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The Fe-Mn alloys are potential candidates for biodegradable implant applications. However, the very low degradation rates of Fe-Mn alloys in the physiological environment are a major disadvantage. In this study, the degradation rate of a Fe-20Mn alloy was improved using the groove pressing (GP) technique. Hot rolled sheets of 2 mm thickness were subjected to GP operation at 1000°C. Uniform fine-grained (UFG) Fe-Mn alloys were obtained using the GP technique. The influence of GP on the microstructure, mechanical properties, degradation behavior in simulated body fluid (SBF), surface wettability, biomineralization, and cytocompatibility was investigated and compared to the annealed (A Fe-Mn) and rolled (R Fe-Mn) sample. The groove-pressed Fe-Mn (G Fe-Mn) alloy had a grain size of approximately 40 ± 16 μm whereas the A Fe-Mn and R Fe-Mn samples had grain sizes of 303 ± 81 and 117 ± 14.5 μm, respectively. Enhanced strength and elongation were also observed with the G Fe-Mn sample. The potentiodynamic polarization test showed the highest I corr , lowest polarization resistance, and lowest E corr for the G Fe-Mn sample among all other samples indicating its higher degradation rate. The weight loss data from immersion tests also shows that the percentage of weight loss increases with time indicating the accelerated degradation behavior of the sample. The static immersion test showed an enhancement in weight loss of 0.46 ± 0.02% and 1.02 ± 0.05% for R Fe-Mn and G Fe-Mn samples, respectively, than A Fe-Mn sample (0.31 ± 0.03%) after 56 days in immersion in SBF. The greater biomineralization tendency in UFG materials is confirmed by the G Fe-Mn sample's stronger hydroxyapatite deposition. When compared to the A Fe-Mn and R Fe-Mn samples, the G Fe-Mn sample has a better wettability, which promotes higher cell adhesion and vitality, showing higher biocompatibility. This study demonstrates that Fe-20Mn processed by GP has potential applications for the manufacture of biodegradable metallic implants., (© 2024 Wiley Periodicals LLC.)

In this study, we have formulated a novel apatite bone cements derived from natural sources (i.e. eggshell and fishbone) with improved qualities that is, porosity, resorbability, biological activity, and so forth. The naturally-derived apatite bone cement (i.e. FBDEAp) was prepared by mixing hydroxyapatite (synthesized from fishbone) and tricalcium phosphate (synthesized from eggshell) as a solid phase with a liquid phase (a dilute acidic blend of cement binding accelerator and biopolymers like gelatin and chitosan) with polysorbate (as liquid porogen) to get a desired bone cement paste. The prepared cement paste sets within the clinically acceptable setting time (≤20 min), easily injectable (>85%) through hands and exhibits physiological pH stability (7.3-7.4). The pure apatite phased bone cement was confirmed by x-ray diffraction and Fourier transform infrared spectroscopy analyses. The FBDEAp bone cement possesses acceptable compressive strength (i.e. 5-7 MPa) within trabecular bone range and is resorbable up to 28% in simulated body fluid solution within 12 weeks of incubation at physiological conditions. The FBDEAp is macroporous in nature (average pore size ~50-400 μm) with interconnected pores verified by SEM and micro-CT analyses. The FBDEAp showed significantly increased MG63 cell viability (>125% after 72 h), cell adhesion, proliferation, and key osteogenic genes expression levels (up to 5-13 folds) compared to the synthetically derived, synthetic and eggshell derived as well as synthetic and fishbone derived bone cements. Thus, we strongly believe that our prepared FBDEAp bone cement can be used as potential trabecular bone substitute in orthopedics., (© 2024 Wiley Periodicals LLC.)

Antibiotic-loaded bioactive bone substitutes are widely used for treating various orthopedic diseases and prophylactically to avoid post implantation infection. Calcium deficient hydroxyapatite (also known as apatitic bone cement) is a potential bioactive bone substitute in orthopedics due to its chemical composition similar to that of natural bone minerals. In this study, fabrication of mannitol (a solid porogen) incorporated injectable synthetic (Syn) and eggshell derived (ESD) apatitic bone cements loaded with antibiotics (gentamicin/meropenem/ rifampicin/vancomycin) was investigated. The release kinetics of the antibiotics were studied by fitting them with different kinetic models. All the antibiotics-loaded apatitic bone cements set within clinically accepted setting time (20 ± 2 min) and with good injectability (>70%). The antibiotics released from these bone cements were found to be controlled and sustained throughout the study time. Weibull and Gompertz (applies in least initial burst and sustain drug release rate models) were the best models to predict the release behavior. They cements had acceptable compressive strength (6-10 MPa; in the range of trabecular bone) and were biodegradable (21%-27% within 12 weeks of incubation) in vitro in simulated body fluids at physiological conditions. These bone cements showed excellent antibacterial activity from day 1 onwards and no bacterial colony was found from day 3 onwards. The viability of MG63 cells in vitro after 72 h was significantly higher after 24 h (i.e., ~110%). The cells were well attached and spread over the surface of the cements with extended morphology. The ESD antibiotic-loaded apatitic bone cements showed better injectability, degradation and cytocompatibility compared when compared to Syn antibiotic-loaded apatitic bone cements. Thus, we believe that the ESD antibiotic-loaded apatitic bone cements are suitable as potential injectable bone substitutes to avoid post-operative implant associated and other acute or chronic bone infections., (© 2023 Wiley Periodicals LLC.)

Biomimicry is becoming deep-rooted as part of bioceramics owing to its numerous functional advantages. Naturally occurring hydroxyapatite (HA) apart from primary nano structures are also characterised by various ionic substitutions. The ease of accommodating such key elements into the HA lattice is known to enhance bone healing properties of bioceramics. In this work, hydroxyapatite synthesized via biomimetic approach was substituted with individual as well as multiple cations for potential applications in bone repair. Ion substitutions of Sr, Mg and Zn was carried out on HA for the first time by using Serratia grown in a defined biomineralization medium. The individual ions of varying concentration substituted in Serratia HA (SHA) (Sr SHA, Mg SHA and Zn SHA) were analysed for crystallinity, functional groups, morphology and crystal size. All three showed decreased crystallinity, phase purity, large agglomerated aggregates and needle-shaped morphologies. Fourier transform infrared spectroscopy (FTIR) spectra indicated increased carbonate content of 5.8% resembling that of natural bone. Additionally, the reduced O-H intensities clearly portrayed disruption of HA lattice and subsequent ion-substitution. The novelty of this study lies primarily in investigating the co-substitution of a combination of 1% Sr, Zn and Mg in SHA and establishing the associated change in bone parameters. Scanning electron microscope (SEM) and transmission electron microscope (TEM) images clearly illustrated uniform nano-sized agglomerates of average dimensions of 20-50 nm length and 8-15 nm width for Sr SHA; 10-40 nm length and 8-10 nm width for both Zn SHA and Mg SHA and 40-70 nm length and 4-10 nm width in the case of 1% Sr, Zn, Mg SHA. In both individual as well as co-substitutions, significant peak shifts were not observed possibly due to the lower concentrations. However, cell volumes increased in both cases due to presence of Sr 2+ validating its dominant integration into the SHA lattice. Rich trace ion deposition was presented by energy dispersive X-ray spectroscopy (EDS) and quantified using inductively coupled plasma optical emission spectrometer (ICP-OES). In vitro cytotoxicity studies in three cell lines viz. NIH/3T3 fibroblast cells, MG-63 osteosarcoma cells and RAW 264.7 macrophages showed more than 90% cell viability proving the biocompatible nature of 1% Sr, Zn and Mg in SHA. Microbial biomineralization by Serratia produced nanocrystals of HA that mimicked "bone-like apatite" as evidenced by pure phase, carbonated groups, reduced crystallinity, nano agglomerates, variations in cell parameters, rich ion deposition and non-toxic nature. Therefore ion-substituted and co-substituted biomineralized nano SHA appears to be a suitable candidate for applications in biomedicine addressing bone injuries and aiding regeneration as a result of its characteristics close to that of the human bone., (© 2023. The Author(s).)

Calcium deficient hydroxyapatite (CDHA)-based apatite forming bone cements are well known for their bioactivity and bioresorbability. The formulation of CDHA-based cements with improved macroporosity, injectability, and resorbability has been investigated. The solid phase consists of nanocrystalline hydroxyapatite (HA) and tricalcium phosphate (β-TCP). The liquid phase is diluted acetic acid with disodium hydrogen phosphate as binding accelerator along with gelatin and chitosan to improve the injectability. A porogen agent either mannitol (as solid porogen) or polysorbate (as liquid porogen) is also used to improve the porosity. All combined in fine-tuned composition results in optimal bone cements. The cement sets within the clinically preferred setting time (≤20 min) and injectability (>70%) and also stable at physiological pH (i.e., ~7.3-7.4). The XRD and FT-IR analysis confirmed the formation of CDHA phase on day 7 when the after-set cement immersed under phosphate buffer solution (PBS) at physiological conditions. The cements were found to have acceptable compressive strength for trabecular bone substitute. The cements were macroporous in nature with average pore size between 50 and 150 μm and were interconnected as confirmed by SEM, micro-CT and MIP analysis. The prepared cements are degradable up to 22% and 19% in simulated body fluid and PBS respectively within 10 weeks of immersion at physiological conditions. The cements exhibit higher viability (%) (>110%) with L929 and MG63 cells compared to the control after 3 days of incubation. They also show increased proliferation, well spreading and extended filopodia with MG63 cells. Overall, the developed apatite forming bone cements seems to be suitable for low or non-load bearing orthopedic applications., (© 2022 Wiley Periodicals LLC.)

Introduction: The aim of this study was to evaluate the effect of functionalized nanoparticle photodynamic therapy on Nano hardness of root dentin METHODOLOGY: Fifty single rooted lower premolars were decoronated and sectioned into two halves. Then the samples were embedded horizontally in to the acrylic resin to expose the dentin surface. Baseline nanohardness was done at midroot level using a Nanohardness tester. Exposed dentin surfaces were immersed in the following irrigating solutions Post treatment nanohardness testing was done and results were analyzed statistically RESULTS: In general, all the samples in their respective groups had significant change in nanohardness following immersion in irrigant solutions except in NaOCl + EDTA and saline group. CSRB-np and PLGA-MBnp showed increased nanohardness (P = 0.005 and P = 0.007 respectively). Whereas NaOCl + EDTA + CHX showed decrease in nanohardness (P = 0.04). With regards to Modulus of elasticity (MOE), CSRB-np showed significant difference (P = 0.002) compared to the other groups. MOE increased in CSRB-np and PLGA-MBnp while it decreased in all the other groups., Conclusion: In this study, the improvement of nanohardness and modulus of elasticity following the immersion of root dentin in CSRB-np solution was demonstrated., (Copyright © 2020 Elsevier B.V. All rights reserved.)

Curdlan, an insoluble and neutral polysaccharide, was produced from Agrobacterium sp. ATCC 31750 and chemically modified with dimethylaminoethyl (DMAE) group to introduce gene binding ability. The resulting DMAE-curdlan was crosslinked with curdlan nanoparticles using epichlorohydrin. The prepared nanoparticles are spherical with an average diameter of 523 ± 195 nm, stable and are highly biocompatible with differentiated THP-1 macrophages with viability of above 90%. They are taken up more efficiently by RAW 264.7 macrophage cells than by L929 fibroblast cells. They increase the expression of M1 macrophage marker genes, TNFα and CXCL10, and decrease the expression of M2 marker, CD206, indicating their ability to activate M1 phenotype and aid in tumor regression. They are also capable of delivering siRNA to human macrophage-like cells efficiently and inhibit ~59% of the expression of target MMP-9 protein. These results indicate that this modified curdlan-based nanoparticle is a promising vehicle for the delivery of siRNAs to macrophages, which could open up treatment strategies for a range of diseases., (Copyright © 2019 Elsevier B.V. All rights reserved.)

Calcium phosphate (CaP) bioceramics closely resemble the natural human bone, which is a main reason for their popularity as bone substitutes. However, this compositional similarity makes it difficult to distinguish CaPs, especially in particulate form, from native bone by imaging modalities such as X-ray radiography, computed tomography (CT), and magnetic resonance imaging (MRI) to monitor the healing progress. External contrast agents can improve the imaging contrast of CaPs but can affect their physicochemical properties and can produce artifacts. In this work, we have attempted to improve the contrast of CaP nanoparticles via ion substitutions for multimodal imaging. Calcium-deficient hydroxyapatite (CDHA) nanoparticles with silver (Ag), gadolinium (Gd), and iron (Fe) substitution were prepared by a microwave-accelerated wet chemical process to improve the contrast in CT, T1 (spin-lattice), and T2 (spin-spin) MRI relaxation modes, respectively. Ag, Gd, and Fe were substituted at 0.25, 0.5, and 0.25 at.%, respectively. The ion-substituted CDHA (ICDHA) was found to be phase pure by X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FT-IR). Transmission electron microscopy (TEM) images showed that the ICDHA nanoparticles were platelet shaped and of 52 ± 2 nm length and 6 ± 1 nm width. The ICDHA showed high contrast in X-ray and CT compared to CDHA. The vibrating sample magnetometry (VSM) studies showed the ICDHA to exhibit paramagnetic behavior compared to diamagnetic CDHA, which was further confirmed by improved contrast in T1 and T2 MRI mode. In addition, the in vitro tetracycline drug loading and release was studied to investigate the capability of these nanoparticles for antibiotic drug delivery. It was found that a burst release profile was observed for 24 h with 47-52% tetracycline drug release. The ICDHA nanoparticles also showed in vitro antibacterial activity against Staphylococcus aureus and Escherichia coli due to Ag, which was further enhanced by antibiotic loading. In vitro biocompatibility studies showed that the triple-ion-substituted ICDHA nanoparticles were cytocompatible. Thus, the ion-substituted CDHA nanoparticles can have potential theranostic applications due to their multimodal image contrast, antibacterial activity, and drug delivery potential. Future work will be conducted with actual bone samples in vitro or in animal models.

A dual local drug delivery system (DDS) composed of calcium phosphate bioceramic nanocarriers aimed at treating the antibacterial, anti-inflammatory, and bone-regenerative aspects of periodontitis has been developed. Calcium-deficient hydroxyapatite (CDHA, Ca/P = 1.61) and tricalcium phosphate (β-TCP) were prepared by microwave-accelerated wet chemical synthesis method. The phase purity of the nanocarriers was confirmed by x-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FT-IR), while the transmission electron microscopy (TEM) confirmed their nanosized morphology. CDHA was selected as carrier for the antibiotic (tetracycline) while TCP was chosen as the anti-inflammatory drug (ibuprofen) carrier. Combined drug release profile was studied in vitro from CDHA/TCP (CTP) system and compared with a HA/TCP (BCP) biphasic system. The tetracycline and ibuprofen release rate was 71 and 23% from CTP system as compared to 63 and 20% from BCP system. CTP system also showed a more controlled drug release profile compared to BCP system. Modeling of drug release kinetics from CTP system indicated that the release follows Higuchi model with a non-typical Fickian diffusion profile. In vitro biological studies showed the CTP system to be biocompatible with significant antibacterial and anti-inflammatory activity. In vivo implantation studies on rat cranial defects showed greater bone healing and new bone formation in the drug-loaded CTP system compared to control (no carrier) at the end of 12 weeks. The in vitro and in vivo results suggest that the combined drug delivery platform can provide a comprehensive management for all bone infections requiring multi-drug therapy.

Electrospraying has tremendous potential to prepare submicron to nano size ceramic particles with novel properties. In this study, a sol-gel assisted electrospraying has been used to synthesise phase controlled apatite (hydroxyapatite, HA and calcium deficient hydroxyapatite, CDHA) particles. Variation in particle size was also achieved by controlling the process parameters. The particles were non cytotoxic, induced proliferation of osteoblast-like cells (HOS) and internalised by the cells. Increased alkaline phosphatase, collagen and calcium deposition confirmed the mineralisation of cells. Expression of osteopontin, osteocalcin and alkaline phosphatase genes further ascertained that the particles promoted osteogenic commitment of the rat bone marrow-derived mesenchymal stem cells (rBMSCs). The particles also showed better loading and release of tetracycline drug than accelerated microwave synthesised apatite particles. The methodology for synthesis of ceramic particles may have avenues for a wide range of biomedical applications. © 2017 Wiley Periodicals, Inc. J Biomed Mater Res Part B: Appl Biomater, 106B: 1941-1954, 2018., (© 2017 Wiley Periodicals, Inc.)

Tissue engineering aims to fabricate and functionalise constructs that mimic the native extracellular matrix (ECM) in the closest way possible to induce cell growth and differentiation in both in vitro and in vivo conditions. Development of scaffolds that can function as tissue substitutes or augment healing of tissues is an essential aspect of tissue regeneration. Although there are many techniques for achieving this biomimicry in 2D structures and 2D cell cultures, translation of successful tissue regeneration in true 3D microenvironments is still in its infancy. Electrospinning, a well known electrohydrodynamic process, is best suited for producing and functionalising, nanofibrous structures to mimic the ECM. A systematic control of the processing parameters coupled with novel process innovations, has recently resulted in novel 3D electrospun structures. This chapter gives a brief account of the various 3D electrospun structures that are being tried as tissue engineering scaffolds. Combining electrospinning with other 3D structure forming technologies, which have shown promising results, has also been discussed. Electrospinning has the potential to bridge the gap between what is known and what is yet to be known in fabricating 3D scaffolds for tissue regeneration.

Conventional glass-ionomer cements (GIC) are one of the most prevalent dental restorative materials, but their use is limited by their relatively low mechanical strength. Efforts have been made to improve the mechanical properties by addition of various fillers of which nano-sized particles appears to be a promising strategy. In the current study, effect of addition of nanochitosan particles in GIC (NCH-GIC) on compressive strength, flexural strength, wear resistance and fluoride release has been evaluated and compared with conventional GIC (C-GIC). Nanochitosan was synthesized by ionic cross linking method and its particle size was found to be 110-235nm. Nanochitosan was mixed with glass ionomer powder at a concentration of 10wt.% and cement samples were prepared. NCH-GIC had significantly higher compressive strength values which could be attributed to early formation of aluminium polysalts. Similarly, flexural strength of NCH-GIC (21.26MPa) was significantly higher than C-GIC (12.67MPa). Wear resistance was also found to increase due to better integrated interface between the glass particle and polymer matrix bonding in NCH-GIC. Fluoride release was significantly higher in NCH-GIC compared to C-GIC for 7 days. It can be anticipated that addition of nanochitosan to GIC will improve the anti-cariogenic and mechanical properties for high strength applications., (Copyright © 2017 Elsevier B.V. All rights reserved.)

AZ31 magnesium alloy was coated with polycaprolactone (PCL) nano-fibrous layer using electrospinning technique so as to control degradation in physiological environment. Before coating, the alloy was treated with HNO3 to have good adhesion between the coating and substrate. To elucidate the role of pre-treatment and coating, samples only with PCL coating as well as HNO3 treatment only were prepared for comparison. Best coating adhesion of 4B grade by ASTM D3359-09 tape test was observed for pre-treated samples. The effect of coating on in vitro degradation and biomineralization was studied using supersaturated simulated body fluid (SBF 5×). The weight loss and corrosion results obtained by immersion test showed that the combination of HNO3 pre-treatment and PCL coating is very effective in controlling the degradation rate and improving bioactivity. Cytotoxicity studies using L6 cells showed that PCL coated sample has better cell adhesion and proliferation compared to uncoated samples. Nano-fibrous PCL coating combined with prior acid treatment seems to be a promising method to tailor degradation rate with enhanced bioactivity of Mg alloys., (Copyright © 2016 Elsevier B.V. All rights reserved.)

The objective of the present work is to investigate the role of different grain sizes produced by equal channel angular pressing (ECAP) on the degradation behavior of magnesium alloy using in vitro and in vivo studies. Commercially available AZ31 magnesium alloy was selected and processed by ECAP at 300°C for up to four passes using route Bc. Grain refinement from a starting size of 46μm to a grain size distribution of 1-5μm was successfully achieved after the 4th pass. Wettability of ECAPed samples assessed by contact angle measurements was found to increase due to the fine grain structure. In vitro degradation and bioactivity of the samples studied by immersing in super saturated simulated body fluid (SBF 5×) showed rapid mineralization within 24h due to the increased wettability in fine grained AZ31 Mg alloy. Corrosion behavior of the samples assessed by weight loss and electrochemical tests conducted in SBF 5× clearly showed the prominent role of enhanced mineral deposition on ECAPed AZ31 Mg in controlling the abnormal degradation. Cytotoxicity studies by MTT colorimetric assay showed that all the samples are viable. Additionally, cell adhesion was excellent for ECAPed samples particularly for the 3rd and 4th pass samples. In vivo experiments conducted using New Zealand White rabbits clearly showed lower degradation rate for ECAPed sample compared with annealed AZ31 Mg alloy and all the samples showed biocompatibility and no health abnormalities were noticed in the animals after 60days of in vivo studies. These results suggest that the grain size plays an important role in degradation management of magnesium alloys and ECAP technique can be adopted to achieve fine grain structures for developing degradable magnesium alloys for biomedical applications., (Copyright © 2015 Elsevier B.V. All rights reserved.)

Several synthetic scaffolds are being developed using polymers, ceramics and their composites to overcome the limitations of auto- and allografts. Polymer-ceramic composites appear to be the most promising bone graft substitute since the natural bone itself is a composite of collagen and hydroxyapatite. Ceramics provide strength and osteoconductivity to the scaffold while polymers impart flexibility and resorbability. Natural polymers have an edge over synthetic polymers because of their biocompatibility and biological recognition property. But, very few natural polymer-ceramic composites are available as commercial products, and those few are predominantly based on type I collagen. Disadvantages of using collagen include allergic reactions and pathogen transmission. The commercial products also lack sufficient mechanical properties. This review summarizes the recent developments of biocomposite materials as bone scaffolds to overcome these drawbacks. Their characteristics, in vitro and in vivo performance are discussed with emphasis on their mechanical properties and ways to improve their performance., (Copyright © 2015 Elsevier B.V. All rights reserved.)

Nanotechnology has tremendous potential for the management of infectious diseases caused by multi-drug resistant bacteria, through the development of newer antibacterial materials and efficient modes of antibiotic delivery. Calcium phosphate (CaP) bioceramics are commonly used as bone substitutes due to their similarity to bone mineral and are widely researched upon for the treatment of bone infections associated with bone loss. CaPs can be used as local antibiotic delivery agents for bone infections and can be substituted with antibacterial ions in their crystal structure to have a wide spectrum, sustained antibacterial activity even against drug resistant bacteria. In the present work, a dual mode antibiotic delivery system with antibacterial ion substituted calcium deficient hydroxyapatite (CDHA) nanoparticles has been developed. Antibacterial ions such as zinc, silver, and strontium have been incorporated into CDHA at concentrations of 6, 0.25-0.75, and 2.5-7.5 at. %, respectively. The samples were found to be phase pure, acicular nanoparticles of length 40-50 nm and width 5-6 nm approximately. The loading and release profile of doxycycline, a commonly used antibiotic, was studied from the nanocarriers. The drug release was studied for 5 days and the release profile was influenced by the ion concentrations. The release of antibacterial ions was studied over a period of 21 days. The ion substituted CDHA samples were tested for antibacterial efficacy on Staphylococcus aureus and Escherichia coli by MIC/MBC studies and time-kill assay. AgCDHA and ZnCDHA showed high antibacterial activity against both bacteria, while SrCDHA was weakly active against S. aureus. Present study shows that the antibiotic release can provide the initial high antibacterial activity, and the sustained ion release can provide a long-term antibacterial activity. Such dual mode antibiotic and antibacterial ion release offers an efficient and potent way to treat an incumbent drug resistant infection.

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., (Copyright © 2014 Elsevier Ltd. All rights reserved.)

Eggshell is an attractive natural source of calcium for the synthesis of hydroxyapatite (HA) as it contains minor amounts of biologically relevant elements such as Mg, Sr, and Si. The mineral phase of the human bone is essentially a calcium deficient hydroxyapatite (CDHA) which shows more bioactivities and absorbance than stoichiometric HA does. Hence, we have attempted to develop a protein delivery system based on eggshell derived CDHA (ECDHA) nanoparticles for bone tissue engineering. Nanoparticles with Ca/P molar ratio of 1.67, 1.61 and 1.51 to form CDHAs with compositions covering the properties of stable HA phase (Ca/P=1.67) to degradable tricalcium phosphate (TCP) phase (Ca/P=1.5) were synthesized by microwave-accelerated wet chemical synthesis using eggshell as well as synthetic calcium hydroxide as calcium precursors. The delivery profiles of bovine serum albumin (BSA), a model protein by the nanocarriers, were studied. Both eggshells derived and synthetic CDHA samples showed maximum amount of loading of 57% and 37%, respectively at a Ca/P ratio of 1.51, comparing to stoichiometric HA. ECDHA also showed a much more BSA release (25%) than synthetically derived CDHA (6.5%) did. To further improve the release profile, alginate coating was carried out on CDHA nanoparticles and the BSA release profiles were evaluated. A maximum release of 65% was observed for alginate coated ECDHA at a Ca/P ratio of 1.51 for a period of 2 days. The ECDHA nanoparticle with a Ca/P ratio similar to degradable TCP and with alginate coating seems to be an ideal protein delivery agent., (Copyright © 2014 Elsevier B.V. All rights reserved.)

Nano-hydroxyapatite (nHA) reinforced magnesium composite (Mg-nHA) was fabricated by friction stir processing (FSP). The effect of smaller grain size and the presence of nHA particles on controlling the degradation of magnesium were investigated. Grain refinement from 1500μm to ≈3.5μm was observed after FSP. In vitro bioactivity studies by immersing the samples in supersaturated simulated body fluid (SBF 5×) indicate that the increased hydrophilicity and pronounced biomineralization are due to grain refinement and the presence of nHA in the composite respectively. Electrochemical test to assess the corrosion behavior also clearly showed the improved corrosion resistance due to grain refinement and enhanced biomineralization. Using MTT colorimetric assay, cytotoxicity study of the samples with rat skeletal muscle (L6) cells indicate marginal increase in cell viability of the FSP-Mg-nHA sample. The composite also showed good cell adhesion., (Copyright © 2014 Elsevier B.V. All rights reserved.)

Current treatment of periodontal infections includes mechanical debridement, administration of antibiotics and bone grafting. Oral administration of antibiotics results in undesirable side effects, while current modes of local administration are affected by problems concerning allergic response to the polymeric carrier agents. We have developed an osteoconductive drug delivery system composed of apatitic nanocarriers capable of providing sustained delivery of drugs in the periodontium. Calcium deficient hydroxyapatite (CDHA) nanocarriers of different Ca/P ratios were synthesized and characterized using the x-ray diffraction method, transmission electron microscopy, inductively coupled plasma atomic emission spectroscopy, Fourier transform infrared spectroscopy and the BET gas isotherm method. Loading and release studies performed with tetracycline showed a sustained release of up to 88% in phosphate buffered saline over a period of five days. Antibacterial activity studies showed that the tetracycline loaded CDHA (TC-CDHA) nanocarriers were effective against S. aureus and E. coli bacteria. The biocompatibility of the TC-CDHA nanocarriers was demonstrated using an alamar blue assay and further characterized by cell uptake studies. Interestingly, cell uptake of drug loaded CDHA also increased the cellular proliferation of human periodontal ligament fibroblast cells. Hence, it can be concluded that the CDHA nanocarriers are ideal drug delivery agents and have bone regenerative potential for local periodontal applications.

Friction stir processing (FSP) was successfully adopted to fabricate nano-hydroxyapatite (nHA) reinforced AZ31 magnesium alloy composite as well as to achieve fine grain structure. The combined effect of grain refinement and the presence of embedded nHA particles on enhancing the biomineralization and controlling the degradation of magnesium were studied. Grain refinement from 56 to ~4 and 2 μm was observed at the stir zones of FSP AZ31 and AZ31-nHA composite respectively. The immersion studies in super saturated simulated body fluid (SBF 5×) for 24 h suggest that the increased wettability due to fine grain structure and nHA particles present in the AZ31-nHA composite initiated heterogeneous nucleation which favored the early nucleation and growth of calcium-phosphate mineral phase. The nHA particles as nucleation sites initiated rapid biomineralization in the composite. After 72 h of immersion the degradation due to localized pitting was observed to be reduced by enhanced biomineralization in both the FSPed AZ31 and the composite. Also, best corrosion behavior was observed for the composite before and after immersion test. MTT assay using rat skeletal muscle (L6) cells showed negligible toxicity for all the processed and unprocessed samples. However, cell adhesion was observed to be more on the composite due to the small grain size and incorporated nHA.

Wear resistant TiB-TiN reinforced Ti6Al4V alloy composite coatings were deposited on Ti substrate using laser based additive manufacturing technology. Ti6Al4V alloy powder premixed with 5wt% and 15wt% of boron nitride (BN) powder was used to synthesize TiB-TiN reinforcements in situ during laser deposition. Influences of laser power, scanning speed and concentration of BN on the microstructure, mechanical, in vitro tribological and biological properties of the coatings were investigated. Microstructural analysis of the composite coatings showed that the high temperature generated due to laser interaction with Ti6Al4V alloy and BN results in situ formation of TiB and TiN phases. With increasing BN concentration, from 5wt% to 15wt%, the Young's modulus of the composite coatings, measured by nanoindentation, increased from 170±5GPa to 204±14GPa. In vitro tribological tests showed significant increase in the wear resistance with increasing BN concentration. Under identical test conditions TiB-TiN composite coatings with 15wt% BN exhibited an order of magnitude less wear rate than CoCrMo alloy-a common material for articulating surfaces of orthopedic implants. Average top surface hardness of the composite coatings increased from 543±21HV to 877±75HV with increase in the BN concentration. In vitro biocompatibility and flow cytometry study showed that these composite coatings were non-toxic, exhibit similar cell-materials interactions and biocompatibility as that of commercially pure titanium (CP-Ti) samples. In summary, excellent in vitro wear resistance, high stiffness and suitable biocompatibility make these composite coatings as a potential material for load-bearing articulating surfaces towards orthopaedic implants., (© 2013 Elsevier Ltd. All rights reserved.)

Groove pressing (GP) has been successfully adopted to achieve fine grain size up to 7 μm in AZ31 magnesium alloy with an initial grain size of 55 μm. The effect of microstructural evolution and surface features on wettability, corrosion resistance, bioactivity and cell adhesion were investigated with an emphasis to study the influence of deposited phases when the samples were immersed in simulated body fluid (SBF 5×). The role of microstructure was also evaluated without any surface treatments or coatings on the material. GPed samples exhibit improved hydrophilicity compared to the annealed sample. After immersion in SBF, specimens were characterized using scanning electron microscopy (SEM), energy dispersive X-ray (EDAX) analysis and X-ray diffraction (XRD) methods. More amount of white precipitates composed of hydroxyapatite and magnesium phosphate along with magnesium hydroxide was observed on the surfaces of groove pressed specimens as compared to the annealed specimens with an increase in immersion time in SBF. Corrosion behavior of the samples estimated using potentiodynamic polarization curves indicate good corrosion resistance for GPed samples before and after immersion in SBF. The MTT assay using rat skeletal muscle (L6) cells revealed that both the processed and unprocessed samples are nontoxic and cell adhesion was promising for GPed sample., (Copyright © 2013 Elsevier B.V. All rights reserved.)

Glass ionomer cements (GICs) are clinically attractive filling materials often employed in the field of dentistry as restorative and luting materials. The present work aims to formulate bioactive nanocrystalline calcium deficient hydroxyapatite (nCDHA)-GIC composite cements with improved mechanical and resorption properties of the set cement than GICs. The nCDHA was synthesized via an accelerated microwave process and characterized by X-ray powder diffraction (XRD) and Fourier transform infrared spectroscopy (FT-IR) methods. The synthesized nCDHA was mixed with GIC in different compositions (5, 10 and 15 wt%) maintaining the powder to liquid ratio. Cylinders of dimensions 8 mm height and 4 mm diameter were formed using a Teflon mold following a conventional cement forming technique. The XRD and FT-IR of the cylinders showed increased intensity and characteristic bands of CDHA with increase in nCDHA content. The surface cracks and the elemental composition of the set cements were analyzed by scanning electron microscopy (SEM) and energy dispersive X-ray analysis (EDX). Decreased surface hardness was observed for composite cements with increase in nCDHA addition. The cement cylinders were tested for ionic release in Millipore water (pH=7) via inductive coupled plasma (ICP) spectroscopy and in demineralization solution of pH=5 to find out the weight loss in an acidic environment at 37 °C performed periodically for 5 weeks. The ionic release percentage, weight loss and compressive strength were observed to increase with an increase in nCDHA addition., (Copyright © 2011 Elsevier Ltd. All rights reserved.)

Regeneration of fractured or diseased bones is the challenge faced by current technologies in tissue engineering. The major solid components of human bone consist of collagen and hydroxyapatite. Collagen (Col) and hydroxyapatite (HA) have potential in mimicking natural extracellular matrix and replacing diseased skeletal bones. More attention has been focused on HA because of its crystallographic structure similar to inorganic compound found in natural bone and extensively investigated due to its excellent biocompatibility, bioactivity and osteoconductivity properties. In the present study, electrospun nanofibrous scaffolds are fabricated with collagen (80 mg/ml) and Col/HA (1:1). The diameter of the collagen nanofibers is around 265 +/- 0.64 nm and Col/HA nanofibers are 293 +/- 1.45 nm. The crystalline HA (29 +/- 7.5 nm) loaded into the collagen nanofibers are embedded within nanofibrous matrix of the scaffolds. Osteoblasts cultured on both scaffolds and show insignificant level of proliferation but mineralization was significantly (p < 0.001) increased to 56% in Col/HA nanofibrous scaffolds compared to collagen. Energy dispersive X-ray analysis (EDX) spectroscopy results proved the presence of higher level of calcium and phosphorous in Col/HA nanocomposites than collagen nanofibrous scaffolds grown osteoblasts. The results of the present study suggested that the designed electrospun nanofibrous scaffold (Col/HA) have potential biomaterial for bone tissue engineering.

The eggshell waste has been value engineered to a nanocrystalline hydroxyapatite (HA) by microwave processing. To highlight the advantages of eggshell as calcium precursor in the synthesis of HA (OHA), synthetic calcium hydroxide was also used to form HA (SHA) following similar procedure and were compared with a commercially available pure HA (CHA). All the HAs were characterized by X-ray powder diffraction (XRD) method, Fourier transform infrared (FT-IR) spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM) and specific surface area measurements. Nanocrystalline nature of OHA is revealed through characteristic broad peaks in XRD patterns, platelets of length 33-50 nm and width 8-14 nm in TEM micrograph and size calculations from specific surface area measurements. FT-IR spectra showed characteristic bands of HA and additionally peaks of carbonate ions. The cell parameter calculations suggest the formation of carbonated HA of B-type. The OHA exhibits superior sinterability in terms of hardness and density than both SHA and CHA may be due to larger surface area of its spherulite structure. The in vitro dissolution study shows longer stability in phosphate buffer and cell culture test using osteoblast cells establishes biocompatibility of OHA.

The silver (0.5-3 at %) substituted nanosize hydroxyapatites (AgHAs) were synthesized by microwave processing. The X-ray diffraction (XRD) peaks are very broad, indicating that the AgHAs were of nanosize (30 nm). Transmission electron microscopy analysis shows needle-like morphology of AgHA, having length 60-70 nm and width 15-20 nm. The AgHA phase was stable up to 700 degrees C without any secondary phases. The antibacterial effect of AgHA against Escherichia coli and Staphylococcus aureus was observed by spread plate method, even for low concentration of silver ions (0.5%) with 1 x 10(5) cells/mL of respective bacterial culture, after a 48 h incubation period. However, some colonies of E. coli were seen with a high dose of 1 x 10(8) cells/mL after 24 h. The zone of inhibition by disc diffusion test method was found to vary with the amount of silver in the sintered AgHA pellets, for both the bacteria, after 24 h of inoculation. Osteoblast cell attachment in varying density was noticed on AgHA samples with 0.5, 1.0, and 1.5% silver substitution. However, osteoblast spreading was significantly greater on 0.5% AgHA compared to 1.0 or 1.5% substituted AgHA samples. Thus, the low amount of AgHA has a potential of minimizing the risk of bacterial contamination, without compromising the bioactivity, and is expected to display greater biological efficacy in terms of osseointegration.

Rapid synthesis of calcium deficient hydroxyapatite (CDHA, Ca(10-x)(HPO4)x(PO4)(6-x)(OH)(2-x)) with Ca/P ratio 1.5 was done by precipitation using calcium nitrate tetra-hydrate and phosphoric acid and subsequently subjecting to microwave irradiation in a domestic microwave oven for 15 min. Transmission electron microscopy analysis shows needle like morphology of CDHA having length 16-39 nm and width 7-16 nm. The synthesized CDHA has the characteristic HPO4(2-) vibration band at 875 cm(-1) in Fourier transform infrared (FT-IR) spectra. The X-ray powder diffraction (XRD) analysis shows a pattern corresponding to stoichiometric hydroxyapatite (HA) with broad peaks suggesting that CDHA particles were nanosized. Fourier transform Raman spectroscopy (FT-Raman) do not indicate any fluorescence band that is characteristic of non-stoichiometric HA. The thermal decomposition of CDHA to beta tricalcium phosphate (beta-TCP) was also studied for the additional confirmation. The nanosized CDHA was found to be stable up to 600 degrees C.

The partial conversion of coralline hydroxyapatite (HA) into tricalcium phosphate (TCP) catalyzed by the thermal decomposition of silver oxide was investigated. The thermal analysis of HA powder mixed with 5 mol % Ag2O indicated the decomposition of silver oxide to be around 550 degrees C in the presence of HA. Subsequently a functional gradient structure was formed by spreading silver oxide on one surface of the HA compact of diameter 10 mm and then firing at 700 degrees C in air. The X-ray powder diffraction analysis confirmed the formation of alpha-TCP induced by the Ag2O decomposition. The content of alpha-TCP of the sintered pellet was found to decrease with the increasing depth from the surface of the pellet. In vitro solubility study in phosphate buffer of pH 7.2 showed the stability of the biphasic material as in between HA and TCP., (Copyright 2000 Kluwer Academic Publishers)

The combined effect of titanium dioxide and silver oxide on the in situ formation of biphasic calcium phosphate ceramics was investigated. Titania (5-20 mol%) was mixed with pure hydroxyapatite (HA) or HA containing Ag2O (10-20 mol%) and was heated to 900 degrees C for 12 h. The sintered samples were found to contain tricalcium phosphate (beta-TCP) and other phases along with HA depending upon the amount as well as the type of the additives used as evidenced by X-ray powder diffraction (XRD) and fourier transform infrared (FT-IR) spectroscopic studies. Enhanced TCP formation with reduced impurity phases was observed with TiO2-Ag2O addition. In vitro solubility study in phosphate buffer at physiological conditions shows the resorbable nature of these materials. A functionally graded material (FGM) structure was formed by spreading TiO2-Ag2O mixture on the surface of the HA green compact and heating at 900 degrees C. The FGM shows gradient structure of TCP and HA from the surface to the interior of the pellet in addition to titania and silver phases.