Synthesis Of Nano-hydroxyapatite Research Articles

Impact of Alkaline Immersion Time on Nano-Hydroxyapatite Synthesis from Broiler Eggshells with Electrochemical Method Using Constant Direct Current (CDC)

Calcium phosphate is widely used in biomaterials, especially as a bone substitute. One of the calcium phosphate compounds that is widely used is hydroxyapatite. In biomedical applications, nano-sized hydroxyapatite particles have better bioactivity than coarse crystals. Hydroxyapatite can be synthesized from various sources of calcium and phosphate. Broiler eggshells were chosen as a source of calcium in this study because they have a relatively high calcium content. The method used in the synthesis of nano-hydroxyapatite in this research is the electrochemical method. This research aims to examine the effect of varying NaOH immersion time on the size and structure of calcium phosphate particles produced using an electrochemical method made from chicken egg shells. The synthesis of nano-hydroxyapatite from chicken egg shells was carried out in 4 stages: material preparation, electrolysis, precipitate immersion, and characterization. Nanometer-sized particles can be acquired through an immersion process lasting at least four hours, and it is observed that the longer the duration of immersion, the greater the resemblance of the resulting structure to hydroxyapatite.

О применении нанотехнологий в ветеринарной и человеческой ортопедии: имплантация и протезирование

The field of orthopedic implant materials has advanced greatly in recent years, with synthetic materials on the forefront of development. The use of biocompatible polymers has allowed for the creation of materials capable of reproducing anatomical structures, resorbing over time, or eliciting specific biological responses. Polyurethanes are particularly suitable for mechanical orthopedic devices, and nanotechnology has emerged as a critical component in improving orthopedic implants. Synthetic materials also allow for the modeling of implant behavior, thus increasing the likelihood of successful implantation procedures. The development of new composite coating methods that better mimic bone structure would lead to the creation of a new generation of orthopedic implants with improved implant integration and bone healing. The addition of antibiotics to nanohydroxyapatite mixtures has been shown to prevent bacterial growth, increasing the chances of successful infection treatment and reducing the risk of implant rejection. The use of spherical nanoparticles in nanohydroxyapatite synthesis allows for the creation of powders that can be formed into any desired shape, such as screws, plates, and other forms. In conclusion, synthetic materials hold the significant potential for improving orthopedic implant technology, offering a range of possibilities for reproducing anatomical structures, eliciting biological responses, and resorbing over time. The use of polyurethanes, nanotechnology, and composite coatings offers promising avenues for future development, while the addition of antibiotics to nanohydroxyapatite mixtures and the use of spherical nanoparticles in synthesis represent significant advances in the field.

A study on the development of scaffold fabrication using citric acid polyester – nanohydroxyapatite composite

ABSTRACT. Nano hydroxyapatite (n-HAp) and its composites have shown a great development in the field of tissue regeneration and in controlled drug delivery due to its good biocompatibility and bioactivity behavior. Furthermore, HAp-based nanocomposites enhance mechanical properties. These synthetic HAp nanocomposites can also be tailored to fabricate scaffold with controlled porosity which facilitate the growth of the cell in the field of tissue engineering. In this paper, we focus on the synthesis of nano hydroxyapatite (n-HAp) by sol-gel method. The synthesized nano powders were calcined at 500 oC and characterized by FT-IR, XRD and TEM. We have also described the synthesis of citric acid-based polyester by melt polycondensation method without adding catalyst. The monomers used were citric acid, 1,6-hexane diol and sebacic acid. The corresponding synthesized n-HAp/polyester composite have potential application in soft tissue engineering. The structures of polyester and its nanocomposite were studied by FT-IR and 1H NMR spectral studies. The thermal and mechanical properties of polyester, composites and cytotoxicity activity (MTT assay) using vero cells were also studied. Porous scaffold of the nano HAp/Polyester was fabricated by solvent-casting particulate leaching technique which is useful in the development of tissue engineering applications. SEM and TEM studies were carried out for nano HAp, polyester, composites and scaffold.
 
 KEY WORDS: Cytotoxicity, Polycondensation, Sol-gel, Solvent-casting, Tissue engineering
 Bull. Chem. Soc. Ethiop. 2022, 36(4), 923-934. 
 DOI: https://dx.doi.org/10.4314/bcse.v36i4.17

Synthesis of nano hydroxyapatite from Hypopthalmichthys molitrix (silver carp) bone waste by two different methods: a comparative biophysical and in vitro evaluation on osteoblast MG63 cell lines.

More than a thousand tonnes of fish bone wastes can be transformed into biomedical products annually. Alkaline hydrolysis and thermal calcification were used to create nanosized hydroxyapatite (HAp) crystals from Silver carp bone wastes. Biophysical tests were used to determine the nano size and chemical composition of synthesised hydroxyapatite. Alkaline hydrolysis hydroxyapatite (AH-HAp) was 58.3nm, while Thermal calcination hydroxyapatite (TC-HAp) was 64.3nm in size, confirmed by Atomic Force Microscopy. Energy Dispersive X-ray Analysis studies showed Ca/P (Calcium phosphate) ratio of AH-HAp to be 1.65, whereas TC-HAp as 1.45, confirming AH-HAp to be organically rich along with a similar Ca/P ratio as natural HAp. Fourier Transform Infrared Spectroscopy spectra indicated HAp formation from both procedures, however AH-HAp had superior crystallinity than TC-HAp confirmed from X-Ray Diffraction spectra. MG63 osteoblast cell lines showed 91% cell viability in cytotoxicity studies and 70.1% proliferation efficiency in Alkaline Phosphatase assay, which was higher than TC-HAp. The present study shows that HAp produced via alkaline hydrolysis has better biocompatibility which enhances its applicability as a biomaterial, than HAp synthesized through thermal calcination, which tends to incinerate organic moieties.

The calcination temperature effect in the synthesis of nanohydroxyapatite: characterization and its application as a nanocarrier

Drug delivery is the process of administering drugs at a specific amount in a specific site. Hydroxyapatite (HA) is reported as a drug carrier because of its unique properties such as high biodegradability, biocompatibility and drug-loading capacity, easy preparation, sterilization and cost-effective production. In the present study, the nanohydroxyapatite was synthesized at various calcination temperatures by the sol–gel route. The results revealed that the synthesized HA at 700 °C had the highest crystallinity. Moreover, the loading content of ampicillin was studied on HA samples synthesized at different calcination temperatures. It is considered that synthesized HA at 500 °C provided appropriate surface for ampicillin loading. The synthesized HA was characterized by scanning electron microscopy, X-ray diffraction, Fourier transform infrared and UV/Vis spectroscopy techniques before and after ampicillin loading.

Optimization of a lab scale and pilot scale conversion of eggshell biowaste into hydroxyapatite using microwave reactor

The high demand for synthetic hydroxyapatite for biomedical applications is on the rise day by day at the same time, there is a pressing need for producing hydroxyapatite (HA) at an economically viable cost to make the treatment affordable to everyone. In order to meet this objective, recycling of waste to value added products and cost effective methods suitable for scaling up the process are being attempted by researchers. In this report, an attempt has been made to optimize the parameters for the synthesis of nano HA from eggshell biowaste using well explored microwave method by employing a lab scale and pilot scale microwave reactors. Several parameters such as pH, organic modifier concentration and microwave power against volume of the reaction mixture has been studied from the view point of enhancing the yield of the product. The preliminary experiments done using lab scale reactor helped the optimization of pH and EDTA concentration. From the lab scale experiments, we found that the yield was directly proportional to the microwave power. The parameters optimized in the lab scale has been carried over to the pilot scale reactor. The results from pilot scale reactor revealed that although the microwave power from pilot scale reactor is considerably higher than that of the maximum power (900 W) of the lab scale reactor there is no significant difference in the yield of the product but the microwave irradiation time has reduced considerably which is almost in proportion to the power of the reactor. Parameters optimized from these batch processes will be useful for devising new scaling up process such as continuous flow methods.

Synthesis of Nano-Hydroxyapatite from Snakehead (<i>Channa striata</i>) Fish Bone and its Antibacterial Properties

Nano-hydroxyapatite was synthesized by coprecipitation method and tested its antibacterial properties. Nano-hydroxyapatite was synthesized using CaO precursors from snakehead (Channa striata) fish bones and (NH4)2HPO4. The synthesis was carried out with temperature variations of 30, 60, 80, and 100 °C. Antibacterial activity was determined using two types of bacteria, namely gram-positive and gram-negative. The XRD spectra show that the highest peak is hydroxyapatite synthesized at a temperature of 100 °C. Hydroxyapatite produced from various synthesis temperatures has the size of nanoparticles in the range 37.32-49.27 nm. The nano-hydroxyapatite functional groups are characterized using FTIR, the analysis indicate the presence of OH, CO32‒ and PO43‒. The molar ratio Ca/P is obtained of 1.71 approaching theoretical hydroxyapatite of 1.67. The resulted nano-hydroxyapatite has significant antibacterial properties to Escherichia coli and Staphylococcus aureus.

Synthesis of Nanohydroxyapatite from Cuttlefish Bone (Sepia sp.) Using Milling Method.

The synthesis of nanohydroxyapatite from cuttlefish bone (Sepia sp.) has been done by using High Energy Milling (HEM) and its characterization in vitro as bone repair. This study aimed to determine the effect of the milling process on microscopic properties and mechanical properties of nano-HA through XRD, TEM, and compressive strength tests. The hydroxyapatite (HA) used in this study consisted of 1M CaCO3 from aragonite which was extracted from cuttlefish lamella bone (Sepia sp.) and 0.6 M NH4H2PO4, which was hydrothermally processed at 200°C for 12 h and then sintered at 900°C for 1h. Parameter milling includes the variation of milling time, i.e., 3 h, 6 h, and 9 h at rotational speed of 350 rpm. An increase in milling time causes a decrease in HA particle size. This is shown from the results of TEM at the milling time of 9 h with the smallest size up to 65 nm. The result of cell viability test showed that all samples are not toxic with cell viability value of >80%. The milling time of 9 h was an optimum condition with a compressive strength of 4.35952 MPa that can be applied to cancellous bone.

GDMS Analysis Of Calcium Carbonate Naturaly Doped By REE, Phospates And Other Impurities

A mathematical model was developed for calculation of types and intensities of molecular interferences and simulation of mass-spectra at GDMS analysis of non-conducting samples with the use of a secondary cathode. An improved design of the cell with Ta-secondary cathode were suggested enhancing the matrix to tantalum ion current ratio and sensitivity of the analysis in ca. 1.5 orders of magnitude. The model have been used for interpretation of complicate mass-spectra of calcium carbonate naturally doped with REE, phosphates and other impurities. Comparison calculated and experimental mass-spectra of VG9000 instrument demonstrates good agreement and allows select the most suitable isotopes and rejecting wrong molecular peaks. It have been shown that electrons in glow discharge plasma have different temperatures in different zones that reveals itself as separate Boltzmann populations of ionization levels for molecules, metal atoms and argon atoms/ions. Calcium carbonate is widely used for many application including as precursor for nano-hydroxyapatite synthesis. Calcium carbonate was precipitated from natural mine waters and was used as model object having high number of various impurities allowing to investigate the impact of complicate molecular ions, determine necessary resolving power of the GD-instruments to meet required detection limit.

Effects of ultrasonic agitation time on wet chemical synthesis of nanohydroxyapatite

In this study, the synthesis of the nanohydroxyapatite (nHAp) powders by way of wet chemical method is reported. Calcium nitrate tetrahydrate (Ca(NO3)2·H2O) and dibasic ammonium phosphate ((NH4)2HPO4) were used as calcium and phosphorus sources, respectively. The effect of ultrasonic agitation time has been systematically studied between 30 and 150 min at the temperature of 70°C. Structural, morphological, spectroscopic and thermal analysis have been carried out by way of X-ray powder diffraction, scanning electron microscopy, Fourier-transform infrared spectroscopy and Raman spectroscopy and thermogravimetry–differential scanning calorimetry analysis. It is shown that the ultrasonic agitation conditions significantly affect the crystallite size, dislocation density and microstrain of the powders calculated by way of the Debye–Scherrer formula. Thermal analyses reveal that the ultrasonic agitation treatment has a very beneficial effect on the fabrication of the powders by the wet chemical method due to the inhibition of physisorbed and chemisorbed water and the calcium deficiency. Magnetic stirring treatment is found to lead to larger nHAp nanoparticle agglomerations due to more water absorption. The results offer a promising route towards the scalable synthesis of the pure-phase nHAp powders with controllable structural and morphological properties, which could be useful in various types of basic and applied research on HAp-based materials.

Effect of Current Density on Nano-Hydroxyapatite Synthesis from Chicken Eggshell Using Electrochemical Method with Constant Direct Current (CDC)

Effect of Current Density on Nano-Hydroxyapatite Synthesis from Chicken Eggshell Using Electrochemical Method with Constant Direct Current (CDC)

Effect of pH on Nano-Hydroxyapatite Synthesis from Chicken Eggshell Prepared by Electrochemical Method

Effect of pH on Nano-Hydroxyapatite Synthesis from Chicken Eggshell Prepared by Electrochemical Method

Properties of iron-containing nanohydroxyapatite-based composites

The paramagnetic properties of compounds resulting from the synthesis of nanohydroxyapatite in the presence of Fe(III) ions have been studied by electron paramagnetic resonance, Mossbauer spectroscopy, and magnetochemistry. Based on the obtained results on the mechanism of the reaction between an orthophosphoric acid solution and an aqueous calcium hydroxide suspension, we have found conditions for incorporating Fe(III) impurity ions into hydroxyapatite. We have studied samples differing in the sequence in which reagents were mixed and in hydroxyapatite crystallite formation conditions. It has been shown that, in all instances, the composition and properties of the iron-containing phases in the composites depend significantly on both synthesis and heat treatment conditions.

Greener Synthesis of Nano Hydroxyapatite using Fatty acids template for the application of Tissue Engineering Nano Hydroxyapatite: Fatty acids Synthesis and Characterizations

Nano-hydroxyapatite (nano-HAp) is significant import as a bio-ceramic material for use in orthopedic applications because of its comparability in size, crystallography and substance creation with human hard tissue. In this present study, the biologically high interest of nano-HAp was synthesized as green template mode approaches using the various fatty acids like linoleic acid, lauric acid, and oleic acid. The influence of the fatty acid for the formations nano- HAp structure and nature of fatty acid during synthesis was investigated. The nano-HAp functionality, crystallinity, and morphology were determined by FTIR, XRD, and SEM techniques, respectively. The biocompatibility of HAp on MG63 cell line was confirmed by in vitro MTT assay method. The in-vitro studies showed better biocompatibility and cell proliferation results on the template assist synthesized nHAP. These results indicate that nHAp form the green methodology could be a promising material for bone tissue engineering.

Synthesis of nanohydroxyapatite in the presence of iron(III) ions

The effect of small amounts of iron(III) ions on the morphology, phase composition, and structure of the products of the hydroxyapatite (HAP) synthesis has been studied by electron microscopy, X-ray powder diffraction, and Mossbauer spectroscopy methods. It has been demonstrated that the introduction of dopant iron(III) ions into the reaction mixture at different stages of HAP formation makes it possible to control crystal growth, morphology, and phase composition. The iron ions are not incorporated into the HAP crystal structure; rather, they form their proper nanophase, as well as adsorption clusters on the HAP surface.

Sono-synthesis of nanohydroxyapatite: Effects of process parameters

Hydroxyapatite (HA) [Ca10(PO4)6(OH)2] is a bioactive ceramic with excellent osteoconductive properties. This characteristic helps HA to be integrated into the bone without provoking an immune reaction, thus making it a useful biocompatible material for load bearing bone implant. In this study, nanohydroxyapatite (NHA) was synthesised using a precipitation method assisted with ultrasonication. The process parameters such as ultrasonic time (t) (10–30min), ultrasonic amplitude (A) (50–70%), solution temperature (T) (50–90°C), and solution pH (7–9) were varied on the basis of single factor and their effects on NHA synthesis was investigated. Besides that, the effect of calcination on the NHA powder morphology was also studied by varying the calcination time (2, 4 and 6h) and temperature (400, 800 and 1200°C). The characterisations of the synthesised NHA powder were conducted using thermogravimetric analysis (TGA), field emission scanning electron microscope (FESEM), energy-dispersive X-ray spectroscopy (EDX), X-ray diffraction (XRD), Brunauer–Emmett–Teller (BET), transmission electron microscope (TEM), zeta-sizer and Fourier transform infrared spectroscopy (FTIR). It was found that nano-sized HA particles can be produced at optimum set of process parameters of t=25min, T=90°C, A=65%, and pH=8. Results revealed that the thermal stability, morphology and crystallinity of the NHA powder was further improved by calcinating the powder at optimum temperature and time of 800°C and 2 h, respectively.

Synthesis of Nano Hydroxyapatite: Application in Drug Delivery of Sulfasalazine

In this work we synthesized Nano hydroxyapatite (HAp) by Solgel method, Then we functionalized hydroxyapatite nanoparticle by use of 3-Aminopropyl trimethoxysilane (APTMS) , to improve the loading and control release of sulfasalazine drug bonded to APTMS. The drug release patterns from Sulfasalazine loaded HAp nanoparticles at pH value 8 For 6h, Sulfasalazine loaded functionalized HAp nanoparticles (Sulfasalazine loaded HApAPTMS) at pH value 8 as in the intestine for 48h. Moreover, the functionalized HAp showed relatively slower release rate of sulfasalazine compare with non functionalized HAp. because the strong ionic interaction between NH2 group in sulfasalazine in HAp-APTMS. On other side, the functionalized HAp loaded more drug than pure HAp. The synthesized nanoparticles and functionalized HAp characterized by Scanning Electron Microscopy (SEM), X-ray Diffraction (XRD), Fourier transform infrared (FT-IR) and UV/Vis analysis techniques. Then the obtained material was studied in the simulated body fluid (SBF) to this investigated storage and release properties.

Preparation and coating of nano-ceramic on orthopaedic implant material using electrostatic spray deposition

The objective of the present manuscript was the synthesis of nano hydroxyapatite (n-HA) and its coating on orthopaedic implant material. The synthesis of n-HA has been achieved using wet chemical method. The elemental analysis and FTIR spectrum confirmed the formation of n-HA having a Ca/P ratio of 1.71. The AFM and XRD results showed the nano dimensions of hydroxyapatite (HA) in the range of 25–35 nm. Scanning electron micrographs (SEM) showed a flake-like structure of n-HA having sharp edges. The n-HA was further coated on orthopaedic implant material (titanium alloy, Ti6Al4V), using the electrostatic spray deposition (EDS) technique. The surface roughness of Ti alloy increased from 2.34 μm to 2.77 μm after coating with n-HA and corrosion resistance improved drastically. XRD pattern of n-HA coated Ti alloy however showed broadening of HA associated peak, reflecting change from crystalline to amorphous phase of n-HA.

Synthesis of Nano-hydroxyapatite via Microbial Method and Its Characterization

Nanoparticles of hydroxyapatite were successfully synthesized by microbial method at ambient temperature and pressure, using calcium chloride and specific substrate as reactants. The compositional and morphological properties of products of the syntheses were studied by means of X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM), and thermogravimetric analysis (TGA). The characterization data obtained showed that the phase composition, functional groups, and surface morphology of samples obtained by microbial method were mainly similar to that by chemical precipitation method. The hydroxyapatite powder was shown to be nanometer-grade in size and sphere-like in shape.

Influence of the Precipitation Temperature on Properties of Nanohydroxyapatite Powder for the Fabrication of Highly Porous Bone Scaffolds

The aim of the present work is to study the influence of the precipitation temperature in the synthesis of nanohydroxyapatite (n-HAp) on the properties of the resulting n-HAp powder for the fabrication of highly porous scaffolds for bone tissue engineering. The n-HAp powder was obtained by a wet precipitation technique starting from calcium nitrate tetrahydrate (Ca (NO3)2*4H2O) and phosphoric acid (H3PO4) at different temperatures: 10°C, 37°C and 50°C. Highly porous scaffolds were fabricated using the three different powders by the sponge replica method and sintering at 1300°C. Combined X-ray diffraction (XRD) and transmission electron microscopy (TEM) analyses on powders indicated that on increasing the precipitation temperature the formation of pure n-HAp is accelerated, without significant changes in particles morphology and size. Scaffolds characterized by high porosity (89%) and good compressive strength (0.53 MPa for n-HAp prepared at 37°C) were obtained. XRD analyses on sintered n-HAp confirmed the thermal stability of the material. Therefore, the as-synthesized n-HAp powder can be successfully used for the fabrication of highly porous scaffolds as bone substitutes.