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Method for preparing different particle sizes of porous beta-TCP microspheres by oil-in-water type solid emulsification

An oil-in-water microsphere technology, which is applied in the preparation of microspheres, prostheses, and pharmaceutical formulations, can solve the problems of success rate, high cost, and complexity of introducing antigenic substances, and achieve good biocompatibility and operation Simple, Widely Applicable Effects

Inactive Publication Date: 2017-06-27
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Although methods for preparing microspheres with different particle sizes while maintaining a porous structure have been reported from time to time in recent years, some methods have problems such as complexity, high cost, introduction of antigenic substances, and low success rate.

Method used

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  • Method for preparing different particle sizes of porous beta-TCP microspheres by oil-in-water type solid emulsification
  • Method for preparing different particle sizes of porous beta-TCP microspheres by oil-in-water type solid emulsification
  • Method for preparing different particle sizes of porous beta-TCP microspheres by oil-in-water type solid emulsification

Examples

Experimental program
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Embodiment 1

[0026] Weigh 3.9618g (NH4) 2 HPO 4 , 11.8075gCa (NO 3 ) 2 4H 2 Dissolve O in deionized water, and dilute to volume with a 100mL volumetric flask. 100mL(NH4) 2 HPO 4 The solution was slowly added dropwise to 90mL Ca(NO 3 ) 2 In the solution, the pH of the solution was adjusted to 7 with ammonia water. After the solution was aged for 24 hours, it was filtered, and the resulting precipitate was washed 5 times with deionized water, and the precipitate was placed in a refrigerator at -21°C for freeze-drying to obtain a nanoscale hydroxyapatite precursor. Weigh 0.5g of PVB and dissolve it in 10mL of dichloromethane solvent, stir for 12 hours, then weigh 1g of hydroxyapatite precursor and add it into the solution, and continue to stir for 3 hours to obtain a slurry. Dissolve 5g of PVA in 500mL of deionized water to obtain a PVA solution. Add the slurry dropwise to the PVA solution at 8°C and a rotation speed of 200rpm. After stirring for 3 hours, filter and wash with deioniz...

Embodiment 2

[0029] Weigh 0.5g of PVB and dissolve it in 15mL of dichloromethane solvent, stir for 12 hours, then weigh 1g of the hydroxyapatite precursor prepared in Example 1 and add it into the solution, stir for 3 hours to obtain a slurry. Dissolve 5g of PVA in 500mL of deionized water to obtain a PVA solution. Add the slurry dropwise to the PVA solution at 8°C and a rotation speed of 200rpm, stir for 3 hours, filter, wash with deionized water for 5 times, and freeze the obtained solid. After drying, precursor microspheres were obtained. The precursor microspheres were sintered in a muffle furnace to obtain porous β-TCP microspheres. The sintering procedure was as follows: from room temperature to 600°C, the heating rate was controlled at 2°C / min, kept at 600°C for 2 hours, and then heated at 5°C / min. The heating rate was raised from 600°C to 1100°C at a rate of min, kept at this temperature for 2 hours, and finally cooled to room temperature.

[0030] image 3 It is the SEM image of...

Embodiment 3

[0032] Weigh 0.5g of PVB and dissolve it in 10mL of dichloromethane solvent, stir for 12 hours, then weigh 1g of the hydroxyapatite precursor prepared in Example 1 and add it into the solution, stir for 3 hours to obtain a slurry. Dissolve 5g of PVA in 500mL of deionized water to obtain a PVA solution. Add the slurry dropwise to the PVA solution at 8°C and a rotation speed of 400rpm, stir for 3 hours, filter, wash with deionized water for 5 times, and freeze the obtained solid. After drying, precursor microspheres were obtained. The precursor microspheres were sintered in a muffle furnace to obtain porous β-TCP microspheres. The sintering procedure was as follows: from room temperature to 600°C, the heating rate was controlled at 2°C / min, kept at 600°C for 2 hours, and then heated at 5°C / min. The heating rate was raised from 600°C to 1100°C at a rate of min, kept at this temperature for 2 hours, and finally cooled to room temperature.

[0033] Figure 4 It is the SEM image of ...

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Abstract

The invention discloses a method for preparing different particle sizes of porous beta-TCP microspheres by oil-in-water type solid emulsification. The method includes the steps of subjecting a calcium nitrate solution and a hydrogen phosphate solution to mixed reaction to obtain a hydroxyapatite precursor, dispersing the hydroxyapatite precursor into a polyvinyl butyral-dichloromethane solution to obtain a mixed solution, subjecting the mixed solution and a polyvinyl alcohol solution to mixed reaction to obtain precursor microspheres, and sintering to obtain a target product, namely the porous beta-TCP microspheres. The method has the advantages that the particle size of the microspheres is controlled through oil-phase concentration and a rotation speed, and the prepared beta-TCP microspheres are porous, controllable in size and excellent in biocompatibility and can be applied to the field of biological materials such as bone tissue engineering.

Description

technical field [0001] The invention belongs to the technical field of biomaterials, and in particular relates to a method for preparing porous β-TCP microspheres with different particle sizes by using oil-in-water solid emulsification. Background technique [0002] Treatment of bone tissue damage caused by congenital diseases, accidents, tissue lesions, etc. is a major problem in orthopedics. The self-healing or healing difficulty caused by bone tissue damage has derived a lot of treatment methods to achieve the normal life activities of patients. Traditional treatment methods include cartilage drilling, autologous or allogeneic cartilage transplantation, etc. However, these methods have their own defects and are difficult to be widely used in clinic. Bone tissue engineering scaffolds emerged as the times require, which overcome or improve the above difficulties and bring benefits to patients with bone tissue injuries. [0003] Calcium phosphate is an important inorganic...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J13/02A61L27/56A61L27/50A61L27/12
CPCA61L27/12A61L27/50A61L27/56A61L2400/06A61L2430/02B01J13/02
Inventor 王友法赵洋籽戴红莲
Owner WUHAN UNIV OF TECH
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