Method for preparing hydroxyapatite nano-structure microspheres

A technology of hydroxyapatite and nanostructure, applied in the direction of nanotechnology, chemical instruments and methods, phosphorus compounds, etc., to achieve obvious slow-release effect, simple preparation process, and good biocompatibility

Inactive Publication Date: 2011-08-17
HEFEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method is relatively simple, but only one shape of hollow spherical nano-hydroxyapatite is o...

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  • Method for preparing hydroxyapatite nano-structure microspheres
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  • Method for preparing hydroxyapatite nano-structure microspheres

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Embodiment 1

[0027] The preparation method of hydroxyapatite nanostructure microspheres in this embodiment is as follows:

[0028]Take 2mL of 0.4mol / L calcium chloride and 2mL of 0.24mol / L diammonium hydrogen phosphate solution and mix, the solution appears turbid, after adjusting the pH of the system to 1 with 1mol / L hydrochloric acid, the solution becomes clear, and the molar ratio n( Urea): n(Ca 2+ )=5:1, n(disodium edetate):n(Ca 2+ )=1:50, V(glycerol):V(H 2 (O)=9:1 add urea, edetate disodium and glycerol, the solution total volume is 40mL after completely dissolving, the concentration of calcium chloride is 0.02mol / L, and the concentration of diammonium hydrogen phosphate is 0.012mol / L , the solution was transferred to a 50mL autoclave, and a solvothermal synthesis reaction was performed at 100° C. for 5 hours to obtain hydroxyapatite nanostructure microspheres.

[0029] Depend on figure 1 a and figure 2 a, b analysis shows that the product is a hexagonal hydroxyapatite hollow na...

Embodiment 2

[0031] The preparation method of hydroxyapatite nanostructure microspheres in this embodiment is as follows:

[0032] Take 10mL of 0.4mol / L calcium chloride and 10mL of 0.24mol / L diammonium hydrogen phosphate solution and mix respectively, the solution appears turbid, after the pH of the system is adjusted to 0.5 with 2mol / L hydrochloric acid, the solution becomes clear, and the molar ratio n( Urea): n(Ca 2+ )=3:1, n(citric acid):n(Ca 2+ )=1:30, V(glycerol):V(H 2 (2)=1:1 add urea, citric acid and glycerol, after dissolving completely, total solution volume is 40mL, and calcium chloride concentration is 0.1mol / L, and diammonium hydrogen phosphate concentration is 0.06mol / L, and solution is transferred to A 50mL autoclave adopts a solvothermal synthesis reaction at 85°C for 10 hours to obtain hydroxyapatite nanostructured microspheres.

[0033] Depend on figure 1 b and figure 2 c, d analysis shows that the product is a hexagonal hydroxyapatite solid nanostructure microsphe...

Embodiment 3

[0035] The preparation method of hydroxyapatite nanostructure microspheres in this embodiment is as follows:

[0036] Take 20mL of 0.4mol / L calcium chloride and 20mL of 0.24mol / L diammonium hydrogen phosphate solution and mix, the solution appears turbid, adjust the pH of the system to 3.5 with 0.5mol / L nitric acid, and the solution becomes clear. (Urea): n(Ca 2+ )=10:1, n(disodium edetate):n(Ca 2+ )=1:25 add urea and disodium edetate, the total volume of the solution after dissolution is 40mL, the concentration of calcium chloride is 0.2mol / L, the concentration of diammonium hydrogen phosphate is 0.12mol / L, and the solution is transferred to The 50mL autoclave adopts solvothermal synthesis reaction at 140°C for 3 hours to obtain hydroxyapatite nanostructure microspheres.

[0037] Depend on figure 1 c and figure 2 e, f analysis shows that the product is hexagonal hydroxyapatite solid nanostructure microspheres. composed of nanosheets. The specific surface area of ​​the ...

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Abstract

The invention discloses a method for preparing hydroxyapatite nano-structure microspheres, which comprises the following steps of: mixing a calcium source and a phosphorus source in a molar ratio of n(Ca2+) to n(PO43-) of 5:3; adding water into the mixture and regulating the pH of a system to the range of 0.5 to 3.5 by acid; then adding a chelating agent and urea; adding glycerine; and preparing the hydroxyapatite nano-structure microspheres by a solvent thermal synthesis method, wherein the volume ratio of glycerine to water is 0-12:1 and the concentration of the calcium source is in the range of 0.02 to 0.2mol/L. The method adopts a one-step synthesis mode. A surfactant is not used. The method has simple preparation process and relatively mild reaction condition. The hydroxyapatite nano-structure microspheres have good biocompatibility and large specific surface area and have loading rate and obvious release effect when being used as a medicament release carrier.

Description

1. Technical field [0001] The invention relates to a preparation method of hydroxyapatite nanostructured microspheres and their application as drug slow-release carriers. 2. Background technology [0002] Hydroxyapatite (Ca 10 (PO 4 ) 6 (OH) 2 ) is the main inorganic component in the bones and teeth of vertebrates, has good biocompatibility, high chemical stability, and does not produce harmful substances after degradation. Hollow nanostructures such as hollow nanospheres, hollow capsules, and nanotubes have the characteristics of large internal space, low density, large specific surface area, and strong surface permeability, which make them have broad application prospects in catalysts, drug release, and transportation. . Nanostructured hydroxyapatite has attracted the attention of scientific and technological personnel in recent years in the fields of catalyst carrier, bone defect filling, bioseparation, heavy metal adsorption and separation, especially in drug sustai...

Claims

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Application Information

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IPC IPC(8): C01B25/32B82Y40/00A61K47/02
Inventor 张卫新张晓静杨则恒
Owner HEFEI UNIV OF TECH
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