ceramic scaffolds are universally used to induct the tissue growth for bone repair and replacement, and serve to support the adhesion, transfer, proliferation and differentiation of cells. Impregnation of polyurethane sponges with a ceramic slurry is adopted to produce highly porous HA ceramic scaffolds with a 3D interconnected structure. However, high porosity always accompanies a decrease in the strength of the HA ceramic scaffolds. Therefore, it is significant to improve the strength of the HA ceramic scaffolds with highly interconnected porosity so that they are more suitable in clinical applications. In this work, highly porous HA ceramic scaffolds are first produced by the polymer impregnation approach, and subsequently further sintered by hot isostatic pressing (HIP). The phase composition, macro- and micro-porous structure, sintering and mechanical properties of the porous HA scaffolds are investigated by x-ray diffraction (XRD), scanning electron microscopy (SEM), nanoindentation analysis and compressive test. The experimental results show that the nanohardness and compressive strength of HIP-sintered porous HA ceramics are higher than those of commonly sintered HA scaffolds. The HIP technique can effectively improve the sintering property and densification of porous HA ceramic scaffolds, so inducing an increase in the compression strength. PMID:18458404

  7. 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

  8. Influence of hydroxyapatite crystallization temperature and concentration on stress transfer in wet-spun nanohydroxyapatite-chitosan composite fibres.

    PubMed

    Xie, J Z; Hein, S; Wang, K; Liao, K; Goh, K L

    2008-06-01

    Hydroxyapatite possesses appropriate osteoconductivity and biocompatibility for hard-tissue replacement implants but suffers from brittleness. One approach to overcome this problem is to incorporate nanometre hydroxyapatite (nHA) into a polymer matrix, such as chitosan, to yield a hydroxyapatite-chitosan (HC) composite. Here, a novel HC composite was synthesized and its elastic properties were investigated by varying (1) nHA concentration and (2) crystallization temperature (T), where T is a parameter which influences the morphology of the crystals. Crystals of nHA were precipitated at T = 40 degrees C and 100 degrees C, blended in a chitosan matrix, and wet-spun to yield fibres of HC composites at 5, 15, 20 and 40% concentrations (mass fraction of nHA). Scanning electron microscopy and energy-dispersive x-ray spectroscopy revealed a uniform distribution of nanocrystallites within the fibre. Tensile testing revealed that HC fibres, which comprised nHA treated at T = 100 degrees C, possessed low tensile strength, sigma(0), and stiffness, E, at low nHA concentrations but high sigma(0) and E at higher concentrations, i.e. beyond a 15% mass fraction of nHA. However, with nHA treated at T = 40 degrees C, the fibres yielded high sigma(0) and E at low nHA concentrations but low sigma(0) and E at high concentrations. The results strongly implicate the underlying effect of crystallite morphology on stress transfer at different concentrations. PMID:18477816

  9. Chalcogenide glass microsphere laser.

    PubMed

    Elliott, Gregor R; Murugan, G Senthil; Wilkinson, James S; Zervas, Michalis N; Hewak, Daniel W

    2010-12-01

    Laser action has been demonstrated in chalcogenide glass microsphere. A sub millimeter neodymium-doped gallium lanthanum sulphide glass sphere was pumped at 808 nm with a laser diode and single and multimode laser action demonstrated at wavelengths between 1075 and 1086 nm. The gallium lanthanum sulphide family of glass offer higher thermal stability compared to other chalcogenide glasses, and this, along with an optimized Q-factor for the microcavity allowed laser action to be achieved. When varying the pump power, changes in the output spectrum suggest nonlinear and/or thermal effects have a strong effect on laser action. PMID:21165022

  10. Photonic crystal microspheres

    NASA Astrophysics Data System (ADS)

    Zhokhov, A. A.; Masalov, V. M.; Sukhinina, N. S.; Matveev, D. V.; Dolganov, P. V.; Dolganov, V. K.; Emelchenko, G. A.

    2015-11-01

    Spherical samples of photonic crystals formed by colloidal SiO2 nanoparticles were synthesized. Synthesis of microspheres from 160 nm, 200 nm and 430 nm diameter colloidal nanoparticles was performed over a wide size range, from 5 μm to 50 μm. The mechanism of formation of void microparticles exceeding 50 μm is discussed. The spectral measurements verified the association of the spectra with the peaks of selective reflection from the cubic lattice planes. The microparticle morphology is characterized by scanning electron microscopy (SEM).

  11. Cytocompatibility and osteogenesis evaluation of HA/GCPU composite as scaffolds for bone tissue engineering.

    PubMed

    Du, Jingjing; Zou, Qin; Zuo, Yi; Li, Yubao

    2014-01-01

    Porous scaffolds for bone repair were prepared from newly designed segmented aliphatic polyurethane based on glyceride of castor oil and isophorone diisocyanate. To promote the scaffolds' biological and mechanical properties, hydroxyapatite powder was incorporated into the polymer matrix. The scaffold (named as HA/GCPU) with 40 wt% HA had an average pore size of 500 μm and a compressive strength of 4.6 MPa. The in vitro cell culture studies demonstrated that the HA/GCPU scaffold owned good cytocompatibility. The scaffold and cell-seeded scaffold were implanted in defects (Ф3 mm × 3 mm) of femoral condyle of Sprague-Dawley rats, respectively. New bone could extensively form in both the scaffold and cell-seeded scaffold. It indicates that the HA/GCPU composite scaffold has good prospect for bone repair and regeneration. PMID:24657710

  12. 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

  13. 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. PMID:21850513

  14. Na-doped hydroxyapatite coating on carbon/carbon composites: Preparation, in vitro bioactivity and biocompatibility

    NASA Astrophysics Data System (ADS)

    Li, Hejun; Zhao, Xueni; Cao, Sheng; Li, Kezhi; Chen, Mengdi; Xu, Zhanwei; Lu, Jinhua; Zhang, Leilei

    2012-12-01

    Na-doped hydroxyapatite (Na-HA) coating was directly prepared onto carbon/carbon (C/C) composites using electrochemical deposition (ECD) and the mean thickness of the coating is approximately 10 ± 2 μm. The formed Na-HA crystals which are Ca-deficient, are rod-like with a hexagonal cross section. The Na/P molar ratios of the coating formed on C/C substrate is 0.097. During the deposition, the Na-HA crystals grow in both radial and longitudinal directions, and faster along the longitudinal direction. The pattern formation of crystal growth leads to dense coating which would help to increase the bonding strength of the coating. The average shear bonding strength of Na-HA coating on C/C is 5.55 ± 0.77 MPa. The in vitro bioactivity of the Na-HA coated C/C composites were investigated by soaking the samples in a simulated body fluid (SBF) for 14 days. The results indicate that the Na-HA coated C/C composites can rapidly induce bone-like apatite nucleation and growth on its surface in SBF. The in vitro cellular biocompatibility tests reveal that the Na-HA coating was better to improve the in vitro biocompatibility of C/C composites compared with hydroxyapatite (HA) coating. It was suggested that the Na-HA coating might be an effective method to improve the surface bioactivity and biocompatibility of C/C composites.

  15. In Vitro Evaluation of Hydroxyapatite-Coated Titanium Implant with Atmospheric Plasma Treatment.

    PubMed

    Lee, Hyo-Jin; Kwon, Tae-Yub; Kim, Kyo-Han; Kang, Seong Soo; Choi, Seok Hwa; Kwon, Soon-Taek; Cho, Dae-Hyun; Son, Jun Sik

    2015-08-01

    Plasma treatments are becoming a popular method for modifying the characteristics of a range of substrate surfaces. Atmospheric pressure plasma (APP) is cost-efficient, safe and simple compared to high-pressure plasma. This study examined the effects of a low-temperature APP treatment of a hydroxyapatite (HA)-coated Ti (HA-Ti) surface. The APP treatment made the HA-Ti surfaces more hydrophilic without changing surface morphologies. The APP-treated HA-Ti (APP-HA-Ti) surface showed enhanced cell spreading, cell proliferation, and alkaline phosphatase (ALP) levels with more developed cellular networks, and the formed extracellular matrix (ECM) was fused perfectly with the HA substrate than that on the HA-Ti surface. In conclusion, an APP treatment is a potential surface-modifying method that can enhance the cell affinity at the early stages in vitro. PMID:26369123

  16. Hydroxyapatite for Keratoprosthesis Biointegration

    PubMed Central

    Wang, Liqiang; Jeong, Kyung Jae; Chiang, Homer H.; Zurakowski, David; Behlau, Irmgard; Chodosh, James; Dohlman, Claes H.; Langer, Robert

    2011-01-01

    Purpose. Integration of keratoprosthesis with the surrounding cornea is very important in preventing bacterial invasion, which may cause ocular injury. Here the authors investigated whether hydroxyapatite (HAp) coating can improve keratoprosthesis (KPro) biointegration, using polymethyl methacrylate (PMMA)—the principal component of the Boston KPro—as a model polymer. Methods. HAp coatings were induced on PMMA discs after treatment with concentrated NaOH and coating with poly-dopamine (PDA) or polydopamine and then with 11-mercaptoundecanoic acid (11-MUA). Coatings were characterized chemically (Fourier transform infrared spectroscopy [FTIR], energy dispersive X-ray spectroscopy [EDX]) and morphologically (SEM) and were used as substrates for keratocyte growth in vitro. Cylinders of coated PMMA were implanted in porcine corneas ex vivo for 2 weeks, and the force required to pull them out was measured. The inflammatory reaction to coated discs was assessed in the rabbit cornea in vivo. Results. FTIR of the coatings showed absorption bands characteristic of phosphate groups, and EDX showed that the Ca/P ratios were close to those of HAp. By SEM, each method resulted in morphologically distinct HAp films; the 11-MUA group had the most uniform coating. The hydroxyapatite coatings caused comparable enhancement of keratocyte proliferation compared with unmodified PMMA surfaces. HAp coating significantly increased the force and work required to pull PMMA cylinders out of porcine corneas ex vivo. HAp coating of implants reduced the inflammatory response around the PMMA implants in vivo. Conclusions. These results are encouraging for the potential of HAp-coated surfaces for use in keratoprostheses. PMID:21849419

  17. A functionally graded titanium/hydroxyapatite film obtained by sputtering.

    PubMed

    Ozeki, Kazuhide; Yuhta, Toshio; Fukui, Yasuhiro; Aoki, Hideki; Nishimura, Ikuya

    2002-03-01

    A functionally graded film of titanium/hydroxyapatite (HA) was prepared on a titanium substrate using a radio frequency magnetron sputtering. The ratio of titanium to HA was controlled by moving the target shutter. The film was composed of five layers, with overall film thickness of 1 microm. The HA was concentrated close to the surface, while the titanium concentration increased with proximity to the substrate. The bonding strength between the film and the substrate was 15.2 MPa in a pull-out test and the critical load from a scratch test was 58.85 mN. The corresponding values of a pure HA sputtered film were 8.0 MPa and 38.47 mN, respectively. The bonding strength of a pure HA plasma spray coating was 10.4 MPa in the pull-out test. The graded film and the pure HA film were sputter-coated to a thickness of 1 microm on titanium columns (10 mm in length and 4 mm in diameter). These columns were implanted in diaphyses of the femora of six adult dogs and a push-out test was carried out after 2, 4, and 12 weeks. After 12 weeks, the push-out strengths of the graded film, the pure HA film and the non-coated columns were 3.7, 3.5, and 1.0 MPa. PMID:15348621

  18. Osteogenic responses to zirconia with hydroxyapatite coating by aerosol deposition.

    PubMed

    Cho, Y; Hong, J; Ryoo, H; Kim, D; Park, J; Han, J

    2015-03-01

    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

  19. 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

  20. Lysozyme loading and release from Se doped hydroxyapatite nanoparticles.

    PubMed

    Wang, Yanhua; Hao, Hang; Zhang, Shengmin

    2016-04-01

    Element-substituted hydroxyapatite (HA) based nanocomposites have become a promising therapeutic material for improving bone defect repair. Selenium substituted HA nanoparticles can both induce apoptosis of bone tumor cells and enhance osteointegration. However, the effect of selenite ions on the proteins in combination with the HA nanoparticles remains to be elucidated. Here, we investigated the influence of selenium doping concentration on the loading and release of lysozyme (LSM) as a model protein drug. The selenium substituted HA-LSM composites with different doping concentrations were synthesized and characterized. The subsequent delivery of lysozyme was studied in a phosphate buffer solution (PBS). We found that selenium substituted HA-LSM composites with Se:P=10% showed the highest amount of lysozyme loading (41.7%), whereas the amount of lysozyme loaded in undoped HA nanoparticles was the lowest (34.1%). The doped selenium interacts with lysozyme molecules, which leads to the increase of β-sheet and unordered, and the decrease of self-association, α-helix and β-turns in protein structures. Moreover, selenium addition significantly slows the protein release from HA-LSM composites. The composites with Se:P=10% release lysozyme at the slightly slower rate among the samples with different Se doping concentrations. It also shows that the released lysozyme retains most of its enzymatic activity. PMID:26838882

  1. Hydroxyapatite/metal composite coatings formed by electrocodeposition.

    PubMed

    Dasarathy, H; Riley, C; Coble, H D; Lacefield, W R; Maybee, G

    1996-05-01

    Early bone infusion by cementless fixation of composite orthopedic and dental implants consisting of metallic substrates and bioceramics is well documented. Calcium phosphate ceramics in general and hydroxyapatite (HA) in particular have been the most popular of the bioceramics used for coating metals. Here, a non-line of sight coating procedure by electrocodeposition is reported for mechanically fixing HA particles in a metal matrix. Analyses of the coating showed excellent adhesion to the substrate and no structural transformation in either crystallinity or stoichiometry. Adhesion and surface coverage of HA depended upon the particle size. As a demonstration of the coating procedure's non-line of sight applicability, it was successfully used to coat titanium rods sintered with small titanium spheres. PMID:8731152

  2. Nano hydroxyapatite-coated implants improve bone nanomechanical properties.

    PubMed

    Jimbo, R; Coelho, P G; Bryington, M; Baldassarri, M; Tovar, N; Currie, F; Hayashi, M; Janal, M N; Andersson, M; Ono, D; Vandeweghe, S; Wennerberg, A

    2012-12-01

    Nanostructure modification of dental implants has long been sought as a means to improve osseointegration through enhanced biomimicry of host structures. Several methods have been proposed and demonstrated for creating nanotopographic features; here we describe a nanoscale hydroxyapatite (HA)-coated implant surface and hypothesize that it will hasten osseointegration and improve its quality relative to that of non-coated implants. Twenty threaded titanium alloy implants, half prepared with a stable HA nanoparticle surface and half grit-blasted, acid-etched, and heat-treated (HT), were inserted into rabbit femurs. Pre-operatively, the implants were morphologically and topographically characterized. After 3 weeks of healing, the samples were retrieved for histomorphometry. The nanomechanical properties of the surrounding bone were evaluated by nanoindentation. While both implants revealed similar bone-to-implant contact, the nanoindentation demonstrated that the tissue quality was significantly enhanced around the HA-coated implants, validating the postulated hypothesis. PMID:23045363

  3. Nano-hydroxyapatite and its applications in preventive, restorative and regenerative dentistry: a review of literature

    PubMed Central

    Pepla, Erlind; Besharat, Lait Kostantinos; Palaia, Gaspare; Tenore, Gianluca; Migliau, Guido

    2014-01-01

    Summary 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. PMID:25506416

  4. Effects of incorporation of HA/ZrO(2) into glass ionomer cement (GIC).

    PubMed

    Gu, Y W; Yap, A U J; Cheang, P; Khor, K A

    2005-03-01

    Glass ionomer cements (GICs) are a class of bioactive cements that bond directly to bone. In this paper, a new bioactive hydroxyapatite (HA)/zirconia (ZrO(2))-filled GIC composite was developed to improve the biocompatibility and bioactivity of the GICs with the surrounding bone and connective tissues. Nano-sized HA/30 wt% ZrO(2) powders were heat treated at 700 degrees Celsius and 800 degrees Celsius for 3 h to elucidate the influence of the crystallinity of composite powders on the performance of HA/ZrO(2)-GICs. The effects of different volume percentages of HA/ZrO(2) powders (4, 12, 28 and 40 vol%) substituted within GICs were investigated based on their microhardness, compressive strength and diametral tensile strength. The HA/ZrO(2)-GICs composite was soaked in distilled water for 1 day and 1 week before subjecting the samples to mechanical testing. Results showed that the glass and HA/ZrO(2) particles were distributed uniformly in the GIC matrix. The substitution of highly crystalline HA/ZrO(2) improved the mechanical properties of the HA/ZrO(2)-GICs due to the slow resorption rate for highly crystalline powders in distilled water. The mechanical properties of HA/ZrO(2)-GICs increased with increasing soak time due to the continuous formation of aluminium salt bridges, which improved the final strength of the cements. The compositions 4 and 12 vol% HA/ZrO(2)-GICs exhibited superior mechanical properties than the original GICs. The mechanical properties of HA/ZrO(2)-GICs were found to be much better than those of HA-GICs because ZrO(2) has the attributes of high strength, high modulus, and is significantly harder than glass and HA particles. Furthermore, ZrO(2) does not dissolve with increasing soaking time. PMID:15350775

  5. Particle Tracking of Fluorescent Microspheres

    NASA Astrophysics Data System (ADS)

    Kaminski, Zofia; Mueller, Joachim; Berk, Serkan

    2010-10-01

    In this research, the diffusion coefficients of the fluorescent microspheres and the relation of those coefficients to particle radius were investigated. An additional focus was to see how well the measured radius of the microspheres compared to the radius as reported by the manufacturer and to measure the distribution of radii in a sample. This study further developed the critical process of ensuring particle movement within the sample volume and made preliminary sample measurements.The methods developed for tracking microspheres will later be used to determine the radii of virus like particles (VLPs), which are a non-infectious model system of the HIV virus. Results from our measurements will be reported.

  6. Microsphere based saliva diagnostics

    NASA Astrophysics Data System (ADS)

    Rissin, David M.; DiCesare, Christopher; Hayman, Ryan B.; Blicharz, Timothy M.; Walt, David R.

    2005-11-01

    Saliva presents a minimally invasive alternative medium to blood for performing diagnostics1. Microsphere sensors for ions, small organic molecules, and proteins are currently being developed and optical microarrays containing thousands of these sensors will be used for simultaneous multi-analyte analysis. The fiber bundle platform in use is 1mm in diameter and contains approximately 50,000 individually addressable 3.1μm fibers, each with an etched well capable of housing a single 3.1μm microsphere sensor. Micron-sized bead-based chemistries are produced in house, followed by deposition onto a fiber-optic bundle platform, allowing for multiplexed analysis. The ultimate goal is to develop a universal diagnostic system using saliva as the diagnostic medium. This platform will permit multiplexed analysis of a sample by integrating microfluidics with the optical arrays loaded with sensors capable of detecting relevant biomarkers associated with a wide range of disease states. Disease states that are currently under investigation include end stage renal disease (ESRD) and Sjoegrens Syndrome (SS).

  7. Effects of the Reinforcement Morphology on the Fatigue Properties of Hydroxyapatite Reinforced Polymers

    PubMed Central

    Kane, Robert J.; Converse, Gabriel L.; Roeder, Ryan K.

    2008-01-01

    The objective of this study was to examine the effects of the hydroxyapatite (HA) reinforcement morphology and content on the fatigue behavior of HA reinforced high density polyethylene (HDPE). To this end, HDPE was reinforced with 20 and 40 vol% of either HA whiskers or an equiaxed HA powder, and tested in four-point bending fatigue under simulated physiological conditions. The fatigue life, mechanical property degradation and failure surfaces were compared between experimental groups. HDPE reinforced with HA whiskers exhibited a four- to five-fold increase (p < 0.001, T-test) in fatigue life compared to an equiaxed powder for either the 20 and 40 vol% reinforcement level. Composites containing 40 vol% HA exhibited decreased fatigue life compared to those with 20 vol% HA for either reinforcement morphology (p < 0.0001, ANOVA). HA whisker reinforced HDPE exhibited less stiffness loss, permanent deformation (creep) and energy dissipation at a given number of cycles compared to HA powder. Thus, HA whisker reinforced HDPE was more tolerant of fatigue damage due to either microcracking or polymer plasticity. Scanning electron microscopy of failure surfaces and surface microcracks showed evidence of toughening by uncracked ligaments, crack tip plasticity, polymer fibril bridging and HA whisker pullout. The results of this study suggest that the use of HA whiskers, in place of HA powder, is a straightforward means to improve the fatigue life and damage tolerance of HA reinforced polymers for synthetic bone substitutes. PMID:19578474

  8. Hydroxyapatite fiber reinforced poly(alpha-hydroxy ester) foams for bone regeneration

    NASA Technical Reports Server (NTRS)

    Thomson, R. C.; Yaszemski, M. J.; Powers, J. M.; Mikos, A. G.; McIntire, L. V. (Principal Investigator)

    1998-01-01

    A process has been developed to manufacture biodegradable composite foams of poly(DL-lactic-co-glycolic acid) (PLGA) and hydroxyapatite short fibers for use in bone regeneration. The processing technique allows the manufacture of three-dimensional foam scaffolds and involves the formation of a composite material consisting of a porogen material (either gelatin microspheres or salt particles) and hydroxyapatite short fibers embedded in a PLGA matrix. After the porogen is leached out, an open-cell composite foam remains which has a pore size and morphology defined by the porogen. By changing the weight fraction of the leachable component it was possible to produce composite foams with controlled porosities ranging from 0.47 +/- 0.02 to 0.85 +/- 0.01 (n = 3). Up to a polymer:fiber ratio of 7:6, short hydroxyapatite fibers served to reinforce low-porosity PLGA foams manufactured using gelatin microspheres as a porogen. Foams with a compressive yield strength up to 2.82 +/- 0.63 MPa (n = 3) and a porosity of 0.47 +/- 0.02 (n = 3) were manufactured using a polymer:fiber weight ratio of 7:6. In contrast, high-porosity composite foams (up to 0.81 +/- 0.02, n = 3) suitable for cell seeding were not reinforced by the introduction of increasing quantities of hydroxyapatite short fibers. We were therefore able to manufacture high-porosity foams which may be seeded with cells but which have minimal compressive yield strength, or low porosity foams with enhanced osteoconductivity and compressive yield strength.

  9. Corrosion behavior of plasma sprayed hydroxyapatite and hydroxyapatite-silicon oxide coatings on AISI 304 for biomedical application

    NASA Astrophysics Data System (ADS)

    Singh, Gurpreet; Singh, Hazoor; Sidhu, Buta Singh

    2013-11-01

    The objective of this study is to evaluate corrosion resistance of plasma sprayed hydroxyapatite (HA) and HAsbnd silicon oxide (SiO2) coated AISI 304 substrates. In HAsbnd SiO2 coatings, 10 wt% SiO2 and 20 wt% SiO2 was mixed with HA. The feedstock and coatings were characterized by X-ray diffraction and scanning electron microscopy/energy dispersive X-ray spectroscopy. The corrosion resistance was determined for the uncoated and coated samples. The corrosion resistance of the AISI 304 was found more after the deposition of the HAsbnd SiO2 coatings rather than HA coating and uncoated. All the coatings were crack free after 24 h dipping in Ringer's solution for electrochemical corrosion testing.

  10. A comparative study of zinc, magnesium, strontium-incorporated hydroxyapatite-coated titanium implants for osseointegration of osteopenic rats.

    PubMed

    Tao, Zhou-Shan; Zhou, Wan-Shu; He, Xing-Wen; Liu, Wei; Bai, Bing-Li; Zhou, Qiang; Huang, Zheng-Liang; Tu, Kai-kai; Li, Hang; Sun, Tao; Lv, Yang-Xun; Cui, Wei; Yang, Lei

    2016-05-01

    Surface modification techniques have been applied to generate titanium implant surfaces that promote osseointegration for the implants in cementless arthroplasty. However, its effect is not sufficient for osteoporotic bone. Zinc (Zn), magnesium (Mg), and strontium (Sr) present a beneficial effect on bone growth, and positively affect bone regeneration. The aim of this study was to confirm the different effects of the fixation strength of Zn, Mg, Sr-substituted hydroxyapatite-coated (Zn-HA-coated, Mg-HA-coated, Sr-HA-coated) titanium implants via electrochemical deposition in the osteoporotic condition. Female Sprague-Dawley rats were used for this study. Twelve weeks after bilateral ovariectomy, all animals were randomly divided into four groups: group HA; group Zn-HA; group Mg-HA and group Sr-HA. Afterwards, all rats from groups HA, Zn-HA, Mg-HA and Sr-HA received implants with hydroxyapatite containing 0%, 10% Zn ions, 10% Mg ions, and 10% Sr ions. Implants were inserted bilaterally in all animals until death at 12 weeks. The bilateral femurs of rats were harvested for evaluation. All treatment groups increased new bone formation around the surface of titanium rods and push-out force; group Sr-HA showed the strongest effects on new bone formation and biomechanical strength. Additionally, there are significant differences in bone formation and push-out force was observed between groups Zn-HA and Mg-HA. This finding suggests that Zn, Mg, Sr-substituted hydroxyapatite coatings can improve implant osseointegration, and the 10% Sr coating exhibited the best properties for implant osseointegration among the tested coatings in osteoporosis rats. PMID:26952418

  11. Effect of different sintering methods on bioactivity and release of proteins from PLGA microspheres.

    PubMed

    Dormer, Nathan H; Gupta, Vineet; Scurto, Aaron M; Berkland, Cory J; Detamore, Michael S

    2013-10-01

    Macromolecule release from poly(d,l-lactide-co-glycolide) (PLGA) microspheres has been well-characterized, and is a popular approach for delivering bioactive signals from tissue-engineered scaffolds. However, the effect of some processing solvents, sterilization, and mineral incorporation (when used in concert) on long-term release and bioactivity has seldom been addressed. Understanding these effects is of significant importance for microsphere-based scaffolds, given that these scaffolds are becoming increasingly more popular, yet growth factor activity following sintering and/or sterilization is heretofore unknown. The current study evaluated the 6-week release of transforming growth factor (TGF)-β3 and bone morphogenetic protein (BMP)-2 from PLGA and PLGA/hydroxyapatite (HAp) microspheres following exposure to ethanol (EtOH), dense phase carbon dioxide (CO2), or ethylene oxide (EtO). EtO was chosen based on its common use in scaffold sterilization, whereas EtOH and CO2 were chosen given their importance in sintering microspheres together to create scaffolds. Release supernatants were then used in an accelerated cell stimulation study with human bone marrow stromal cells (hBMSCs) with monitoring of gene expression for major chondrogenic and osteogenic markers. Results indicated that in microspheres without HAp, EtOH exposure led to the greatest amount of delivery, while those treated with CO2 delivered the least growth factor. In contrast, formulations with HAp released almost half as much protein, regardless of EtOH or CO2 exposure. Notably, EtO exposure was not found to significantly affect the amount of protein released. Cell stimulation studies demonstrated that eluted protein samples performed similarly to positive controls in PLGA-only formulations, and ambiguously in PLGA/HAp composites. In conclusion, the use of EtOH, subcritical CO2, and EtO in microsphere-based scaffolds may have only slight adverse effects, and possibly even desirable effects in some

  12. 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

  13. Hydroxyapatite coating of an acetabular prosthesis. Effect on stability.

    PubMed

    Moilanen, T; Stocks, G W; Freeman, M A; Scott, G; Goodier, W D; Evans, S J

    1996-03-01

    We report the radiological and clinical outcome of a press-fit (SLF) acetabular component at two to three years in two groups of patients having primary total hip replacement. In 69 the implant was coated with hydroxyapatite (HA) and in 40 it was uncoated. The stability of the cup was assessed by measurement of proximal migration and change in the angle of inclination. The clinical results in the two groups did not differ significantly, and the mean proximal linear wear was similar in both. Fewer radiolucent lines (RLLs) were seen on the radiographs of cups coated with HA. The mean proximal migration was studied by calculating regression lines for each patient using migration measurements: for the SLF+HA group the mean slope was 0.06 mm/year and for the SLF-HA group 0.20 mm/year (p = 0.22). The change in the angle of inclination during follow-up was also consistently smaller in HA-coated cups. Using regression methods the SLF+HA group had a mean slope of 0.08 degrees/year and the SLF-HA group 0.44 degrees/year and the SLF-HA group 0.44 degrees/year (p = 0.023). Partial HA coating appeared to have no effect on the clinical outcome or on the rate of wear of polyethylene, but there was a trend towards a reduced rate of proximal migration, and a significant reduction in rotational migration and the number of radiolucent lines. This suggests that HA coating enhances the stability of this acetabular component. PMID:8666624

  14. Intrinsic magnetism and hyperthermia in bioactive Fe-doped hydroxyapatite.

    PubMed

    Tampieri, Anna; D'Alessandro, Teresa; Sandri, Monica; Sprio, Simone; Landi, Elena; Bertinetti, Luca; Panseri, Silvia; Pepponi, Giancarlo; Goettlicher, Joerg; Bañobre-López, Manuel; Rivas, Jose

    2012-02-01

    The use of magnetic activation has been proposed to answer the growing need for assisted bone and vascular remodeling during template/scaffold regeneration. With this in mind, a synthesis procedure was developed to prepare bioactive (Fe2+/Fe3+)-doped hydroxyapatite (Fe-HA), endowed with superparamagnetic-like properties. This new class of magnetic hydroxyapatites can be potentially employed to develop new magnetic ceramic scaffolds with enhanced regenerative properties for bone surgery; in addition, magnetic Fe-HA can find application in anticancer therapies, to replace the widely used magnetic iron oxide nanoparticles, whose long-term cytotoxicity was recently found to reach harmful levels. An extensive physicochemical, microstructural and magnetic characterization was performed on the obtained Fe-HA powders, and demonstrated that the simultaneous addition of Fe2+ and Fe3+ ions during apatite nucleation under controlled synthesis conditions induces intrinsic magnetization in the final product, minimizing the formation of magnetite as secondary phase. This result potentially opens new perspectives for biodevices aimed at bone regeneration and for anti-cancer therapies based on hyperthermia. PMID:22005331

  15. Hydroxyapatite electrodeposition on anodized titanium nanotubes for orthopedic applications

    NASA Astrophysics Data System (ADS)

    Parcharoen, Yardnapar; Kajitvichyanukul, Puangrat; Sirivisoot, Sirinrath; Termsuksawad, Preecha

    2014-08-01

    Nanotubes modification for orthopedic implants has shown interesting biological performances (such as improving cell adhesion, cell differentiation, and enhancing osseointegration). The purpose of this study is to investigate effect of titanium dioxide (TiO2) nanotube feature on performance of hydroxyapatite-coated titanium (Ti) bone implants. TiO2 nanotubes were prepared by anodization using ammonium fluoride electrolyte (NH4F) with and without modifiers (PEG400 and Glycerol) at various potential forms, and times. After anodization, the nanotubes were subsequently annealed. TiO2 nanotubes were characterized by scanning electron microscope and X-ray diffractometer. The amorphous to anatase transformation due to annealing was observed. Smooth and highly organized TiO2 nanotubes were found when high viscous electrolyte, NH4F in glycerol, was used. Negative voltage (-4 V) during anodization was confirmed to increase nanotube thickness. Length of the TiO2 nanotubes was significantly increased by times. The TiO2 nanotube was electrodeposited with hydroxyapatite (HA) and its adhesion was estimated by adhesive tape test. The result showed that nanotubes with the tube length of 560 nm showed excellent adhesion. The coated HA were tested for biological test by live/dead cell straining. HA coated on TiO2 nanotubes showed higher cells density, higher live cells, and more spreading of MC3T3-E1 cells than that growing on titanium plate surface.

  16. Glass microsphere lubrication

    NASA Technical Reports Server (NTRS)

    Geiger, Michelle; Goode, Henry; Ohanlon, Sean; Pieloch, Stuart; Sorrells, Cindy; Willette, Chris

    1991-01-01

    The harsh lunar environment eliminated the consideration of most lubricants used on earth. Considering that the majority of the surface of the moon consists of sand, the elements that make up this mixture were analyzed. According to previous space missions, a large portion of the moon's surface is made up of fine grained crystalline rock, about 0.02 to 0.05 mm in size. These fine grained particles can be divided into four groups: lunar rock fragments, glasses, agglutinates (rock particles, crystals, or glasses), and fragments of meteorite material (rare). Analysis of the soil obtained from the missions has given chemical compositions of its materials. It is about 53 to 63 percent oxygen, 16 to 22 percent silicon, 10 to 16 percent sulfur, 5 to 9 percent aluminum, and has lesser amounts of magnesium, carbon, and sodium. To be self-supporting, the lubricant must utilize one or more of the above elements. Considering that the element must be easy to extract and readily manipulated, silicon or glass was the most logical choice. Being a ceramic, glass has a high strength and excellent resistance to temperature. The glass would also not contaminate the environment as it comes directly from it. If sand entered a bearing lubricated with grease, the lubricant would eventually fail and the shaft would bind, causing damage to the system. In a bearing lubricated with a solid glass lubricant, sand would be ground up and have little effect on the system. The next issue was what shape to form the glass in. Solid glass spheres was the only logical choice. The strength of the glass and its endurance would be optimal in this form. To behave as an effective lubricant, the diameter of the spheres would have to be very small, on the order of hundreds of microns or less. This would allow smaller clearances between the bearing and the shaft, and less material would be needed. The production of glass microspheres was divided into two parts, production and sorting. Production includes the

  17. 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

  18. Laser-assisted production of tricalcium phosphate nanoparticles from biological and synthetic hydroxyapatite in aqueous medium

    NASA Astrophysics Data System (ADS)

    Boutinguiza, M.; Pou, J.; Lusquiños, F.; Comesaña, R.; Riveiro, A.

    2011-04-01

    Pulsed laser ablation technique has attracted great attention as a method for preparing nanoparticles. In this work, calcined fish bones and synthetic hydroxyapatite, have been used as target to be ablated in de-ionized water with a pulsed CO 2 laser to produce calcium phosphate nanoparticles. The obtained nanoparticles were amorphous and spherical in shape with a mean diameter of about 25 nm. The microanalyses revealed that nanoparticles obtained from the synthetic HA undergo transformation to tricalcium phosphate. While nanoparticles obtained from the biological hydroxyapatite mostly preserve the composition of precursor material.

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

    NASA Astrophysics Data System (ADS)

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

    2014-10-01

    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.

  20. Surface modification of titanium by nano-TiO 2/HA bioceramic coating

    NASA Astrophysics Data System (ADS)

    He, G.; Hu, J.; Wei, S. C.; Li, J. H.; Liang, X. H.; Luo, E.

    2008-11-01

    A nano-TiO 2/hydroxyapatite composite bioceramic coating was developed and applied to the surfaces of pure titanium discs by the sol-gel method. A TiO 2 anatase bioceramic coating was utilized in the inner layer, which could adhere tightly to the titanium substrate. A porous hydroxyapatite (HA) bioceramic coating was utilized in the outer layer, which has higher solubility and better short-term bioactivity. Conventional HA coatings and commercially pure titanium were used as controls. X-ray diffraction (XRD) and scanning electron microscopy (SEM) were employed to characterize the crystallization, surface morphology, and thickness of the coatings. The bioactivities of the coatings were evaluated by in vitro osteoblast cultures. Results showed that the nano-TiO 2/HA composite bioceramic coating exhibited good crystallization and homogeneous, nano-scale surface morphology. In addition, the nano-TiO 2/HA coating adhered tightly to the substrate, and the in vitro osteoblast cultures exhibited satisfactory bioactivity.

  1. Characterization, mechanical properties and corrosion resistance of biocompatible Zn-HA/TiO2 nanocomposite coatings.

    PubMed

    Mirak, Mohammad; Alizadeh, Morteza; Ghaffari, Mohammad; Ashtiani, Mohammad Najafi

    2016-09-01

    Biocompatible Zinc-hydroxyapatite-titania and Zinc-hydroxyapatite nanocomposite coatings have been prepared by electrodeposition on NiTi shape memory alloy. Structures of coatings were characterized using X-ray diffraction (XRD). It was found that addition of TiO2 particles cause to reduction of crystallite size of coating. Scanning Electronic Microscope (SEM) observation showed that the Zn-HA/TiO2 coating consists of plate-like regions which can express that this plate-like structure can facilitate bone growth. X-ray photoelectron microscope (XPS) was performed to investigation of chemical state of composite coating and showed that Zinc matrix was bonded to oxygen. high-resolution transmission electron microscope (HRTEM) result illustrated the crystalline structure of nanocomposite coating. Mechanical behavior of coating was evaluated using microhardness and ball on disk wear test. The TiO2 incorporated composite coatings exhibited the better hardness and anti-wear performance than the Zn-HA coatings. Polarization measurements have been used to evaluate the electrochemical coatings performance. The Zn-HA/TiO2 composite coatings showed the highest corrosion resistance compared with Zn-HA and bare NiTi. PMID:27232830

  2. Comparative evaluation of biocompatibility of dense nanostructured and microstructured Hydroxyapatite/Titania composites.

    PubMed

    Farzin, A; Ahmadian, M; Fathi, M H

    2013-05-01

    This work deals with the biocompatibility of dense nano- and micro-structured Hydroxyapatite/Titania composites prepared by two step and conventional sintering, respectively. By application of two step sintering, it was shown that the final grain size of HA-15 wt.% TiO2 is maintained lower than 100 nm while by the application of conventional sintering it reaches higher than 100 nm. Biocompatibility of the dense bulks was evaluated by cell attachment and proliferation experiments. Cell morphology, and viability on each nano- and micro-structured Hydroxyapatite/Titania composites were examined at different time points. The nanostructured HA/Titania dense bulk exhibited higher cell viability than a microstructured one. In addition, the effects of ionic products from nano- and micro-structured bulk dissolution on osteoblasts were studied. The MTT test confirmed that the products from nanostructured HA/Titania dense bulk significantly promoted osteoblast proliferation within a certain concentration range. PMID:23498255

  3. 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. PMID:27157760

  4. Hydroxyapatite thin films synthesized by Pulsed Laser Deposition onto titanium mesh implants for cranioplasty applications

    NASA Astrophysics Data System (ADS)

    Duta, L.; Stan, G. E.; Popescu, A. C.; Socol, G.; Miroiu, F. M.; Mihailescu, I. N.; Ianculescu, A.; Poeata, I.; Chiriac, A.

    2013-06-01

    We report on the synthesis of advanced nanostructured hydroxyapatite thin films onto 3D titanium (Ti) mesh substrates by Pulsed Laser Deposition method. Morphological and structural investigations as well as pull-out tests proved the stoichiometric transfer of crystalline hydroxyapatite (HA) films along with their good adherence. In vivo tests were performed on 12 patients (six with simple Ti mesh, six with Ti mesh biofunctionalized with HA). The tomodensitometry analysis of the cranial control scans evidenced the process of osseogenesis. For four patients with implanted HA/Ti mesh structures, the modification of the value obtained on Hounsfield scale was observed at the level of implant, proving the progress of osseointegration. We conclude that the structures exhibit excellent bonding strength and functionality, and are suitable for neurosurgical applications.

  5. Effects of strontium ions on growth and dissolution of hydroxyapatite and on bone mineral detection.

    PubMed

    Christoffersen, J; Christoffersen, M R; Kolthoff, N; Bärenholdt, O

    1997-01-01

    Preparation and analyses of a series of hydroxyapatites (HA) containing 1-10 mol % of Ca2+ replaced by Sr2+ is reported. The solubility of these apatites is found to increase with increasing content of Sr2+, 10% SrHA dissolves faster than CaHA at given values of Ca2+ and phosphate concentrations, but with a similar rate at the same degree of saturation. Sr2+ is found to inhibit the rates of both dissolution and growth of CaHA and 10% SrHA at pH 7.2, CaHA being more strongly inhibited by Sr2+ than 10% SrHA. The effect of partial substitution of Ca2+ in hydroxyapatite by Sr2+ on bone mineral content (BMC) and bone mineral density (BMD) measured by dual energy X-ray absorptiometry has been studied using three commercial densitometers. Extrapolating the absorption data for up to 10% replacement of Ca2+ by Sr2+ to 100% substitution of Ca2+ by Sr2+ in HA leads to an apparent increase in BMC or BMD of about a factor of 10. This factor is in agreement with theoretical calculations using attenuation coefficients of the atoms concerned. It is concluded that existing BMC scanners register artificially high values of BMC if the bone contains significant amounts of Sr2+ or other metal ions with atomic number larger than calcium. PMID:8988347

  6. Study on the Mechanical Properties of Three-Dimensional Directly Binding Hydroxyapatite Powder.

    PubMed

    Wang, Yanen; Li, Xinpei; Wei, Qinghua; Yang, Mingming; Wei, Shengmin

    2015-05-01

    In the three-dimensional directly fabricating hydroxyapatite composite artificial bone scaffold process, the liquid bio-binder is sprayed on the surface of bioceramics powder layer. The spraying volume and the powder size directly influence the mechanical properties of the bone scaffold and the future biodegradation performance. When the size of powder is stable, the amount of binder spraying will directly affect the mechanical strength of bone scaffold. In order to figure out the solidification mechanism of α-n-butyl cyanoacrylate (NBCA) bio-binder on the hydroxyapatite (HA) powder layer, the molecular dynamics simulation method is applied to investigate the binding energy shifts between NBCA on HA crystallographic planes. The mechanical properties can be deduced from this methodology; furthermore, the Knoop identification experiments are used to investigate the effective elastic modules of pure HA system and HA/NBCA composite model. Both the simulation and the experiments results elucidate that HA (110) has the highest binding energy with NBCA as the high planar atom density and the mechanical properties of HA/NBCA mixed system are stronger than the pure HA system on three-dimensional crystallographic; in this sense, the bone scaffolds with different strengths could be fabricated by controlling various NBCA binders liquid doses on the surface of HA powder layers during the 3D printing process. PMID:25556069

  7. Low-Energy Plasma Spray (LEPS) Deposition of Hydroxyapatite/Poly-ɛ-Caprolactone Biocomposite Coatings

    NASA Astrophysics Data System (ADS)

    Garcia-Alonso, Diana; Parco, Maria; Stokes, Joseph; Looney, Lisa

    2012-01-01

    Thermal spraying is widely employed to deposit hydroxyapatite (HA) and HA-based biocomposites on hip and dental implants. For thick HA coatings (>150 μm), problems are generally associated with the build-up of residual stresses and lack of control of coating crystallinity. HA/polymer composite coatings are especially interesting to improve the pure HA coatings' mechanical properties. For instance, the polymer may help in releasing the residual stresses in the thick HA coatings. In addition, the selection of a bioresorbable polymer may enhance the coatings' biological behavior. However, there are major challenges associated with spraying ceramic and polymeric materials together because of their very different thermal properties. In this study, pure HA and HA/poly-ɛ-caprolactone (PCL) thick coatings were deposited without significant thermal degradation by low-energy plasma spraying (LEPS). PCL has never been processed by thermal spraying, and its processing is a major achievement of this study. The influence of selected process parameters on microstructure, composition, and mechanical properties of HA and HA/PCL coatings was studied using statistical design of experiments (DOE). The HA deposition rate was significantly increased by the addition of PCL. The average porosity of biocomposite coatings was slightly increased, while retaining or even improving in some cases their fracture toughness and microhardness. Surface roughness of biocomposites was enhanced compared with HA pure coatings. Cell culture experiments showed that murine osteoblast-like cells attach and proliferate well on HA/PCL biocomposite deposits.

  8. Endothelial cell migration and morphogenesis on silk fibroin scaffolds containing hydroxyapatite electret.

    PubMed

    Nakamura, Miho; Soya, Tomoko; Hiratai, Rumi; Nagai, Akiko; Hashimoto, Kazuaki; Morita, Ikuo; Yamashita, Kimihiro

    2012-04-01

    The purpose of this study was to evaluate the effects of composite wound dressing films made of silk fibroin (SF) containing hydroxyapatite (HA) or polarized HA (pHA) powders on endothelial cell (EC) behaviors that have important roles in the wound-healing process. XRD revealed the SF films to be semicrystalline, with a broad peak centered at about 20.7° which is characteristic of β-sheets embedded within an amorphous matrix. The SF composite films with 0.6 (w/v)% in concentration of HA powder (HA/SF) or pHA powder (pHA/SF) contained HA crystals of amorphous and silk II crystalline structures. SEM observation showed that there were differences in SF morphology between HA/SF and pHA/SF. The pHA/SF exhibited a furry texture around the pHA crystals, most likely due to the stored charged and zeta potentials. The HA/SF and pHA/SF films enhanced EC migration compared with that on the SF film. The number of migrated cells on the HA/SF and pHA/SF was ~1.5 times larger than that on the SF. The quantitative analysis of the endothelial morphogenesis indicated that the pHA/SF film enhanced the formation of capillary-like structures compared with SF and HA/SF. Thus, pHA/SF may potentially stimulate and contribute to the enhancement of angiogenesis in the wound-healing process. PMID:22275235

  9. Bacterial Cellulose-Hydroxyapatite Nanocomposites for Bone Regeneration

    PubMed Central

    Saska, S.; Barud, H. S.; Gaspar, A. M. M.; Marchetto, R.; Ribeiro, S. J. L.; Messaddeq, Y.

    2011-01-01

    The aim of this study was to develop and to evaluate the biological properties of bacterial cellulose-hydroxyapatite (BC-HA) nanocomposite membranes for bone regeneration. Nanocomposites were prepared from bacterial cellulose membranes sequentially incubated in solutions of CaCl2 followed by Na2HPO4. BC-HA membranes were evaluated in noncritical bone defects in rat tibiae at 1, 4, and 16 weeks. Thermogravimetric analyses showed that the amount of the mineral phase was 40%–50% of the total weight. Spectroscopy, electronic microscopy/energy dispersive X-ray analyses, and X-ray diffraction showed formation of HA crystals on BC nanofibres. Low crystallinity HA crystals presented Ca/P a molar ratio of 1.5 (calcium-deficient HA), similar to physiological bone. Fourier transformed infrared spectroscopy analysis showed bands assigned to phosphate and carbonate ions. In vivo tests showed no inflammatory reaction after 1 week. After 4 weeks, defects were observed to be completely filled in by new bone tissue. The BC-HA membranes were effective for bone regeneration. PMID:21961004

  10. 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.

  11. 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.

  12. Electrophoretic deposition of composite hydroxyapatite-silica-chitosan coatings

    SciTech Connect

    Grandfield, K.; Zhitomirsky, I.

    2008-01-15

    Electrophoretic deposition (EPD) method has been developed for the fabrication of nanocomposite silica-chitosan coatings. Cathodic deposits were obtained on various conductive substrates using suspensions of silica nanoparticles in a mixed ethanol-water solvent, containing dissolved chitosan. Co-deposition of silica and hydroxyapatite (HA) nanoparticles resulted in the fabrication of HA-silica-chitosan coatings. The deposition yield has been studied at a constant voltage mode at various deposition durations. The method enabled the formation of coatings of different thickness in the range of up to 100 {mu}m. Deposit composition, microstructure and porosity can be varied by variation of HA and silica concentration in the suspensions. It was demonstrated that EPD can be used for the fabrication of HA-silica-chitosan coatings of graded composition and laminates. The method enabled the deposition of coatings containing layers of silica-chitosan and HA-chitosan nanocomposites using suspensions with different HA and silica content. Obtained coatings were studied by X-ray diffraction, thermogravimetric and differential thermal analysis, scanning electron microscopy and energy dispersive spectroscopy. The mechanism of deposition is discussed.

  13. Converting ultrasonic induction heating deposited monetite coating to Na-doped HA coating on H 2O 2-treated C/C composites by a two-step hydrothermal method

    NASA Astrophysics Data System (ADS)

    Xin-bo, Xiong; Jian-feng, Hung; Xie-rong, Zeng; Cen-cen, Chu

    2011-10-01

    a monetite coating on H 2O 2-treated C/C composites was prepared by ultrasonic induction heating (UIH) technology. Subsequently, this coating was subjected to an ammonia hydrothermal treatment to form a undoped hydroxyapatite (U-HA) coating. Finally, the as-prepared U-HA coating was placed in a NaOH solution and hydrothermally treated to produce the other hydroxyapatite (Na-HA) coating. The structure, morphology and chemical composition of the two HA coatings were characterized by XRD, FTIR, SEM and EDS, the adhesiveness and local mechanical properties, e.g. nanohardness and Young's modulus of the two HA coatings to C/C composites was evaluated by a scratch test and nanoindentation technique respectively. The results showed that the two HA coatings had the alike morphology and crystallization. But, compared with the U-HA coating, the Na-HA coating was doped with Na ions, and gave a Ca/P ratio close to a stoichiometric hydroxyapatite, and thus showed a higher nano-indentation value, Young's modulus, and larger bonding strength. These results verified the strengthened effect of Na ion in hydroxyapatite coating on carbon/carbon (C/C) composities.

  14. Synthesis and photoluminescence study of flower-like hydroxyapatite nanostructure for bioprobe applications

    NASA Astrophysics Data System (ADS)

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

    2013-02-01

    Biocompatible luminescent materials have received much attention for the development of novel bioprobes. In the present work, we have synthesized the flower-like hydroxyapatite (HA) nanostructure from eggshell biowaste via a simple and rapid microwave conversion process. The synthesized product is identified as Mg containing B-type carbonated HA. It showed an intense blue emission between 360 nm to 550 nm with maximum around 430 nm under UV light excitation (λex= 344 nm). This blue emission might result from the carbonate related impurities present in the structure of HA and it can be a potential luminescent material for the development biocompatible probes.

  15. Characterization of Hydroxyapatite-Glass Composites Using Terahertz Time-Domain Spectroscopy

    NASA Astrophysics Data System (ADS)

    Yatongchai, C.; Wren, A. W.; Sundaram, S. K.

    2015-01-01

    Terahertz time-domain spectroscopy (THz-TDS) is presented as a tool for characterization of the hydroxyapatite (HA)-glass composites. The materials under investigation are composites of HA and a calcium zinc silicate glass. Our results show that the refractive index and dielectric constant in THz frequencies provide a reliable determination of glass content of these composites. In addition, the THz-TDS is used to morphological changes in HA during simulated body fluid (SBF) incubation. Our results demonstrate that the THz-TDS can be a promising non-destructive tool.

  16. Characterization of Hydroxyapatite-Glass Composites Using Terahertz Time-Domain Spectroscopy

    NASA Astrophysics Data System (ADS)

    Yatongchai, C.; Wren, A. W.; Sundaram, S. K.

    2014-08-01

    Terahertz time-domain spectroscopy (THz-TDS) is presented as a tool for characterization of the hydroxyapatite (HA)-glass composites. The materials under investigation are composites of HA and a calcium zinc silicate glass. Our results show that the refractive index and dielectric constant in THz frequencies provide a reliable determination of glass content of these composites. In addition, the THz-TDS is used to morphological changes in HA during simulated body fluid (SBF) incubation. Our results demonstrate that the THz-TDS can be a promising non-destructive tool.

  17. Formation and Characterization of Crystalline Hydroxyapatite Coating with the (002) Texture

    NASA Astrophysics Data System (ADS)

    Grubova, I.; Priamushko, T.; Chudinova, E.; Surmeneva, M.; Korneva, O.; Epple, M.; Prymak, O.; Shulepov, I.; Surmenev, R.

    2016-02-01

    This study reports the effect of titanium (Ti) microstructure on the mechanical properties and surface wettability of thin (<800 nm) hydroxyapatite (HA) coating deposited via radio-frequency (RF) magnetron sputtering. It was revealed that the sand-blasting (SB) and acid etching (AE) of Ti prior deposition led to a wide range of surface roughness in nano/micro scale. After nanostructured HA coating deposition such physico-mechanical characteristics as nanohardness H, Young's modulus E, H/E ratio and H3/E2 were significantly improved. Moreover, HA coatings exhibited improved wear resistance, lower friction coefficient and ability of the coating to wetting.

  18. Biodegradation rate of shellac coated bovine hydroxyapatite for bone filler material

    NASA Astrophysics Data System (ADS)

    Triyono, Joko; Triyono, Susilowati, Endang; Murdiyantara, Suci Anindya

    2016-03-01

    This work reports on the effect of shellac coated hydroxyapatite (HA) on the biodegradation rate. The HA was processed from bovine bone. Shellac was derived from the resinous secretion of the lac insect. The aims of the addition of shellac solution is to know how the biodegradation rate material in the Phosphate Buffered Saline (PBS) solution. The four different of shellac solutions (2,5%; 5%; 7,5%; and 10% weight) coated HA scaffoldand one ratio as a control. It was concluded that the ability of biodegradation rate a materialwas not influenced by the ratio of shellac. All materials were biodegradedwhen they were soaked in PBS solution.

  19. Effects of rheological properties on ice-templated porous hydroxyapatite ceramics.

    PubMed

    Zhang, Yan; Zhou, Kechao; Bao, Yinxiang; Zhang, Dou

    2013-01-01

    Freeze casting of aqueous suspension was investigated as a method for fabricating hydroxyapatite (HA) porous ceramics with lamellar structures. The rheological properties of HA suspensions employed in the ice-templated process were investigated systematically. Well aligned lamellar pores and dense ceramic walls were obtained successfully in HA porous ceramics with the porosity of 68-81% and compressive strength of 0.9-2.4 MPa. The results exhibited a strong correlation between the rheological properties of the employed suspensions and the morphology and mechanical properties of ice-templated porous HA ceramics, in terms of lamellar pore characteristics, porosities and compressive strengths. The ability to produce aligned pores and achieve the manipulation of porous HA microstructures by controlling the rheological parameters were demonstrated, revealing the potential of the ice-templated method for the fabrication of HA scaffolds in biomedical applications. PMID:25428079

  20. Biomimetic mineralization of nano-sized, needle-like hydroxyapatite with ultrahigh capacity for lysozyme adsorption.

    PubMed

    Ma, Yi; Zhang, Juan; Guo, Shanshan; Shi, Jie; Du, Wenying; Wang, Zheng; Ye, Ling; Gu, Wei

    2016-11-01

    Because of its superior biocompatibility, hydroxyapatite (HA) has been widely exploited as a promising vehicle to deliver a broad range of therapeutics in a variety of biological systems. Herein, we report a biomimetic process to prepare nano-sized, colloidal stable HA with needle-like morphology by using carboxymethyl cellulose (CMC) as the template. It was revealed that the needle-like HA was transformed from the spherical amorphous calcium phosphate (ACP) nanoparticles after a 14-day period of aging under ambient conditions. The needle-like HA/CMC exhibited an ultra-high lysozyme adsorption capacity up to 930-940mg/g. Moreover, a sustained and pH-sensitive release of adsorbed lysozyme from HA/CMC was evidenced. Therefore, our biomimetic needle-like HA/CMC nanoparticles hold great potential in serving as an efficient carrier for the delivery and controlled release of lysozyme. PMID:27524053

  1. Nanostructural Characteristics of Vacuum Cold-Sprayed Hydroxyapatite/Graphene-Nanosheet Coatings for Biomedical Applications

    NASA Astrophysics Data System (ADS)

    Liu, Yi; Huang, Jing; Li, Hua

    2014-10-01

    Development of novel biocompatible nanomaterials has provided insights into their potential biomedical applications. Bulk fabrication of the nanomaterials in the form of coatings remains challenging. Here, we report hydroxyapatite (HA)/graphene-nanosheet (GN) composite coatings deposited by vacuum cold spray (VCS). Significant shape changes of HA nanograins during the coating deposition were revealed. The nanostructural features of HA together with curvature alternation of GN gave rise to dense structures. Based on the microstructural characterization, a structure model was proposed to elucidate the nanostructural characteristics of the HA-GN nanocomposites. Results also showed that addition of GN significantly enhanced fracture toughness and elastic modulus of the HA-based coatings, which is presumably accounted for by crack bridging offered by GN in the composites. The VCS HA-GN coatings show potential for biomedical applications for the repair or replacement of hard tissues.

  2. 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.

  3. Photocatalytic Deposition of Hydroxyapatite onto a Titanium Dioxide Nanotubular Layer with Fine Tuning of Layer Nanoarchitecture.

    PubMed

    Ulasevich, Sviatlana A; Poznyak, Sergey K; Kulak, Anatoly I; Lisenkov, Aleksey D; Starykevich, Maksim; Skorb, Ekaterina V

    2016-04-26

    A new effective method of photocatalytic deposition of hydroxyapatite (HA) onto semiconductor substrates is proposed. A highly ordered nanotubular TiO2 (TNT) layer formed on titanium via its anodization is chosen as the photoactive substrate. The method is based on photodecomposition of the phosphate anion precursor, triethylphosphate (TEP), on the semiconductor surface with the following reaction of formed phosphate anions with calcium cations presented in the solution. HA can be deposited only on irradiated areas, providing the possibility of photoresist-free HA patterning. It is shown that HA deposition can be controlled via pH, light intensity, and duration of the process. Energy-dispersive X-ray spectroscopy profile analysis and glow discharge optical emission spectroscopy of HA-modified TNT prove that HA deposits over the entire TNT depth. High biocompatibility of the surfaces is proven by protein adsorption and pre-osteoblast cell growth. PMID:26991479

  4. Inhibition of hydroxyapatite formation by osteopontin phosphopeptides.

    PubMed Central

    Pampena, David A; Robertson, Karen A; Litvinova, Olga; Lajoie, Gilles; Goldberg, Harvey A; Hunter, Graeme K

    2004-01-01

    Osteopontin (OPN) is an acidic phosphoglycoprotein that is believed to function in the prevention of soft tissue calcification. In vitro studies have shown that OPN can inhibit the formation of hydroxyapatite (HA) and other biologically relevant crystal phases, and that this inhibitory activity requires phosphorylation of the protein; however, it is not known which phosphorylated residues are involved. We have synthesized peptides corresponding to four phosphoserine-containing sequences in rat OPN: OPN7-17, containing phosphoserines 10 and 11; OPN41-52, containing phosphoserines 46 and 47; OPN248-264, containing phosphoserines 250, 257 and 262; and OPN290-301, containing phosphoserines 295-297. The abilities of these peptides to inhibit de novo HA formation were determined using a constant-composition autotitration assay. All four OPN phosphopeptides caused a dose-dependent increase in nucleation lag time, but did not significantly affect subsequent formation of the crystals. However, OPN41-52 (inhibitory constant 73.5 min/microM) and OPN290-301 (72.2 min/microM) were approx. 4 times more potent inhibitors than OPN7-17 (19.7 min/microM) and OPN247-264 (16.3 min/microM). 'Scrambling' the amino acid sequence of OPN290-301 resulted in decreased potency (45.6 min/microM), whereas omission of the phosphate groups from this peptide caused a greater decrease (5.20 min/microM). These findings have identified phosphorylated sequences that are important for the ability of rat bone OPN to inhibit HA crystal formation, and suggest that negative-charge density is an important factor in this activity. PMID:14678013

  5. Calcium Deficient Hydroxyapatite for Medical Application Prepared by Hydrothermal Method

    NASA Astrophysics Data System (ADS)

    Ioku, Koji; Kamitakahara, Masanobu; Ikeda, Tohru

    2010-11-01

    Hydrothermal processing plays a key role in the synthesis of biomaterials with excellent biocompatibility in the physiological environment. Especially, calcium phosphates are paid to much attention for the regenerative medicine. Two kinds of porous materials of hydroxyapatite with 70% porosity were prepared. One of them is a newly developed calcium-deficient hydroxyapatite composed of rod-shaped particles of about 20 μm in length synthesized hydrothermally (HHA) and the other one is the stoichiometric hydroxyapatite (SHA) prepared by the conventional sintering method. These materials were used for animal implantation tests to compare these biological responses. In the rabbit femur, implanted HHA was slowly resorbed and then most of the implanted HHA was resorbed after 72 weeks. The implanted SHA was unresorbed throughout the experimental period. The volume of newly formed bone and the number of osteoclasts in the implanted region were significantly larger in HHA than in SHA after 24 weeks. Results in the present research suggested that the activity of osteoclasts correlated to the bone forming activity of osteoblasts. The method to synthesize biodegradable pure calcium-deficient HA is expected to provide adequate biodegradability and bone replaceability.

  6. Synthesis of fluorapatite–hydroxyapatite nanoparticles and toxicity investigations

    PubMed Central

    Montazeri, N; Jahandideh, R; Biazar, Esmaeil

    2011-01-01

    In this study, calcium phosphate nanoparticles with two phases, fluorapatite (FA; Ca10(PO4)6F2) and hydroxyapatite (HA; Ca10(PO4)6(OH)2), were prepared using the solgel method. Ethyl phosphate, hydrated calcium nitrate, and ammonium fluoride were used, respectively, as P, Ca, and F precursors with a Ca:P ratio of 1:72. Powders obtained from the sol-gel process were studied after they were dried at 80°C and heat treated at 550°C. The degree of crystallinity, particle and crystallite size, powder morphology, chemical structure, and phase analysis were investigated by scanning electron microscopy (SEM), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), and Zetasizer experiments. The results of XRD analysis and FTIR showed the presence of hydroxyapatite and fluorapatite phases. The sizes of the crystallites estimated from XRD patterns using the Scherrer equation and the crystallinity of the hydroxyapatite phase were about 20 nm and 70%, respectively. Transmission electron microscope and SEM images and Zetasizer experiments showed an average size of 100 nm. The in vitro behavior of powder was investigated with mouse fibroblast cells. The results of these experiments indicated that the powders were biocompatibile and would not cause toxic reactions. These compounds could be applied for hard-tissue engineering. PMID:21499417

  7. Synthesis of fluorapatite-hydroxyapatite nanoparticles and toxicity investigations.

    PubMed

    Montazeri, N; Jahandideh, R; Biazar, Esmaeil

    2011-01-01

    In this study, calcium phosphate nanoparticles with two phases, fluorapatite (FA; Ca(10)(PO(4))(6)F(2)) and hydroxyapatite (HA; Ca(10)(PO(4))(6)(OH)(2)), were prepared using the solgel method. Ethyl phosphate, hydrated calcium nitrate, and ammonium fluoride were used, respectively, as P, Ca, and F precursors with a Ca:P ratio of 1:72. Powders obtained from the sol-gel process were studied after they were dried at 80°C and heat treated at 550°C. The degree of crystallinity, particle and crystallite size, powder morphology, chemical structure, and phase analysis were investigated by scanning electron microscopy (SEM), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), and Zetasizer experiments. The results of XRD analysis and FTIR showed the presence of hydroxyapatite and fluorapatite phases. The sizes of the crystallites estimated from XRD patterns using the Scherrer equation and the crystallinity of the hydroxyapatite phase were about 20 nm and 70%, respectively. Transmission electron microscope and SEM images and Zetasizer experiments showed an average size of 100 nm. The in vitro behavior of powder was investigated with mouse fibroblast cells. The results of these experiments indicated that the powders were biocompatible and would not cause toxic reactions. These compounds could be applied for hard-tissue engineering. PMID:21499417

  8. Mechanical properties of hydroxyapatite whisker reinforced polyetherketoneketone composite scaffolds.

    PubMed

    Converse, Gabriel L; Conrad, Timothy L; Roeder, Ryan K

    2009-12-01

    The apparent mechanical properties of hydroxyapatite (HA) whisker reinforced polyetherketoneketone (PEKK) scaffolds were evaluated in unconfined, uniaxial compression to investigate the effects of the porosity (75%, 82.5% and 90%), HA content (0, 20 and 40 vol%) and mold temperature (350, 365 and 375 ( composite function)C). Increased porosity resulted in a non-linear decrease in the elastic modulus and yield strength for both reinforced and unreinforced PEKK scaffolds, as expected. The increase in elastic modulus and yield strength with increased relative density followed a power-law, similar to trabecular bone and other open-cell foams. HA whisker reinforcement generally resulted in an increased elastic modulus from 0 to 20 vol% HA and a subsequent decrease from 20 to 40 vol% HA, while the yield strength and strain were decreased in scaffolds with 40 vol% HA compared to those with 0 or 20 vol% HA. Increased mold temperature resulted in an increased elastic modulus, yield strength and yield strain. These effects enabled the mechanical properties to be tailored to mimic human trabecular bone. The elastic modulus was greater than 50 MPa, and the yield strength was greater than 0.5 MPa, for scaffolds with 75% porosity at all combinations of reinforcement level and mold temperature. Scaffolds with 75% porosity and 20 vol% HA molded at 375 ( composite function)C exhibited a mean elastic modulus and yield strength of 149 MPa and 2.2 MPa, respectively, which was the highest of the conditions investigated in this study and similar to human vertebral trabecular bone. Therefore, HA whisker reinforced PEKK scaffolds may be advantageous for permanent implant fixation, including interbody spinal fusion. PMID:19716108

  9. Properties of Nanostructured Hydroxyapatite Prepared by a Spray Drying Technique.

    PubMed

    Chow, Laurence C; Sun, Limin; Hockey, Bernard

    2004-01-01

    In previous studies nano sized hydroxyapatite (HA) particles were prepared by solgel or precipitation methods, in which the products were washed by aqueous or non-aqueous liquids to remove impurities or undesired components. The washing is know to modify the surfaces of the cystalline particles. This study evaluated properties of nano HA materials prepared by a spray drying method in which the HA product was not exposed to any liquid after its formation. The spray drying apparatus consisted of a nozzle that sprayed an acidic calcium phosphate solution in the form of a fine mist into a stream of filtered air flowing through a heated glass column. The water and volatile acid were evaporated by the time the mist reached the end of the column, and the fine particles were collected by an electrostatic precipitator. Powder x ray diffraction patterns suggested the material was amorphous, exhibiting a single broad peak at 30.5° 2θ. However, high resolution transmission electron microscopic analysis showed that the particles, some of which were 5 nm in size, exhibited well ordered HA lattice fringes. Small area diffraction patterns were indicative of HA. Fourier transfer infrared spectroscopy showed patterns of typical of HA with small amounts of HPO4 (2-). The thermodynamic solubility product of the nano HA was 3.3 × 10(-94) compared to 1 × 10(-117) for macro scale crystalline HA. These results showed that a spray drying technique can be used to prepare nanometer sized crystalline HA that have significantly different physicochemical properties than those of its bulk-scale counterpart. PMID:27366633

  10. Properties of Nanostructured Hydroxyapatite Prepared by a Spray Drying Technique

    PubMed Central

    Chow, Laurence C.; Sun, Limin; Hockey, Bernard

    2004-01-01

    In previous studies nano sized hydroxyapatite (HA) particles were prepared by solgel or precipitation methods, in which the products were washed by aqueous or non-aqueous liquids to remove impurities or undesired components. The washing is know to modify the surfaces of the cystalline particles. This study evaluated properties of nano HA materials prepared by a spray drying method in which the HA product was not exposed to any liquid after its formation. The spray drying apparatus consisted of a nozzle that sprayed an acidic calcium phosphate solution in the form of a fine mist into a stream of filtered air flowing through a heated glass column. The water and volatile acid were evaporated by the time the mist reached the end of the column, and the fine particles were collected by an electrostatic precipitator. Powder x ray diffraction patterns suggested the material was amorphous, exhibiting a single broad peak at 30.5° 2θ. However, high resolution transmission electron microscopic analysis showed that the particles, some of which were 5 nm in size, exhibited well ordered HA lattice fringes. Small area diffraction patterns were indicative of HA. Fourier transfer infrared spectroscopy showed patterns of typical of HA with small amounts of HPO42−. The thermodynamic solubility product of the nano HA was 3.3 × 10−94 compared to 1 × 10−117 for macro scale crystalline HA. These results showed that a spray drying technique can be used to prepare nanometer sized crystalline HA that have significantly different physicochemical properties than those of its bulk-scale counterpart. PMID:27366633

  11. 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

  12. 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

    Filová, Elena; Suchý, Tomáš; Sucharda, Zbyněk; Supová, Monika; Zaloudková, Margit; Balík, Karel; Lisá, Věra; Slouf, 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

  13. Fabrication of glass microspheres with conducting surfaces

    DOEpatents

    Elsholz, William E.

    1984-01-01

    A method for making hollow glass microspheres with conducting surfaces by adding a conducting vapor to a region of the glass fabrication furnace. As droplets or particles of glass forming material pass through multiple zones of different temperature in a glass fabrication furnace, and are transformed into hollow glass microspheres, the microspheres pass through a region of conducting vapor, forming a conducting coating on the surface of the microspheres.

  14. Fabrication of glass microspheres with conducting surfaces

    DOEpatents

    Elsholz, W.E.

    1982-09-30

    A method for making hollow glass microspheres with conducting surfaces by adding a conducting vapor to a region of the glass fabrication furnace. As droplets or particles of glass forming material pass through multiple zones of different temperature in a glass fabrication furnace, and are transformed into hollow glass microspheres, the microspheres pass through a region of conducting vapor, forming a conducting coating on the surface of the microspheres.

  15. 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. PMID:19627776

  16. In vitro study on the degradation of lithium-doped hydroxyapatite for bone tissue engineering scaffold.

    PubMed

    Wang, Yaping; Yang, Xu; Gu, Zhipeng; Qin, Huanhuan; Li, Li; Liu, Jingwang; Yu, Xixun

    2016-09-01

    Li-doped hydroxyapatite (LiHA) which is prepared through introducing low dose of Li into hydroxyapatite (HA) has been increasingly studied as a bone tissue-engineered scaffold. The degradation properties play a crucial role in the success of long-term implantation of a bone tissue-engineered construct. Herein, the in vitro degradation behaviors of LiHA scaffolds via two approaches were investigated in this study: solution-mediated degradation and osteoblast-mediated degradation. In solution-mediated degradation, after being immersed in simulated body fluid (SBF) for some time, some characteristics of these scaffolds (such as release of ionized lithium and phosphate, pH change, mechanical properties, cytocompatibility and SEM surface characterization) were systematically tested. A similar procedure was also employed to research the degradation behaviors of LiHA scaffolds in osteoblast-mediated degradation. The results suggested that the degradation in SBF and degradation in culture medium with cell existed distinguishing mechanisms. LiHA scaffolds were degraded via a hydrolytic mechanism when they were soaked in SBF. Upon degradation, an apatite precipitation (layer) was formed on the surfaces of scaffolds. While a biological mechanism was presented for the degradation of scaffolds in cell-mediated degradation. Compared with pure HA, LiHA scaffolds had a better effect on the growth of osteoblast cells, meanwhile, the release amount of PO4(3-) in a degradation medium indicated that osteoblasts could accelerate the degradation of LiHA due to the more physiological activities of osteoblast. According to the results from compressive strength test, doping Li into HA could enhance the strength of HA. Moreover, the results from MTT assay and SEM observation showed that the degradation products of LiHA scaffolds were beneficial to the proliferation of osteoblasts. The results of this research can provide the theoretical basis for the clinical application of LiHA scaffolds

  17. Elaboration of the hydroxyapatite with different precursors and application for the retention of the lead.

    PubMed

    Meski, S; Ziani, S; Khireddine, H; Yataghane, F; Ferguene, N

    2011-01-01

    Carbonate hydroxyapatite (CHAP) was synthesized from different precursors; synthetic (CaCO3 and Ca(OH)2) and natural (egg shell before and after calcinations at 900 degrees C) under different conditions and characterized by using TG/DTG analysis, X-ray powder diffraction (XRD) method and Fourier transform infrared (FT-IR) spectroscopy techniques. The results of these analyses indicate that the four powders present the same structure of hydroxyapatite. Furthermore the four powders obtained were used for the retention of lead. The results obtained indicated that all powders present high adsorption capacity for lead, but from environmental and economic views, the hydroxyapatite synthesized from eggshell no calcined (HA2) is most advantageous. The influence of different sorption parameters, such as: initial metal concentration, equilibration time, solution pH and sorbent dosage was studied and discussed. PMID:21977625

  18. Hydrothermal fabrication of hydroxyapatite on the PEG-grafted surface of wood from Chinese Glossy Privet

    NASA Astrophysics Data System (ADS)

    Wang, Ning; Cai, Chuanjie; Cai, Dongqing; Cheng, Junjie; Li, Shengli; Wu, Zhengyan

    2012-10-01

    Wood-hydroxyapatite composite material was developed by depositing hydrated calcium hydrogen phosphate (HCHP) on the surface of wood from Chinese Glossy Privet (CGP) with polyethylene glycol (PEG, HO(CH2CH2O)nH) as the grafting agent and subsequent hydrothermal vapor treatment. The results illustrated that HCHP could adhere quickly and strongly on the PEG-grafted wood surface. Moreover, this HCHP could be efficiently transformed to hydroxyapatite (HA, Ca10(PO4)6(OH)2) by hydrothermal vapor treatment. IR, XRD analysis and SEM observation indicated that the fabricated hydroxyapatite was pure and its morphology was uniform and microporous. This work provides a new fabricating approach of biocompatible material which may have some potential applications as bone-repairing material.

  19. XPS and bioactivity study of the bisphosphonate pamidronate adsorbed onto plasma sprayed hydroxyapatite coatings

    NASA Astrophysics Data System (ADS)

    McLeod, Kate; Kumar, Sunil; Smart, Roger St. C.; Dutta, Naba; Voelcker, Nicolas H.; Anderson, Gail I.; Sekel, Ron

    2006-12-01

    This paper reports the use of X-ray photoelectron spectroscopy (XPS) to investigate bisphosphonate (BP) adsorption onto plasma sprayed hydroxyapatite (HA) coatings commonly used for orthopaedic implants. BPs exhibit high binding affinity for the calcium present in HA and hence can be adsorbed onto HA-coated implants to exploit their beneficial properties for improved bone growth at the implant interface. A rigorous XPS analysis of pamidronate, a commonly used nitrogenous BP, adsorbed onto plasma sprayed HA-coated cobalt-chromium substrates has been carried out, aimed at: (a) confirming the adsorption of this BP onto HA; (b) studying the BP diffusion profile in the HA coating by employing the technique of XPS depth profiling; (c) confirming the bioactivity of the adsorbed BP. XPS spectra of plasma sprayed HA-coated discs exposed to a 10 mM aqueous BP solution (pamidronate) for periods of 1, 2 and 24 h showed nitrogen and phosphorous photoelectron signals corresponding to the BP, confirming its adsorption onto the HA substrate. XPS depth profiling of the 2 h BP-exposed HA discs showed penetration of the BP into the HA matrix to depths of at least 260 nm. The bioactivity of the adsorbed BP was confirmed by the observed inhibition of osteoclast (bone resorbing) cell activity. In comparison to the HA sample, the HA sample with adsorbed BP exhibited a 25-fold decrease in primary osteoclast cells.

  20. Characterization of dicalcium phosphate dihydrate cements prepared using a novel hydroxyapatite-based formulation.

    PubMed

    Alge, Daniel L; Santa Cruz, Grace; Goebel, W Scott; Chu, Tien-Min Gabriel

    2009-04-01

    Dicalcium phosphate dihydrate (DCPD) cements are typically prepared using beta-tricalcium phosphate (beta-TCP) as the base component. However, hydroxyapatite (HA) is an interesting alternative because of its potential for reducing cement acidity, as well as modulating cement properties via ionic substitutions. In the present study, we have characterized DCPD cements prepared with a novel formulation based on monocalcium phosphate monohydrate (MCPM) and HA. Cements were prepared using a 4:1 MCPM:HA molar ratio. The reactivity of HA in this system was verified by showing DCPD formation using poorly crystalline HA, as well as highly crystalline HA. Evaluation of cements prepared with poorly crystalline HA revealed that setting occurs rapidly in the MCPM/HA system, and that the use of a setting regulator is necessary to maintain workability of the cement paste. Compressive testing showed that MCPM/HA cements have strengths comparable to what has previously been published for DCPD cements. However, preliminary in vitro analysis of cement degradation revealed that conversion of DCPD to HA may occur much more rapidly in the MCPM/HA system compared to cements prepared with beta-TCP. Future studies should investigate this property further, as it could have important implications for the use of HA-based DCPD cement formulations. PMID:19349655

  1. Microspheres and their methods of preparation

    DOEpatents

    Bose, Anima B; Yang, Junbing

    2015-03-24

    Carbon microspheres are doped with boron to enhance the electrical and physical properties of the microspheres. The boron-doped carbon microspheres are formed by a CVD process in which a catalyst, carbon source and boron source are evaporated, heated and deposited onto an inert substrate.

  2. Synthesis and Characterization of Collagen Scaffolds Reinforced by Eggshell Derived Hydroxyapatite for Tissue Engineering.

    PubMed

    Padmanabhan, Sanosh Kunjalukkal; Salvatore, Luca; Gervaso, Francesca; Catalano, Massimo; Taurino, Antonietta; Sannino, Alessando; Licciulli, Antonio

    2015-01-01

    In this work, we synthesized porous nanohydroxyapatite/collagen composite scaffold (nHA-COL), which resemble extracellular matrices in bone and cartilage tissues. Nano hydroxyapatite (nHA) was successfully nucleated in to the collagen matrix using hen eggshell as calcium biogenic source. Porosity was evaluated by apparent and theoretical density measurement. Porosity of all scaffolds was in the range of 95-98%. XRD and TEM analyses show the purity and size of nucleated HA around 10 nm and selected area electron diffraction (SAED) analysis reveals the polycrystalline nature of nucleated HA. SEM analysis reveals (i) all the scaffolds have interconnected pores with an average pore diameter of 130 micron and (ii) aggregates of hydroxyapatite were strongly embedded in the collagen matrix for both composite scaffolds compared with pure collagen scaffold. EDS analysis shows the Ca/P stoichiometric ratio around 1.67 and FTIR reveals the chemical interaction between the collagen molecule and HA particles. The testing of mechanical properties evidenced that incorporation of HA resulted in up to a two-fold increase in compressive modulus with high reinforcement level (-7 kPa for 50HA-50COL) compared to pure collagen scaffold. PMID:26328390

  3. Multilayered polymer microspheres by thermal imprinting during microsphere growth.

    PubMed

    Takekoh, Ryu; Li, Wen-Hui; Burke, Nicholas A D; Stöver, Harald D H

    2006-01-11

    Modulation of the polymerization temperature in precipitation polymerizations was used to form onion-type polymer microspheres consisting of multiple nested layers. Specifically, the copolymerization of chloromethylstyrene and divinylbenzene-55 in acetonitrile, at temperatures ramping between 65 and 75 degrees C, led to monodisperse, cross-linked microspheres of about 10 mum diameter that have radial density profiles closely reflecting the thermal profiles used. This thermal imprinting is attributed to the copolymer formed being close to its theta point during the polymerization. As the microspheres grow by continuously capturing oligomers from solution, the resulting transient surface gel layer expands and contracts with temperature, and thus records the reaction temperature profile in the form of a corresponding density profile, even as it cross-links. PMID:16390152

  4. 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

  5. Advances in Microsphere Insulation Systems

    NASA Astrophysics Data System (ADS)

    Allen, M. S.; Baumgartner, R. G.; Fesmire, J. E.; Augustynowicz, S. D.

    2004-06-01

    Microsphere insulation, typically consisting of hollow glass bubbles, combines in a single material the desirable properties that other insulations only have individually. The material has high crush strength, low density, is noncombustible, and performs well in soft vacuum. Microspheres provide robust, low-maintenance insulation systems for cryogenic transfer lines and dewars. They also do not suffer from compaction problems typical of perlite that result in the necessity to reinsulate dewars because of degraded thermal performance and potential damage to its support system. Since microspheres are load bearing, autonomous insulation panels enveloped with lightweight vacuum-barrier materials can be created. Comprehensive testing performed at the Cryogenics Test Laboratory located at the NASA Kennedy Space Center demonstrated competitive thermal performance with other bulk materials. Test conditions were representative of actual-use conditions and included cold vacuum pressure ranging from high vacuum to no vacuum and compression loads from 0 to 20 psi. While microspheres have been recognized as a legitimate insulation material for decades, actual implementation has not been pursued. Innovative microsphere insulation system configurations and applications are evaluated.

  6. Synthesis and characterization of hydroxyapatite nanofiber by chemical precipitation method using surfactants

    SciTech Connect

    Gao, Shan; Sun, Kangning; Li, Aimin; Wang, Hongyou

    2013-03-15

    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 by 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.

  7. Hydroxyapatite-hybridized chitosan/chitin whisker bionanocomposite fibers for bone tissue engineering applications.

    PubMed

    Pangon, Autchara; Saesoo, Somsak; Saengkrit, Nattika; Ruktanonchai, Uracha; Intasanta, Varol

    2016-06-25

    Biomimetic nanofibrous scaffolds derived from natural biopolymers for bone tissue engineering applications require good mechanical and biological performances including biomineralization. The present work proposes the utility of chitin whisker (CTWK) to enhance mechanical properties of chitosan/poly(vinyl alcohol) (CS/PVA) nanofibers and to offer osteoblast cell growth with hydroxyapatite (HA) mineralization. By using diacid as a solvent, electrospun CS/PVA nanofibrous membranes containing CTWK can be easily obtained. The dimension stability of nanofibrous CS/PVA/CTWK bionanocomposite is further controlled by exposing to glutaraldehyde vapor. The nanofibrous membranes obtained allow mineralization of HA in concentrated simulated body fluid resulting in an improvement of Young's modulus and tensile strength. The CTWK combined with HA in bionanocomposite is a key to promote osteoblast cell adhesion and proliferation. The present work, for the first time, demonstrates the use of CTWKs for bionanocomposite fibers of chitosan and its hydroxyapatite biomineralization with the function in osteoblast cell culture. These hydroxyapatite-hybridized CS/PVA/CTWK bionanocomposite fibers (CS/PVA/CTWK-HA) offer a great potential for bone tissue engineering applications. PMID:27083834

  8. Evaluation of the novel three-dimensional porous poly (L-lactic acid)/nano-hydroxyapatite composite scaffold.

    PubMed

    Huang, Jianghong; Xiong, Jianyi; Liu, Jianquan; Zhu, Weimin; Chen, Jielin; Duan, Li; Zhang, Jufeng; Wang, Daping

    2015-01-01

    To determine the optimal ratio of nano-hydroxyapatite (n-HA) to polylactic acid (PLLA) in the novel three-dimensional porous PLLA/n-HA composite scaffolds, low-temperature rapid prototyping technology was employed to fabricate the composite materials with different n-HA contents. Mechanical properties and degradation behaviors of the composites were examined, and the scaffold microstructure and n-HA dispersion were observed by scanning electron microscope (SEM). Mechanical tests demonstrated that the tensile strength of the composite material gradually decreased with an increase in n-HA content. When the n-HA content reached 20 wt%, the bending strength of the composite material peaked at 138.5 MPa. SEM images demonstrated that the optimal content of n-HA was 20 wt% as the largest interconnected pore size that can be seen, with a porosity as high as 80%. In vitro degradation experiments demonstrated that the pH value of the material containing solution gradually decreased in a time-dependent manner, with a simultaneous weakening of the mechanical properties. In vitro study using rat osteoblast cells showed that the composite scaffolds were biocompatible; the 20 wt% n-HA scaffold offered particular improvement to rat osteoblast cell adhesion and proliferation compared to other compositions. It was therefore concluded that 20 wt% n-HA is the optimal nano-hydroxyapatite (n-HA) to polylactic acid (PLLA) ratio, with promise for bone tissue engineering. PMID:26405972

  9. The impact of the RGD peptide on osteoblast adhesion and spreading on zinc-substituted hydroxyapatite surface.

    PubMed

    Mavropoulos, Elena; Hausen, Moema; Costa, Andrea M; Alves, Gutemberg; Mello, Alexandre; Ospina, C A; Mir, M; Granjeiro, José M; Rossi, Alexandre M

    2013-05-01

    The incorporation of zinc into the hydroxyapatite structure (ZnHA) has been proposed to stimulate osteoblast proliferation and differentiation. Another approach to improve cell adhesion and hydroxyapatite (HA) performance is coating HA with adhesive proteins or peptides such as RGD (arginine-glycine-aspartic acid). The present study investigated the adhesion of murine osteoblastic cells to non-sintered zinc-substituted HA disks before and after the adsorption of RGD. The incorporation of zinc into the HA structure simultaneously changed the topography of disk's surface on the nanoscale and the disk's surface chemistry. Fluorescence microscopy analyses using RGD conjugated to a fluorescein derivative demonstrated that ZnHA adsorbed higher amounts of RGD than non-substituted HA. Zinc incorporation into HA promoted cell adhesion and spreading, but no differences in the cell density, adhesion and spreading were detected when RGD was adsorbed onto ZnHA. The pre-treatment of disks with fetal bovine serum (FBS) greatly increased the cell density and cell surface area for all RGD-free groups, overcoming the positive contribution of zinc to cell adhesion. The presence of RGD on the ZnHA surface impaired the effects of FBS pre-treatment possibly due to competition between FBS proteins and RGD for surface binding sites. PMID:23494616

  10. Degradation behavior of hydroxyapatite/poly(lactic-co-glycolic) acid nanocomposite in simulated body fluid

    SciTech Connect

    Liuyun, Jiang; Chengdong, Xiong; Lixin, Jiang; Lijuan, Xu

    2013-10-15

    Graphical abstract: In this manuscript, we initiated a systematic study to investigate the effect of HA on thermal properties, inner structure, reduction of mechanical strength, surface morphology and the surface deposit of n-HA/PLGA composite with respect to the soaking time. The results showed that n-HA played an important role in improving the degradation behavior of n-HA/PLGA composite, which can accelerate the degradation of n-HA/PLGA composite and endow it with bioactivity, after n-HA was detached from PLGA during the degradation, so that n-HA/PLGA composite may have a more promising prospect of the clinical application than pure PLGA as bone fracture internal fixation materials, and the results would be of reference significance to predict the in vivo degradation and biological properties. - Highlights: • Effect of n-HA on degradation behavior of n-HA/PLGA composite was investigated. • Degradation behaviors of n-HA/PLGA and PLGA were carried out in SBF for 6 months. • Viscosity, thermal properties, inner structure and bending strength were tested. • n-HA can accelerate the degradation and endows it with bioactivity. - Abstract: To investigate the effect of hydroxyapatite(HA) on the degradation behavior of hydroxyapatite/poly(lactic-co-glycolic) acid (HA/PLGA) nanocomposite, the degradation experiment of n-HA/PLGA composite and pure PLGA were carried out by soaking in simulated body fluid(SBF) at 37 °C for 1, 2, 4 and 6 months. The change of intrinsic viscosity, thermal properties, inner structure, bending strength reduction, surface morphology and the surface deposit of n-HA/PLGA composite and pure PLGA with respect to the soaking time were investigated by means of UbbeloHde Viscometer, differential scanning calorimeter (DSC), scanning electron microscope(SEM), electromechanical universal tester, a conventional camera and X-ray diffraction (XRD). The results showed that n-HA played an important role in improving the degradation behavior of n-HA

  11. Development of dental composites with reactive fillers that promote precipitation of antibacterial-hydroxyapatite layers.

    PubMed

    Aljabo, Anas; Abou Neel, Ensanya A; Knowles, Jonathan C; Young, Anne M

    2016-03-01

    The study aim was to develop light-curable, high strength dental composites that would release calcium phosphate and chlorhexidine (CHX) but additionally promote surface hydroxyapatite/CHX co-precipitation in simulated body fluid (SBF). 80 wt.% urethane dimethacrylate based liquid was mixed with glass fillers containing 10 wt.% CHX and 0, 10, 20 or 40 wt.% reactive mono- and tricalcium phosphate (CaP). Surface hydroxyapatite layer thickness/coverage from SEM images, Ca/Si ratio from EDX and hydroxyapatite Raman peak intensities were all proportional to both time in SBF and CaP wt.% in the filler. Hydroxyapatite was, however, difficult to detect by XRD until 4 weeks. XRD peak width and SEM images suggested this was due to the very small size (~10 nm) of the hydroxyapatite crystallites. Precipitate mass at 12 weeks was 22 wt.% of the sample CaP total mass irrespective of CaP wt.% and up to 7 wt.% of the specimen. Early diffusion controlled CHX release, assessed by UV spectrometry, was proportional to CaP and twice as fast in water compared with SBF. After 1 week, CHX continued to diffuse into water but in SBF, became entrapped within the precipitating hydroxyapatite layer. At 12 weeks CHX formed 5 to 15% of the HA layer with 10 to 40 wt.% CaP respectively. Despite linear decline of strength and modulus in 4 weeks from 160 to 101 MPa and 4 to 2.4 GPa, respectively, upon raising CaP content, all values were still within the range expected for commercial composites. The high strength, hydroxyapatite precipitation and surface antibacterial accumulation should reduce tooth restoration failure due to fracture, aid demineralised dentine repair and prevent subsurface carious disease respectively. PMID:26706532

  12. Materials processing and in-vivo animal studies of nitrided hydroxyapatite bioceramics

    NASA Astrophysics Data System (ADS)

    Rashid, Nancy Elizabeth

    2000-10-01

    Calcium phosphate bioceramics are currently being used in medicine and dentistry, for reconstruction or repair of diseased or injured bone, but with limited success. Incorporating nitrogen into phosphate glasses has resulted in improved properties, and it is proposed that similar benefits may be gained from nitriding calcium phosphate bioceramics for bone implants as well. This work focuses on processing of hydroxyapatite and tricalcium phosphate bioceramics nitrided by using solid, liquid, gas and ion sources. These materials were characterized by chemical, structural, mechanical, and biological methods to determine both the material structure and their suitability as implant materials. Calcium nitride and NaPON glass were unsatisfactory sources of nitrogen for hydroxyapatite (HA) and/or tricalcium phosphate (TCP) ceramics. Calcium nitride, Ca3N2, is reacts with water vapor in the air, releasing ammonia, and leaving behind crystals of calcium oxide, CaO. The calcium oxide byproduct decreases the chemical stability of hydroxyapatite and HA/TCP composites in simulated body fluid. Sodium phosphorus oxynitride (NaPON) glass, in the form of a liquid sintering aid for HA, produces an inhomogeneous, composite as well. Hydroxyapatite heated at 800C in an ammonia atmosphere produces a homogeneous material with up to 2 wt% N. Infrared spectroscopy indicates cyanamide ions, CN22-, are formed by the incorporated nitrogen and impurity carbon. The use of 15N-doped ammonia results in an 15N NMR peak at 83.2 ppm, indicating P--N bonding. Raman spectroscopy may also indicate P--N bonding, but it is inconclusive. In a limited study, nitrogen may decrease the hardness and fracture toughness of the phosphate ceramic, hydroxyapatite, contrary to results expected for nitrogen in phosphate glasses. Nitrogen ions are incorporated in hydroxyapatite by ion implantation, with lower energies producing higher nitrogen contents. The highest concentration achieved was 3.55 wt% N, as determined

  13. 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. PMID:25390283

  14. Sulfobetaine as a zwitterionic mediator for 3D hydroxyapatite mineralization

    PubMed Central

    Liu, Pingsheng; Song, Jie

    2013-01-01

    Both positively and negatively charged residues play pivotal roles in recruiting precursor ions or ion clusters, and lowering interfacial energy in natural biomineralization process. Synergistic utilization of opposite charges, however, has rarely been implemented in the design of cytocompatible synthetic scaffolds promoting hydroxyapatite (HA)-mineralization and osteointegration. We report the use of cytocompatible zwitterionic sulfobetaine ligands to enable 3-dimensional in vitro mineralization of HA across covalently crosslinked hydrogels. The overall charge-neutral zwitterionic hydrogel effectively recruited oppositely charged precursor ions while overcame excessive swelling exhibited by anionic and cationic hydrogels under physiological conditions, resulting in denser and structurally well-integrated mineralized composites. Further controls over the size, content, and spatial distribution of the mineral domains within the zwitterionic hydrogel are accomplished by facile adjustments of hydrogel crosslinking densities and the supersaturation rate governing heterogeneous mineral nucleation and growth. These findings should inspire many creative uses of zwitterionic polymers and polymer coatings for skeletal tissue repair and regeneration. PMID:23332320

  15. In vitro bioactivity and cytocompatibility properties of spark plasma sintered HA-Ti composites.

    PubMed

    Kumar, Alok; Dhara, Sharmistha; Biswas, Krishanu; Basu, Bikramjit

    2013-02-01

    The present study reports the results of the detailed in vitro bioactivity and cytocompatibility properties of the hydroxyapatite (HA) and the HA-titanium (HA-Ti) composite with varying amount of Ti (5, 10, and 20 wt %), densified using spark plasma sintering process (SPS). Using this technique and tailoring suitable processing parameters, it has been possible to retain both HA and Ti in the sintered ceramics. Importantly, the uniquely designed SPS processing with suitably chosen parameters enables in achieving better mechanical properties, such as higher indentation fracture toughness (~1.5 MPa m(1/2) ) in HA-Ti composites compared with HA. X-ray diffraction and scanning electron microscopic (SEM) observations reveal good bioactivity of the HA-Ti composites with the formation of thick, flaky, and porous apatite layer when immersed in simulated body fluid at 37°C and pH of 7.4. Atomic absorption spectroscopic analysis of the simulated body fluid solution reveals dynamic changes in Ca(+2) ion concentration with more dissolution of Ca(+2) ion from the HA-20Ti composite. However, the measurements with inductively coupled plasma spectrometer do not record dissolution of Ti(+4) ions. Transmission electron microscopic analysis indicates weak crystalline nature of the apatite and confirms the formation of fine-scale apatite crystals. MTT assay, fluorescence, and SEM study demonstrate good cell viability and cell adhesion/proliferation of the Saos -2 cells, cultured on the developed composites under standard culture condition, and the difference in cell viability has been discussed in reference to substrate composition and roughness. Overall, HA-Ti composites exhibit comparable and even better in vitro bioactivity and cytocompatibility properties than HA. PMID:23281190

  16. Comparison of microstructures and phase compositions of artificial and bone-derived hydroxyapatites by transmission electron microscopy and energy dispersive electron spectroscopy.

    PubMed

    Lee, Jong Kook

    2014-11-01

    Biological problems associated with sintered implants fabricated from artificially synthesized hydroxyapatite include selective dissolution at grain boundaries, microstructural disintegration in the body due to particle loosening, and slow crack growth at the implant surface. In addition, mechanical degradation has been shown to be significant, thus limiting their application as load-bearing medical implants. In contrast, bone-derived hydroxyapatite bioceramics have highly dissolution-resistant properties and excellent biocompatibility in the body. They are also easy to synthesize by thermal decomposition of animal bone. In this study, microstructural observations and crystal phase analysis of bone-derived hydroxyapatite were investigated by TEM and EDS using sintered hydroxyapatite samples. In addition, a comparative investigation into elemental distributions and the microstructures of artificial hydroxyapatite, bovine, and tuna bone-derived hydroxyapatites was performed. Bone-derived HA consists mainly of HA and a small amount of MgO. Hot-pressed HA compacts showed homogeneous microstructures and densities of 95-97%, however, grain sizes and microstructures varied with the starting powders. PMID:25958617

  17. Calcining influence on the powder properties of hydroxyapatite.

    PubMed

    Patel, N; Gibson, I R; Ke, S; Best, S M; Bonfield, W

    2001-02-01

    The effect of different calcination temperatures on the powder characteristics and the sintered density of synthetic hydroxyapatite (HA) powders, produced using two different processing routes, was examined. Powders were produced by either drying, milling and sieving an as-precipitated HA or by spray-drying a slurry of precipitated HA. Calcining the two powders at temperatures between 400 and 1000 degrees C did not significantly affect the powder particle size. The specific surface areas of the two powders, however, were reduced from 70-80 m2/g for a calcination temperature of 400 degrees C to approximately 5-7 m2/g for 1000 degrees C. Analysis of the surfaces of the HA powders using scanning electron microscopy (SEM) illustrated the coarsening and subsequent sintering of the sub-micron crystallites that constitute a powder particle as the calcination temperature increased, corresponding to the decrease in surface area of the powders. The sintered densities of the final ceramics were not significantly affected by calcining the powders. Microhardness measurements of ceramics prepared from powders calcined at different temperatures showed no significant variations with calcination temperature or powder processing method. The results of this study have illustrated that for applications where HA may be used in powder form, for example in plasma-spraying and for the production of HA-polymer composites, calcining the HA will significantly affect the powder properties, namely the surface area and morphology of the powders. For applications requiring HA in a dense ceramic form, for example as granules or blocks, calcining the powders does not significantly affect the properties of the final ceramic. PMID:15348326

  18. Nanocrystalline hydroxyapatite coatings on titanium: a new fast biomimetic method.

    PubMed

    Bigi, Adriana; Boanini, Elisa; Bracci, Barbara; Facchini, Alessandro; Panzavolta, Silvia; Segatti, Francesco; Sturba, Luigina

    2005-07-01

    We obtained a fast biomimetic deposition of hydroxyapatite (HA) coatings on Ti6Al4V substrates using a slightly supersaturated Ca/P solution, with an ionic composition simpler than that of simulated body fluid (SBF). At variance with other fast deposition methods, which produce amorphous calcium phosphate coatings, the new proposed composition allows one to obtain nanocrystalline HA. Soaking in supersaturated Ca/P solution results in the deposition of a uniform coating in a few hours, whereas SBF, or even 1.5SBF, requires 14 days to deposit a homogeneous coating on the same substrates. The coating consists of HA globular aggregates, which exhibit a finer lamellar structure than those deposited from SBF. The extent of deposition increases on increasing the immersion time. Transmission electron microscope (TEM) images recorded on the material detached from the coating show that the deposition is constituted of thin nanocrystals. Electron diffraction (ED) patterns recorded from most of the crystals exhibit the presence of rings, which can be indexed as reflections characteristic of HA. Furthermore, several HA single-crystal spot ED images were obtained from individual crystals. PMID:15664635

  19. Template synthesis and characterization of highly ordered lamellar hydroxyapatite

    NASA Astrophysics Data System (ADS)

    Liu, Chao; Ji, Xiujie; Cheng, Guoxiang

    2007-06-01

    Surfactant template synthesis attracts great attention in the fields of biomaterials and functional materials. In this study, highly ordered lamellar hydroxyapatite (Lα-HA) powder was synthesized by a surfactant templating method in water-ethanol. Ca(NO 3) 2 and (NH 4) 2HPO 4 were used as calcium and phosphorus sources, respectively. Sodium dodecyl sulphonate (SDS, C 12H 25SO 3Na) acted as the template. X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR) analyses showed that HA is the only crystal phase in Lα-HA. Transmission electron microscope (TEM) observation further proved this regular lamellar structure detected by XRD. The repeat periodicity of the structure is about 3.6 nm observed by TEM, which is in well accordance with the XRD data (3.16 nm). The selected area electron diffraction (SAED) results indicated that Lα-HA was a polycrystalline structure. The formation of Lα-HA could be explained by a surfactant template.

  20. Bioactive rosette nanotube-hydroxyapatite nanocomposites improve osteoblast functions.

    PubMed

    Sun, Linlin; Zhang, Lijie; Hemraz, Usha D; Fenniri, Hicham; Webster, Thomas J

    2012-09-01

    Inspired from biological systems, small synthetic organic molecules expressing the hydrogen bonding arrays of the DNA bases guanine and cytosine were prepared, and their self-assembly into rosette nanotubes (RNTs) was investigated. Due to their unique biological, physicochemical, and mechanical properties, RNTs could serve as the next generation of injectable orthopedic materials. In this study, a self-assembling module (termed twin base linkers or TBL) was synthesized, and the corresponding RNTs were used as bioactive components in composites of poly (2-hydroxyethyl methacrylate) (pHEMA) and hydroxyapatite (HA) nanoparticles (termed TBL/HA/pHEMA). The properties of these composites were characterized for solidification time, surface morphology, mechanical properties, and cytocompatibility. The experimental conditions were optimized to achieve solidification within 2-40 min, offering a range of properties for orthopedic applications. Composites with 20 wt% HA nanoparticles had a compressive strength (37.1 MPa) and an ultimate tensile stress (14.7 MPa) similar to that of a natural vertebral disc (5-30 MPa). Specifically, the TBL (0.01 mg/mL)/HA(20 wt%)/pHEMA composites improved long-term functions of osteoblasts (or bone-forming cells) in terms of collagen synthesis, alkaline phosphatase activity, and calcium deposition. Moreover, this composite inhibited fibroblast adhesion, thus decreasing the potential for undesirable fibrous tissue formation. In summary, this in vitro study provided evidence that TBL/HA/pHEMA composites are promising injectable orthopedic implant materials that warrant further mechanistic and in vivo studies. PMID:22530958

  1. Increased risk of revision of acetabular cups coated with hydroxyapatite

    PubMed Central

    Lazarinis, Stergios; Kärrholm, Johan

    2010-01-01

    Background Hydroxyapatite (HA) is the main inorganic component of bone, and HA coating is widely used on acetabular cups in hip arthroplasty. It has been suggested that this surface finish improves cup survival. Methods All patients registered in the Swedish Hip Arthroplasty Register between 1992 and 2007 with an uncemented acetabular implant that was available either with or without HA coating were identified. 8,043 total hip arthroplasties (THAs) with the most common cup types (Harris-Galante, Romanus, and Trilogy) were investigated. A Cox regression model including type of coating, age, sex, primary diagnosis, cup type, and type of stem fixation was used to calculate adjusted risk ratios (RRs) for the risk of revision. Results HA coating was a risk factor for cup revision due to aseptic loosening (adjusted RR 1.7; 95% CI: 1.3–2). Age at primary arthroplasty of < 50 years, a diagnosis of pediatric hip disease, the use of a cemented stem, and the Romanus and Harris-Galante cup types were also associated with statistically significantly increased risk of cup revision due to aseptic loosening. Interpretation Our findings question the routine use of HA-coated cups in primary total hip arthroplasty. With some designs, this practice may even increase the risk of loosening—resulting in revision surgery. PMID:19968603

  2. Hydroxyapatite ceramics from hydrothermally prepared powders

    SciTech Connect

    Lin, C.H.; Huang, C.W.; Chang, S.C.

    1994-12-31

    Hydroxyapatite (Ca{sub 5}(PO{sub 4}){sub 3}(OH)) is an effective material for artificial human bone production. Hydroxyapatite powders were hydrothermally produced in this work by reacting Ca(OH){sub 2} with Na{sub 3}PO{sub 4}{center_dot}12H{sub 2}O in an autoclave at various temperature and for various times. The particle size of hydroxyapatite was observed to be very fine, uniform, around 50 nm, as well as independent of reaction time. The hydroxyapatite powders were compacted and sintered at various temperatures for 2 hrs. The density, grain size, and hardness of the hydroxyapatite ceramics were measured and compared with those of the hydroxyapatite ceramics produced by the powders from the commercial source. The hydroxyapatite ceramics from the hydrothermal powders were found to have a higher density, smaller grain size, and higher hardness. After the hydroxyapatite ceramics were dipped in a simulated biological body liquid for 10 days, the density and hardness of the hydroxyapatite ceramics from the hydrothermal powders were less deteriorated than those of the hydroxyapatite ceramics from the commercial powder.

  3. Modeling the Formation of Polyimide Microspheres

    NASA Technical Reports Server (NTRS)

    Pipes, R. B.; Weiser, E. S.; Gonsoulin, B.; Hubert, P.

    2002-01-01

    High temperature polyimide microspheres have been developed from polyimide solid residuum by a simple inflation process. Microspheres have been fabricated from several polyimide precursors through the use of a circulating air oven. Microsphere formation and final physical property characterization have been limited to simple mechanical and thermal testing. The present paper focuses on developing an understanding of microsphere formation through simple geometric rules for an incompressible polymeric material and microscopic observations of precursor residuum inflation. Inflation kinematics of the hollow polyimide microspheres as a function of time and temperature is discussed.

  4. Polarization Dependent Whispering Gallery Modes in Microspheres

    NASA Technical Reports Server (NTRS)

    Adamovsky, Grigory (Inventor); Wrbanek, Susan Y. (Inventor)

    2016-01-01

    A tunable resonant system is provided and includes a microsphere that receives an incident portion of a light beam generated via a light source, the light beam having a fundamental mode, a waveguide medium that transmits the light beam from the light source to the microsphere, and a polarizer disposed in a path of the waveguide between the light source and the microsphere. The incident portion of the light beam creates a fundamental resonance inside the microsphere. A change in a normalized frequency of the wavelength creates a secondary mode in the waveguide and the secondary mode creates a secondary resonance inside the microsphere.

  5. Mechanisms of uranium interactions with hydroxyapatite: Implications for groundwater remediation

    USGS Publications Warehouse

    Fuller, C.C.; Bargar, J.R.; Davis, J.A.; Piana, M.J.

    2002-01-01

    The speciation of U(VI) sorbed to synthetic hydroxyapatite was investigated using a combination of U LIII-edge XAS, synchrotron XRD, batch uptake measurements, and SEM-EDS. The mechanisms of U(VI) removal by apatite were determined in order to evaluate the feasibility of apatitebased in-situ permeable reactive barriers (PRBs). In batch U(VI) uptake experiments with synthetic hydroxyapatite (HA), near complete removal of dissolved uranium (>99.5%) to <0.05 ??M was observed over a range of total U(VI) concentrations up to equimolar of the total P in the suspension. XRD and XAS analyses of U(VI)-reacted HA at sorbed concentrations ???4700 ppm U(VI) suggested that uranium(VI) phosphate, hydroxide, and carbonate solids were not present at these concentrations. Fits to EXAFS spectra indicate the presence of Ca neighbors at 3.81 A??. U-Ca separation, suggesting that U(VI) adsorbs to the HA surfaces as an inner-sphere complex. Uranium(VI) phosphate solid phases were not detected in HA with 4700 ppm sorbed U(VI) by backscatter SEM or EDS, in agreement with the surface complexation process. In contrast, U(VI) speciation in samples that exceeded 7000 ppm sorbed U(VI) included a crystalline uranium(VI) phosphate solid phase, identified as chernikovite by XRD. At these higher concentrations, a secondary, uranium(VI) phosphate solid was detected by SEM-EDS, consistent with chernikovite precipitation. Autunite formation occurred at total U:P molar ratios ???0.2. Our findings provide a basis for evaluating U(VI) sorption mechanisms by commercially available natural apatites for use in development of PRBs for groundwater U(VI) remediation.

  6. Mesoporous Fe{sub 3}O{sub 4}/hydroxyapatite composite for targeted drug delivery

    SciTech Connect

    Gu, Lina; He, Xiaomei; Wu, Zhenyu

    2014-11-15

    Highlights: • Mesoporous Fe{sub 3}O{sub 4}/hydroxyapatite composite was synthesized by a simple, efficient and environmental friendly method. • The prepared material had a large surface area, high pore volume, and good magnetic separability. • DOX-loaded Fe{sub 3}O{sub 4}/hydroxyapatite composite exhibited surprising slow drug release behavior and pH-dependent behavior. - Abstract: In this contribution, we introduced a simple, efficient, and green method of preparing a mesoporous Fe{sub 3}O{sub 4}/hydroxyapatite (HA) composite. The as-prepared material had a large surface area, high pore volume, and good magnetic separability, which made it suitable for targeted drug delivery systems. The chemotherapeutic agent doxorubicin (DOX) was used to investigate the drug release behavior of Fe{sub 3}O{sub 4}/HA composite. The drug release profiles displayed a little burst effect and pH-dependent behavior. The release rate of DOX at pH 5.8 was larger than that at pH 7.4, which could be attributed to DOX protonation in acid medium. In addition, the released DOX concentrations remained at 0.83 and 1.39 μg/ml at pH 7.4 and 5.8, respectively, which indicated slow, steady, and safe release rates. Therefore, the as-prepared Fe{sub 3}O{sub 4}/hydroxyapatite composite could be an efficient platform for targeted anticancer drug delivery.

  7. 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.

  8. 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. PMID:26116779

  9. 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

  10. Production of monodisperse, polymeric microspheres

    NASA Technical Reports Server (NTRS)

    Rembaum, Alan (Inventor); Rhim, Won-Kyu (Inventor); Hyson, Michael T. (Inventor); Chang, Manchium (Inventor)

    1990-01-01

    Very small, individual polymeric microspheres with very precise size and a wide variation in monomer type and properties are produced by deploying a precisely formed liquid monomer droplet, suitably an acrylic compound such as hydroxyethyl methacrylate into a containerless environment. The droplet which assumes a spheroid shape is subjected to polymerizing radiation such as ultraviolet or gamma radiation as it travels through the environment. Polymeric microspheres having precise diameters varying no more than plus or minus 5 percent from an average size are recovered. Many types of fillers including magnetic fillers may be dispersed in the liquid droplet.

  11. 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. PMID:27349789

  12. The influence of silanisation on the mechanical and degradation behaviour of PLGA/HA composites.

    PubMed

    Naik, Ashutosh; Best, Serena M; Cameron, Ruth E

    2015-03-01

    This study investigates the influence of silanisation on the mechanical and degradation behaviour of PLGA/HA composites. Three different silanes (mercaptopropyl trimethoxy silane (MPTMS), aminopropyl trimethoxy silane (APTMS) and aminopropyltriethoxy silane (APTES)) were applied to HA substrates in order to study the effect of head group (which binds to the polymer) and tail group (which binds to the surface hydroxyl groups in HA). A composite of hydroxyapatite (HA) and poly(d,l lactide-co-glycolide (50:50)) (PLGA) was investigated. The influence of concentration, the reaction time, drying temperature and substrate surface on silanisation was examined. TGA was used to detect the degree of silanisation. HA with MPTMS (1wt.% MPTMS with reaction time of 1h) was used as filler in PLGA-30wt.% HA composites for an in-vitro degradation study carried out in PBS. In addition, the mechanical properties of the composites were studied. Silanisation affects the properties of the composite by improving the bonding at the interface and hence it was found to influence the plastic mechanical properties rather than the elastic mechanical properties or the degradation profile of the composite. PMID:25579967

  13. Tunable Delivery of Bioactive Peptides from HA Biomaterials and Allograft Bone Using Variable Length Polyglutamate Domains

    PubMed Central

    Culpepper, Bonnie K.; Webb, William M.; Bonvallet, Paul P.; Bellis, Susan L.

    2013-01-01

    Hydroxyapatite (HA) biomaterials and allograft bone are common alternatives to autogenous grafts, however these materials lack the strong osteoinductive potential of autologous bone. Previous studies have established that polyglutamate domains, which bind selectively to HA, can be engineered onto bioactive peptides as a mechanism for coupling osteoinductive signals onto HA and allograft. In the current investigation, we adapted the polyglutamate approach to tailor delivery of a model collagen-derived peptide, DGEA, by manipulating the number of glutamates in the HA binding domain. Specifically, DGEA was modified with diglutamate (E2-DGEA), tetraglutamate (E4-DGEA) or heptaglutamate (E7-DGEA), and it was found that initial peptide binding to HA and allograft was significantly enhanced as the number of glutamates increased. We also determined that the rate of release of polyglutamate-DGEA from substrates over a 5-day interval increased proportionally as the number of glutamate residues was decreased. Additionally, we tuned the peptide release rate by creating mixtures of E2-DGEA, E4-DGEA and E7-DGEA, and observed that release kinetics of the mixtures were distinct from pure solutions of each respective peptide. These collective results suggest that variable length polyglutamate domains provide an effective mechanism for controlled delivery of osteoregenerative peptides on HA-containing bone graft materials. PMID:23625466

  14. Evaluation of human osteoblastic cell response to plasma-sprayed silicon-substituted hydroxyapatite coatings over titanium substrates.

    PubMed

    Gomes, Pedro S; Botelho, Cláudia; Lopes, Maria A; Santos, José D; Fernandes, Maria H

    2010-08-01

    Silicon-substituted hydroxyapatite (Si-HA) coatings have been plasma sprayed over titanium substrates (Ti-6Al-4V) aiming to improve the bioactivity of the constructs for bone tissue repair/regeneration. X-ray diffraction analysis of the coatings has shown that, previous to the thermal deposition, no secondary phases were formed due to the incorporation of 0.8 wt % Si into HA crystal lattice. Partial decomposition of hydroxyapatite, which lead to the formation of the more soluble phases of alpha- and beta-tricalcium phosphate and calcium oxide, and increase of amorphization level only occurred following plasma spraying. Human bone marrow-derived osteoblastic cells were used to assess the in vitro biocompatibility of the constructs. Cells attached and grew well on the Si-HA coatings, putting in evidence an increased metabolic activity and alkaline phosphatase expression comparing to control, i.e., titanium substrates plasma sprayed with hydroxyapatite. Further, a trend for increased differentiation was also verified by the upregulation of osteogenesis-related genes, as well as by the augmented deposition of globular mineral deposits within established cell layers. Based on the present findings, plasma spraying of Si-HA coatings over titanium substrates demonstrates improved biological properties regarding cell proliferation and differentiation, comparing to HA coatings. This suggests that incorporation of Si into the HA lattice could enhance the biological behavior of the plasma-sprayed coating. PMID:20574971

  15. Mechanical properties of hydroxyapatite thin films for applications in medical implants

    NASA Astrophysics Data System (ADS)

    Kim, Hyunbin; Catledge, Shane A.; Camata, Renato P.; Vohra, Yogesh K.; Lacefield, William R.

    2002-03-01

    Pulsed laser deposition (PLD) allows control over the structure and composition of hydroxyapatite (HA) coatings used on orthopedic and dental implants. It enables the optimization of the coating mechanical properties that are critical for good implant performance. In this paper we have studied the mechanical properties of crystalline HA films deposited by PLD (Nd:YAG laser, 532 nm). HA films with thickness in the sub-micron range were deposited on Ti6Al4V and X-ray diffraction of the films reveals high HA crystallinity. Atomic force microscopy was performed to study film morphology. Nanoindentation measurements on the coatings have yielded hardness of (4.9 ± 1.1) GPa and elastic modulus of (105 ± 18) GPa, establishing the usefulness of the coatings for implant applications, as they meet current standards of clinically approved implant coatings. Scratch tests results and a new PLD strategy for nanostructured HA films under development in our group will be discussed.

  16. Hydroxyapatite coatings on nanotubular titanium dioxide thin films prepared by radio frequency magnetron sputtering.

    PubMed

    Shin, Jinho; Lee, Kwangmin; Koh, Jeongtae; Son, Hyeju; Kim, Hyunseung; Lim, Hyun-Pil; Yun, Kwidug; Oh, Gyejeong; Lee, Seokwoo; Oh, Heekyun; Lee, Kyungku; Hwang, Gabwoon; Park, Sang-Won

    2013-08-01

    In this study, hydroxyapatite (HA) was coated on anodized titanium (Ti) surfaces through radio frequency magnetron sputtering in order to improve biological response of the titanium surface. All the samples were blasted with resorbable blasting media (RBM). RBM-blasted Ti surface, anodized Ti surface, as-sputtered HA coating on the anodized Ti surface, and heat-treated HA coating on the anodized Ti surface were prepared. The samples were characterized using scanning electron microscopy and X-ray photoemission spectroscopy, and biologic responses were evaluated. The top of the TiO2 nanotubes was not closed by HA particles when the coating time is less than 15 minutes. It was demonstrated that the heat-treated HA was well-crystallized and this enhanced the cell attachment of the anodized Ti surface. PMID:23882839

  17. A new approach to enhancement of bone formation by electrically polarized hydroxyapatite.

    PubMed

    Teng, N C; Nakamura, S; Takagi, Y; Yamashita, Y; Ohgaki, M; Yamashita, K

    2001-10-01

    An electrical field may affect osteogenesis. Since we found that hydroxyapatite (HA) ceramics may be polarizable, we hypothesized that electrically polarized HA may foster production of new bone in vivo. Both polarized and non-polarized HA ceramics were inserted into the subperiosteum spaces at the parietal bone area of rats. After 2, 4, and 8 weeks, the implant sites were examined histologically. Morphometric analysis revealed that new bone formation was accelerated on the negatively charged surface of the polarized HA (N-surface) at 2 weeks. The newly formed bone approached maturation at 4 weeks and was thicker on the N-surface than in the controls. By 8 weeks, newly formed bone in the controls was almost the same as that on the N-surface. These findings suggest that polarized HA is biocompatible and that bone formation on the N-surface is enhanced in the early stage of bone healing. PMID:11706953

  18. Pulsed laser deposition of silicon substituted hydroxyapatite coatings from synthetical and biological sources

    NASA Astrophysics Data System (ADS)

    Solla, E. L.; González, P.; Serra, J.; Chiussi, S.; León, B.; López, J. García

    2007-12-01

    Silicon substituted hydroxyapatite (Si-HA) is a new material with an enhanced bioactibity and it can be produced by chemical synthesis. Nevertheless, the coating of metallic substrates with a bioactive material is a common method nowadays to improve its integration with the receptor bone. Si-HA films were deposited by pulsed laser deposition (PLD), using targets composed of mixtures of HA with different Si containing sources such as SiO 2 and diatomaceous earth. The Si-HA films were characterized in terms of structure and chemical composition by spectroscopic techniques (FTIR, XPS), and several ion beam techniques (RBS, PIXE). The analysis revealed that the Si is successfully incorporated into the HA structure, as well as traces of other elements such as Na, Fe or K.

  19. Development of a synthetic bone scaffold using porous hydroxyapatite for bone repair.

    PubMed

    Mustaffa, R; Besar, I; Andanastuti, M

    2008-07-01

    In this study, porous hydroxyapatite (HA) samples were fabricated via sponge techniques with the aid of sago as part of the binder mixture. Development processes for the production of porous bone graft substitutes are studied using polyurethane sponge. To obtain the optimum amount of binder for successful fabrication of porous HA were done. Initially, porous HA powder was synthesized using calcium hydroxide and orthorphosphoric acid. Meanwhile, sago was mixed with PVA in a certain ratio to be used as binder for preparing the porous HA. After a series of investigative tests were conducted to characterize the sintered samples, the use of the sago and polymeric mixture was found to successfully aid the fabrication of porous HA samples. In this investigation, comparison of physical and mechanical characteristics between samples prepared using difference techniques was made. PMID:19025001

  20. [Preparation and characterization of nano-hydroxyapatite/polyurethane composite bio-film].

    PubMed

    Dong, Zhihong; Li, Yubao; Zhang, Li; Zou, Qin

    2009-06-01

    Through Hydroxyl (-OH) reacting with isocyanate group (-NCO), 13 Wt% nano-hydroxyapatite (n-HA)/polyurethane (PU) composite guided bone regeneration membrane was synthesized by use of solvent evaporation method. Its surface character was analyzed by XRD, IR, TG, contact angle, water absorption, elongation and combustion test and SEM. The results indicate that nano-HA/PU has good homogeneity,the interface between the inorganic mineral and organic polymer is optimized to create proper combination; that n-HA crystals are similar to the apatite crystals in natural bone, HA/PU composite membrane has good hydrophilicity mechanical behavior; and that many pores are observed on the membrane which help cells' metabolism. So the HA/PU composite membrane, thus prepared, has the potential for use in guided bone regeneration and tissue engineering. PMID:19634670

  1. Osteolysis from a press-fit hydroxyapatite-coated implant. A case study.

    PubMed

    Bloebaum, R D; Dupont, J A

    1993-04-01

    The clinical and histological results of hydroxyapatite (HA) coating separation from a press-fit total hip arthroplasty 3.3 years after surgery are documented. Semiquantitative histological analysis showed grade 3+ mononuclear histiocytes and giant cells present in the retrieved capsule and periprosthetic tissues. Grade 3+ (titanium alloy, HA, and polyethylene) particles could be seen throughout the tissues. Backscattered electron and correlated elemental analysis confirmed that the HA coating had migrated to the articulating surface of the polyethylene insert causing third-body wear. The authors suggest that the orthopedic surgeon be cautioned in the routine use of HA-coated implants if osteolysis associated with HA separation and migration is to be avoided. PMID:8386748

  2. Electrospun polyvinyl alcohol-collagen-hydroxyapatite nanofibers: a biomimetic extracellular matrix for osteoblastic cells

    NASA Astrophysics Data System (ADS)

    Song, Wei; Markel, David C.; Wang, Sunxi; Shi, Tong; Mao, Guangzhao; Ren, Weiping

    2012-03-01

    The failure of prosthesis after total joint replacement is due to the lack of early implant osseointegration. In this study polyvinyl alcohol-collagen-hydroxyapatite (PVA-Col-HA) electrospun nanofibrous meshes were fabricated as a biomimetic bone-like extracellular matrix for the modification of orthopedic prosthetic surfaces. In order to reinforce the PVA nanofibers, HA nanorods and Type I collagen were incorporated into the nanofibers. We investigated the morphology, biodegradability, mechanical properties and biocompatibility of the prepared nanofibers. Our results showed these inorganic-organic blended nanofibers to be degradable in vitro. The encapsulated nano-HA and collagen interacted with the PVA content, reinforcing the hydrolytic resistance and mechanical properties of nanofibers that provided longer lasting stability. The encapsulated nano-HA and collagen also enhanced the adhesion and proliferation of murine bone cells (MC3T3) in vitro. We propose the PVA-Col-HA nanofibers might be promising modifying materials on implant surfaces for orthopedic applications.

  3. Preparation and Functional Assessment of Composite Chitosan-Nano-Hydroxyapatite Scaffolds for Bone Regeneration

    PubMed Central

    Reves, Benjamin T.; Jennings, Jessica A.; Bumgardner, Joel D.; Haggard, Warren O.

    2012-01-01

    Composite chitosan-nano-hydroxyapatite microspheres and scaffolds prepared using a co-precipitation method have shown potential for use in bone regeneration. The goal of this research was to improve the functional properties of the composite scaffolds by modifying the fabrication parameters. The effects of degree of deacetylation (DDA), drying method, hydroxyapatite content and an acid wash on scaffold properties were investigated. Freeze-dried 61% DDA scaffolds degraded faster (3.5 ± 0.5% mass loss) than air-dried 61% DDA scaffolds and 80% DDA scaffolds, but had a lower compressive modulus of 0.12 ± 0.01 MPa. Air-dried 80% DDA scaffolds displayed the highest compressive modulus (3.79 ± 0.51 MPa) and these scaffolds were chosen as the best candidate for use in bone regeneration. Increasing the amount of hydroxyapatite in the air-dried 80% DDA scaffolds did not further increase the compressive modulus of the scaffolds. An acid wash procedure at pH 6.1 was found to increase the degradation of air-dried 80% DDA scaffolds from 1.3 ± 0.1% to 4.4 ± 0.4%. All of the formulations tested supported the proliferation of SAOS-2 cells. PMID:24956519

  4. Development of porous polyurethane/strontium-substituted hydroxyapatite composites for bone regeneration.

    PubMed

    Sariibrahimoglu, Kemal; Yang, Wanxun; Leeuwenburgh, Sander C G; Yang, Fang; Wolke, Joop G C; Zuo, Yi; Li, Yubao; Jansen, John A

    2015-06-01

    Polyurethane (PU) has been widely used for the biomedical applications but its potential for bone regeneration is limited due to its lack of osteoconductive properties. Strontium substituted hydroxyapatite (SrHA) particles, on the other hand, are known to exhibit a positive effect on bone formation. Therefore, the aim of this study was to (i) develop porous polyurethane scaffolds containing strontium SrHA nanoparticles (PU/SrHA) and (ii) compare their in vitro biological performance for applications in bone regeneration to PU scaffolds. SrHA and HA was synthesized using a conventional wet-chemical neutralization reaction at temperatures of 25, 50, and 80°C. Chemical analysis was performed by inductively coupled plasma-optical emission spectrometry. Synthesizing temperatures at 25 and at 50°C were selected for the composite preparation (abbreviated as HA-25, SrHA-25, HA-50, and SrHA-50, respectively). PU was synthesized from isophorone diisocyanate, polytetramethylene ether glycol, and 1,4-butanediol. Composite scaffolds were prepared by addition of HA or SrHA nanoparticles into PU scaffolds during polymer preparation. The results showed that the Sr content in HA nanoparticles increased with increasing synthesis temperature. The addition of nanoparticles decreased the elongation-at-break and tensile strength, but significantly increased the surface wettability of the PU scaffolds. In vitro degradation tests demonstrated that release of cations was significantly higher from PU/SrHA-50 composite scaffolds. Cell culture tests indicated that PU composites containing either HA or SrHA nanoparticles increased proliferation of bone marrow stem cells as compared to plain PU scaffolds, whereas osteogenic differentiation was not affected by the incorporation of HA nanoparticles irrespective of the incorporation of Sr. PMID:25203691

  5. Primary human osteoblast culture on 3D porous collagen-hydroxyapatite scaffolds.

    PubMed

    Jones, Gemma L; Walton, Robin; Czernuszka, Jan; Griffiths, Sarah L; El Haj, Alicia J; Cartmell, Sarah H

    2010-09-15

    There is a need in tissue-engineering for 3D scaffolds that mimic the natural extracellular matrix of bone to enhance cell adhesion, proliferation, and differentiation. The scaffold is also required to be degradable. A highly porous scaffold has been developed to incorporate two of the extracellular components found in bone-collagen and hydroxyapatite (HA). The scaffold's collagen component is an afibrillar monomeric type I atelocollagen extracted from foetal calf's skin. This provided a novel environment for the inclusion of HA powder. Five hundred thousand primary human osteoblasts were seeded onto 4 mm cubed scaffolds that varied in ratio of HA to collagen. Weight ratios of 1:99, 25:75, 50:50, and 75:25 hydroxyapatite:collagen (HA:Collagen) were analysed. The scaffolds plus cells were cultured for 21 days. DNA assays and live/dead viability staining demonstrated that all of the scaffolds supported cell proliferation and viability. An alkaline phosphatase assay showed similar osteoblast phenotype maintenance on all of the 3D scaffolds analysed at 21 days. MicroCT analysis demonstrated an increase in total sample volume (correlating to increase in unmineralised matrix production). An even distribution of HA throughout the collagen matrix was observed using this technique. Also at 3 weeks, reductions in the percentage of the mineralised phase of the constructs were seen. These results indicate that each of the ratios of HA/collagen scaffolds have great potential for bone tissue engineering. PMID:20694991

  6. Comparison of Physical-chemical and Mechanical Properties of Chlorapatite and Hydroxyapatite Plasma Sprayed Coatings

    PubMed Central

    Demnati, Imane; Grossin, David; Marsan, Olivier; Bertrand, Ghislaine; Collonges, Gérard; Combes, Christèle; Parco, Maria; Braceras, Inigo; Alexis, Joel; Balcaen, Yannick; Rey, Christian

    2015-01-01

    Chlorapatite can be considered a potential biomaterial for orthopaedic applications. Its use as plasma-sprayed coating could be of interest considering its thermal properties and particularly its ability to melt without decomposition unlike hydroxyapatite. Chlorapatite (ClA) was synthesized by a high-temperature ion exchange reaction starting from commercial stoichiometric hydroxyapatites (HA). The ClA powder showed similar characteristics as the original industrial HA powder, and was obtained in the monoclinic form. The HA and ClA powders were plasma-sprayed using a low-energy plasma spraying system with identical processing parameters. The coatings were characterized by physical-chemical methods, i.e. X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR) and Raman spectroscopy, including distribution mapping of the main phases detected such as amorphous calcium phosphate (ACP), oxyapatite (OA), and HA or ClA. The unexpected formation of oxyapatite in ClA coatings was assigned to a side reaction with contaminating oxygenated species (O2, H2O). ClA coatings exhibited characteristics different from HA, showing a lower content of oxyapatite and amorphous phase. Although their adhesion strength was found to be lower than that of HA coatings, their application could be an interesting alternative, offering, in particular, a larger range of spraying conditions without formation of massive impurities. PMID:25893015

  7. New composite materials based on alginate and hydroxyapatite as potential carriers for ascorbic acid.

    PubMed

    Ilie, Andreia; Ghiţulică, Cristina; Andronescu, Ecaterina; Cucuruz, Andrei; Ficai, Anton

    2016-08-30

    The purpose of this article was to obtain prolonged drug release systems in which the drug (ascorbic acid) to reach intact the target area in an environment that is able to control the administration of the active component by chemical or physiological pathways. As support for drug, it was used a material based on calcium phosphate - hydroxyapatite and a natural polymer - alginate, since it is one of the most investigated composite materials for medical applications due to its positive response to biological testing: bioactivity, biocompatibility and osteoconductivity. Three composites with different ratios between alginate and hydroxyapatite were obtained: (a) Alg/HA/AA 1:1 (the mass ratio between Alg and HA being of 1:1), (b) Alg/HA/AA 1:3 (Alg:HA mass ratio of 1:3) and (c) Alg/HA/AA 3:1 (Alg:HA mass ratio of 3:1). The synthesized materials were characterized using X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM) and to observe the drug release process, UV-vis spectroscopy. PMID:26784979

  8. Microwave-assisted synthesis of porous chitosan-modified montmorillonite-hydroxyapatite composite scaffolds.

    PubMed

    Kar, Sumanta; Kaur, Tejinder; Thirugnanam, A

    2016-01-01

    In this study, a porous chitosan-organically modified montmorillonite-hydroxyapatite (CS-OM-HA) composite scaffold was developed by combining microwave irradiation and gas foaming method. Hydroxyapatite (HA) particles of size ∼ 65 nm were synthesized and characterized by X-ray diffraction (XRD) and attenuated total reflectance-Fourier transform infrared (ATR-FTIR) spectroscopy. The prepared composite scaffolds were characterized using ATR-FTIR, XRD, mercury intrusion porosimeter (MIP) and scanning electron microscopy (SEM) studies. The synergistic effect of HA and OM on the mechanical and in vitro biological properties (swelling, degradation, protein adsorption and bioactivity) of the composite scaffolds were evaluated. Swelling, degradation, mechanical property, bioactivity and protein adsorption studies of CS-OM-HA composite scaffolds have shown desirable results in comparison with the pure CS and CS-OM composite scaffolds. CS-OM-HA composite scaffolds were also found to be non-cytotoxic to MG 63 osteoblast cell lines. From the study, it can be concluded that the novel CS-OM-HA composite scaffold with improved mechanical and in vitro biological properties has wide potential in non-load bearing bone tissue engineering applications. PMID:26505953

  9. Production of hydroxyapatite layers on the plasma electrolytically oxidized surface of titanium alloys.

    PubMed

    Lugovskoy, Alex; Lugovskoy, Svetlana

    2014-10-01

    Hydroxyapatite (HA) is a bioactive material that is widely used for improving the osseointegration of titanium dental implants. Titanium can be coated with HA by various methods, such as chemical vapor deposition (CVD), thermal spray, or plasma spray. HA coatings can also be grown on titanium surfaces by hydrothermal, chemical, and electrochemical methods. Plasma electrolytic oxidation (PEO), or microarc oxidation (MAO), is an electrochemical method that enables the production of a thick porous oxide layer on the surface of a titanium implant. If the electrolyte in which PEO is performed contains calcium and phosphate ions, the oxide layer produced may contain hydroxyapatite. The HA content can then be increased by subsequent hydrothermal treatment. The HA thus produced on titanium surfaces has attractive properties, such as a high porosity, a controllable thickness, and a considerable density, which favor its use in dental and bone surgery. This review summarizes the state of the art and possible further development of PEO for the production of HA on Ti implants. PMID:25175246

  10. 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.

  11. Effect of Nano-HA/Collagen Composite Hydrogels on Osteogenic Behavior of Mesenchymal Stromal Cells.

    PubMed

    Hayrapetyan, Astghik; Bongio, Matilde; Leeuwenburgh, Sander C G; Jansen, John A; van den Beucken, Jeroen J J P

    2016-06-01

    This study aimed to comparatively evaluate the in vitro effect of nanosized hydroxyapatite and collagen (nHA/COL) based composite hydrogels (with different ratios of nHA and COL) on the behavior of human mesenchymal stromal cells (MSCs), isolated from either adipose tissue (AT-MSCs) or bone marrow (BM-MSCs). We hypothesized that (i) nHA/COL composite hydrogels would promote the osteogenic differentiation of MSCs in an nHA concentration dependent manner, and that (ii) AT-MSCs would show higher osteogenic potential compared to BM-MSCs, due to their earlier observed higher proliferation and osteogenic differentiation potential in 2D in vitro cultures [1]. The obtained results indicated that AT-MSCs show indeed high proliferation, differentiation and mineralization capacities in nHA/COL constructs compared to BM-MSCs, but this effect was irrespective of nHA concentration. Based on the results of alkaline phosphatase (ALP) activity and osteocalcin (OCN) protein level, the osteogenic differentiation of BM-MSCs started in the beginning of the culture period and for AT-MSCs at the end of the culture period. At a molecular level, both cell types showed high expression of osteogenic markers (bone morphogenic protein 2 [BMP2], runt-related transcription factor 2 [RUNX2], OCN or COL1) in both an nHA concentration and time dependent manner. In conclusion, AT-MSCs demonstrated higher osteogenic potential in nHA/COL based 3D micro-environments compared to BM-MSCs, in which proliferation and osteogenic differentiation were highly promoted in a time dependent manner, irrespective of nHA amount in the constructs. The fact that AT-MSCs showed high proliferation and mineralization potential is appealing for their application in future pre-clinical research as an alternative cell source for BM-MSCs. PMID:26803618

  12. 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

  13. Processing and mechanical behavior of lamellar structured degradable magnesium-hydroxyapatite implants.

    PubMed

    Ratna Sunil, B; Ganapathy, C; Sampath Kumar, T S; Chakkingal, Uday

    2014-12-01

    Multilayered (laminated) composites exhibit tunable mechanical behavior compared to bulk materials due to the presence of more interfaces and therefore magnesium based composites are gaining wide popularity as biodegradable materials targeted for temporary implant applications. The objective of the present work is to fabricate magnesium based lamellar metal matrix composites (MMCs) for degradable implant applications. Nano-hydroxyapatite (HA) powder was selected as the secondary phase and lamellar structured magnesium-nano-hydroxyapatite (Mg-HA) composites of 8, 10 and 15wt% HA were fabricated by ball milling and spark plasma sintering. It was found that HA particles were coated on the Mg flakes after 20h of ball milling carried out using tungsten carbide (WC) as the milling media. Spark plasma sintering of the milled powders resulted in the formation of lamellar structure of Mg with the presence of HA and magnesium oxide (MgO) at the inter-lamellar sites of the composites. Phase analysis of the milled powder by an X-ray diffraction (XRD) method confirms the presence of HA and MgO along with Mg after sintering. Corrosion behavior of the composites investigated by potentiodynamic polarization tests shows a reduction in the inter-lamellar corrosion with increase in HA content and the best corrosion resistance is found for the Mg-10% HA composite. This composite also exhibits maximum Vickers hardness. Young׳s modulus and fracture toughness measured by nano-indentation method were higher for the Mg-8% HA composite. The results thus suggest that lamellar structured Mg composites with 8% and 10% HA show promise for temporary degradable orthopedic implant applications because of their improved corrosion resistance and superior mechanical properties. PMID:25241282

  14. Preparation and characterization of magnesium/carbonate co-substituted hydroxyapatites.

    PubMed

    Gibson, I R; Bonfield, W

    2002-07-01

    A new synthesis/processing method has been devised to produce magnesium/carbonate co-substituted hydroxyapatite ceramics that do not decompose to tricalcium phosphate (TCP) on sintering. Using this method, a series of magnesium/carbonate co-substituted hydroxyapatite (Mg/CO(3)-HA) compositions, containing between 0 and 0.35 wt % Mg and approximately 0.9 wt % CO(3) were prepared. Sintering the Mg/CO(3)-HA compositions in a CO(2)/H(2)O atmosphere yields a single crystalline phase that appears to be identical to stoichiometric HA. In contrast, when the compositions were prepared in the absence of carbonate and were sintered in air, the phase composition was a biphasic mixture of HA and TCP e.g. for 0.25 wt % Mg substitution the phase composition was approximately 60%HA/40% TCP. Clearly, both the synthesis route and the processing (i.e. sintering) route are of importance in the production of a single-phase Mg/CO(3)-HA ceramic. Fourier transform infrared (FTIR) spectroscopy has indicated that the Mg/CO(3)-HA ceramics still contained carbonate groups after sintering at 1200 degrees C. Chemical analysis by X-ray fluorescence spectroscopy (XRF) and C-H-N analysis has shown that the cation/anion molar ratio (i.e. [Ca+Mg]/[P+C/2]) of the different compositions were 1.68(+/-0.01), which is equivalent to the Ca/P molar ratio of stoichiometric HA. Although the magnesium/carbonate co-substitution had a positive effect in preventing phase decomposition during sintering, it appeared to have a negative effect on the densification of the MgCO(3)-HA ceramics, compared to stoichiometric HA. PMID:15348578

  15. In vitro osteoclast formation and resorption of silicon-substituted hydroxyapatite ceramics.

    PubMed

    Friederichs, Robert J; Brooks, Roger A; Ueda, Masato; Best, Serena M

    2015-10-01

    Materials that participate in bone remodeling at the implant/tissue interface represent a modern tissue engineering approach with the aim of balancing implant resorption and nascent tissue formation. Silicon-substituted hydroxyapatite (SiHA) ceramics are capable of stimulating new bone formation, but little is known about their interaction with osteoclasts (OC). The effects of soluble silicate and SiHA on OCs were investigated in this study. Soluble silicate below 500 μM did not stimulate cell metabolism at 4 days or alter resorption area at 7 days on calcium phosphate discs. On sintered ceramics, OC numbers were similar on HA, Si0.3 HA (0.5 wt % Si) and Si0.5 HA (1.2 wt % Si) after 21 days in vitro, but actin ring sealing zone morphology on SiHA resembled that commonly found on bone or on carbonate-substituted hydroxyapatite (CHA). Smaller and thicker actin rings on SiHA as compared to HA were probably the result of altered surface chemistry and solubility differences. The more stable sealing zones and increased lattice solubility likely contributed to increased individual pit volumes observed on Si0.5 HA. The delayed formation of OCs on Si0.5 HA (lower numbers at day 14) excludes earlier differentiation as a possible mechanism of increased individual OC pit volumes at later times (day 21). Materials characterization of Si containing biomaterials remains paramount as the Si type and amounts can subsequently impact downstream OC behaviour in a complex manner. PMID:25847383

  16. Improve the Strength of PLA/HA Composite Through the Use of Surface Initiated Polymerization and Phosphonic Acid Coupling Agent

    PubMed Central

    Wang, Tongxin; Chow, Laurence C.; Frukhtbeyn, Stanislav A.; Ting, Andy Hai; Dong, Quanxiao; Yang, Mingshu; Mitchell, James W.

    2011-01-01

    Bioresorbable composite made from degradable polymers, e.g., polylactide (PLA), and bioactive calcium phosphates, e.g., hydroxyapatite (HA), are clinically desirable for bone fixation, repair and tissue engineering because they do not need to be removed by surgery after the bone heals. However, preparation of PLA/HA composite from non-modified HA usually results in mechanical strength reductions due to a weak interface between PLA and HA. In this study, a calcium-phosphate/phosphonate hybrid shell was developed to introduce a greater amount of reactive hydroxyl groups onto the HA particles. Then, PLA was successfully grafted on HA by surface-initiated polymerization through the non-ionic surface hydroxyl groups. Thermogravimetric analysis indiated that the amount of grafted PLA on HA can be up to 7 %, which is about 50 % greater than that from the literature. PLA grafted HA shows significantly different pH dependent ζ-potential and particle size profiles from those of uncoated HA. By combining the phosphonic acid coupling agent and surface initiated polymerization, PLA could directly link to HA through covalent bond so that the interfacial interaction in the PLA/HA composite can be significantly improved. The diametral tensile strength of PLA/HA composite prepared from PLA-grafted HA was found to be over twice that of the composite prepared from the non-modified HA. Moreover, the tensile strength of the improved composite was 23 % higher than that of PLA alone. By varying additional variables, this approach has the potential to produce bioresorbable composites with improved mechanical properties that are in the range of natural bones, and can have wide applications for bone fixation and repair in load-bearing areas. PMID:22399838

  17. Coralline hydroxyapatite in complex acetabular reconstruction.

    PubMed

    Wasielewski, Ray C; Sheridan, Kate C; Lubbers, Melissa A

    2008-04-01

    This retrospective study examined whether a coralline hydroxyapatite bone graft substitute adequately repaired bone defects during complex acetabular reconstructions. Seventeen patients who underwent acetabular revision using Pro Osteon 500 were assessed to determine whether any cups required re-revision, whether bone had incorporated into the coralline hydroxyapatite grafts, and whether the coralline hydroxyapatite grafts resorbed with time. At latest follow-up, no cups required re-revision, but 1 had failed. Radiographic evidence of bone incorporation was observed in every coralline hydroxyapatite graft. Graft resorption was not observed. PMID:19292282

  18. Synthesis and characterization of porous hydroxyapatite and hydroxyapatite coatings

    SciTech Connect

    Nieh, T G; Choi, B W; Jankowski, A F

    2000-10-25

    A technique is developed to construct bulk hydroxyapatite (HAp) with different cellular structures. The technique involves the initial synthesis of nanocrystalline hydroxyapatite powder from an aqueous solution using water-soluble compounds and then followed by spray drying into agglomerated granules. The granules were further cold pressed and sintered into bulks at elevated temperatures. The sintering behavior of the HAp granules was characterized and compared with those previously reported. Resulting from the fact that the starting HAp powders were extremely fine, a relatively low activation energy for sintering was obtained. In the present study, both porous and dense structures were produced by varying powder morphology and sintering parameters. Porous structures consisting of open cells were constructed. Sintered structures were characterized using scanning electron microscopy and x-ray tomography. In the present paper, hydroxyapatite coatings produced by magnetron sputtering on silicon and titanium substrates will also be presented. The mechanical properties of the coatings were measured using nanoindentation techniques and microstructures examined using transmission electron microscopy.

  19. The enamel protein amelotin is a promoter of hydroxyapatite mineralization.

    PubMed

    Abbarin, Nastaran; San Miguel, Symone; Holcroft, James; Iwasaki, Kengo; Ganss, Bernhard

    2015-05-01

    Amelotin (AMTN) is a recently discovered protein that is specifically expressed during the maturation stage of dental enamel formation. It is localized at the interface between the enamel surface and the apical surface of ameloblasts. AMTN knock-out mice have hypomineralized enamel, whereas transgenic mice overexpressing AMTN have a compact but disorganized enamel hydroxyapatite (HA) microstructure, indicating a possible involvement of AMTN in regulating HA mineralization directly. In this study, we demonstrated that recombinant human (rh) AMTN dissolved in a metastable buffer system, based on light scattering measurements, promotes HA precipitation. The mineral precipitates were characterized by scanning and transmission electron microscopy and electron diffraction. Colloidal gold immunolabeling of AMTN in the mineral deposits showed that protein molecules were associated with HA crystals. The binding affinity of rh-AMTN to HA was found to be comparable to that of amelogenin, the major protein of the forming enamel matrix. Overexpression of AMTN in mouse calvaria cells also increased the formation of calcium deposits in the culture medium. Overexpression of AMTN during the secretory stage of enamel formation in vivo resulted in rapid and uncontrolled enamel mineralization. Site-specific mutagenesis of the potential serine phosphorylation motif SSEEL reduced the in vitro mineral precipitation to less than 25%, revealing that this motif is important for the HA mineralizing function of the protein. A synthetic short peptide containing the SSEEL motif was only able to facilitate mineralization in its phosphorylated form ((P)S(P) SEEL), indicating that this motif is necessary but not sufficient for the mineralizing properties of AMTN. These findings demonstrate that AMTN has a direct influence on biomineralization by promoting HA mineralization and suggest a critical role for AMTN in the formation of the compact aprismatic enamel surface layer during the maturation

  20. Nanostructuring and texturing of pulsed laser deposited hydroxyapatite thin films

    NASA Astrophysics Data System (ADS)

    Kim, Hyunbin; Catledge, Shane; Vohra, Yogesh; Camata, Renato; Lacefield, William

    2003-03-01

    Hydroxyapatite (HA) [Ca_10(PO_4)_6(OH)_2] is commonly deposited onto orthopedic and dental metallic implants to speed up bone formation around devices, allowing earlier stabilization in a patient. Pulsed laser deposition (PLD) is a suitable means of placing thin HA films on these implants because of its control over stoichiometry, crystallinity, and nanostructure. These characteristics determine the mechanical properties of the films that must be optimized to improve the performance of load-bearing implants and other devices that undergo bone insertion. We have used PLD to produce nanostructured and preferentially oriented HA films and evaluated their mechanical properties. Pure, highly crystalline HA films on Ti-6Al-4V substrates were obtained using a KrF excimer laser (248nm) with energy density of 4-8 J/cm^2 and deposition temperature of 500-700^rcC. Scanning electron and atomic force microscopies reveal that our careful manipulation of energy density and substrate temperature has led to films made up of HA grains in the nanometer scale. Broadening of x-ray diffraction peaks as a function of deposition temperature suggests it may be possible to control the film nanostructure to a great extent. X-ray diffraction also shows that as the laser energy density is increased in the 4-8 J/cm^2 range, the hexagonal HA films become preferentially oriented along the c-axis perpendicular to the substrate. Texture, nanostructure, and phase make-up all significantly influence the mechanical properties. We will discuss how each of these factors affects hardness and Young's modulus of the HA films as measured by nanoindentation.

  1. The deposition of strontium-substituted hydroxyapatite coatings.

    PubMed

    Boyd, Adrian R; Rutledge, L; Randolph, L D; Mutreja, I; Meenan, B J

    2015-02-01

    Strontium substituted hydroxyapatite (SrHA) coatings have received a lot of interest recently as strontium (Sr) has been shown to have the dual benefit of promoting bone formation and reducing bone resorption, in vivo. In this work, SrHA coatings were deposited onto polycrystalline titanium surfaces using radio frequency (RF) magnetron co-sputtering and compared to those deposited from HA alone. In particular, the influence of different levels of Sr-substitution of the sputtering targets (5 and 13% Sr-substituted HA targets) on the properties of the deposited coatings produced at a low discharge power level (150 W) were investigated using FTIR, XPS, XRD, ToFSIMS and AFM techniques (both before and after annealing at 500 °C). The results show that Sr could be successfully incorporated into the HA lattice to form SrHA coatings and that they contained no other impurities. However, the coating produced from the 13% Sr-substituted target had a higher Ca+Sr/P ratio (1.95±0.14) and Sr content when compared to the coating produced from the 5% Sr-substituted target (1.58±0.20). The deposition rate also decreased with increasing Sr content of the sputtering targets. Furthermore, as the Sr content of the coatings increased, so did the preferred 002 orientation of the coating along with increased surface roughness and heterogeneity of the surface features. Therefore, this study has shown that RF magnetron sputtering offers a means to control attendant properties of Sr-substituted HA, such as the crystallinity, stoichiometry, phase purity and surface topography. PMID:25631262

  2. Development of Risperidone PLGA Microspheres

    PubMed Central

    D'Souza, Susan; Faraj, Jabar A.; Giovagnoli, Stefano; DeLuca, Patrick P.

    2014-01-01

    The aim of this study was to design and evaluate biodegradable PLGA microspheres for sustained delivery of Risperidone, with an eventual goal of avoiding combination therapy for the treatment of schizophrenia. Two PLGA copolymers (50 : 50 and 75 : 25) were used to prepare four microsphere formulations of Risperidone. The microspheres were characterized by several in vitro techniques. In vivo studies in male Sprague-Dawley rats at 20 and 40 mg/kg doses revealed that all formulations exhibited an initial burst followed by sustained release of the active moiety. Additionally, formulations prepared with 50 : 50 PLGA had a shorter duration of action and lower cumulative AUC levels than the 75 : 25 PLGA microspheres. A simulation of multiple dosing at weekly or 15-day regimen revealed pulsatile behavior for all formulations with steady state being achieved by the second dose. Overall, the clinical use of Formulations A, B, C, or D will eliminate the need for combination oral therapy and reduce time to achieve steady state, with a smaller washout period upon cessation of therapy. Results of this study prove the suitability of using PLGA copolymers of varying composition and molecular weight to develop sustained release formulations that can tailor in vivo behavior and enhance pharmacological effectiveness of the drug. PMID:24616812

  3. An amphiphilic degradable polymer/hydroxyapatite composite with enhanced handling characteristics promotes osteogenic gene expression in bone marrow stromal cells.

    PubMed

    Kutikov, Artem B; Song, Jie

    2013-09-01

    Electrospun polymer/hydroxyapatite (HA) composites combining biodegradability with osteoconductivity are attractive for skeletal tissue engineering applications. However, most biodegradable polymers such as poly(lactic acid) (PLA) are hydrophobic and do not blend with adequate interfacial adhesion with HA, compromising the structural homogeneity, mechanical integrity and biological performance of the composite. To overcome this challenge, we combined a hydrophilic polyethylene glycol (PEG) block with poly(d,l-lactic acid) to improve the adhesion of the degradable polymer with HA. The amphiphilic triblock copolymer PLA-PEG-PLA (PELA) improved the stability of HA-PELA suspension at 25wt.% HA content, which was readily electrospun into HA-PELA composite scaffolds with uniform fiber dimensions. HA-PELA was highly extensible (failure strain>200% vs. <40% for HA-PLA), superhydrophilic (∼0° water contact angle vs. >100° for HA-PLA), and exhibited an 8-fold storage modulus increase (unlike deterioration for HA-PLA) upon hydration, owing to the favorable interaction between HA and PEG. HA-PELA also better promoted osteochondral lineage commitment of bone marrow stromal cells in unstimulated culture and supported far more potent osteogenic gene expression upon induction than HA-PLA. We demonstrate that the chemical incorporation of PEG is an effective strategy to improve the performance of degradable polymer/HA composites for bone tissue engineering applications. PMID:23791675

  4. An amphiphilic degradable polymer/hydroxyapatite composite with enhanced handling characteristics promotes osteogenic gene expression in bone marrow stromal cells

    PubMed Central

    Kutikov, Artem B.; Song, Jie

    2013-01-01

    Electrospun polymer/hydroxyapatite (HA) composites combining biodegradability with osteoconductivity are attractive for skeletal tissue engineering applications. However, most biodegradable polymers such as PLA are hydrophobic and do not blend with adequate interfacial adhesion with HA, compromising the structural homogeneity, mechanical integrity, and biological performance of the composite. To overcome this challenge, we incorporated a hydrophilic polyethylene glycol (PEG) block to poly(D,L-lactic acid) to improve the adhesion of the degradable polymer with HA. The amphiphilic triblock copolymer PLA-PEG-PLA (PELA) improved the stability of HA-PELA suspension at 25 wt% HA content, which was readily electrospun into HA-PELA composite scaffolds with uniform fiber dimensions. HA-PELA was highly extensible (failure strain >200% vs. <40% for HA-PLA), superhydrophilic (~0° water contact angle vs. >100° for HA-PLA), and exhibited an 8-fold storage modulus increase (unlike deterioration for HA-PLA) upon hydration, owing to the favorable interaction between HA and PEG. HA-PELA also better promoted osteochondral lineage commitment of bone marrow stromal cells in unstimulated culture and supported far more potent osteogenesis upon induction than HA-PLA. We demonstrate that the chemical incorporation of PEG is an effective strategy to improve the performance of degradable polymer/HA composites for bone tissue engineering applications. PMID:23791675

  5. Microspheres and nanoparticles from ultrasound

    NASA Astrophysics Data System (ADS)

    Suh, Won Hyuk

    Improved preparations of various examples of monodispersed, porous, hollow, and core-shell metal and semiconductor nanoparticles or nanowires have been developed. Now titania microspheres and nanoparticles and silica microspheres can be synthesized using an inexpensive high frequency (1.7 MHz) ultrasonic generator (household humidifier; ultrasonic spray pyrolysis; USP). Morphology and pore size of titania microspheres were controlled by the silica to Ti(IV) ratio and silica particle size. Fine tuning the precursor ratio affords sub-50 nm titania nanoparticles as well. In terms of silica microspheres, morphology was controlled by the silica to organic monomer ratio. In liquids irradiated with high intensity ultrasound (20 kHz; HIUS), acoustic cavitation produces high energy chemistry through intense local heating inside the gas phase of collapsing bubbles in the liquid. HIUS and USP confine the chemical reactions to isolated sub-micron reaction zones, but sonochemistry does so in a heated gas phase within a liquid, while USP uses a hot liquid droplet carried by a gas flow. Thus, USP can be viewed as a method of phase-separated synthesis using submicron-sized droplets as isolated chemical reactors for nanomaterial synthesis. While USP has been used to create both titania and silica spheres separately, there are no prior reports of titania-silica composites. Such nanocomposites of metal oxides have been produced, and by further manipulation, various porous structures with fascinating morphologies were generated. Briefly, a precursor solution was nebulized using a commercially available household ultrasonic humidifier (1.7 MHz ultrasound generator), and the resulting mist was carried in a gas stream of air through a quartz glass tube in a hot furnace. After exiting the hot zone, these microspheres are porous or hollow and in certain cases magnetically responsive. In the case of titania microspheres, they are rapidly taken up into the cytoplasm of mammalian cells and

  6. PCL/chitosan/Zn-doped nHA electrospun nanocomposite scaffold promotes adipose derived stem cells adhesion and proliferation.

    PubMed

    Ghorbani, Fereshteh Mohammad; Kaffashi, Babak; Shokrollahi, Parvin; Seyedjafari, Ehsan; Ardeshirylajimi, Abdolreza

    2015-03-15

    Chitosan (Ch), and poly(ɛ-caprolactone) (PCL), widely used as biomaterials with desirable properties for tissue engineering applications, were both blended with zinc-doped hydroxyapatite nanoparticles(nZnHA) and electrospun into nanofibrous scaffolds using formic acid/acetic acid. The rationale behind this study was to demonstrate that presence of small quantities of Zn(2+) ions doped in HA nanoparticles can improve biocompatibility of PCL/Ch blends. SEM observation revealed that average fiber diameter was increased from about 136 nm for a PCL/Ch blend, to around 210 nm for PCL/Ch/nZnHA nanocomposite. PCL/Ch/nZnHA scaffolds offered higher elastic modulus (about 3-fold) and tensile strength (nearly 1.5-fold) than the corresponding PCL/Ch scaffolds. In-vitro biocompatibility studies using human adipose derived stem cells (hAD-MSCs), demonstrated that the presence of only 5 wt% nZnHA in PCL/Ch/nZnHA nanocomposites enhanced hAD-MSCs' attachment compared to PCL/Ch and PCL/Ch/nHA. Finally, hAD-MSCs proliferation occurred at significantly higher rates of 1.5, 1.3 and 1.2 times on PCL/Ch/nZnHA scaffold compared to PCL, PCL/Ch and PCL/Ch/nHA, respectively. PMID:25542118

  7. Mitochondria and nuclei dual-targeted heterogeneous hydroxyapatite nanoparticles for enhancing therapeutic efficacy of doxorubicin.

    PubMed

    Xiong, Hui; Du, Shi; Ni, Jiang; Zhou, Jianping; Yao, Jing

    2016-07-01

    Dual-targeted nanoparticles have been increasingly used to realize greater anti-proliferation effect by attacking double key sites of tumor cells. In order to retain nuclei inhibition effect and enhance DOX-induced apoptosis by mitochondrial pathway simultaneously, hyaluronic acid (HA) modified hydroxyapatite (HAP) nanoparticles (HAP-HA), the functional calcium-based tumor targeting nanoparticles, have been developed. In this nanosystem, HA acts as an active tumor-targeting ligand to bind the CD44 receptors which are overexpressed on the surface of tumor cells while HAP can load and deliver DOX to both nuclei and mitochondria of tumor cells. In this study, DOX-loaded HAP-HA nanoparticles (DOX/HAP-HA) exhibited satisfactory drug loading efficiency which was up to 214.55 ± 51.05 μg mg(-1) and showed a uniform nano-scaled particle size. The mitochondrial and nuclei targetability of DOX/HAP-HA was confirmed by confocal laser scanning microscopy analyses. Besides, western blot assay demonstrated that DOX/HAP-HA could markedly enhance mitochondrial cytochrome C leakage and thereby activate apoptotic cascade associated with it. In addition, in vivo anti-tumor efficacy and toxicity evaluation of DOX/HAP-HA indicated that DOX/HAP-HA was more effective and less harmful compared to other groups. DOX/HAP-HA might be a new promising targeted delivery system for effective cancer therapy. PMID:27105438

  8. Electrodeposition of porous hydroxyapatite/calcium silicate composite coating on titanium for biomedical applications

    NASA Astrophysics Data System (ADS)

    Huang, Yong; Han, Shuguang; Pang, Xiaofeng; Ding, Qionqion; Yan, Yajing

    2013-04-01

    A novel method of electrolytic porous hydroxyapatite/calcium silicate (HA/CaSiO3) composite coating was conducted on pure titanium in a mixed solution of nano-SiO2, Ca(NO3)2 and NH4H2PO4. SEM observation showed that the composite layer was porous, thereby providing abundant sites for the osteoblast adhesion. XRD results showed that the composite coating was mainly composed of HA and CaSiO3. Bond strength testing exhibited that HA-CaSiO3/Ti had higher bond strength than HA/Ti. The HA/CaSiO3 coating was more corrosion resistant than the HA coating based on the polarization tests. In vitro cell experiments demonstrated that both the HA and HA/CaSiO3 coatings showed better cell response than the bared titanium. In addition, the proliferation of MC3T3-E1 osteoblast cells grown on the HA/CaSiO3 coating were remarkably higher than those on the bared Ti and pure HA coating.

  9. Effects of zinc-substituted nano-hydroxyapatite coatings on bone integration with implant surfaces*

    PubMed Central

    Zhao, Shi-fang; Dong, Wen-jing; Jiang, Qiao-hong; He, Fu-ming; Wang, Xiao-xiang; Yang, Guo-li

    2013-01-01

    Objective: The purpose of this study was to investigate the effects of a zinc-substituted nano-hydroxyapatite (Zn-HA) coating, applied by an electrochemical process, on implant osseointegraton in a rabbit model. Methods: A Zn-HA coating or an HA coating was deposited using an electrochemical process. Surface morphology was examined using field-emission scanning electron microscopy. The crystal structure and chemical composition of the coatings were examined using an X-ray diffractometer (XRD) and Fourier transform infrared spectroscopy (FTIR). A total of 78 implants were inserted into femurs and tibias of rabbits. After two, four, and eight weeks, femurs and tibias were retrieved and prepared for histomorphometric evaluation and removal torque (RTQ) tests. Results: Rod-like HA crystals appeared on both implant surfaces. The dimensions of the Zn-HA crystals seemed to be smaller than those of HA. XRD patterns showed that the peaks of both coatings matched well with standard HA patterns. FTIR spectra showed that both coatings consisted of HA crystals. The Zn-HA coating significantly improved the bone area within all threads after four and eight weeks (P<0.05), the bone to implant contact (BIC) at four weeks (P<0.05), and RTQ values after four and eight weeks (P<0.05). Conclusions: The study showed that an electrochemically deposited Zn-HA coating has potential for improving bone integration with an implant surface. PMID:23733429

  10. Cancellous bone healing around strontium-doped hydroxyapatite in osteoporotic rats previously treated with zoledronic acid.

    PubMed

    Li, Yunfeng; Shui, Xueping; Zhang, Li; Hu, Jing

    2016-04-01

    Bisphosphonates (BPs) are potent anti-osteoporotic agents. Strontium-doped hydroxyapatite (HA) (SrHA) has been reported to increase bone density and improve trabecular microarchitecture in osteoporotic animals. But information about the effect of SrHA on the surrounding bone tissue in osteoporotic animals previously on BPs treatment is limited. We hypothesize that SrHA will induce increased bone density in the vicinity of the material when compared to HA, even in osteoporotic animals previously treated with BPs. HA and 10%SrHA (HA with 10 mol % calcium substituted by strontium) implants were prepared and characterized by scanning electronic microscopy (SEM), X-ray photoemission spectroscopy (XPS), and X-ray diffraction (XRD). Osteoporotic animal model was established by bilateral ovariectomy. Twelve weeks later, all OVX rats accepted subcutaneous injection of zoledronic acid (ZOL) at the dose of 1.5 μg/kg weekly for another twelve weeks. Subsequently, rod-shaped HA and SrHA implants were inserted in the distal femur of the OVX animals previously treated with ZOL. Eight weeks after implantation, specimens were harvested for histological and micro-computed tomography (micro-CT) analysis. Compared to HA, 10%SrHA raised the percent bone volume by 32.7%, the mean trabecular thickness by 36.5%, the mean trabecular number by 34.3%, the mean connectivity density by 38.4%, while the mean trabecular separation showed no significant difference. 10%SrHA also increased the bone area density by 36.3% in histological analysis. Results from this study indicated that 10%SrHA increased bone density and improved trabecular microarchitecture around implants in osteoporotic animals previously treated with ZOL when compared to HA. PMID:25891947

  11. Phase stability and biological property evaluation of plasma sprayed hydroxyapatite coatings for orthopedic and dental applications.

    PubMed

    Vahabzadeh, Sahar; Roy, Mangal; Bandyopadhyay, Amit; Bose, Susmita

    2015-04-01

    In this work we have investigated the effects of strontium (Sr) dopant on in vitro protein release kinetics and in vivo osteogenic properties of plasma sprayed hydroxyapatite (HA) coatings, along with their dissolution behavior. Plasma sprayed HA coatings are widely used in load-bearing implants. Apart from osseointegration, the new generation of HA coating is expected to deliver biomolecules and/or drugs that can induce osteoinduction. This paper reports the preparation of crystalline and amorphous HA coatings on commercially pure titanium (Cp-Ti) using inductively coupled radio frequency (RF) plasma spray, and their stability at different solution pH. Coatings prepared at 110 mm working distance from the nozzle showed an average Ca ion release of 18 and 90 ppm in neutral and acidic environments, respectively. Decreasing the working distance to 90 mm resulted in the formation of a coating with less crystalline HA and phases with higher solubility products, and consequently higher dissolution over 32 days. A 92% release of a model protein bovine serum albumin (BSA) in phosphate buffer with pH of 7.4 was measured for Sr-doped HA (Sr-HA) coating, while only a 72% release could be measured for pure HA coating. Distortion of BSA during adsorption on coatings revealed a strong interaction between the protein and the coating, with an increase in α-helix content. Osteoid formation was found on Sr-HA implants as early as 7 weeks post implantation compared to HA coated and uncoated Ti implants. After 12 weeks post implantation, osteoid new bone was formed on HA implants; whereas, bone mineralization started on Sr-HA samples. While no osteoid was formed on bare Ti surfaces, bone was completely mineralized on HA and Sr-HA coatings after 16 weeks post implantation. Our results show that both phase stability and chemistry can have a significant influence toward in vitro and in vivo response of HA coatings on Ti implants. PMID:25638672

  12. Freeze-cast hydroxyapatite scaffolds for bone tissue engineering applications.

    PubMed

    Fu, Qiang; Rahaman, Mohamed N; Dogan, Fatih; Bal, B Sonny

    2008-06-01

    Freeze casting of aqueous suspensions was investigated as a method for preparing porous hydroxyapatite (HA) scaffolds for eventual application to bone tissue engineering. Suspensions of HA particles (10-20 volume percent) were frozen unidirectionally in a cylindrical mold placed on a cold steel substrate (-20 degrees C). After sublimation of the ice, sintering for 3 h at 1350 degrees C produced constructs with dense HA lamellae, with porosity of approximately 50%, and inter-lamellar pore widths of 5-30 microm. These constructs had compressive strengths of 12 +/- 1 MPa and 5 +/- 1 MPa in the directions parallel and perpendicular to the freezing direction, respectively. Manipulation of the microstructure was achieved by modifying the solvent composition of the suspension used for freeze casting. The use of water-glycerol mixtures (20 wt% glycerol) resulted in the production of constructs with finer pores (1-10 microm) and a larger number of dendritic growth connecting the HA lamellae, and higher strength. On the other hand, the use of water-dioxane mixtures (60 wt% dioxane) resulted in a cellular-type microstructure with larger pores (90-110 microm). The mechanical response showed high strain tolerance (5-10% at the maximum stress), high strain for failure (>20%) and sensitivity to the loading rate. The favorable mechanical behavior of the porous constructs, coupled with the ability to modify their microstructure, indicates the potential of the present freeze casting route for the production of porous scaffolds for bone tissue engineering. PMID:18458369

  13. Development and Characterization of Biphasic Hydroxyapatite/β-TCP Cements

    PubMed Central

    Gallinetti, Sara; Canal, Cristina; Ginebra, Maria-Pau; Ferreira, J

    2014-01-01

    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. Ca2+ 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. PMID:25866411

  14. Enhancement of hydroxyapatite formation by laser-liquid-solid interaction

    NASA Astrophysics Data System (ADS)

    Pramatarova, Liliana; Pecheva, Emilia; Petrov, Todor S.; Minkovski, Nikolai I.; Kondyurin, Alexey; Pramatarova, Radina

    2004-06-01

    In this paper the use of stainless steel, silicon and silica glass substrates for the growth of hydroxyapatite (HA, widely used as artificial bone material), induced by a laser-liquid-solid-interaction is reported. The method allows growing of HA layer by using the interaction between a laser beam and a liquid precursor solution, as well as laser irradiation of the substrate during the laser-liquid interaction. The scanned laser beam (pulsed CuBr laser) is directed at the solid substrate, which is immersed in the solution, which resembles the ion composition and concentrations of the human blood plasma (simulated body fluid, SBF). The set-up includes an open deposition system, which allows the introduction of the laser beam led by a scanning system. It is shown that the proposed method enhances the HA formation, in comparison with the traditional methods of prolonged soaking in SBF. The HA layers grown in this manner are investigated by Light Microscopy (LM), Scanning Electron Microscopy (SEM), Energy Dispersive X-ray (EDX) Spectroscopy, X-ray Diffraction (XRD), Fourier Transform Infrared (FTIR) and Raman Spectroscopy.

  15. Hydroxyapatite Formation on a Novel Dental Cement in Human Saliva

    PubMed Central

    Engstrand, Johanna; Unosson, Erik; Engqvist, Håkan

    2012-01-01

    Dental materials have to meet high standards regarding mechanical strength and handling properties. There is however only a limited amount of research that has been devoted to natural formation of hydroxyapatite (HA) in contact with the materials. The objective of the current investigation was to study the surface reactions occurring in human salvia on a novel dental cement. Ceramir Crown & Bridge, a bioceramic luting agent intended for permanent cementation of conventional oral prosthetics, was evaluated by immersing discs made from the cement in human saliva and phosphate buffered saline (PBS) for seven days, after which they were dried and analyzed. The analytical methods used in order to verify HA formation on the surface were grazing incidence X-ray diffraction (GI-XRD), scanning electron microscopy (SEM), and X-ray photoelectron spectroscopy (XPS). All results showed that HA was formed on the surfaces of samples stored in saliva as well as on samples stored in PBS. The possibility of a dental luting cement to promote natural formation of HA at the tooth interface increases the stability and durability of the system and could help prevent secondary caries. PMID:23056955

  16. Analysis of human alveolar osteoblast behavior on a nano-hydroxyapatite substrate: an in vitro study

    PubMed Central

    2014-01-01

    Background Nano-hydroxyapatite (nHA) is a potential ideal biomaterial for bone regeneration. However, studies have yet to characterize the behavior of human osteoblasts derived from alveolar bone on nHA. Thus, the aim of the present study was to evaluate the influence of nHA on the adhesion, proliferation and differentiation of these alveolar bone-derived cells. Methods Primary human alveolar osteoblasts were collected from the alveolar ridge of a male periodontal patient during osseous resective surgery and grown on culture plates coated with either polylysine or polylysine with nano-hydroxyapatite (POL/nHA) composite. The cells were grown and observed for 14 days, and then assessed for potential modifications to osteoblasts homeostasis as evaluated by quantitative reverse transcriptase-polymerase chain reaction (real time RT-PCR), scanning electron microscopy and atomic force microscopy. Results Real time PCR revealed a significant increase in the expression of the selected markers of osteoblast differentiation (bone morphogenetic protein (BMP)-2,-5,-7, ALP, COLL-1A2, OC, ON) in cells grown on the POL/nHA substrate. In addition, as compared with the POL surface, cells grown on the POL/nHA substrate demonstrated better osteoconductive properties, as demonstrated by the increase in adhesion and spreading, likely as a result of the increased surface roughness of the composite. Conclusions The increased expression of BMPs and osteoinductive biomarkers suggest that nano-hydroxyapatite may stimulate the proliferation and differentiation of local alveolar osteoblasts and thus encourage bone regeneration at sites of alveolar bone regeneration. PMID:24650194

  17. Segmental stability in orthognathic surgery: hydroxyapatite/Poly-l-lactide osteoconductive composite versus titanium miniplate osteosyntheses.

    PubMed

    Landes, Constantin A; Ballon, Alexander; Tran, Andreas; Ghanaati, Shahram; Sader, Robert

    2014-09-01

    Hydroxyapatite was included into F-u-HA/PLLA (unsintered hydroxyapatite - Poly l-lactide) composite osteosynthesis material for its documented osteoconductive capacity. This study investigates segmental retention capacities and outcome stability using F-u-HA/PLLA composite osteosyntheses in orthognathic surgery. Of fifty patients in total, 25 patients were osteofixated with F-u-HA/PLLA osteoconductive bioabsorbable osteosyntheses and compared to a group of 25 patients treated with titanium miniplates. The F-u-HA/PLLA group included 14 maxillary advancements, 4 setbacks, 13 impactions, 5 elongations at A-point; the titanium group included 20 maxillary advancements, 2 setbacks, 11 impactions and 11 elongations. In the mandible the F-u-HA/PLLA group included 13 advancements at B-point, 11 setbacks, 16 clockwise rotations and 8 counterclockwise rotations at the Gonial angle (Ar-Go-Gn); the titanium group included 9 mandibular advancements, 5 setbacks, 8 clockwise rotations and 6 counterclockwise rotations at Ar-Go-Gn. Segmental stability and relapse were assessed comparing preoperative, postoperative and follow-up roentgen cephalometrics at 22 ± 11 months on average in F-u-HA/PLLA cases, 24 ± 22 months on average in the titanium group. All absolute operative movements were nonsignificant in the F-u-HA/PLLA cases compared to the titanium osteosynthesis cases. Relapses were nonsignificant but there was greater vertical relapse in maxillary impactions with titanium osteosyntheses. Throughout this study, F-u-HA/PLLA composite osteosyntheses appeared as stable as titanium miniplates. It can therefore be concluded, although from a limited number of patients, that the investigated osteoconductive osteosynthesis can be used in a similar way to titanium miniplates in orthognathic surgery. Compared to earlier studies using other bioabsorbable polymers in the literature, F-u-HA/PLLA proved to be more stable in segmental retention. PMID:24534684

  18. Effect of blending HA-g-PLLA on xanthohumol-loaded PLGA fiber membrane.

    PubMed

    Qiao, Tiankui; Jiang, Suchen; Song, Ping; Song, Xiaofeng; Liu, Qimin; Wang, Lijuan; Chen, Xuesi

    2016-10-01

    Electropsun poly (lactide-co-glycolide) (PLGA) fiber membrane loaded xanthohumol (XN) has been developed using a co-solvent system of chloroform and dimethylformamide. To enhance its biological functionality as bone tissue engineering scaffolds, 5wt% hydroxyapatite grafted poly (l-lactic acid) (HA-g-PLLA) is blended into the spinning solution. The purpose of the present work is to disclose the effect of blending HA-g-PLLA on the corresponding properties of the medicated fiber membrane including morphology, thermodynamics, wettability, drug release, mechanics as well as cytotoxicity. XN and HA-g-PLLA can be well blended with PLGA to make fibers. Blending HA-g-PLLA not only turns amorphous XN/PLGA fiber membrane into crystal structure, but also changes the membranous wettability. Various medicated membranes exhibit the sustained release profiles. Drug release rate of the ternary membrane with HA-g-PLLA is slower compared to the binary XN/PLGA, and for the ternary membrane, the drug release accelerates with increasing XN content. A model is proposed to account for the drug release process. Tensile testing shows that at 10% of XN, the comprehensive mechanics of the ternary is preferable to the binary. At the same time, these fiber membranes are no cytotoxicity. PMID:27343844

  19. Improving mechanical and biological properties of macroporous HA scaffolds through composite coatings.

    PubMed

    Zhao, J; Lu, X; Duan, K; Guo, L Y; Zhou, S B; Weng, J

    2009-11-01

    Interconnected porous hydroxyapatite (HA) scaffolds are widely used for bone repair and replacement, owing to their ability to support the adhesion, transfer, proliferation and differentiation of cells. In the present study, the polymer impregnation approach was adopted to produce porous HA scaffolds with three-dimensional (3D) porous structures. These scaffolds have an advantage of highly interconnected porosity (approximately 85%) but a drawback of poor mechanical strength. Therefore, the as-prepared HA scaffolds were lined with composite polymer coatings in order to improve the mechanical properties and retain its good bioactivity and biocompatibility at the same time. The composite coatings were based on poly(D,L-lactide) (PDLLA) polymer solutions, and contained single component or combination of HA, calcium sulfate (CS) and chondroitin sulfate (ChS) powders. The effects of composite coatings on scaffold porosity, microstructure, mechanical property, in vitro mineralizing behavior, and cell attachment of the resultant scaffolds were investigated. The results showed that the scaffolds with composite coatings resulted in significant improvement in both mechanical and biological properties while retaining the 3D interconnected porous structure. The in vitro mineralizing behaviors were mainly related to the compositions of CS and ChS powders in the composite coatings. Excellent cell attachments were observed on the pure HA scaffold as well as the three types of composite scaffolds. These composite scaffolds with improved mechanical properties and bioactivities are promising bone substitutes in tissue engineering fields. PMID:19679453

  20. On the structural, mechanical, and biodegradation properties of HA/β-TCP robocast scaffolds.

    PubMed

    Houmard, Manuel; Fu, Qiang; Genet, Martin; Saiz, Eduardo; Tomsia, Antoni P

    2013-10-01

    Hydroxyapatite/β-tricalcium phosphate (HA/β-TCP) composite scaffolds have shown great potential for bone-tissue engineering applications. In this work, ceramic scaffold with different HA/β-TCP compositions (pure HA, 60HA/40β-TCP, and 20HA/80β-TCP) were fabricated by a robotic-assisted deposition (robocasting) technique using water-based hydrogel inks. A systematic study was conducted to investigate the porosity, mechanical property, and degradation of the scaffolds. Our results indicate that, at a similar volume porosity, the mechanical strength of the sintered scaffolds increased with the decreasing rod diameter. The compressive strength of the fabricated scaffolds (porosity ≈ 25-80 vol %) varied between ∼3 and ∼50 MPa, a value equal or higher than that of human cancellous bone (2-12 MPa). Although there was a slight increase of Ca and P ions in water after 5 month, no noticeable degradation of the scaffolds in SBF or water was observed. Our findings from this work indicate that composite calcium phosphate scaffolds with customer-designed chemistry and architecture may be fabricated by a robotic-assisted deposition method. PMID:23650043

  1. Electrophoretic deposition of double-layer HA/Al composite coating on NiTi.

    PubMed

    Karimi, Esmaeil; Khalil-Allafi, Jafar; Khalili, Vida

    2016-01-01

    In order to improve the bioactivity of NiTi alloys, which are being known as the suitable materials for biomedical applications, numerous NiTi disks were electrophoretically coated by hetero-coagulated hydroxyapatite/aluminum composite coatings in three main voltages from suspensions with different Al concentrations. In this paper, the amount of Ni ions release and bioactivity of prepared samples as well as bonding strength of the coating to substrate were investigated. The surface characterization of the coating by XRD, EDX, SEM, and FTIR showed that HA particles bonded by Al particles. It caused the formation of a free crack coating on NiTi disks. Moreover, the bonding strength of HA/Al coatings to NiTi substrate were improved by two times as compared to that of the pure HA coatings. Immersing of coated samples in SBF for 1 week showed that apatite formation ability was improved on HA/Al composite coating and Ni ions release from the surface of composite coating decreased. These results induce the appropriate bioactivity and biocompatibility of the deposited HA/Al composite coatings on NiTi disks. PMID:26478383

  2. Microsphere coated substrate containing reactive aldehyde groups

    NASA Technical Reports Server (NTRS)

    Rembaum, Alan (Inventor); Yen, Richard C. K. (Inventor)

    1984-01-01

    A synthetic organic resin is coated with a continuous layer of contiguous, tangential, individual microspheres having a uniform diameter preferably between 100 Angstroms and 2000 Angstroms. The microspheres are an addition polymerized polymer of an unsaturated aldehyde containing 4 to 20 carbon atoms and are covalently bonded to the substrate by means of high energy radiation grafting. The microspheres contain reactive aldehyde groups and can form conjugates with proteins such as enzymes or other aldehyde reactive materials.

  3. Calcium silicate ceramic scaffolds toughened with hydroxyapatite whiskers for bone tissue engineering

    SciTech Connect

    Feng, Pei; Wei, Pingpin; Li, Pengjian; Gao, Chengde; Shuai, Cijun; Peng, Shuping

    2014-11-15

    Calcium silicate possessed excellent biocompatibility, bioactivity and degradability, while the high brittleness limited its application in load-bearing sites. Hydroxyapatite whiskers ranging from 0 to 30 wt.% were incorporated into the calcium silicate matrix to improve the strength and fracture resistance. Porous scaffolds were fabricated by selective laser sintering. The effects of hydroxyapatite whiskers on the mechanical properties and toughening mechanisms were investigated. The results showed that the scaffolds had a uniform and continuous inner network with the pore size ranging between 0.5 mm and 0.8 mm. The mechanical properties were enhanced with increasing hydroxyapatite whiskers, reached a maximum at 20 wt.% (compressive strength: 27.28 MPa, compressive Young's modulus: 156.2 MPa, flexural strength: 15.64 MPa and fracture toughness: 1.43 MPa·m{sup 1/2}) and then decreased by addition of more hydroxyapatite whiskers. The improvement of mechanical properties was due to whisker pull-out, crack deflection and crack bridging. Moreover, the degradation rate decreased with the increase of hydroxyapatite whisker content. A layer of bone-like apatite was formed on the scaffold surfaces after being soaked in simulated body fluid. Human osteoblast-like MG-63 cells spread well on the scaffolds and proliferated with increasing culture time. These findings suggested that the calcium silicate scaffolds reinforced with hydroxyapatite whiskers showed great potential for bone regeneration and tissue engineering applications. - Highlights: • HA whiskers were incorporated into CS to improve the properties. • The scaffolds were successfully fabricated by SLS. • Toughening mechanisms was whisker pull-out, crack deflection and bridging. • The scaffolds showed excellent apatite forming ability.

  4. Glass microspheres for medical applications

    NASA Astrophysics Data System (ADS)

    Conzone, Samuel David

    Radioactive dysprosium lithium borate glass microspheres have been developed as biodegradable radiation delivery vehicles for the radiation synovectomy treatment of rheumatoid arthritis. Once injected into a diseased joint, the microspheres deliver a potent dose of radiation to the diseased tissue, while a non-uniform chemical reaction converts the glass into an amorphous, porous, hydrated dysprosium phosphate reaction product. The non-radioactive, lithium-borate component is dissolved from the glass (up to 94% weight loss), while the radioactive 165Dy reacts with phosphate anions in the body fluids, and becomes "chemically" trapped in a solid, dysprosium phosphate reaction product that has the same size as the un-reacted glass microsphere. Ethylene diamine tetraacetate (EDTA) chelation therapy can be used to dissolve the dysprosium phosphate reaction product after the radiation delivery has subsided. The dysprosium phosphate reaction product, which formed in vivo in the joint of a Sprague-Dawley rat, was dissolved by EDTA chelation therapy in <1 week, without causing any detectable joint damage. The combination of dysprosium lithium borate glass microspheres and EDTA chelation therapy provides an unique "tool" for the medical community, which can deliver a large dose (>100 Gy) of localized beta radiation to a treatment site within the body, followed by complete biodegradability. The non-uniform reaction process is a desirable characteristic for a biodegradable radiation delivery vehicle, but it is also a novel material synthesis technique that can convert a glass to a highly porous materials with widely varying chemical composition by simple, low-temperature, glass/solution reaction. The reaction product formed by nonuniform reaction occupies the same volume as the un-reacted glass, and after drying for 1 h at 300°C, has a specific surface area of ≈200 m2/g, a pore size of ≈30 nm, and a nominal crushing strength of ≈10 MPa. Finally, rhenium glass

  5. Improved biocompatibility of hydroxyapatite thin film prepared by aerosol deposition.

    PubMed

    Park, Dong-Soo; Kim, In-Sook; Kim, Hyeongil; Chou, Alex Hung Kuo; Hahn, Byung-Dong; Li, Long-Hao; Hwang, Soon-Jung

    2010-08-01

    Technical development for an efficient coating of bioactive materials improves the characteristics of a fully functional implant. The aim of this study was to investigate the osteoinductive effect of a newly developed hydroxyapatite (HA)-coating technique using aerosol deposition without post-heat treatment [room temperature (RT) group] on the titanium (Ti) dental implant in vitro and in vivo, compared with that of HA coating with post-heat treatment (HT-400 group) or machined surface (control group). Cell proliferation or attachment on the HA-coated Ti surface was assessed using tetrazolium salt, WST-8 or scanning electron microscopy (SEM). Human osteoblasts (HOB) on RT group were well attached and grew alike in the control or HT-400 group. The alkaline phosphatase activity of HOB cultured on RT and HT-400 group was significantly higher than the control group (p < 0.05). Evaluation by SEM, TEM, and XRD demonstrated that aerosol deposition facilitated HA particles to form a dense and uniform HA layer in the RT group despite no post-heating. In a rabbit tibia model (n = 3), the ratios of bone implant contact and bone area in the RT group (49.88%, 86.05%) were greater than in the HT-400 group (38.82%, 77.34%) or the control (28.31%, 73.86%). The finding of this study showed that the HA coating using aerosol deposition without post-heat treatment has a good biocompatibility, and provide a promoting strategy to enhance osseointegration in the application of the dental implant. PMID:20574972

  6. Hydroxyapatite nanocrystals as a smart, pH sensitive, delivery system for kiteplatin.

    PubMed

    Lelli, Marco; Roveri, Norberto; Marzano, Cristina; Hoeschele, James D; Curci, Alessandra; Margiotta, Nicola; Gandin, Valentina; Natile, Giovanni

    2016-08-16

    Hydroxyapatite (HA) nanocrystals are important inorganic constituents of biological hard tissues in vertebrates and have been proposed as a bone substitute or a coating material for prostheses in biomedicine. Hydroxyapatite is also amenable for its capacity to bind to a great variety of biomolecules and therapeutic agents. As drug carriers, apatite nanoparticles also have the advantage of pH dependent solubility and low toxicity. Thus HA nanoparticles are negligibly soluble at physiological pH but their dissolution is accelerated at lower pH such as that typically found in the vicinity of tumors. In the present study we have investigated the adsorption on and the release from biomimetic HA nanoparticles of two platinum derivatives of cis-1,4-diaminocyclohexane ([PtX2(cis-1,4-DACH)], X2 = Cl2 (1) and 1,1-cyclobutanedicarboxylate (CBDCA, 2)). The first of the two compounds proved to be active against colon cancer cells also resistant to oxaliplatin. The release has been investigated as a function of pH to mimic the different physiological environments of healthy tissues and tumors, and the in vitro cytotoxicity of the releasates from the HA matrices has been assessed against various human cancer cell lines. The results fully confirmed the potential of 1-loaded HA nanoparticles as bone-specific drug delivery devices. PMID:27397134

  7. Porous bioactive scaffold of aliphatic polyurethane and hydroxyapatite for tissue regeneration.

    PubMed

    Wang, Li; Li, Yubao; Zuo, Yi; Zhang, Li; Zou, Qin; Cheng, Lin; Jiang, Hong

    2009-04-01

    In this study, a new hydroxyapatite (HA)/polyurethane (PU) composite porous scaffold was developed by in situ polymerization. Aliphatic isophorone diisocyanate as a nontoxic and safe agent was adopted to produce the rigid segment in polyurethane polymerization. Hydroxyapatite powder was compounded in a PU polymer matrix during the polymeric process. The macrostructure and morphology as well as mechanical strength of the scaffolds were characterized by FTIR, XRD, DSC and SEM. The results show that the isophorone diisocyanate can react mildly with hydroxyl (-OH) groups of castor oil and a mild foaming action caused by the release of CO2 gas occurred simultaneously in the reactive process, thus producing a uniform porous structure of HA/PU scaffold. The HA/PU composite scaffold with a high HA content of about 60 wt% has a porosity of more than 78% and a pore size from 100 microm to 800 microm. The HA/PU scaffold exhibited good cytocompatibility estimated by co-culturing the scaffold with MG63 cells through MTT test. The porous composite scaffold has good homogenization and a perfect three-dimensional structure for cell migration and bone tissue ingrowth, and should have good prospects for bone tissue regeneration. PMID:19208942

  8. Poly-L-lactic acid/hydroxyapatite electrospun nanocomposites induce chondrogenic differentiation of human MSC.

    PubMed

    Spadaccio, Cristiano; Rainer, Alberto; Trombetta, Marcella; Vadalá, Gianluca; Chello, Massimo; Covino, Elvio; Denaro, Vincenzo; Toyoda, Yoshiya; Genovese, Jorge A

    2009-07-01

    Cartilage and bone tissue engineering has been widely investigated but is still hampered by cell differentiation and transplant integration issues within the constructs. Scaffolds represent the pivotal structure of the engineered tissue and establish an environment for neo-extracellular matrix synthesis. They can be associated to signals to modulate cell activity. In this study, considering the well reported role of hydroxyapatite (HA) in cartilage repair, we focused on the putative chondrogenic differentiation of human mesenchymal stem cells (hMSCs) following culture on membranes of electrospun fibers of poly-L-lactic acid (PLLA) loaded with nanoparticles of HA. hMSCs were seeded on PLLA/HA and bare PLLA membranes and cultured in basal medium, using chondrogenic differentiation medium as a positive control. After 14 days of culture, SOX-9 positive cells could be detected in the PLLA/HA group. Cartilage specific proteoglycan immunostain confirmed the presence of neo-extracellular-matrix production. Co-expression of CD29, a typical surface marker of MSCs and SOX-9, suggested different degrees in the differentiation process. We developed a hydroxyapatite functionalized scaffold with the aim to recapitulate the native histoarchitecture and the molecular signaling of osteochondral tissue to facilitate cell differentiation toward chondrocyte. PLLA/HA nanocomposites induced differentiation of hMSCs in a chondrocyte-like phenotype with generation of a proteoglycan based matrix. This nanocomposite could be an amenable alternative scaffold for cartilage tissue engineering using hMSCs. PMID:19418224

  9. Pulsed laser deposition of hydroxyapatite on titanium substrate with titania interlayer.

    PubMed

    Rajesh, P; Muraleedharan, C V; Komath, Manoj; Varma, Harikrishna

    2011-03-01

    Pulsed laser deposition (PLD) has been used to deposit hydroxyapatite (HA) ceramic over titanium substrate with an interlayer of titania. PLD has been identified as a potential candidate for bioceramic coatings over metallic substrates to be used as orthopedic and dental implants because of better process control and preservation of phase identity of the coating component. However, direct deposition of hydroxyapatite on titanium at elevated temperature results in the formation of natural oxide layer along with some perovskites like calcium titanate at the interface. This leads to easy debonding of ceramic layer from the metal and thereby affecting the adhesion strength. In the present study, adherent and stable HA coating over Ti6Al4V was achieved with the help of an interlayer of titania. The interlayer was made to a submicron level and HA was deposited consecutively to a thickness of around one micron by exposing to laser ablation at a substrate temperature of 400°C. The deposited phase was identified to be phase pure HA by X-ray diffraction, scanning electron microscopy, energy dispersive X-ray analysis, and inductively coupled plasma spectrometry. The mechanical behavior of coating evaluated by scratch test indicates that the adhesion strength of HA coating was improved with the presence of titania interlayer. PMID:21234791

  10. 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.

  11. Coupling system to a microsphere cavity

    NASA Technical Reports Server (NTRS)

    Iltchenko, Vladimir (Inventor); Maleki, Lute (Inventor); Yao, Steve (Inventor); Wu, Chi (Inventor)

    2002-01-01

    A system of coupling optical energy in a waveguide mode, into a resonator that operates in a whispering gallery mode. A first part of the operation uses a fiber in its waveguide mode to couple information into a resonator e.g. a microsphere. The fiber is cleaved at an angle .PHI. which causes total internal reflection within the fiber. The energy in the fiber then forms an evanescent field and a microsphere is placed in the area of the evanescent field. If the microsphere resonance is resonant with energy in the fiber, then the information in the fiber is effectively transferred to the microsphere.

  12. 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

  13. Electron microscopy of biomaterials based on hydroxyapatite

    SciTech Connect

    Suvorova, E. I. Klechkovskaya, V. V.; Komarov, V. F.; Severin, A. V.; Melikhov, I. V.; Buffat, P. A.

    2006-10-15

    Three types of biomaterials based on hydroxyapatite are synthesized and investigated. Hydroxyapatite nanocrystals or microcrystals precipitated from low-temperature aqueous solutions serve as the initial material used for preparing spherical porous granules approximately 300-500 {mu}m in diameter. Sintering of hydroxyapatite crystals at a temperature of 870 deg. C for 2 h or at 1000 deg. C (for 3 h) + 1200 deg. C (for 2 h) brings about the formation of solid ceramics with different internal structures. According to the electron microscopic data, the ceramic material prepared at 870 deg. C is formed by agglomerated hydroxyapatite nanocrystals, whereas the ceramics sintered at 1200 deg. C (with a bending strength of the order of 100 MPa) are composed of crystal blocks as large as 2 {mu}m. It is established that all the biomaterials have a single-phase composition and consist of the hydroxyapatite with a structure retained up to a temperature of 1200 deg. C.

  14. 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. PMID:23348918

  15. The role of phosphorylation in dentin phosphoprotein peptide absorption to hydroxyapatite surfaces: a molecular dynamics study

    PubMed Central

    Villarreal-Ramirez, Eduardo; Garduño-Juarez, Ramon; Gericke, Arne; Boskey, Adele

    2015-01-01

    Dentin phosphoprotein (DPP) is a protein expressed mainly in dentin and to a lesser extent in bone. DPP has a disordered structure, rich in glutamic acid, aspartic acid and phosphorylated serine/threonine residues. It has a high capacity for binding to calcium ions and to hydroxyapatite (HA) crystal surfaces. We used molecular dynamics (MD) simulations as a method for virtually screening interactions between DPP motifs and HA. The goal was to determine which motifs are absorbed to HA surfaces. For these simulations, we considered five peptides from the human DPP sequence. All-atom MD simulations were performed using GROMACS, the peptides were oriented parallel to the {100} HA crystal surface, the distance between the HA and the peptide was 3 nm. The system was simulated for 20 ns. Preliminary results show that for the unphosphorylated peptides, the acidic amino acids present an electrostatic attraction where their side chains are oriented towards HA. This attraction, however, is slow to facilitate bulk transport to the crystal surface. On the other hand, the phosphorylated (PP) peptides are rapidly absorbed on the surface of the HA with their centers of mass closer to the HA surface. More importantly, the root mean square fluctuation (RMSF) indicates that the average structures of the phosphorylated peptides are very inflexible and elongate, while that of the unphosphorylated peptides are flexible. Radius of gyration (Rg) analysis showed the compactness of un-phosphorylated peptides is lower than phosphorylated peptides. Phosphorylation of the DPP peptides is necessary for binding to HA surfaces. PMID:25158198

  16. 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. PMID:22606041

  17. Nanomechanical properties of electrospun composite scaffolds based on polycaprolactone and hydroxyapatite.

    PubMed

    Tyagi, Parul; Catledge, Shane A; Stanishevsky, Andrei; Thomas, Vinoy; Vohra, Y K

    2009-08-01

    Fibrous nanocomposite scaffolds were electrospun from dispersions of hydroxyapatite nanoparticles (nanoHA) in polycaprolactone (PCL) with varying nanoHA contents (from 0% to 50% by weight). Such scaffolds were produced to mimic the nano-features of the extracellular matrix (ECM) for natural bone tissue regeneration. NanoHA was found to be well dispersed in the PCL fibers up to the addition of 30 wt%, whereas beads and agglomeration of HA particles was observed above this nanoHA concentration. The structural and morphological characterizations were evaluated by scanning electron microscopy (SEM), Fourier-Transform Infrared Spectroscopy (FTIR), and X-ray Diffraction (XRD). The average fiber diameter decreased with increased nanoHA concentration. The nanomechanical properties of the as-spun fibrous scaffolds as well as pressure-consolidated (pelletized) composites were evaluated by nanoindentation. Elastic modulus increased with increasing HA content, but was especially pronounced for 40-50% HA content where the indenter tip is more likely to probe agglomerated HA particles. PMID:19928159

  18. Engineering nanocages with polyglutamate domains for coupling to hydroxyapatite biomaterials and allograft bone.

    PubMed

    Culpepper, Bonnie K; Morris, David S; Prevelige, Peter E; Bellis, Susan L

    2013-03-01

    Hydroxyapatite (HA) is the principal constituent of bone mineral, and synthetic HA is widely used as a biomaterial for bone repair. Previous work has shown that polyglutamate domains bind selectively to HA and that these domains can be utilized to couple bioactive peptides onto many different HA-containing materials. In the current study we have adapted this technology to engineer polyglutamate domains into cargo-loaded nanocage structures derived from the P22 bacteriophage. P22 nanocages have demonstrated significant potential as a drug delivery system due to their stability, large capacity for loading with a diversity of proteins and other types of cargo, and ability to resist degradation by proteases. Site-directed mutagenesis was used to modify the primary coding sequence of the P22 coat protein to incorporate glutamate-rich regions. Relative to wild-type P22, the polyglutamate-modified nanocages (E2-P22) exhibited increased binding to ceramic HA disks, particulate HA and allograft bone. Furthermore, E2-P22 binding was HA selective, as evidenced by negligible binding of the nanocages to non-HA materials including polystyrene, agarose, and polycaprolactone (PCL). Taken together these results establish a new mechanism for the directed coupling of nanocage drug delivery systems to a variety of HA-containing materials commonly used in diverse bone therapies. PMID:23312905

  19. 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. PMID:26369028

  20. Densification Process of OH Controlled Hydroxyapatite Ceramics by Spark Plasma Sintering

    SciTech Connect

    Kawagoe, D.; Koga, Y.; Ishida, E. H.; Ioku, K.

    2006-05-15

    Calcium hydroxyapatite, Ca10(PO4)6(OH)2:HA, is the inorganic principle component of natural bones and teeth. It has been already suggested that the amount of OH ion in the crystal structure of HA is closely related to the biocompatibility. The amount of OH ion in current HA, however, has not been controlled. In order to prepare more functional HA ceramics, the amount of OH ion must be controlled. In this study, HA ceramics with different OH amount were prepared from fine HA crystals by spark plasma sintering (SPS). In order to reveal the ideal sintering conditions for preparation of transparent ceramics, densification process on SPS was investigated. The samples were pressed uniaxialy under 60 MPa, and then they were heated by SPS at 800 deg. C, 900 deg. C and 1000 deg. C for 10 min with the heating rate of 25 deg. C{center_dot}min-1. The quantity of OH ion in HA ceramics sintered by SPS was decreased with increasing temperature of sintering. Transparent HA ceramics were prepared by SPS at 900 deg. C and 1000 deg. C. In analysis of the densification behavior during sintering of HA by SPS, dominant sintering mechanism was plastic flow of densification. Transparent ceramics should be the most suitable materials to investigate the interface between human cells and ceramics.

  1. Engineering nanocages with polyglutamate domains for coupling to hydroxyapatite biomaterials and allograft bone

    PubMed Central

    Culpepper, Bonnie K.; Morris, David S.; Prevelige, Peter E.; Bellis, Susan L.

    2013-01-01

    Hydroxyapatite (HA) is the principal constituent of bone mineral, and synthetic HA is widely used as a biomaterial for bone repair. Previous work has shown that polyglutamate domains bind selectively to HA and that these domains can be utilized to couple bioactive peptides onto many different HA-containing materials. In the current study we have adapted this technology to engineer polyglutamate domains into cargo-loaded nanocage structures derived from the P22 bacteriophage. P22 nanocages have demonstrated significant potential as a drug delivery system due to their stability, large capacity for loading with a diversity of proteins and other types of cargo, and ability to resist degradation by proteases. Site-directed mutagenesis was used to modify the primary coding sequence of the P22 coat protein to incorporate glutamate-rich regions. Relative to wild-type P22, the polyglutamate-modified nanocages (E2-P22) exhibited increased binding to ceramic HA disks, particulate HA and allograft bone. Furthermore, E2-P22 binding was HA selective, as evidenced by negligible binding of the nanocages to non-HA materials including polystyrene, agarose, and polycaprolactone (PCL). Taken together these results establish a new mechanism for the directed coupling of nanocage drug delivery systems to a variety of HA-containing materials commonly used in diverse bone therapies. PMID:23312905

  2. Discrete deposition of hydroxyapatite nanoparticles on a titanium implant with predisposing substrate microtopography accelerated osseointegration

    NASA Astrophysics Data System (ADS)

    Nishimura, Ichiro; Huang, Yuhong; Butz, Frank; Ogawa, Takahiro; Lin, Audrey; Wang, Chiachien Jake

    2007-06-01

    We report here a new versatile method to deposit discrete hydroxyapatite (HA) nanoparticles on a titanium (Ti) implant with predisposing substrate microtopography, which exhibited an unexpectedly robust biological effect. Commercially pure Ti substrates were treated with 3-aminopropyltriethoxysilane, on which HA nanoparticles (20 nm) were deposited and chemically bonded to TiO2. The HA deposition rate was linearly related to the treatment time and HA nanoparticles were deposited on up to 50% of the substrate surface. As a result, the discrete deposition of HA nanoparticles generated novel 20-40 nm nanotopography on the Ti substrate with microtopography that was smooth (turned) or roughened by double acid etching (DAE). The experimental implants with or without HA nanoparticles were surgically placed in rat femur and an implant push-in test was performed after two weeks of healing. The deposition of HA nanoparticles on the DAE surface increased the mechanical withstanding load by 129% and 782% as compared to the control DAE and turned implants, respectively. Micro-computed tomography-based 3D bone morphometry revealed equivalent bone volumes around the DAE implant with or without HA nanoparticles. These data suggest that the discrete deposition of HA nanoparticles accelerates the early osseointegration process, likely through increased shear bonding strengths.

  3. Laser ablation in titanium implants followed by biomimetic hydroxyapatite coating: Histomorphometric study in rabbits.

    PubMed

    Faeda, Rafael Silveira; Spin-Neto, Rubens; Marcantonio, Elcio; Guastaldi, Antonio Carlos; Marcantonio, Elcio

    2012-07-01

    Titanium surface texture and chemistry modification successfully improves the host response and consequently the bone-to-implant contact surrounding dental implants. The aim of the present study was to investigate, using histomorphometrical-analysis, the effects of titanium surface modification by laser-ablation (Nd:YAG) followed by thin chemical deposition of HA. Forty-eight rabbits received one implant by tibiae of AS-machined (MS), laser-modified (LMS), or biomimetic hydroxyapatite-coated (HA) surface. Bone-to-implant contact (BIC) and bone area (BBT) were evaluated after 4, 8, and 12 weeks, at cortical and cancellous regions. Average BIC in the cortical region was higher (P < 0.001) on the LMS and HA implants for all periods, with no differences between LMS and HA. For the cancellous area, the LMS and HA implants showed higher (P < 0.01) BIC than MS at the initial periods. The LMS and HA showed similar values in the cortical region, but a tendency of higher values for HA in the cancellous region was observed in all periods. For the BBT, the differences were found only between HA and MS after 4 weeks in the cortical region (P < 0.05), and after 12 weeks in the cancellous area (P < 0.05). Our results showed that HA biomimetic coating preceded by laser treatment induced the contact osteogenesis and allowed the formation of a more stable bone-implant interface, even in earlier periods. PMID:22389308

  4. Sol-Gel-Derived Hydroxyapatite-Carbon Nanotube/Titania Coatings on Titanium Substrates

    PubMed Central

    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/TiO2) double layer coatings were successfully developed on titanium (Ti) substrates intended for biomedical applications. A TiO2 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/TiO2 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/TiO2 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/TiO2 coatings on Ti substrates might be a promising material for bone replacement. PMID:22606041

  5. PLGA/nHA hybrid nanofiber scaffold as a nanocargo carrier of insulin for accelerating bone tissue regeneration

    NASA Astrophysics Data System (ADS)

    Haider, Adnan; Gupta, Kailash Chandra; Kang, Inn-Kyu

    2014-06-01

    The development of tissue engineering in the field of orthopedic surgery is booming. Two fields of research in particular have emerged: approaches for tailoring the surface properties of implantable materials with osteoinductive factors as well as evaluation of the response of osteogenic cells to these fabricated implanted materials (hybrid material). In the present study, we chemically grafted insulin onto the surface of hydroxyapatite nanorods (nHA). The insulin-grafted nHAs (nHA-I) were dispersed into poly(lactide-co-glycolide) (PLGA) polymer solution, which was electrospun to prepare PLGA/nHA-I composite nanofiber scaffolds. The morphology of the electrospun nanofiber scaffolds was assessed by field emission scanning electron microscopy (FESEM). After extensive characterization of the PLGA/nHA-I and PLGA/nHA composite nanofiber scaffolds by Fourier transform infrared spectroscopy (FTIR), X-ray diffraction spectroscopy (XRD), X-ray photoelectron spectroscopy (XPS), energy-dispersive X-ray spectrometry (EDS), and transmission electron microscopy (TEM), the PLGA/nHA-I and PLGA/nHA (used as control) composite nanofiber scaffolds were subjected to cell studies. The results obtained from cell adhesion, alizarin red staining, and Von Kossa assay suggested that the PLGA/nHA-I composite nanofiber scaffold has enhanced osteoblastic cell growth, as more cells were proliferated and differentiated. The fact that insulin enhanced osteoblastic cell proliferation will open new possibilities for the development of artificial scaffolds for bone tissue regeneration.

  6. 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

  7. Effect of strontium-containing hydroxyapatite bone cement on bone remodeling following hip replacement.

    PubMed

    Ni, Guo X; Lin, Jian H; Chiu, Peter K Y; Li, Zhao Y; Lu, William W

    2010-01-01

    It is uncertain whether the use of bioactive bone cement has any beneficial effect on local bone adaptation following hip replacement. In this study, twelve goats underwent cemented hip hemiarthroplasty unilaterally, with either PMMA bone cement or strontium-containing hydroxyapatite (Sr-HA) bioactive bone cement. Nine months later, the femoral cortical bones at different levels were analyzed by microhardness testing and micro-CT scanning. Extensive bone remodeling was found at proximal and mid-levels in both PMMA and Sr-HA groups. However, with regard to the differences of bone mineral density, cortical bone area and bone hardness between implanted and non-implanted femur, less decreases were found in Sr-HA group than PMMA group at proximal and mid-levels, and significant differences were shown for bone area and hardness at proximal level. The results suggested that the use of Sr-HA cement might alleviate femoral bone remodeling after hip replacement. PMID:19728042

  8. Effect of silver additive on physicochemical properties of hydroxyapatite applied to reconstructive surgery

    NASA Astrophysics Data System (ADS)

    Zhuk, I. V.; Rasskazova, L. A.; Korotchenko, N. M.

    2015-11-01

    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 (CCa2+.103, 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 samples 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.

  9. Nano-hydroxyapatite composite biomaterials for bone tissue engineering--a review.

    PubMed

    Venkatesan, Jayachandran; Kim, Se-Kwon

    2014-10-01

    In recent years, significant development has been achieved in the construction of artificial bone with ceramics, polymers and metals. Nano-hydroxyapatite (nHA) is widely used bioceramic material for bone graft substitute owing to its biocompatibility and osteoconductive properties. nHA with chitin, chitosan, collagen, gelatin, fibrin, polylactic acid, polycaprolactone, poly(lactic-co-glycolic) acid, polyamide, polyvinyl alcohol, polyurethane and polyhydroxybutyrate based composite scaffolds have been explored in the present review for bone graft substitute. This article further reviews the preparative methods, chemical interaction, biocompatibiity, biodegradation, alkaline phosphatase activity, mineralization effect, mechanical properties and delivery of nHA-based nanocomposites for bone tissue regeneration. The nHA based composite biomaterials proved to be promising biomaterials for bone tissue engineering. PMID:25992432

  10. Compression molding of aerogel microspheres

    DOEpatents

    Pekala, R.W.; Hrubesh, L.W.

    1998-03-24

    An aerogel composite material produced by compression molding of aerogel microspheres (powders) mixed together with a small percentage of polymer binder to form monolithic shapes in a cost-effective manner is disclosed. The aerogel composites are formed by mixing aerogel microspheres with a polymer binder, placing the mixture in a mold and heating under pressure, which results in a composite with a density of 50--800 kg/m{sup 3} (0.05--0.80 g/cc). The thermal conductivity of the thus formed aerogel composite is below that of air, but higher than the thermal conductivity of monolithic aerogels. The resulting aerogel composites are attractive for applications such as thermal insulation since fabrication thereof does not require large and expensive processing equipment. In addition to thermal insulation, the aerogel composites may be utilized for filtration, ICF target, double layer capacitors, and capacitive deionization. 4 figs.

  11. Compression molding of aerogel microspheres

    DOEpatents

    Pekala, Richard W.; Hrubesh, Lawrence W.

    1998-03-24

    An aerogel composite material produced by compression molding of aerogel microspheres (powders) mixed together with a small percentage of polymer binder to form monolithic shapes in a cost-effective manner. The aerogel composites are formed by mixing aerogel microspheres with a polymer binder, placing the mixture in a mold and heating under pressure, which results in a composite with a density of 50-800 kg/m.sup.3 (0.05-0.80 g/cc). The thermal conductivity of the thus formed aerogel composite is below that of air, but higher than the thermal conductivity of monolithic aerogels. The resulting aerogel composites are attractive for applications such as thermal insulation since fabrication thereof does not require large and expensive processing equipment. In addition to thermal insulation, the aerogel composites may be utilized for filtration, ICF target, double layer capacitors, and capacitive deionization.

  12. Biodegradable microspheres for parenteral delivery.

    PubMed

    Sinha, V R; Trehan, A

    2005-01-01

    Nowadays, emphasis is being laid to development of controlled release dosage forms. Interest in this technology has increased steadily over the past few years. Although oral administration of drugs is a widely accepted route of drug delivery, bioavailability of drug often varies as a result of gastrointestinal absorption, degradation by first-pass effect, and hostile environment of gastrointestinal tract. Transdermal administration for percutaneous absorption of drug is limited by the impermeable nature of the stratum corneum. Ocular and nasal delivery is also unfavorable because of degradation by enzymes present in eye tissues and nasal mucosa. Hence, the parenteral route is the most viable approach in such cases. Of the various ways of achieving long-term parenteral drug delivery, biodegradable microspheres are one of the better means of controlling the release of drug over a long time. Because of the lipidic nature of liposomes, problems such as limited physical stability and difficulty of freeze-drying are encountered. Similarly, for emulsions, stability on long-term basis and in suspensions, rheological changes during filling, injecting, and storage poses limitation. Also, in all these systems, the release rate cannot be tailored to the needs of the patient. Parenteral controlled-release formulations based on biodegradable microspheres can overcome these problems and can control the release of drug over a predetermined time span, usually in the order of days to weeks to months. Various FDA-approved controlled-release parenteral formulations based on these biodegradable microspheres are available on the market, including Lupron Depot Nutropin Depot and Zoladex. This review covers various molecules encapsulated in biodegradable microspheres for parenteral delivery. PMID:16566705

  13. Microspheres in Plasma Display Panels

    NASA Technical Reports Server (NTRS)

    2006-01-01

    Filling small bubbles of molten glass with gases is just as difficult as it sounds, but the technical staff at NASA is not known to shy away from a difficult task. When Microsphere Systems, Inc. (MSI), of Ypsilanti, Michigan, and Imaging Systems Technology, Inc. (IST), of Toledo, Ohio, were trying to push the limits of plasma displays but were having difficulty with the designs, NASA s Glenn Garrett Morgan Commercialization Initiative (GMCI) assembled key personnel at Glenn Research Center and Ohio State University for a brainstorming session to come up with a solution for the companies. They needed a system that could produce hollow, glass micro-sized spheres (microspheres) that could be filled with a variety of gasses. But the extremely high temperature required to force the micro-sized glass bubbles to form at the tip of a metal nozzle resulted in severe discoloration of the microspheres. After countless experiments on various glass-metal combinations, they had turned to the GMCI for help. NASA experts in advanced metals, ceramics, and glass concluded that a new design approach was necessary. The team determined that what was needed was a phosphate glass composition that would remain transparent, and they went to work on a solution. Six weeks later, using the design tips from the NASA team, Tim Henderson, president of MSI, had designed a new system in which all surfaces in contact with the molten glass would be ceramic instead of metal. Meanwhile, IST was able to complete a Phase I Small Business Innovation Research (SBIR) grant supported by the National Science Foundation (NSF) and supply a potential customer with samples of the microspheres for evaluation as filler materials for high-performance insulations.

  14. 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.

  15. Robocasting nanocomposite scaffolds of poly(caprolactone)/hydroxyapatite incorporating modified carbon nanotubes for hard tissue reconstruction.

    PubMed

    Dorj, Biligzaya; Won, Jong-Eun; Kim, Joong-Hyun; Choi, Seong-Jun; Shin, Ueon Sang; Kim, Hae-Won

    2013-06-01

    Nanocomposite scaffolds with tailored 3D pore configuration are promising candidates for the reconstruction of bone. Here we fabricated novel nanocomposite bone scaffolds through robocasting. Poly(caprolactone) (PCL)-hydroxyapatite (HA) slurry containing ionically modified carbon nanotubes (imCNTs) was robotic-dispensed and structured layer-by-layer into macrochanneled 3D scaffolds under adjusted processing conditions. Homogeneous dispersion of imCNTs (0.2 wt % relative to PCL-HA) was achieved in acetone, aiding in the preparation of PCL-HA-imCNTs slurry with good mixing property. Incorporation of imCNTs into PCL-HA composition significantly improved the compressive strength and elastic modulus of the robotic-dispensed scaffolds (~1.5-fold in strength and ~2.5-fold in elastic modulus). When incubated in simulated body fluid (SBF), PCL-HA-imCNT nanocomposite scaffold induced substantial mineralization of apatite in a similar manner to the PCL-HA scaffold, which was contrasted in pure PCL scaffold. MC3T3-E1 cell culture on the scaffolds demonstrated that cell proliferation levels were significantly higher in both PCL-HA-imCNT and PCL-HA than in pure PCL, and no significant difference was found between the nanocomposite scaffolds. When the PCL-HA-imCNT scaffold was implanted into a rat subcutaneous tissue for 4 weeks, soft fibrous tissues with neo-blood vessels formed well in the pore channels of the scaffolds without any significant inflammatory signs. Tissue reactions in PCL-HA-imCNT scaffold were similar to those in PCL-HA scaffold, suggesting incorporated imCNT did not negate the beneficial biological roles of HA. While more long-term in vivo research in bone defect models is needed to confirm clinical availability, our results suggest robotic-dispensed PCL-HA-imCNT nanocomposite scaffolds can be considered promising new candidate matrices for bone regeneration. PMID:23184729

  16. 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

  17. Preparation and characterization of NiW-nHA composite catalyst for hydrocracking.

    PubMed

    Zhou, Gang; Hou, Yongzhao; Liu, Lei; Liu, Hongru; Liu, Can; Liu, Jing; Qiao, Huiting; Liu, Wenyong; Fan, Yubo; Shen, Shituan; Rong, Long

    2012-12-21

    The synthesis, characterization and catalytic capability of the NiW-nano-hydroxyapatite (NiW-nHA) composite were investigated in this paper. The NiW-nHA catalyst was prepared by a co-precipitation method. Then Fourier transform infrared (FT-IR) spectroscopy, transmission electron microscopy (TEM), X-ray diffraction (XRD) and energy dispersive spectroscopy (EDX) were used to analyze this material. In addition, the catalytic capacity of the NiW-nHA composite was also examined by FT-IR and gas chromatography (GC). The results of FT-IR analysis indicated that Ni, W and nHA combined closely. TEM observation revealed that this catalyst was needle shaped and the crystal retained a nanometer size. XRD data also suggested that a new phase of CaWO(4) appeared and the lattice parameters of nHA changed in this system. nHA was the carrier of metals. The rates of Ni/W-loading were 73.24% and 65.99% according to the EDX data, respectively. Furthermore, the conversion of 91.88% Jatropha oil was achieved at 360 °C and 3 MPa h(-1) over NiW-nHA catalyst. The straight chain alkanes ranging from C(15) to C(18) were the main components in the production. The yield of C(15)-C(18) alkanes was up to 83.56 wt%. The reaction pathway involved hydrocracking of the C═C bonds of these triglycerides from Jatropha oil. This paper developed a novel non-sulfided catalyst to obtain a "green biofuel" from vegetable oil. PMID:23128670

  18. Cellular proliferation, cellular viability, and biocompatibility of HA-ZnO composites.

    PubMed

    Saha, Naresh; Dubey, Ashutosh K; Basu, Bikramjit

    2012-01-01

    One of the important issues in the development of hydroxyapatite (HA)-based biomaterials is the prosthetic infection, which limits wider use of monolithic HA despite superior cellular response. Recently, we reported that ZnO addition to HA can induce bactericidal property. It is therefore important to assess how ZnO addition influences the cytotoxicity property and cell adhesion/proliferation on HA-ZnO composite surfaces in vitro. In the above perspective, the objective of this study is to investigate the cell type and material composition dependent cellular proliferation and viability of pressureless sintered HA-ZnO composites. The combination of cell viability data as well as morphological observations of cultured human osteoblast-like SaOS2 cells and mouse fibroblast L929 cells suggests that HA-ZnO composites containing 10 Wt % or lower ZnO exhibit the ability to support cell adhesion and proliferation. Both SaOS2 and L929 cells exhibit extensive multidirectional network of actin cytoskeleton and cell flattening on the lower ZnO containing (≤10 Wt %) HA-ZnO composites. The in vitro results illustrate how variation in ZnO content can influence significantly the cell vitality, as evaluated using MTT biochemical assay. Also, the critical statistical analysis reveals that ZnO addition needs to be carefully tailored to ensure good in vitro cytocompatibility. The underlying reasons for difference in biological properties are analyzed. It is suggested that surface wettability as well as dissolution of ZnO, both contribute to the observed differences in cellular viability and proliferation. PMID:22102555

  19. Preparation and characterization of NiW-nHA composite catalyst for hydrocracking

    NASA Astrophysics Data System (ADS)

    Zhou, Gang; Hou, Yongzhao; Liu, Lei; Liu, Hongru; Liu, Can; Liu, Jing; Qiao, Huiting; Liu, Wenyong; Fan, Yubo; Shen, Shituan; Rong, Long

    2012-11-01

    The synthesis, characterization and catalytic capability of the NiW-nano-hydroxyapatite (NiW-nHA) composite were investigated in this paper. The NiW-nHA catalyst was prepared by a co-precipitation method. Then Fourier transform infrared (FT-IR) spectroscopy, transmission electron microscopy (TEM), X-ray diffraction (XRD) and energy dispersive spectroscopy (EDX) were used to analyze this material. In addition, the catalytic capacity of the NiW-nHA composite was also examined by FT-IR and gas chromatography (GC). The results of FT-IR analysis indicated that Ni, W and nHA combined closely. TEM observation revealed that this catalyst was needle shaped and the crystal retained a nanometer size. XRD data also suggested that a new phase of CaWO4 appeared and the lattice parameters of nHA changed in this system. nHA was the carrier of metals. The rates of Ni/W-loading were 73.24% and 65.99% according to the EDX data, respectively. Furthermore, the conversion of 91.88% Jatropha oil was achieved at 360 °C and 3 MPa h-1 over NiW-nHA catalyst. The straight chain alkanes ranging from C15 to C18 were the main components in the production. The yield of C15-C18 alkanes was up to 83.56 wt%. The reaction pathway involved hydrocracking of the C&z.dbd;C bonds of these triglycerides from Jatropha oil. This paper developed a novel non-sulfided catalyst to obtain a ``green biofuel'' from vegetable oil.

  20. Strontium and zoledronate hydroxyapatites graded composite coatings for bone prostheses.

    PubMed

    Boanini, Elisa; Torricelli, Paola; Sima, Felix; Axente, Emanuel; Fini, Milena; Mihailescu, Ion N; Bigi, Adriana

    2015-06-15

    Both strontium and zoledronate (ZOL) are known to be useful for the treatment of bone diseases associated to the loss of bone substance. In this work, we applied an innovative technique, Combinatorial Matrix-Assisted Pulsed Laser Evaporation (C-MAPLE), to deposit gradient thin films with variable compositions of Sr-substituted hydroxyapatite (SrHA) and ZOL modified hydroxyapatite (ZOLHA) on Titanium substrates. Compositional gradients were obtained by simultaneous laser vaporization of the two distinct material targets. The coatings display good crystallinity and granular morphology, which do not vary with composition. Osteoblast-like MG63 cells and human osteoclasts were co-cultured on the thin films up to 21 days. The results show that Sr counteracts the negative effect of relatively high concentration of ZOL on osteoblast viability, whereas both Sr and ZOL enhance extracellular matrix deposition. In particular, ZOL promotes type I collagen production, whereas Sr increases the production of alkaline phosphatase. Moreover, ZOL exerts a greater effect than Sr on osteoprotegerin/RANKL ratio and, as a consequence, on the reduction of osteoclast proliferation and activity. The deposition method allows to modulate the composition of the thin films and hence the promotion of bone growth and the inhibition of bone resorption. PMID:25706198

  1. Antibacterial coatings of fluoridated hydroxyapatite for percutaneous implants.

    PubMed

    Ge, Xiang; Leng, Yang; Bao, Chongyun; Xu, Sherry Li; Wang, Renke; Ren, Fuzeng

    2010-11-01

    Percutaneous orthopedic and dental implants require not only good adhesion with bone but also the ability to attach and form seals with connective tissues and the skin. To solve the skin-seal problem of such implants, an electrochemical deposition method was used to modify the surfaces of metallic implants to improve their antibacterial ability and skin seals around them. A dense and uniform fluoridated calcium phosphate coating with a thickness of about 200 nm was deposited on an acid-etched pure titanium substrate by controlling the current density and reaction duration of the electrochemical process. The as-deposited amorphous fluoridated calcium phosphate transformed to fluoridated hydroxyapatite (FHA) after heat treatment at 600°C in a water vapor environment for 3 h. Both single crystal diffraction patterns and high-resolution transmission electron microscope (HRTEM) images confirmed the phase of the fluoridated calcium phosphate after the heat treatment. The antibacterial activities of FHA coatings were tested against Staphylococcus aureus (S. aureus), Escherichia coli (E. coli), and Porphyromonas gingivalis (P. gingivalis) with the film attachment method. The antibacterial activity of FHA coating is much higher than that of pure hydroxyapatite (HA) coating and acid-etched pure titanium surface. The promising features of FHA coating make it suitable for orthopedic and dental applications. PMID:20725973

  2. Study the bonding mechanism of binders on hydroxyapatite surface and mechanical properties for 3DP fabrication bone scaffolds.

    PubMed

    Wei, Qinghua; Wang, Yanen; Li, Xinpei; Yang, Mingming; Chai, Weihong; Wang, Kai; zhang, Yingfeng

    2016-04-01

    In 3DP fabricating artificial bone scaffolds process, the interaction mechanism between binder and bioceramics power determines the microstructure and macro mechanical properties of Hydroxyapatite (HA) bone scaffold. In this study, we applied Molecular Dynamics (MD) methods to investigating the bonding mechanism and essence of binders on the HA crystallographic planes for 3DP fabrication bone scaffolds. The cohesive energy densities of binders and the binding energies, PCFs g(r), mechanical properties of binder/HA interaction models were analyzed through the MD simulation. Additionally, we prepared the HA bone scaffold specimens with different glues by 3DP additive manufacturing, and tested their mechanical properties by the electronic universal testing machine. The simulation results revealed that the relationship of the binding energies between binders and HA surface is consistent with the cohesive energy densities of binders, which is PAM/HA>PVA/HA>PVP/HA. The PCFs g(r) indicated that their interfacial interactions mainly attribute to the ionic bonds and hydrogen bonds which formed between the polar atoms, functional groups in binder polymer and the Ca, -OH in HA. The results of mechanical experiments verified the relationship of Young׳s modulus for three interaction models in simulation, which is PVA/HA>PAM/HA>PVP/HA. But the trend of compressive strength is PAM/HA>PVA/HA>PVP/HA, this is consistent with the binding energies of simulation. Therefore, the Young׳s modulus of bone scaffolds are limited by the Young׳s modulus of binders, and the compressive strength is mainly decided by the viscosity of binder. Finally, the major reasons for differences in mechanical properties between simulation and experiment were found, the space among HA pellets and the incomplete infiltration of glue were the main reasons influencing the mechanical properties of 3DP fabrication HA bone scaffolds. These results provide useful information in choosing binder for 3DP fabrication

  3. Research on the preparation, biocompatibility and bioactivity of magnesium matrix hydroxyapatite composite material.

    PubMed

    Linsheng, Li; Guoxiang, Lin; Lihui, Li

    2016-08-12

    In this paper, magnesium matrix hydroxyapatite composite material was prepared by electrophoretic deposition method. The optimal process parameters of electrophoretic deposition were HA suspension concentration of 0.02 kg/L, aging time of 10 days and voltage of 60 V. Animal experiment and SBF immersion experiment were used to test the biocompatibility and bioactivity of this material respectively. The SD rats were divided into control group and implant group. The implant surrounding tissue was taken to do tissue biopsy, HE dyed and organizational analysis after a certain amount of time in the SD rat body. The biological composite material was soaked in SBF solution under homeothermic condition. After 40 days, the bioactivity of the biological composite material was evaluated by testing the growth ability of apatite on composite material. The experiment results showed that magnesium matrix hydroxyapatite biological composite material was successfully prepared by electrophoretic deposition method. Tissue hyperplasia, connective tissue and new blood vessels appeared in the implant surrounding soft tissue. No infiltration of inflammatory cells of lymphocytes and megakaryocytes around the implant was found. After soaked in SBF solution, a layer bone-like apatite was found on the surface of magnesium matrix hydroxyapatite biological composite material. The magnesium matrix hydroxyapatite biological composite material could promot calcium deposition and induce bone-like apatite formation with no cytotoxicity and good biocompatibility and bioactivity. PMID:27567779

  4. Nanostructured Si, Mg, CO3 2- Substituted Hydroxyapatite Coatings Deposited by Liquid Precursor Plasma Spraying: Synthesis and Characterization

    NASA Astrophysics Data System (ADS)

    Huang, Tao; Xiao, Yanfeng; Wang, Shanling; Huang, Yi; Liu, Xiaoguang; Wu, Fang; Gu, Zhongwei

    2011-06-01

    In this study, a novel liquid precursor plasma spraying (LPPS) process was used to deposit Si, Mg, CO3 2- substituted hydroxyapatite (HA) coatings (alone and cosubstituted) onto Ti-6Al-4V substrates. Salts of silicon, magnesium, and carbonate elements were directly added into the HA liquid precursor for subsequent plasma spraying. The phase composition, structure, and morphology of all HA coatings were characterized by x-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and Fourier transform infrared (FTIR) spectroscopy. The results indicated that the trace elements were successfully incorporated into the HA structure and nanostructured coatings were obtained for all doped HA formulations. The incorporation of trace elements into the HA structure reduced its crystallinity, especially when silicon, magnesium and carbonate ions entered simultaneously into the HA structure. FTIR spectra showed that the Si-HA and Mg-HA coatings had decreased intensities in both the O-H and P-O bands and that the CO3 2--HA coating was mainly a B-type carbonate-substituted HA. The results showed that the LPPS process is an effective and simple method to synthesize trace element substituted biomimetic HA coatings with nanostructure.

  5. 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. PMID:25900356

  6. Thermoplastic polyurethane/hydroxyapatite electrospun scaffolds for bone tissue engineering: effects of polymer properties and particle size.

    PubMed

    Mi, Hao-Yang; Palumbo, SunMi; Jing, Xin; Turng, Lih-Sheng; Li, Wan-Ju; Peng, Xiang-Fang

    2014-10-01

    Thermoplastic polyurethane (TPU)/hydroxyapatite (HA) scaffolds were fabricated via electrospinning. The effects of TPU properties and HA particle size on scaffold physical properties and osteoblast-like cell performance were investigated. It was found that the addition of micro-HA (mHA), which was inlayed in the fiber, decreased the electrospun fiber diameter. On the contrary, nano-HA (nHA), which was either embedded or existed inside of the fiber, increased the fiber diameter for both soft and hard TPUs. The soft TPU had a much lower Young's modulus and higher strain-at-break than the hard TPU. The addition of both mHA and nHA decreased the tensile properties; this decrease was more significant with mHA. The cells on the hard scaffolds actively proliferated and migrated compared to those on the soft scaffolds. On the other hand, cells on the soft scaffolds more effectively induced osteogenesis of human mesenchymal stem cells (hMSCs) than those on the hard scaffolds. In addition, our data suggest that the soft scaffolds with supplementation of nHA further enhanced osteogenesis of hMSCs compared to those without nHA. The soft TPU scaffolds containing nano-HA have the potential to be used in bone tissue engineering applications. PMID:24574168

  7. 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. PMID:26897095

  8. POROUS WALL, HOLLOW GLASS MICROSPHERES

    SciTech Connect

    Sexton, W.

    2012-06-30

    Hollow Glass Microspheres (HGM) is not a new technology. All one has to do is go to the internet and Google{trademark} HGM. Anyone can buy HGM and they have a wide variety of uses. HGM are usually between 1 to 100 microns in diameter, although their size can range from 100 nanometers to 5 millimeters in diameter. HGM are used as lightweight filler in composite materials such as syntactic foam and lightweight concrete. In 1968 a patent was issued to W. Beck of the 3M{trademark} Company for 'Glass Bubbles Prepared by Reheating Solid Glass Particles'. In 1983 P. Howell was issued a patent for 'Glass Bubbles of Increased Collapse Strength' and in 1988 H. Marshall was issued a patent for 'Glass Microbubbles'. Now Google{trademark}, Porous Wall, Hollow Glass Microspheres (PW-HGMs), the key words here are Porous Wall. Almost every article has its beginning with the research done at the Savannah River National Laboratory (SRNL). The Savannah River Site (SRS) where SRNL is located has a long and successful history of working with hydrogen and its isotopes for national security, energy, waste management and environmental remediation applications. This includes more than 30 years of experience developing, processing, and implementing special ceramics, including glasses for a variety of Department of Energy (DOE) missions. In the case of glasses, SRS and SRNL have been involved in both the science and engineering of vitreous or glass based systems. As a part of this glass experience and expertise, SRNL has developed a number of niches in the glass arena, one of which is the development of porous glass systems for a variety of applications. These porous glass systems include sol gel glasses, which include both xerogels and aerogels, as well as phase separated glass compositions, that can be subsequently treated to produce another unique type of porosity within the glass forms. The porous glasses can increase the surface area compared to 'normal glasses of a 1 to 2 order of

  9. Evaluation of Bone Healing on Sandblasted and Acid Etched Implants Coated with Nanocrystalline Hydroxyapatite: An In Vivo Study in Rabbit Femur

    PubMed Central

    Melin Svanborg, Lory; Meirelles, Luiz; Franke Stenport, Victoria; Currie, Fredrik; Andersson, Martin

    2014-01-01

    This study aimed at investigating if a coating of hydroxyapatite nanocrystals would enhance bone healing over time in trabecular bone. Sandblasted and acid etched titanium implants with and without a submicron thick coat of hydroxyapatite nanocrystals (nano-HA) were implanted in rabbit femur with healing times of 2, 4, and 9 weeks. Removal torque analyses and histological evaluations were performed. The torque analysis did not show any significant differences between the implants at any healing time. The control implant showed a tendency of more newly formed bone after 4 weeks of healing and significantly higher bone area values after 9 weeks of healing. According to the results from this present study, both control and nano-HA surfaces were biocompatible and osteoconductive. A submicron thick coating of hydroxyapatite nanocrystals deposited onto blasted and acid etched screw shaped titanium implants did not enhance bone healing, as compared to blasted and etched control implants when placed in trabecular bone. PMID:24723952

  10. Magnetic responsive hydroxyapatite composite scaffolds construction for bone defect reparation

    PubMed Central

    Zeng, Xiao Bo; Hu, Hao; Xie, Li Qin; Lan, Fang; Jiang, Wen; Wu, Yao; Gu, Zhong Wei

    2012-01-01

    Introduction In recent years, interest in magnetic biomimetic scaffolds for tissue engineering has increased considerably. A type of magnetic scaffold composed of magnetic nanoparticles (MNPs) and hydroxyapatite (HA) for bone repair has been developed by our research group. Aim and methods In this study, to investigate the influence of the MNP content (in the scaffolds) on the cell behaviors and the interactions between the magnetic scaffold and the exterior magnetic field, a series of MNP-HA magnetic scaffolds with different MNP contents (from 0.2% to 2%) were fabricated by immersing HA scaffold into MNP colloid. ROS 17/2.8 and MC3T3-E1 cells were cultured on the scaffolds in vitro, with and without an exterior magnetic field, respectively. The cell adhesion, proliferation and differentiation were evaluated via scanning electron microscopy; confocal laser scanning microscopy; and 3-(4,5-Dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide (MTT), alkaline phosphatase, and bone gla protein activity tests. Results The results demonstrated the positive influence of the magnetic scaffolds on cell adhesion, proliferation, and differentiation. Further, a higher amount of MNPs on the magnetic scaffolds led to more significant stimulation. Conclusion The magnetic scaffold can respond to the exterior magnetic field and engender some synergistic effect to intensify the stimulating effect of a magnetic field to the proliferation and differentiation of cells. PMID:22848165

  11. Interfacial stress transfer in a graphene nanosheet toughened hydroxyapatite composite

    NASA Astrophysics Data System (ADS)

    Zhang, L.; Zhang, X. G.; Chen, Y.; Su, J. N.; Liu, W. W.; Zhang, T. H.; Qi, F.; Wang, Y. G.

    2014-10-01

    In recent years, graphene has emerged as potential reinforcing nanofiller in the composites for structural engineering due to its extraordinary high elastic modulus and mechanical strength. As recognized, the transfer of stress from a low modulus matrix to a high-modulus reinforcing graphene and the interfacial behavior at a graphene-matrix interface is the fundamental issue in these composites. In the case of graphene nanosheet (GNS) reinforced hydroxyapatite (HA) composite, this research presented analytical models and simulated that the number of graphene layers of GNSs has little effect on the maximum axial stress (˜0.35 GPa) and the maximum shear stress (˜0.14 GPa) at a GNS-HA interface, and the energy dissipation by GNS pull-out decreases with increasing the number of graphene layers due to weak bonding between them. Also, GNS-HA interfacial delamination and/or GNS rupture were also indentified to be the two key failure mechanisms. The computed results are expected to facilitate a better understanding of the interfacial behavior at a GNS-ceramic interface and to achieve tough ceramics reinforced with GNSs.

  12. Characterization of high velocity oxy-fuel combustion sprayed hydroxyapatite.

    PubMed

    Haman, J D; Lucas, L C; Crawmer, D

    1995-02-01

    Bioceramic coatings, created by the high velocity oxy-fuel combustion spraying of hydroxyapatite (HA) powders onto commercially pure titanium, were characterized in order to determine whether this relatively new coating process can be successfully applied to bioceramic coatings of orthopaedic and dental implants. Fourier transform infrared spectroscopy, X-ray diffraction and scanning electron microscopy were used to characterize both the HA starting powders and coatings. A 12 wk immersion test was conducted and the resulting changes in the coatings were also characterized. Calcium ion release during dissolution was measured with flame atomic absorption during the first 6 weeks of the immersion study. A comparison of powder and coating X-ray diffraction patterns and lattice parameters revealed an HA-type coating with some loss in crystallinity. Fourier transform infrared results showed a partial loss of the OH- group during spraying, however the phosphate groups were still present. Scanning electron microscopy analysis showed a lamellar structure with very close coating-to-substrate apposition. The coatings experienced a loss of calcium during the immersion study, with the greatest release in calcium occurring during the first 6 days of the study. No significant structural or chemical changes were observed during the 12 wk immersion study. These results indicate that the high velocity oxy-fuel process can produce an HA-type coating; however, the process needs further optimization, specifically in the areas of coating-to-substrate bond strength and minimization of phases present other than HA, before it would be recommended for commercial use. PMID:7749000

  13. Electrospun polyurethane/hydroxyapatite bioactive scaffolds for bone tissue engineering: the role of solvent and hydroxyapatite particles.

    PubMed

    Tetteh, G; Khan, A S; Delaine-Smith, R M; Reilly, G C; Rehman, I U

    2014-11-01

    Polyurethane (PU) is a promising polymer to support bone-matrix producing cells due to its durability and mechanical resistance. In this study two types of medical grade poly-ether urethanes Z3A1 and Z9A1 and PU-Hydroxyapatite (PU-HA) composites were investigated for their ability to act as a scaffold for tissue engineered bone. PU dissolved in varying concentrations of dimethylformamide (DMF) and tetrahydrofuran (THF) solvents were electrospun to attain scaffolds with randomly orientated non-woven fibres. Bioactive polymeric composite scaffolds were created using 15 wt% Z3A1 in a 70/30 DMF/THF PU solution and incorporating micro- or nano-sized HA particles in a ratio of 3:1 respectively, whilst a 25 wt% Z9A1 PU solution was doped in ratio of 5:1. Chemical properties of the resulting composites were evaluated by FTIR and physical properties by SEM. Tensile mechanical testing was carried out on all electrospun scaffolds. MLO-A5 osteoblastic mouse cells and human embryonic mesenchymal progenitor cells, hES-MPs were seeded on the scaffolds to test their biocompatibility and ability to support mineralised matrix production over a 28 day culture period. Cell viability was assayed by MTT and calcium and collagen deposition by Sirius red and alizarin red respectively. SEM images of both electrospun PU scaffolds and PU-HA composite scaffolds showed differences in fibre morphology with changes in solvent combinations and size of HA particles. Inclusion of THF eliminated the presence of beads in fibres that were present in scaffolds fabricated with 100% DMF solvent, and resulted in fibres with a more uniform morphology and thicker diameters. Mechanical testing demonstrated that the Young׳s Modulus and yield strength was lower at higher THF concentrations. Inclusion of both sizes of HA particles in PU-HA solutions reinforced the scaffolds leading to higher mechanical properties, whilst FTIR characterisation confirmed the presence of HA in all composite scaffolds. Although

  14. Effects of sol-gel processing parameters on the phases and microstructures of HA films.

    PubMed

    Wang, Diangang; Chen, Chuanzhong; Liu, Xiuna; Lei, Tingquan

    2007-06-15

    Bioactive hydroxyapatite (HA) films were fabricated by a sol-gel method and triethylphosphate and calcium nitrate were used as the phosphorus and calcium precursors, respectively. The effects of the heat treatment temperature, pH level and substrate materials on the phases and microstructures of HA films were studied by X-ray diffraction (XRD), scanning electronic microscopy (SEM) and electronic probe microanalysis (EPMA) and so on. The results show that all the sol-gel films are composed of the phases of HA, CaO, TiO(2) and CaTiO(3). With increasing the calcining temperature, the crystallinity of the films increases, the structure becomes more compact and changes from granular and lamellar to cellular structure, and the Ca/P ratio increases slightly because of the loss of P in the films. The addition of ammonia (adjusting the pH level to be about 7.5) can increase the HA content in the films, and the difference of substrate materials only has a little influence on the microstructure of the sol-gel films. PMID:17353116

  15. Study of the gamma irradiation effects on the PMMA/HA and PMMA/SW

    NASA Astrophysics Data System (ADS)

    Silva, P.; Albano, C.; Perera, R.; Domínguez, N.

    2010-03-01

    The behavior of the poly(methyl methacrylate) (PMMA) under the action of gamma radiation has been sufficiently studied. In this work, we present results from melt flow index (MFI), thermogravimetric analysis (TGA), differential scanning calorimetry (DSC) and electron paramagnetic resonance (EPR) of PMMA composites with hydroxyapatite (HA) and seaweed residues (SW) irradiated with gamma rays at 1.08 kGy/h. Composites of PMMA/HA and PMMA/SW with 10%, 20% and 30% of the filler were prepared. The results show an increase in the MFI values with the integral dose of radiation, being consistent with chain-scission reactions. No EPR signal was observed in pure PMMA, while in the composites, the typical EPR signal of the PMMA radicals was observed, which increased with the amount of HA or SW. When comparing the relative intensities of the EPR signals for both types of composites, a slight increase in the concentration of free radicals generated in the sample with SW respect to that of PMMA/HA composite was obtained. A decay of the total free radical concentration was observed as time elapsed.

  16. BMP-2 Grafted nHA/PLGA Hybrid Nanofiber Scaffold Stimulates Osteoblastic Cells Growth

    PubMed Central

    Haider, Adnan; Kim, Sukyoung; Huh, Man-Woo; Kang, Inn-Kyu

    2015-01-01

    Biomaterials play a pivotal role in regenerative medicine, which aims to regenerate and replace lost/degenerated tissues or organs. Natural bone is a hierarchical structure, comprised of various cells having specific functions that are regulated by sophisticated mechanisms. However, the regulation of the normal functions in damaged or injured cells is disrupted. In order to address this problem, we attempted to artificially generate a scaffold for mimicking the characteristics of the extracellular matrix at the nanoscale level to trigger osteoblastic cell growth. For this purpose, we have chemically grafted bone morphogenetic protein (BMP-2) onto the surface of L-glutamic acid modified hydroxyapatite incorporated into the PLGA nanofiber matrix. After extensive characterization using various spectroscopic techniques, the BMP-g-nHA/PLGA hybrid nanofiber scaffolds were subjected to various in vitro cytocompatibility tests. The results indicated that BMP-2 on BMP-g-nHA/PLGA hybrid nanofiber scaffolds greatly stimulated osteoblastic cells growth, contrary to the nHA/PLGA and pristine PLGA nanofiber scaffold, which are used as control. These results suggest that BMP-g-nHA/PLGA hybrid nanofiber scaffold can be used as a nanodrug carrier for the controlled and targeted delivery of BMP-2, which will open new possibilities for enhancing bone tissue regeneration and will help in the treatment of various bone-related diseases in the future. PMID:26539477

  17. The Tissue Implant Response Surrounding Subcutaneous TCP, HA, And ALCAP Bioceramics.

    PubMed

    Butler, K R; Benghuzzi, Hamed; Tucci, Michelle; Puckett, A D

    2015-01-01

    The objective of this investigation was to quantify and further elucidate the tissue-implant response in the fibrous tissue surrounding tricalcium phosphate (TCP), hydroxyapatite (HA), and aluminum calcium phosphate (ALCAP) implants when implanted subcutaneously. Sixteen animals in four experimental groups (n = 4/group) were implanted with one implant each: Group I (control, TCP), Group II (HA), and Group III (ALCAP). At 90 days post-implantation, the fibrous tissue surrounding the implants was harvested. Sections of stained fibrous tissue were evaluated for the presence of macrophages, fibrocytes, neutrophils, vascularity and thickness for all three groups using semi-automated quantitative methods. The analysis indicated Group III demonstrated a significantly higher number of neutrophils but fewer macrophages and blood vessels per high power field and had a substantially thinner fibrous tissue capsule thickness compared to Groups I and II (alpha=0.05). Group II elicited a greater response of fibroblasts compared to Groups I and III suggesting HA may provide a slightly higher degree of stability to the implant. In total, these findings suggest both TCP and HA behave similarly in vivo when compared to ALCAP and may be better choices for subcutaneous soft-tissue application compared to ALCAP. PMID:25996746

  18. BMP-2 Grafted nHA/PLGA Hybrid Nanofiber Scaffold Stimulates Osteoblastic Cells Growth.

    PubMed

    Haider, Adnan; Kim, Sukyoung; Huh, Man-Woo; Kang, Inn-Kyu

    2015-01-01

    Biomaterials play a pivotal role in regenerative medicine, which aims to regenerate and replace lost/degenerated tissues or organs. Natural bone is a hierarchical structure, comprised of various cells having specific functions that are regulated by sophisticated mechanisms. However, the regulation of the normal functions in damaged or injured cells is disrupted. In order to address this problem, we attempted to artificially generate a scaffold for mimicking the characteristics of the extracellular matrix at the nanoscale level to trigger osteoblastic cell growth. For this purpose, we have chemically grafted bone morphogenetic protein (BMP-2) onto the surface of L-glutamic acid modified hydroxyapatite incorporated into the PLGA nanofiber matrix. After extensive characterization using various spectroscopic techniques, the BMP-g-nHA/PLGA hybrid nanofiber scaffolds were subjected to various in vitro cytocompatibility tests. The results indicated that BMP-2 on BMP-g-nHA/PLGA hybrid nanofiber scaffolds greatly stimulated osteoblastic cells growth, contrary to the nHA/PLGA and pristine PLGA nanofiber scaffold, which are used as control. These results suggest that BMP-g-nHA/PLGA hybrid nanofiber scaffold can be used as a nanodrug carrier for the controlled and targeted delivery of BMP-2, which will open new possibilities for enhancing bone tissue regeneration and will help in the treatment of various bone-related diseases in the future. PMID:26539477

  19. 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.

  20. Integrated Cryogenic Experiment (ICE) microsphere investigation

    NASA Technical Reports Server (NTRS)

    Spradley, I.; Read, D.

    1989-01-01

    The main objective is to determine the performance of microsphere insulation in a 0-g environment and compare its performance to reference insulations such as multilayer insulation. The Lockheed Helium Extended-Life Dewar (HELD) is used to provide superfluid-helium cold sink for the experiment. The use of HELD allows the low-g dynamic properties of Passive Orbital Disconnect Struts (PODS) to be characterized and provides a flight demonstration of the PODS system. The thermal performance of microspheres in 1 and 0 g was predicted, a flight experiment was designed to determine microsphere thermal performance, and the interface was also designed between the experimental package and the shuttle through HELD and the Hitchhiker-M carrier. A single test cell was designed and fabricated. The cell was filled with uncoated glass microspheres and tested with a liquid-nitrogen cold sink. The data were found to agree with predictions of microsphere performance in 1 g.

  1. Polymer microspheres carrying fluorescent DNA probes

    NASA Astrophysics Data System (ADS)

    Chen, Xiaoyu; Dai, Zhao; Zhang, Jimei; Xu, Shichao; Wu, Chunrong; Zheng, Guo

    2010-07-01

    A polymer microspheres carried DNA probe, which was based on resonance energy transfer, was presented in this paper when CdTe quantum dots(QDs) were as energy donors, Au nanoparticles were as energy accepters and poly(4- vinylpyrindine-co-ethylene glycol dimethacrylate) microspheres were as carriers. Polymer microspheres with functional group on surfaces were prepared by distillation-precipitation polymerization when ethylene glycol dimethacrylate was as crosslinker in acetonitrile. CdTe QDs were prepared when 3-mercaptopropionic acid(MPA) was as the stabilizer in aqueous solution. Because of the hydrogen-bonding between the carboxyl groups of MPA on QDs and the pyrindine groups on the microspheres, the QDs were self-assembled onto the surfaces of microspheres. Then, the other parts of DNA probe were finished according to the classic method. The DNA detection results indicated that this novel fluorescent DNA probe system could recognize the existence of complementary target DNA or not.

  2. Multiplexed Microsphere Suspension Array-Based Immunoassays.

    PubMed

    Lin, Andrew; Salvador, Alexandra; Carter, J Mark

    2015-01-01

    ELISA is an extremely powerful tool to detect analytes because of its sensitivity, selectivity, reproducibility and ease of use. Here we describe sandwich immunoassays performed in suspension on spectrally unique microspheres developed by Luminex. Luminex assays offer the benefit of multiplex analysis of large numbers of analytes in a single reaction. Because the microspheres are spectrally unique, many microspheres, each attached to various antibodies, can be added to a single sample. Luminex instruments can distinguish each microsphere and detect the intensity of a reporter signal for each microsphere. Results are reported in Median Fluorescent Intensities for each analyte. Luminex assays can be used to detect up to 500 analytes in a high-throughput format. Luminex refers to this technology as xMAP(®). Here we describe a routine protocol for a Luminex immunoassay. Other Luminex assays would have to be optimized for specific conditions according to their use. PMID:26160569

  3. Laser-Induced Spallation of Microsphere Monolayers.

    PubMed

    Hiraiwa, Morgan; Stossel, Melicent; Khanolkar, Amey; Wang, Junlan; Boechler, Nicholas

    2016-08-01

    The detachment of a semiordered monolayer of polystyrene microspheres adhered to an aluminum-coated glass substrate is studied using a laser-induced spallation technique. The microsphere-substrate adhesion force is estimated from substrate surface displacement measurements obtained using optical interferometry, and a rigid-body model that accounts for the inertia of the microspheres. The estimated adhesion force is compared with estimates obtained using an adhesive contact model together with interferometric measurements of the out-of-plane microsphere contact resonance, and with estimated work of adhesion values for the polystyrene-aluminum interface. Scanning electron microscope images of detached monolayer regions reveal a unique morphology, namely, partially detached monolayer flakes composed of single hexagonal close packed crystalline domains. This work contributes to the fields of microsphere adhesion and contact dynamics, and demonstrates a unique monolayer delamination morphology. PMID:27409715

  4. Integrated Cryogenic Experiment (ICE) microsphere investigation

    SciTech Connect

    Spradley, I.; Read, D.

    1989-09-01

    The main objective is to determine the performance of microsphere insulation in a 0-g environment and compare its performance to reference insulations such as multilayer insulation. The Lockheed Helium Extended-Life Dewar (HELD) is used to provide superfluid-helium cold sink for the experiment. The use of HELD allows the low-g dynamic properties of Passive Orbital Disconnect Struts (PODS) to be characterized and provides a flight demonstration of the PODS system. The thermal performance of microspheres in 1 and 0 g was predicted, a flight experiment was designed to determine microsphere thermal performance, and the interface was also designed between the experimental package and the shuttle through HELD and the Hitchhiker-M carrier. A single test cell was designed and fabricated. The cell was filled with uncoated glass microspheres and tested with a liquid-nitrogen cold sink. The data were found to agree with predictions of microsphere performance in 1 g.

  5. Gas foamed open porous biodegradable polymeric microspheres.

    PubMed

    Kim, Taek Kyoung; Yoon, Jun Jin; Lee, Doo Sung; Park, Tae Gwan

    2006-01-01

    Highly open porous biodegradable polymeric microspheres were fabricated for use as injectable scaffold microcarriers for cell delivery. A modified water-in-oil-in-water (W1/O/W2) double emulsion solvent evaporation method was employed for producing the microspheres. The incorporation of an effervescent salt, ammonium bicarbonate, in the primary W1 droplets spontaneously produced carbon dioxide and ammonia gas bubbles during the solvent evaporation process, which not only stabilized the primary emulsion, but also created well inter-connected pores in the resultant microspheres. The porous microspheres fabricated under various gas foaming conditions were characterized. The surface pores became as large as 20 microm in diameter with increasing the concentration of ammonium bicarbonate, being sufficient enough for cell infiltration and seeding. These porous scaffold microspheres could be potentially utilized for cultivating cells in a suspension manner and for delivering the seeded cells to the tissue defect site in an injectable manner. PMID:16023197

  6. Nanocrystalline spin coated sol-gel hydroxyapatite thin films on Ti substrate: Towards potential applications for implants

    NASA Astrophysics Data System (ADS)

    Carradò, Adele; Viart, Nathalie

    2010-07-01

    Sol-gel spin coating is a promising process to obtain hydroxyapatite (HA) thin films. It is an alternative route to the hydroxyapatite deposition techniques usually employed to cover orthopaedic or dental titanium implant surfaces. The sol-gel (SG) parameters leading to a pure and crystalline HA coatings on Ti substrate were determined. They allow to reach a stoichiometric hydroxyapatite composition (ideal Ca/P atomic ratio 1.67) and a control of the growth of the crystalline phases. The samples, when observed by Scanning Electron Microscopy (SEM), exhibit grains of ca. 200 nm, well adapted for cell proliferation. The crystallisation of the HA films was thoroughly studied by X-Ray diffraction (XRD). The aim of this paper is to validate the sol-gel method as a processing method allowing the control of the mechanical state of the films and, in particular, of the residual stresses (RS) at metal-ceramic interfaces. These stresses were determined on titanium substrates. While the uncoated Ti substrates were in a compressive residual state, the coated ones were in a low tensile state. These results suggest that the sol-gel process is indeed a processing route to obtain HA coated Ti implants.

  7. Hydroxyapatite crystallinity does not affect the repair of critical size bone defects

    PubMed Central

    CONZ, Marcio Baltazar; GRANJEIRO, José Mauro; SOARES, Gloria de Almeida

    2011-01-01

    Objective The physicochemical properties of hydroxyapatite (HA) granules were observed to affect the biological behavior of graft materials. The aim of this work was to analyze the tissue response of two HA granules with different crystallinity and Ca/P ratio in vivo. Material and Methods The HA granules were produced in the Biomaterials Laboratory (COPPE/UFRJ). The testing materials were HA granules presenting a Ca/P molar ratio of 1.60 and 28% crystallinity (HA-1), and a Ca/P molar ratio of 1.67 and 70% crystallinity (HA-2). Both HAs were implanted into a critical-size calvaria rat defects. Results To note, in the control group, the bone defects were filled with blood clot only. Descriptive and histomorphometric analyses after 1, 3, and 6 months postoperatively showed mild inflammatory infiltrate, mainly comprising macrophage-like and multinucleated giant cells, and an increase in the volume density of the fibrous tissues (p<0.05), which was in contrast to the similar volume density of the newly formed bone and biomaterials in relation to the control group. Conclusion Thus, we concluded that HA-1 and HA-2 are biocompatible and non-degradable, and that crystallinity does not affect bone repair of critical size defects. PMID:21655775

  8. In vivo study on hydroxyapatite scaffolds with trabecular architecture for bone repair.

    PubMed

    Appleford, Mark R; Oh, Sunho; Oh, Namsik; Ong, Joo L

    2009-06-15

    The objective of this research was to investigate the bone formation and angio-conductive potential of hydroxyapatite (HA) scaffolds closely matched to trabecular bone in a canine segmental defect after 3 and 12 weeks post implantation. Histomorphometric comparisons were made between naturally forming trabecular bone (control) and defects implanted with scaffolds fabricated with micro-size (M-HA) and nano-size HA (N-HA) ceramic surfaces. Scaffold architecture was similar to trabecular bone formed in control defects at 3 weeks. No significant differences were identified between the two HA scaffolds; however, significant bone in-growth was observed by 12 weeks with 43.9 +/- 4.1% and 50.4 +/- 8.8% of the cross-sectional area filled with mineralized bone in M-HA and N-HA scaffolds, respectively. Partially organized, lamellar collagen fibrils were identified by birefringence under cross-polarized light at both 3 and 12 weeks post implantation. Substantial blood vessel infiltration was identified in the scaffolds and compared with the distribution and diameter of vessels in the surrounding cortical bone. Vessels were less numerous but significantly larger than native cortical Haversian and Volkmann canals reflecting the scaffold architecture where open spaces allowed interconnected channels of bone to form. This study demonstrated the potential of trabecular bone modeled, highly porous and interconnected, HA scaffolds for regenerative orthopedics. PMID:18478555

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

    PubMed

    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

  10. Increased osteoblast adhesion on nanograined hydroxyapatite and tricalcium phosphate containing calcium titanate.

    PubMed

    Ergun, Celaletdin; Liu, Huinan; Halloran, John W; Webster, Thomas J

    2007-03-15

    Depending on the coating method utilized and subsequent heat treatments (such as through the use of plasma-spray deposition), inter-diffusion of atomic species across titanium (Ti) and hydroxyapatite (HA) coatings may result. These events may lead to structural and compositional changes that consequently cause unanticipated HA phase transformations which may clearly influence the performance of an orthopedic implant. Thus, the objective of the present in vitro study was to compare the cytocompatibility properties of chemistries that may form at the Ti:HA interface, specifically HA, tricalcium phosphate (TCP), HA doped with Ti, and those containing calcium titanate (CaTiO(3)). In doing so, results of this study showed that osteoblast (bone-forming cells) adhesion increased with greater CaTiO(3) substitutions in either HA or TCP. Specifically, osteoblast adhesion on HA and TCP composites with CaTiO(3) was almost 4.5 times higher than that over pure HA. Material characterization studies revealed that enhanced osteoblast adhesion on these compacts may be due to increasing shrinkage in the unit lattice parameters and decreasing grain size. Although all CaTiO(3) composites exhibited excellent osteoblast adhesion results, Ca(9)HPO(4)(PO(4))(5)OH phase transformation into TCP/CaTiO(3) increased osteoblast adhesion the most; because of these reasons, these materials should be further studied for orthopedic applications. PMID:17120201

  11. Functionalization of polycaprolactone/hydroxyapatite scaffolds with Usnea lethariiformis extract by using supercritical CO2.

    PubMed

    Fanovich, M A; Ivanovic, J; Zizovic, I; Misic, D; Jaeger, P

    2016-01-01

    Investigation of an integrated supercritical fluid extraction and supercritical solvent impregnation process for fabrication of microporous polycaprolactone-hydroxyapatite (PCL-HA) scaffolds with antibacterial activity is presented. The HA content and particle size as well as the operating conditions of the integrated process is optimized regarding the amount of impregnated antibacterial agent (Usnea lethariiformis extract) in the PCL-HA matrix, scaffold morphology and antibacterial activity against methicillin resistant Staphylococcus aureus (MRSA) strains. High pressure differential scanning calorimetry (HP-DSC) assay reveals that an increasing amount of HA results in decreasing melting temperature as well as crystallinity at an operating pressure of 17 MPa. The PCL-HA composites with micrometric sizes of the HA particles are convenient for being processed by the integrated process due to the simple preparation, a good interaction between the PCL matrix and filler and the advantageous impact on sorption. The scaffold obtained from PCL-HA with 20% of the HA shows the highest impregnation yield at 17 MPa and 35 °C (5.9%) and subsequently also the best bactericidal effect on the tested MRSA strains at an initial bacterial inoculum of 2 × 10(-4)CFU/mL. PMID:26478304

  12. Composite nanofiber mats consisting of hydroxyapatite and titania for biomedical applications.

    PubMed

    Kim, Hong Mi; Chae, Won-Pyo; Chang, Ki-Whan; Chun, Sungsu; Kim, Sukyoung; Jeong, Yongsoo; Kang, Inn-Kyu

    2010-08-01

    Composite nanofiber mats (HA/TiO2) consisting of hydroxyapatite (HA) and titania (TiO2) were fabricated via an electrospinning technique and then collagen (type I) was immobilized on the surface of the HA/TiO2 composite nanofiber mat to improve tissue compatibility. The structure and morphology of the collagen-immobilized composite nanofiber mat (HA/TiO2-col) was investigated using an X-ray diffractometer, electron spectroscopy for chemical analysis, and scanning electron microscope. The potential of the HA/TiO2-col composite nanofiber mat for use as a bone scaffold was assessed by an experiment with osteoblastic cells (MC3T3-E1) in terms of cell adhesion, proliferation, and differentiation. The results showed that the HA/TiO2-col composite nanofiber mats possess better cell adhesion and significantly higher proliferation and differentiation than untreated HA/TiO2 composite nanofiber mats. This result suggests that the HA/TiO2-col composite nanofiber mat has a high-potential for use in the field of bone regeneration and tissue engineering. PMID:20574975

  13. Effect of highly dispersed yttria addition on thermal stability of hydroxyapatite.

    PubMed

    Parente, P; Savoini, B; Ferrari, B; Monge, M A; Pareja, R; Sanchez-Herencia, A J

    2013-03-01

    The capability of the colloidal method to produce yttria (Y(2)O(3)) dispersed hydroxyapatite (HA) has been investigated as an alternative method to the conventional method of mechanical mixing and sintering for developing HA-based materials that could exhibit controllable and enhanced functional properties. A water based colloidal route to produce HA materials with highly dispersed Y(2)O(3) has been applied, and the effect of 10 wt.% Y(2)O(3) addition to HA investigated by thermal analysis, X-ray diffraction and Fourier transform infrared spectroscopy. These measurements evidence a remarkable effect of this Y(2)O(3) addition on decomposition mechanisms of synthetic HA. Results show that incorporation of Y(2)O(3) as dispersed second phase is beneficial because it hinders the decomposition mechanisms of HA into calcium phosphates. This retardation will allow the control of the sintering conditions for developing HA implants with improved properties. Besides, substitution of Ca(2+) with Y(3+) ions appears to promote the formation of OH(-) vacancies, which could improve the conductive properties of HA favorable to osseointegration. PMID:25427499

  14. X-ray peak broadening studies of nanocrystalline hydroxyapatite by Williamson-Hall analysis

    NASA Astrophysics Data System (ADS)

    Venkateswarlu, K.; Chandra Bose, A.; Rameshbabu, N.

    2010-10-01

    Hydroxyapatite (HA) nanoparticles were prepared by microwave synthesis method and the obtained powder is annealed at 800 °C for 2 h. The annealed HA particles were characterized by X-ray diffraction (XRD) and Fourier transform infrared (FTIR) spectroscopy methods. The HA size and morphology were examined using a transmission electron microscope (TEM). The XRD results reveal that the diffraction peaks of the annealed HA were of well crystalline and correspond to the hexagonal crystal structure. The XRD and FTIR results confirm the absence of secondary phases such as β-tricalcium phosphate (β-TCP) and calcium oxide in annealed HA particles. The TEM result confirms the hexagonal structure of annealed HA and the particles were observed to be of ellipsoid-like shaped morphology with less agglomeration. The lattice strain, crystallite size, lattice deformation stress and deformation energy density for annealed (800 °C) HA nanoparticles were estimated by Williamson-Hall-isotropic strain model ( W- H-ISM), W-H-anisotropic strain model ( W- H-ASM) and W-H-energy density model ( W- H-EDM) based on Williamson-Hall ( W- H) plot from powder X-ray diffraction data. The results of estimated average crystallite size of annealed HA by Scherrer and W- H plot methods were compared with TEM results. It is found that the average crystallite size measured by W- H plot methods is in good agreement with TEM results.

  15. Hydroxyapatite coatings with oriented nanoplate and nanorod arrays: Fabrication, morphology, cytocompatibility and osteogenic differentiation.

    PubMed

    Chen, Wei; Tian, Bo; Lei, Yong; Ke, Qin-Fei; Zhu, Zhen-An; Guo, Ya-Ping

    2016-10-01

    Hydroxyapatite (HA) crystals exhibit rod-like shape with c-axis orientation and plate-like shape with a(b)-axis orientation in vertebrate bones and tooth enamel surfaces, respectively. Herein, we report the synthesis of HA coatings with the oriented nanorod arrays (RHACs) and HA coatings with oriented nanoplate arrays (PHACs) by using bioglass coatings as sacrificial templates. After soaking in simulated body fluid (SBF) at 120°C, the bioglass coatings are hydrothermally converted into the HA coatings via a dissolution-precipitation reaction. If the Ca/P ratios in SBF are 2.50 and 1.25, the HA crystals on the coatings are oriented nanorod arrays and oriented nanoplate arrays, respectively. Moreover, the bioglass coatings are treated with SBF at 37°C, plate-like HA coatings with a low crystallinity (SHACs) are prepared. As compared with the Ti6Al4V and SHACs, the human bone marrow stromal cells (hBMSCs) on the RHACs and PHACs have better cell adhesion, spreading, proliferation and osteogenic differentiation because of their moderately hydrophilic surfaces and similar chemical composition, morphology and crystal orientation to human hard tissues. Notably, the morphologies of HA crystals have no obvious effects on cytocompatibility and osteogenic differentiation. Hence, the HA coatings with oriented nanoplate arrays or oriented nanorod arrays have a great potential for orthopedic applications. PMID:27287136

  16. 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

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

    PubMed

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

    2015-07-01

    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

  18. Hydroxyapatite-coated polyurethane for auricular cartilage replacement: an in vitro study.

    PubMed

    Chetty, Avashnee; Steynberg, Tenille; Moolman, Sean; Nilen, Roger; Joubert, Annie; Richter, Wim

    2008-02-01

    Auricular reconstruction remains a major challenge facing reconstructive surgeons owing to the complexity of autogenous transplants. In this study, the development of a three-dimensional custom-made polyurethane (PU) auricular implant with hydroxyapatite (HA) coating is described. The PU implant was produced by computerized tomography (CT) scanning and indirect rapid prototyping. To improve the physiological response of the implant, the PU prototype was coated with a microrough, homogenous layer of HA by a novel solvent-compression coating method. Bioactivity of the HA coated PU substrates was confirmed by apatite formation on the HA coating after 9 days in revised simulated body fluid (pH 7.4). Adhesion strength of the HA coating to the PU surface using the tensile pull-off test revealed partial failure of the coating with an average tensile strength of 1.6 MPa. As an initial stage indication of cytocompatibility for a soft tissue application, in vitro cell culturing on the HA-coated PU substrates using Graham 293 fibroblast cells was performed. After 24 and 72 h, the HA coated surfaces displayed significantly higher cell numbers and metabolically active cells compared with the virgin uncoated PU surfaces. This indicates that HA coated PU surfaces are cytocompatible towards fibroblasts and could potentially be applied to auricular cartilage tissue replacement. PMID:17618497

  19. Characterization of gas tunnel type plasma sprayed hydroxyapatite-nanostructure titania composite coatings

    NASA Astrophysics Data System (ADS)

    Yugeswaran, S.; Kobayashi, A.; Ucisik, A. Hikmet; Subramanian, B.

    2015-08-01

    Hydroxyapatite (HA) can be coated onto metal implants as a ceramic biocompatible coating to bridge the growth between implants and human tissue. Meanwhile many efforts have been made to improve the mechanical properties of the HA coatings without affecting its bioactivity. In the present study, nanostructure titania (TiO2) was mixed with HA powder and HA-nanostructure TiO2 composite coatings were produced by gas tunnel type plasma spraying torch under optimized spraying conditions. For this purpose, composition of 10 wt% TiO2 + 90 wt% HA, 20 wt% TiO2 + 80 wt% HA and 30 wt% TiO2 + 70 wt% HA were selected as the feedstock materials. The phase, microstructure and mechanical properties of the coatings were characterized. The obtained results validated that the increase in weight percentage of nanostructure TiO2 in HA coating significantly increased the microhardness, adhesive strength and wear resistance of the coatings. Analysis of the in vitro bioactivity and cytocompatibility of the coatings were done using conventional simulated body fluid (c-SBF) solution and cultured green fluorescent protein (GFP) labeled marrow stromal cells (MSCs) respectively. The bioactivity results revealed that the composite coating has bio-active surface with good cytocompatibility.

  20. Electrolytic deposition of hydroxyapatite coating on thermal treated Ti-40Zr.

    PubMed

    Hsu, Hsueh-Chuan; Wu, Shih-Ching; Lin, Chih-Hung; Ho, Wen-Fu

    2009-09-01

    In this study, hydroxyapatite (HA) was coated on both thermal treated and untreated Ti-40Zr substrates by means of electrolytic deposition. It was predicted that the HA layer would increase the bioactivity and osteoconductivity of the Ti-40Zr substrate, and a thermal treatment would improve the bonding strength between the HA layer and Ti-40Zr substrate, and prevent the corrosion of the Ti-40Zr substrate. First, the Ti-40Zr samples were annealed at various temperatures (200, 300, 400, 500 and 600 degrees C respectively). After annealing, samples were immersed in a Ca(NO(3))(2).4H(2)O and (NH(4))(3)PO(4).3H(2)O solution for the electrolytic deposition of the HA coating. Various analyses of the coating were conducted, including surface morphology, phase structure, corrosion resistance, biocompatibility, and bond strength between HA and Ti-40Zr. Experimental results indicated that the bonding strength of the HA coating on the thermal treated Ti-40Zr was markedly improved when compared to that of the HA coating on an untreated Ti-40Zr alloy. The corrosion resistance of Ti-40Zr was also improved by the use of the thermal treatment, as shown by a potentiodynamic polarization test. Finally, osteoblast-like cells cultured on the HA coating surface were found to have proliferated on all samples. PMID:19404722

  1. Increase of stability in external fracture fixation by hydroxyapatite-coated bone screws.

    PubMed

    Augat, P; Claes, L; Hanselmann, K F; Suger, G; Fleischmann, W

    1995-01-01

    A major problem in fracture treatment by external fixation is screw loosening, which often results in reduced stability and can lead to prolonged treatment. A load-carrying experiment was conducted to determine whether coating implants with bioactive hydroxyapatite (HA) increases screw stability. Twelve HA-coated ASIF screws with 3 different macroporosities were inserted in 12 sheep that had already been fitted with a 6-pin external fixator for the treatment of a tibial osteotomy. The same number of uncoated polished steel screws served as controls. Although initial stability was not different for HA-coated screws, average removal torque after a 9-week implantation period increased with increasing macroporosity of the HA coating (p < .002). Instability of some screws was accompanied by histologic findings of cartilagenous tissue and proliferation of periosteal callus. Near the threads in the tibial cortex and in the shaft area of the screw were seen large numbers of HA particles that had been sheared off during implantation as well as during screw removal because of high contact forces between the HA coating and bone. Particulate debris of HA particles as well as the release of small bone fragments during explanation is likely to be unavoidable since HA adherence to bone is greater than adherence to steel after several weeks of implantation. PMID:7640445

  2. 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. PMID:26916949

  3. 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

  4. Effect of gun current on the microstructure and crystallinity of plasma sprayed hydroxyapatite coatings

    NASA Astrophysics Data System (ADS)

    Morks, M. F.; Kobayashi, A.

    2007-06-01

    Hydroxyapatite (HA) is a bioactive material because its chemical structure is close to the natural bone. Its bioactive properties make it attractive material in biomedical applications. Gas tunnel type plasma spraying (GTPS) technique was employed in the present study to deposit HA coatings on SUS 304 stainless steel substrate. GTPS is composed of two plasma sources: gun which produces internal low power plasma (1.3-8 kW) and vortex which produces the main plasma with high power level (10-40 kW). Controlling the spraying parameters is the key role for spraying high crystalline HA coatings on the metallic implants. In this study, the arc gun current was changed while the vortex arc current was kept constant at 450 A during the spraying process of HA coatings. The objective of this study is to investigate the influence of gun current on the microstructure, phase crystallinity and hardness properties of HA coatings. The surface morphology and microstructure of as-sprayed coatings were examined by scanning electron microscope. The phase structure of HA coatings was investigated by X-ray diffraction analysis. HA coatings sprayed at high gun current (100 A) are dense, and have high hardness. The crystallinity of HA coatings was decreased with the increasing in the gun current. On the other hand, the hardness was slightly decreased and the coatings suffer from some porosity at gun currents 0, 30 and 50 A.

  5. Development of metal/hydroxyapatite composite surface coatings. Ph.D. Thesis

    SciTech Connect

    Dasarathy, H.

    1992-01-01

    Metal/ceramic composites containing calcium phosphates have shown considerable success in enhancing bone growth into implants, thereby providing cementless fixation. Calcium phosphate occurs in various phases. The extent of compatibility of the composites to the hosts depend upon the phase of the calcium phosphate. A crystalline phase known as hydroxyapatite (HA) which naturally occurs in bones and teeth of animals has proved to enhance bone growth. This work involved development of a composite that will retain both the biological properties of HA and the mechanical properties of the metal. In this method, HA was codeposited electrolytically on a metal substrate in a metal matrix to provide adequate adhesion to the substrate. Codeposited HA on the surface was characterized using FTIR and Raman spectroscopy to ensure that HA structure remained unaltered throughout the conditions employed during the process. The development of the composite was carried out in two phases. Phase 1 consisted of codeposition of HA in a single metal matrix, characterization of HA and testing the viability of the process to all substrate geometry. In the second phase, a process was developed to electrolytically deposit cobalt, chromium, molybdenum alloy (vitallium) and then codeposit HA in that alloy matrix on substrates. The plated alloy was characterized by x-ray photoelectron spectroscopy, x-ray diffraction, energy dispersive spectroscopy and compared with similar analyses for cast vitallium alloy. The deposited alloy was also tested for corrosion and substrate adhesion.

  6. Substituted Hydroxyapatites with Antibacterial Properties

    PubMed Central

    Kolmas, Joanna; Groszyk, Ewa; Kwiatkowska-Różycka, Dagmara

    2014-01-01

    Reconstructive surgery is presently struggling with the problem of infections located within implantation biomaterials. Of course, the best antibacterial protection is antibiotic therapy. However, oral antibiotic therapy is sometimes ineffective, while administering an antibiotic at the location of infection is often associated with an unfavourable ratio of dosage efficiency and toxic effect. Thus, the present study aims to find a new factor which may improve antibacterial activity while also presenting low toxicity to the human cells. Such factors are usually implemented along with the implant itself and may be an integral part of it. Many recent studies have focused on inorganic factors, such as metal nanoparticles, salts, and metal oxides. The advantages of inorganic factors include the ease with which they can be combined with ceramic and polymeric biomaterials. The following review focuses on hydroxyapatites substituted with ions with antibacterial properties. It considers materials that have already been applied in regenerative medicine (e.g., hydroxyapatites with silver ions) and those that are only at the preliminary stage of research and which could potentially be used in implantology or dentistry. We present methods for the synthesis of modified apatites and the antibacterial mechanisms of various ions as well as their antibacterial efficiency. PMID:24949423

  7. Hydrogel microspheres for stabilization of an antioxidant enzyme: effect of emulsion cross-linking of a dual polysaccharide system on the protection of enzyme activity.

    PubMed

    Tang, Deh-Wei; Yu, Shu-Huei; Wu, Wen-Shin; Hsieh, Hao-Ying; Tsai, Yi-Chin; Mi, Fwu-Long

    2014-01-01

    Catalase is an antioxidant enzyme abundant in natural resources. However, the enzyme is usually inactivated by gastric acid and digestive enzymes after oral ingestion. In this study, carboxymethyl chitosan (CM-chitosan) and hyaluronic acid (HA) conjugate hydrogel microspheres have been prepared by an emulsion cross-linking technique to retain the activity of catalase in simulated gastrointestinal (GI) fluids. Cross-linking reduced the swelling capability and increased the resistance toward hyaluronidase digestion of prepared HA-CM-chitosan hydrogel microspheres. Catalase entrapped in the hydrogel microspheres exhibited superior stability over a wide pH range (pH 2.0 and 6.0-8.0) as compared to the native enzyme. The entrapped catalase was also protected against degradation by digestive enzymes. Following the treatments, the catalase-loaded microspheres, in contrast to native catalase, could effectively decrease the intracellular H2O2 level and protect HT-29 colonic epithelial cells against H2O2-induced oxidative damage to preserve cell viability. These results suggested that the HA-CM-chitosan hydrogel microspheres can be used for entrapment, protection and intestinal delivery of catalase for H2O2 scavenging. PMID:24055882

  8. Characteristic of microarc oxidized coatings on titanium alloy formed in electrolytes containing chelate complex and nano-HA

    NASA Astrophysics Data System (ADS)

    Wei, Daqing; Zhou, Yu; Wang, Yaming; Jia, Dechang

    2007-03-01

    Microarc oxidized (MAO) TiO 2-based coatings containing Ca and P on titanium alloy were formed in electrolytes containing nano-hydroxyapatite (nano-HA), calcium and phosphate salts. The effects of HA concentration on the thickness, micropore size and number of the MAO coatings were not pronounced. However, the surfaces of the MAO coatings become rough and the crystallinity of anatase increases with increasing HA concentration. In addition, the Ca and P concentrations on the surfaces of the MAO coatings decrease, since the chelate complex of CaY 2- (Y = [ 2(OOC)NCH 2CH 2N(COO) 2] 4-) and phosphate ions are hindered to be incorporated into the MAO coatings by HA. In vitro experiments indicate that the apatite-forming abilities of the MAO coatings decrease with increasing HA concentration. Furthermore, with increasing HA concentration, the solubility of Ca and P of the MAO coatings decreases, which could lower the supersaturation of the SBF with respect to apatite near the surfaces of the MAO coatings, further leading to the decreased apatite-forming ability. The results indicate that the HA addition in the electrolytes has an important effect on the structure and in vitro bioactivity of the MAO coatings.

  9. Microwave assisted synthesis of nano sized sulphate doped hydroxyapatite

    SciTech Connect

    Alshemary, Ammar Z.; Goh, Yi-Fan; Akram, Muhammad; Razali, Ili Rabihah; Abdul Kadir, Mohammed Rafiq; Hussain, Rafaqat

    2013-06-01

    Highlights: ► Phase pure nano-sized sulphur doped hydroxyapatite has been synthesized. ► TEM analysis confirmed formation of needle shaped structure. ► Lattice parameters and cell volume increased with increase in sulphate doping. ► Crystallite size decreased as sulphate content inside the structure increased. ► Degree of crystallinity decreased with increase in sulphate substitution. - Abstract: Inorganic sulphate is required by all mammalian cells to function properly, it is the fourth most abundant anion in the human plasma. Sulphate ions are the major source of sulphur which is considered an important element for sustenance of life as it is present in the essential amino and is required by cells to function properly. In this study we have successfully substituted sulphate ions (SO{sub 4}{sup 2−}) into hydroxyapatite (Ca{sub 10}(PO{sub 4}){sub 6−x}(SO{sub 4}){sub x}(OH){sub 2−x}) lattice via ion exchange process with phosphate group. Concentration of SO{sub 4}{sup 2−} ions was varied between X = 0.05–0.5, using (Ca (NO{sub 3}){sub 2}·4H{sub 2}O), ((NH{sub 4}){sub 2}HPO{sub 4}) and (Na{sub 2}SO{sub 4}) as starting materials. X-ray diffraction (XRD), Fourier transform IR spectroscopy (FTIR), showed that the substitution of SO{sub 4}{sup 2−} ions into the lattice resulted in peak broadening and reduced peak height due to the amorphous nature and reduced crystallinity of the resulting HA powder. Transmission electron microscopy (TEM) and field emission electron microscopy (FESEM) analysis confirmed the formation of needle shaped particles of 41 nm size with homogenous and uniform distribution of element within the HA structure.

  10. Investigation of the HA film deposited on the porous Ti6Al4V alloy prepared via additive manufacturing

    NASA Astrophysics Data System (ADS)

    Surmeneva, M.; Chudinova, E.; Syrtanov, M.; Koptioug, A.; Surmenev, R.

    2015-11-01

    This study is focused on the use of radio frequency magnetron sputtering to modify the surface of porous Ti6Al4V alloy fabricated via additive manufacturing technology. The hydroxyapatite (HA) coated porous Ti6Al4V alloy was studied in respect with its chemical and phase composition, surface morphology, water contact angle and hysteresis, and surface free energy. Thin nanocrystalline HA film was deposited while its structure with diamond-shaped cells remained unchanged. Hysteresis and water contact angle measurements revealed an effect of the deposited HA films, namely an increased water contact angle and contact angle hysteresis. The increase of the contact angle of the coating-substrate system compared to the uncoated substrate was attributed to the multiscale structure of the resulted surfaces.

  11. Effect of loading time on marginal bone loss around hydroxyapatite-coated implants

    PubMed Central

    Kim, Young-Kyun; Ahn, Kyo-Jin; Yun, Pil-Young; Kim, Minkyoung; Yang, Hong-So; Yi, Yang-Jin

    2013-01-01

    Objectives The objective of this study is compare the rate of marginal bone resorption around hydroxyapatite-coated implants given different loading times in order to evaluate their stability. Materials and Methods The study was conducted retrospectively for one year, targeting 41 patients whose treatment areas were the posterior maxilla and the mandible. Osstem TS III HA (Osstem Implant Co., Busan, Korea) and Zimmer TSV-HA (Zimmer Dental, Carlsbad, CA, USA), which employ the new hydroxyapatite coating technique, were used. The patients were divided into two groups - immediate and delayed loading - and the bone level at the time of loading commencement and after one year of loading was measured using periapical radiography. Differences between the groups were evaluated using Mann-Whitney (α=0.05). Results For all patients as a single group, the survival rate of the implants was 100%, and the mean marginal bone loss was 0.26±0.59 mm. In comparison of the differences by loading, mean marginal bone loss of 0.32±0.69 mm was recorded for the immediate loading group whereas the delayed loading group had mean marginal bone loss of 0.16±0.42 mm. However, the difference was not significant (P>0.05). Conclusion Within the limited observation period of one year, predictable survival rates can be expected when using immediately loaded hydroxyapatite-coated implants. PMID:24471037

  12. 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. PMID:26652351

  13. Diffusion Flame Synthesis of Hydroxyapatite Nanoparticles using Urea Assisted Precursor Solution

    NASA Astrophysics Data System (ADS)

    Widiyastuti; Setiawan, Adhi; Setyawan, Heru; Kusdianto; Nurtono, Tantular; Nia, Suci Madha; Winardi, Sugeng

    2011-12-01

    Hydroxyapatite (HA) or (Ca10(PO4)6(OH)2 has been widely used in orthopedics and dental applications for human bone implant and teeth filler due to their biocompatibility and osteoconductive properties. Fine to nanoparticles of HA with appropriate stoichiometry and purity are preferred because they enhance densification and bioactive properties. Here, we reported the synthesis of hydroxyapatite particles in a diffusion flame reactor. LPG mainly consisting of butane and propane was used as fuel and compressed air was used as oxidizer and carrier gas. The effects of urea adding into precursor on morphology and crystallinity of the generated particles were investigated. Scanning electron microscopy (SEM) and X-ray diffraction (XRD) were used to observe particles morphology and crystallinity, respectively. Purity of the generated particles was analyzed quantitatively from XRD pattern using Rietveld method. Spherical shape of particles morphology was obtained for particles synthesized without urea added into precursor. Increasing fuel flow rate and urea concentration led to further disintegration of the generated particles. Nano sized particles were generated using fuel flow rate of 1 L/min and 30 w% concentration of urea added into precursor. However, increasing urea concentration led to the increase of tricalcium phosphate as a further reaction of hydroxyapatite for flame generated by using LPG as fuel of 1 L/min.

  14. Hydroxyapatite surface modified by L-lactic acid and its subsequent grafting polymerization of L-lactide.

    PubMed

    Qiu, Xueyu; Hong, Zhongkui; Hu, Junli; Chen, Li; Chen, Xuesi; Jing, Xiabin

    2005-01-01

    A new method of surface modification of hydroxyapatite nanoparticles (n-HA) by surface grafting reaction of l-lactic acid and ring-opening polymerization of l-lactide (LLA) was developed. Two modified HA nanoparticles were obtained: HA modified by l-lactic acid (l-HA) and HA grafting with poly(l-lactide) (PLLA; p-HA). The modified surface of n-HA was attested by Fourier transformation infrared, (31)P MAS NMR, and thermal gravimetric analysis. The results showed that l-lactic acid could be easily grafted onto the n-HA surface by forming a Ca carboxylate bond and initiated by the hydroxyl group of the grafted l-lactic acid and LLA could be graft-polymerized onto the n-HA surface in the presence of stannous octanoate. The highest grafting amounts of l-lactic acid and PLLA were about 33 and 22 wt %, respectively. The modified HA/PLLA composites showed good mechanical properties and uniform microstructure. The tensile strength and modulus of the p-HA/PLLA composite containing 15 wt % of p-HA were 67 MPa and 2.1 GPa, respectively, while those of the n-HA/PLLA composites were 45 MPa and 1.7 GPa, respectively. The elongation at the break of the l-HA/PLLA composite containing 15 wt % l-HA could reach 44%, in comparison with 6.5% of the n-HA/PLLA composites containing 15 wt % n-HA. PMID:15877333

  15. 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

  16. Titania-hydroxyapatite nanocomposite coatings support human mesenchymal stem cells osteogenic differentiation.

    PubMed

    Dimitrievska, Sashka; Bureau, Martin N; Antoniou, John; Mwale, Fackson; Petit, Alain; Lima, Rogerio S; Marple, Basil R

    2011-09-15

    In addition to mechanical and chemical stability, the third design goal of the ideal bone-implant coating is the ability to support osteogenic differentiation of mesenchymal stem cells (MSCs). Plasma-sprayed TiO(2)-based bone-implant coatings exhibit excellent long-term mechanical properties, but their applications in bone implants are limited by their bioinertness. We have successfully produced a TiO(2) nanostructured (grain size <50 nm) based coating charged with 10% wt hydroxyapatite (TiO(2)-HA) sprayed by high-velocity oxy-fuel. On Ti64 substrates, the novel TiO(2)-HA coating bond 153× stronger and has a cohesive strength 4× higher than HA coatings. The HA micro- and nano-sized particles covering the TiO(2)-HA coating surface are chemically bound to the TiO(2) coating matrix, producing chemically stable coatings under high mechanical solicitations. In this study, we elucidated the TiO(2)-HA nanocomposite coating surface chemistry, and in vitro osteoinductive potential by culturing human MSCs (hMSCs) in basal and in osteogenic medium (hMSC-ob). We assessed the following hMSCs and hMSC-ob parameters over a 3-week period: (i) proliferation; (ii) cytoskeleton organization and cell-substrate adhesion; (iii) coating-cellular interaction morphology and growth; and (iv) cellular mineralization. The TiO(2) -HA nanocomposite coatings demonstrated 3× higher hydrophilicity than HA coatings, a TiO(2)-nanostructured surface in addition to the chemically bound HA micron- and nano-sized rod to the surface. hMSCs and hMSC-ob demonstrated increased proliferation and osteoblastic differentiation on the nanostructured TiO(2)-HA coatings, suggesting the TiO(2)-HA coatings nanostructure surface properties induce osteogenic differentiation of hMSC and support hMSC-ob osteogenic potential better than our current golden standard HA coating. PMID:21702080

  17. 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

  18. Hydroxyapatite porous scaffold engineered with biological polymer hybrid coating for antibiotic Vancomycin release.

    PubMed

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

    2005-03-01

    The purpose of this study is to improve hydroxyapatite (HA) porous scaffolds via coating with biological polymer-HA hybrids for use as wound healing and tissue regeneration. Highly porous HA scaffolds, fabricated by a polyurethane foam reticulate method, were coated with hybrid coating solution, consisting of poly(epsilon-caprolactone) (PCL), HA powders, and the antibiotic Vancomycin. The PCL to HA ratio was fixed at 1.5 and the drug amounts were varied [drug/(PCL + HA) = 0.02 and 0.04]. For the purpose of comparison, bare HA scaffold without the hybrid coating layer was also loaded with Vancomycin via an immersion-adsorption method. The hybrid coating structure and morphology were observed with Fourier transformed infrared (FT-IR) spectroscopy and scanning electron microscopy (SEM). The effects of the hybrid coating on the compressive mechanical properties and the in vitro drug release of the scaffolds were investigated in comparison with bare HA scaffold. The PCL-HA hybrid coating altered the scaffold pore structure slightly, resulting in thicker stems and reduced porosity. With the hybrid coating, the HA scaffold responded to an applied compressive stress more effectively without showing a brittle failure. This was attributed to the shielding and covering of the framework surface by the coating layer. The encapsulated drugs within the coated scaffold was released in a highly sustained manner as compared to the rapid release of drugs directly adsorbed on the pure HA scaffold. These findings suggest that the coated HA scaffolds expand their applicability in hard tissue regeneration and wound healing substitutes delivering bioactive molecules. PMID:15744609

  19. 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

    2015-08-01

    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. PMID:26179911

  20. Development of nano-sized hydroxyapatite reinforced composites for tissue engineering scaffolds.

    PubMed

    Huang, Jie; Lin, Yu Wan; Fu, Xiao Wei; Best, Serena M; Brooks, Roger A; Rushton, Neil; Bonfield, William

    2007-11-01

    Nano-sized hydroxyapatite (nanoHA) reinforced composites, mimicking natural bone, were produced. Examination by transmission electron microscopy revealed that the nanoHA particles had a rod-like morphology, 20-30 nm in width and 50-80 nm in length. The phase composition of hydroxyapatite was confirmed by X-ray diffraction. The nanoHA particles were incorporated into poly-2-hydroxyethylmethacrylate (PHEMA)/polycaprolactone (PCL) matrix to make new nanocomposites: nanoHA-PHEMA/PCL. Porous nanocomposite scaffolds were then produced using a porogen leaching method. The interconnectivity of the porous structure of the scaffolds was revealed by non-destructive X-ray microtomography. Porosity of 84% was achieved and pore sizes were approximately around 300-400 microm. An in vitro study found that the nanocomposites were bioactive as indicated by the formation of a bone-like apatite layer after immersion in simulated body fluid. Furthermore, the nanocomposites were able to support the growth and proliferation of primary human osteoblast (HOB) cells. HOB cells developed a well organized actin cytoskeletal protein on the nanocomposite surface. The results demonstrate the potential of the nanocomposite scaffolds for tissue engineering applications for bone repair. PMID:17891551

  1. Effect of Hydroxyapatite porous characteristics on healing outcomes in rabbit posterolateral spinal fusion model.

    PubMed

    Motomiya, Makoto; Ito, Manabu; Takahata, Masahiko; Kadoya, Ken; Irie, Kazuharu; Abumi, Kuniyoshi; Minami, Akio

    2007-12-01

    Hydroxyapatite (HA) has been commonly used as a bone graft substitute in various kinds of clinical fields. To improve the healing capability of HA, many studies have been performed to reveal its optimal structural characteristics for better healing outcomes. In spinal reconstruction surgery, non-interconnected porous HAs have already been applied as a bone graft extender in order to avoid autogenous bone harvesting. However, there have been few experimental studies regarding the effects of the structural characteristics of HA in posterolateral lumbar intertransverse process spine fusion (PLF). The aims of this study were to investigate the effect of HA porous characteristics on healing outcomes in a rabbit PLF model in order to elucidate appropriate structural characteristics of HA as a bone graft extender. Thirty-six adult female Japanese White rabbits underwent bilateral intertransverse process fusion at the level of L5-6 without internal fixation. We prepared three types of HA with different porosities: HA with 15% porosity (HA15%), HA with 50% porosity (HA50%), and HA with 85% porosity (HA85%), all of which were clinically available materials. The HA15% and HA50% had few interconnecting pores, whereas the HA85%, which was a recently developed material, had abundant interconnecting pores. All rabbits were randomly divided into the following four groups according to the grafted materials: (1) HA15% + autogenous bone, (2) HA50% + autogenous bone, (3) HA85% + autogenous bone, (4) pure autogenous bone graft. The animals were euthanized at 5 weeks after surgery, and post-mortem analyses including biomechanical testing, radiographical and histological evaluations were performed. There was no statistically significant difference in either fusion rate and/or bending stiffness among the three HA groups. However, in histological and radiological analyses, both bone ingrowth rate and direct bone bonding rate in the HA85% group were significantly higher than those in the HA

  2. Electrospinning Growth Factor Releasing Microspheres into Fibrous Scaffolds

    PubMed Central

    Whitehead, Tonya J.; Sundararaghavan, Harini G.

    2014-01-01

    This procedure describes a method to fabricate a multifaceted substrate to direct nerve cell growth. This system incorporates mechanical, topographical, adhesive and chemical signals. Mechanical properties are controlled by the type of material used to fabricate the electrospun fibers. In this protocol we use 30% methacrylated Hyaluronic Acid (HA), which has a tensile modulus of ~500 Pa, to produce a soft fibrous scaffold. Electrospinning on to a rotating mandrel produces aligned fibers to create a topographical cue. Adhesion is achieved by coating the scaffold with fibronectin. The primary challenge addressed herein is providing a chemical signal throughout the depth of the scaffold for extended periods. This procedure describes fabricating poly(lactic-co-glycolic acid) (PLGA) microspheres that contain Nerve Growth Factor (NGF) and directly impregnating the scaffold with these microspheres during the electrospinning process. Due to the harsh production environment, including high sheer forces and electrical charges, protein viability is measured after production. The system provides protein release for over 60 days and has been shown to promote primary nerve cell growth. PMID:25178038

  3. Precision Extruding Deposition for Freeform Fabrication of PCL and PCL-HA Tissue Scaffolds

    NASA Astrophysics Data System (ADS)

    Shor, L.; Yildirim, E. D.; Güçeri, S.; Sun, W.

    Computer-aided tissue engineering approach was used to develop a novel Precision Extrusion Deposition (PED) process to directly fabricate Polycaprolactone (PCL) and composite PCL/Hydroxyapatite (PCL-HA) tissue scaffolds. The process optimization was carried out to fabricate both PCL and PCL-HA (25% concentration by weight of HA) with a controlled pore size and internal pore structure of the 0°/90° pattern. Two groups of scaffolds having 60 and 70% porosity and with pore sizes of 450 and 750 microns, respectively, were evaluated for their morphology and compressive properties using Scanning Electron Microscopy (SEM) and mechanical testing. The surface modification with plasma was conducted on PCL scaffold to increase the cellular attachment and proliferation. Our results suggested that inclusion of HA significantly increased the compressive modulus from 59 to 84 MPa for 60% porous scaffolds and from 30 to 76 MPa for 70% porous scaffolds. In vitro cell-scaffolds interaction study was carried out using primary fetal bovine osteoblasts to assess the feasibility of scaffolds for bone tissue engineering application. In addition, the results in surface hydrophilicity and roughness show that plasma surface modification can increase the hydrophilicity while introducing the nano-scale surface roughness on PCL surface. The cell proliferation and differentiation were calculated by Alamar Blue assay and by determining alkaline phosphatase activity. The osteoblasts were able to migrate and proliferate over the cultured time for both PCL as well as PCL-HA scaffolds. Our study demonstrated the viability of the PED process to the fabricate PCL and PCL-HA composite scaffolds having necessary mechanical property, structural integrity, controlled pore size and pore interconnectivity desired for bone tissue engineering.

  4. No medium-term advantage of electrochemical deposition of hydroxyapatite in cementless femoral stems

    PubMed Central

    Flatøy, Bernhard; Röhrl, Stephan M; Bøe, Berte; Nordsletten, Lars

    2016-01-01

    Background and purpose Hydroxyapatite has been used for a long time as an adjunct to enhance cementless fixation. The benefit of this is still debated, but new methods of hydroxyapatite deposition have emerged, offering possible gains. In order to investigate this further, we compared the migration pattern and periprosthetic bone remodeling in a cementless femoral stem with either electrochemically deposited hydroxyapatite—called Bonemaster (BM)—or a conventional plasma-sprayed hydroxyapatite (HA) coating. Patients and methods 55 hips were randomized to either BM or HA cementless femoral stems. Patients were followed with radiostereometry (RSA), dual-energy X-ray absorptiometry (DXA), radiographic measurements, and hip questionnaires for 5 years. Results For both stems, migration occurred mainly as subsidence and retroversion during the first 3 months. The BM group had a higher retroversion rate of 0.17° per month during this period, as compared to 0.06° per month for the HA group (p = 0.006). Thereafter, there was almost no movement in any direction for both stem types. Bone resorption occurred mainly during the first year, and subsequently decreased to a rate close to what is seen in normal ageing. The greatest total decrease occurred in Gruen zones 1 and 7, similar in the groups at 5 years. There was a slightly higher resorption rate in Gruen zone 7 from 2 to 5 years in the BM group (1.3% per year; p = 0.04), but in a magnitude that would scarcely affect stem stability or survival. Interpretation There were no clinically relevant differences between the 2 stems regarding stability or periprosthetic bone loss at 5 years. Electrochemically deposited HA does not appear to affect fixation or bone remodeling when compared to conventional plasma spraying at 5 years. Thus, at this point, Bonemaster appears to be safe. PMID:26364953

  5. Nuclear fuel microsphere gamma analyzer

    DOEpatents

    Valentine, Kenneth H.; Long, Jr., Ernest L.; Willey, Melvin G.

    1977-01-01

    A gamma analyzer system is provided for the analysis of nuclear fuel microspheres and other radioactive particles. The system consists of an analysis turntable with means for loading, in sequence, a plurality of stations within the turntable; a gamma ray detector for determining the spectrum of a sample in one section; means for analyzing the spectrum; and a receiver turntable to collect the analyzed material in stations according to the spectrum analysis. Accordingly, particles may be sorted according to their quality; e.g., fuel particles with fractured coatings may be separated from those that are not fractured, or according to other properties.

  6. Solid evacuated microspheres of hydrogen

    DOEpatents

    Turnbull, Robert J.; Foster, Christopher A.; Hendricks, Charles D.

    1982-01-01

    A method is provided for producing solid, evacuated microspheres comprised of hydrogen. The spheres are produced by forming a jet of liquid hydrogen and exciting mechanical waves on the jet of appropriate frequency so that the jet breaks up into drops with a bubble formed in each drop by cavitation. The drops are exposed to a pressure less than the vapor pressure of the liquid hydrogen so that the bubble which is formed within each drop expands. The drops which contain bubbles are exposed to an environment having a pressure just below the triple point of liquid hydrogen and they thereby freeze giving solid, evacuated spheres of hydrogen.

  7. The influence hydroxyapatite nanoparticle shape and size on the properties of biphasic calcium phosphate scaffolds coated with hydroxyapatite-PCL composites.

    PubMed

    Roohani-Esfahani, Seyed-Iman; Nouri-Khorasani, Saied; Lu, Zufu; Appleyard, Richard; Zreiqat, Hala

    2010-07-01

    We developed a composite biphasic calcium phosphate (BCP) scaffold by coating a nanocomposite layer, consisting of hydroxyapatite (HA) nanoparticles and polycaprolactone (PCL), over the surface of BCP. The effects of HA particle size and shape in the coating layer on the mechanical and biological properties of the BCP scaffold were examined. Micro-computerized tomography studies showed that the prepared scaffolds were highly porous (approximately 91%) with large pore size (400-700 microm) and an interconnected porous network of approximately 100%. The HA nanoparticle (needle shape)-composite coated scaffolds displayed the highest compressive strength (2.1 +/- 0.17 MPa), compared to pure HA/beta-TCP (0.1 +/- 0.05 MPa) and to the micron HA - composite coated scaffolds (0.29 +/- 0.07 MPa). These needle shaped scaffolds also showed enhanced elasticity and similar stress-strain profile to natural bone. Needle shaped coated HA/PCL particles induced the differentiation of primary human bone derived cells, with significant upregulation of osteogenic gene expression (Runx2, collagen type I, osteocalcin and bone sialoprotein) and alkaline phosphatase activity compared to other groups. These properties are essential for enhancing bone ingrowth in load-bearing applications. The developed composite scaffolds possessed superior physical, mechanical, elastic and biological properties rendering them potentially useful for bone tissue regeneration. PMID:20398935

  8. Effects of the nano-tubular anodic TiO2 buffer layer on bioactive hydroxyapatite coating.

    PubMed

    Piao, Zhonglie; Qiu, Jijun; Wu, Yongqing; Park, Se-Jeong; He, Weizhen; Timur, A; Ryu, Su-Chak; Kim, Hyung-Kook; Hwang, Yoon-Hwae

    2011-01-01

    We studied the effect of nano-tubular anodic TiO2 buffer layers on hydroxyapatite (HA) coating. The pulsed laser deposition (PLD) method was used to deposit HA on a well arranged nano-tubular anodic TiO2 (NT-ATO) buffer layer prepared by an electrochemical anodization technique. The surface morphology and chemical composition of HA coatings were characterized by using scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS), X-ray diffraction (XRD), and contact angle measurement. We found that crystalline HA coatings show well arranged porous morphologies with a favorable surface wettability. We also found that an anodic nano-tubular TiO2 buffer layer with a relatively short tube length shows a better coating morphology. The deposition process of HA on the nanotubular TiO2 buffer layer was also proposed. PMID:21446441

  9. 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. PMID:25910818

  10. A novel nano hydroxyapatite-incorporated Ni-P coating as an effective inter layer for biological applications.

    PubMed

    Shibli, S M A; Jayalekshmi, A C

    2009-03-01

    Hydroxyapatite (HA) coatings are normally made directly on orthopaedic implants and they possess many demerits such as cracks, irregular phase composition and poor adhesion. The present study had a novel approach of providing a nano-HA and phosphorous-rich electroless nickel (EN) coating as an interlayer on stainless steel (SS) prior to electrodeposition of pure HA coating. The interlayer had the merits of having incorporated with nano HA with rich phosphorous content. The outermost HA coating had excellent adherence and it was found to be free from any defects since it was formed only on the interlayer and not on the direct substrate. The overall coating system revealed high bioactivity when immersed in simulated body fluid (SBF). The present study also highlights the scope of using cost effective SS as the implant substrate instead of titanium as against the current trend of substrate selection. PMID:18987947

  11. On the anisotropic elastic properties of hydroxyapatite.

    NASA Technical Reports Server (NTRS)

    Katz, J. L.; Ukraincik, K.

    1971-01-01

    Experimental measurements of the isotropic elastic moduli on polycrystalline specimens of hydroxyapatite and fluorapatite are compared with elastic constants measured directly from single crystals of fluorapatite in order to derive a set of pseudo single crystal elastic constants for hydroxyapatite. The stiffness coefficients thus derived are given. The anisotropic and isotropic elastic properties are then computed and compared with similar properties derived from experimental observations of the anisotropic behavior of bone.

  12. Solvothermal synthesis of three-dimensional microspherical bismuth oxychloride self-assembled by microspheres

    NASA Astrophysics Data System (ADS)

    Li, Tengfei; Lin, Liyang; Wei, Hongmei; Liang, Guoqiang; Kuang, Xinliang; Liu, Tianmo

    2016-02-01

    Uniform BiOCl microspheres have been synthesized via a facile solvothermal route. The structural features of the as-prepared BiOCl samples were systematically characterized by the X-ray powder diffraction (XRD), and field emission scanning electron microscopy (FE-SEM). The SEM characterization results indicated that BiOCl microspheres possessed a superstructure composed of several hierarchical microspheres, which were assembled by numerous two dimensional nanosheets. This kind of special BiOCl 3D microstructure exhibited a large BET surface area of about 14.24 m2 g-1. Besides, the photocatalytic properties of BiOCl hollow microsphere sample and sheet-like sample were investigated in detail. Significantly, BiOCl hollow microsphere sample presented faster degradation rate toward RhB even under visible light, which should be attributed to the unique BiOCl nanosheets self-assembled hollow microspheres.

  13. Bisphosphonate release profiles from magnetite microspheres.

    PubMed

    Miyazaki, Toshiki; Inoue, Tatsuya; Shirosaki, Yuki; Kawashita, Masakazu; Matsubara, Takao; Matsumine, Akihiko

    2014-10-01

    Hyperthermia has been suggested as a novel, minimally invasive cancer treatment method. After implantation of magnetic nano- or microparticles around a tumour through blood vessels, irradiation with alternating magnetic fields facilitates the efficient in situ hyperthermia even for deep-seated tumours. On the basis of this idea, if the microspheres are capable of delivering drugs, they could be promising multifunctional biomaterials effective for chemotherapy as well as hyperthermia. In the present study, magnetite microspheres were prepared by aggregation of the iron oxide colloid in water-in-oil (W/O) emulsion. The release behaviour of alendronate, a typical bisphosphonate, from the microspheres was examined in vitro as a model of the bone tumour prevention and treatment system. The alendronate was successfully incorporated onto the porous magnetite microspheres in vacuum conditions. The drug-loaded microspheres maintained their original spherical shapes even after shaking in ultrapure water for 3 days, suggesting that they have sufficient mechanical integrity for clinical use. It was attributed to high aggregation capability of the magnetite nanoparticles through van der Waals and weak magnetic attractions. The microspheres showed slow release of the alendronate in vitro, resulting from tight covalent or ionic interaction between the magnetite and the alendronate. The release rate was diffusion-controlled type and well controlled by the alendronate concentration in drug incorporation to the microspheres. PMID:24854985

  14. Detection of Hydroxyapatite in Calcified Cardiovascular Tissues

    PubMed Central

    Lee, Jae Sam; Morrisett, Joel D.; Tung, Ching-Hsuan

    2012-01-01

    Objective The objective of this study is to develop a method for selective detection of the calcific (hydroxyapatite) component in human aortic smooth muscle cells in vitro and in calcified cardiovascular tissues ex vivo. This method uses a novel optical molecular imaging contrast dye, Cy-HABP-19, to target calcified cells and tissues. Methods A peptide that mimics the binding affinity of osteocalcin was used to label hydroxyapatite in vitro and ex vivo. Morphological changes in vascular smooth muscle cells were evaluated at an early stage of the mineralization process induced by extrinsic stimuli, osteogenic factors and a magnetic suspension cell culture. Hydroxyapatite components were detected in monolayers of these cells in the presence of osteogenic factors and a magnetic suspension environment. Results Atherosclerotic plaque contains multiple components including lipidic, fibrotic, thrombotic, and calcific materials. Using optical imaging and the Cy-HABP-19 molecular imaging probe, we demonstrated that hydroxyapatite components could be selectively distinguished from various calcium salts in human aortic smooth muscle cells in vitro and in calcified cardiovascular tissues, carotid endarterectomy samples and aortic valves, ex vivo. Conclusion Hydroxyapatite deposits in cardiovascular tissues were selectively detected in the early stage of the calcification process using our Cy-HABP-19 probe. This new probe makes it possible to study the earliest events associated with vascular hydroxyapatite deposition at the cellular and molecular levels. This target-selective molecular imaging probe approach holds high potential for revealing early pathophysiological changes, leading to progression, regression, or stabilization of cardiovascular diseases. PMID:22877867

  15. Seeing is believing, PLGA microsphere degradation revealed in PLGA microsphere/PVA hydrogel composites.

    PubMed

    Gu, Bing; Sun, Xuanhao; Papadimitrakopoulos, Fotios; Burgess, Diane J

    2016-04-28

    The aim of this study was to understand the polymer degradation and drug release mechanism from PLGA microspheres embedded in a PVA hydrogel. Two types of microspheres were prepared with different molecular weight PLGA polymers (approximately 25 and 7kDa) to achieve different drug release profiles, with a 9-day lag phase and without a lag phase, respectively. The kinetics of water uptake into the microspheres coincided with the drug release profiles for both formulations. For the 25kDa microspheres, minimal water uptake was observed in the early part of the lag phase followed by substantial water uptake at the later stages and in the drug release phase. For the 7kDa microspheres, water uptake occurred simultaneously with drug release. Water uptake was approximately 2-3 times that of the initial microsphere weight for both formulations. The internal structure of the PLGA microspheres was evaluated using low temperature scanning electron microscopy (cryo-SEM). Burst drug release occurred followed by pore forming from the exterior to the core of both microspheres. A well-defined hydrogel/microsphere interface was observed. For the 25kDa microspheres, internal pore formation and swelling occurred before the second drug release phase. The surface layer of the microspheres remained intact whereas swelling, and degradation of the core continued throughout the drug release period. In addition, microsphere swelling reduced glucose transport through the coatings in PBS media and this was considered to be a as a consequence of the increased thickness of the coatings. The combination of the swelling and microdialysis results provides a fresh understanding on the competing processes affecting molecular transport of bioanalytes (i.e. glucose) through these composite coatings during prolonged exposure in PBS. PMID:26965956

  16. Significance of melt-fraction in HVOF sprayed hydroxyapatite particles, splats and coatings.

    PubMed

    Khor, K A; Li, H; Cheang, P

    2004-01-01

    Microstructure characterization and property evaluation of high velocity oxy-fuel (HVOF) sprayed hydroxyapatite (HA) splats and coatings were conducted in the present study as a function of the proportion of melting that occurred in HA particles during HVOF spray. In vitro behavior of single and folded HA splats in simulated body fluid was also investigated. Results showed that phase composition of as-sprayed HA coatings was influenced significantly by the melt fraction in HVOF sprayed particles. Melt fraction of the HA powders were experimentally determined from particle morphology analysis. It was found that the spray parameters and starting powder size influenced the melt fraction of the particles. In vitro investigation of individual HA splats made from different HA particles revealed decisive role of local phase composition in influencing their dissolution/precipitation behavior during the test. Furthermore, Raman spectroscopy qualitative inspection on the sprayed HA particles (partial melted) revealed that thermal decomposition occurred within the melted part rather than the unmelted zone. Young's modulus and micro-hardness of the as-sprayed particles and coatings were determined using nano-indentation technique. The resolidified zone of the sprayed HA particles exhibited an average Young's modulus value of 41.25 GPa. The measured values ranged from 23.1 to 65.3 GPa. The unmelted part of the HA powders showed a markedly narrower range. Young's modulus value of 83.9 GPa (+/-9.4 GPa) was recorded for this region. This succinctly highlight the difference between the unmelted region and melted regions of a HA particle. Young's moduli values measured on HVOF coatings were found to mirror the trend found in the spheroidised particles and splats with apt fidelity. PMID:14643591

  17. 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.

  18. Porous biomorphic silicon carbide ceramics coated with hydroxyapatite as prospective materials for bone implants.

    PubMed

    Gryshkov, Oleksandr; Klyui, Nickolai I; Temchenko, Volodymyr P; Kyselov, Vitalii S; Chatterjee, Anamika; Belyaev, Alexander E; Lauterboeck, Lothar; Iarmolenko, Dmytro; Glasmacher, Birgit

    2016-11-01

    Porous and cytocompatible silicon carbide (SiC) ceramics derived from wood precursors and coated with bioactive hydroxyapatite (HA) and HA-zirconium dioxide (HA/ZrO2) composite are materials with promising application in engineering of bone implants due to their excellent mechanical and structural properties. Biomorphic SiC ceramics have been synthesized from wood (Hornbeam, Sapele, Tilia and Pear) using a forced impregnation method. The SiC ceramics have been coated with bioactive HA and HA/ZrO2 using effective gas detonation deposition approach (GDD). The surface morphology and cytotoxicity of SiC ceramics as well as phase composition and crystallinity of deposited coatings were analyzed. It has been shown that the porosity and pore size of SiC ceramics depend on initial wood source. The XRD and FTIR studies revealed the preservation of crystal structure and phase composition of in the HA coating, while addition of ZrO2 to the initial HA powder resulted in significant decomposition of the final HA/ZrO2 coating and formation of other calcium phosphate phases. In turn, NIH 3T3 cells cultured in medium exposed to coated and uncoated SiC ceramics showed high re-cultivation efficiency as well as metabolic activity. The recultivation efficiency of cells was the highest for HA-coated ceramics, whereas HA/ZrO2 coating improved the recultivation efficiency of cells as compared to uncoated SiC ceramics. The GDD method allowed generating homogeneous HA coatings with no change in calcium to phosphorus ratio. In summary, porous and cytocompatible bio-SiC ceramics with bioactive coatings show a great promise in construction of light, robust, inexpensive and patient-specific bone implants for clinical application. PMID:27524006

  19. Carbon nanotubes in nanocomposites and hybrids with hydroxyapatite for bone replacements.

    PubMed

    Shin, Ueon Sang; Yoon, Il-Kyu; Lee, Gil-Su; Jang, Won-Cheoul; Knowles, Jonathan C; Kim, Hae-Won

    2011-01-01

    Hydroxyapatite (HA), as a bone mineral component, has been an attractive bioceramic for the reconstruction of hard tissues. However, its poor mechanical properties, including low fracture toughness and tensile strength, have been a significant challenge to the application of HA for the replacement of load-bearing and/or large bone defects. Among materials studied to reinforce HA, carbon nanotubes (CNTs: single-walled or multiwalled) have recently gained significant attention because of their unprecedented mechanical properties (high strength and toughness) and physicochemical properties (high surface area, electrical and thermal conductivity, and low weight). Here, we review recent studies of the organization of HA-CNTs at the nanoscale, with a particular emphasis on the functionalization of CNTs and their dispersion within an HA matrix and induction of HA mineralization. The organization of CNTs and HA implemented at the nanoscale can further be developed in the form of coatings, nanocomposites, and hybrid powders to enable potential applications in hard tissue reconstruction. PMID:21776341

  20. 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.

  1. Carbon Nanotubes in Nanocomposites and Hybrids with Hydroxyapatite for Bone Replacements

    PubMed Central

    Shin, Ueon Sang; Yoon, Il-Kyu; Lee, Gil-Su; Jang, Won-Cheoul; Knowles, Jonathan C.; Kim, Hae-Won

    2011-01-01

    Hydroxyapatite (HA), as a bone mineral component, has been an attractive bioceramic for the reconstruction of hard tissues. However, its poor mechanical properties, including low fracture toughness and tensile strength, have been a significant challenge to the application of HA for the replacement of load-bearing and/or large bone defects. Among materials studied to reinforce HA, carbon nanotubes (CNTs: single-walled or multiwalled) have recently gained significant attention because of their unprecedented mechanical properties (high strength and toughness) and physicochemical properties (high surface area, electrical and thermal conductivity, and low weight). Here, we review recent studies of the organization of HA-CNTs at the nanoscale, with a particular emphasis on the functionalization of CNTs and their dispersion within an HA matrix and induction of HA mineralization. The organization of CNTs and HA implemented at the nanoscale can further be developed in the form of coatings, nanocomposites, and hybrid powders to enabl