Fluorescently-labeled hydroxyapatite hollow microsphere and preparation method thereof

A hydroxyapatite and fluorescent labeling technology, applied in the fields of biomedical materials and optical functional materials, can solve the problems of easy attenuation of fluorescence intensity, physiological toxicity, etc., and achieve the effect of avoiding environmental pollution and solving fluorescence attenuation.

Inactive Publication Date: 2014-07-02
KUNMING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to overcome the problems of easy attenuation of fluorescence intensity and physiological toxicity in existing materials, and provide a fluorescent label with adjustable aperture, luminescent color and intensity, good luminescence stability, good physiological compatibility and stable chemical structure Hydroxyapatite hollow microspheres and a preparation method thereof, realized through the following technical scheme

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] A. Eu(NO 3 ) 3 and a calcium hydroxide solution with a concentration of 0.01mol / L, the Eu(NO 3 ) 3 dissolved in a calcium-containing solution to obtain solution I;

[0026] B. Prepare a phosphoric acid solution with a concentration of 0.01mol / L;

[0027] C. According to the molar ratio of Eu ion, Ca ion and phosphate ion is 0.01: 0.99: 0.6, take the solution I obtained in step A and the phosphoric acid solution obtained in step B, and mix the obtained solution I and the phosphoric acid solution under 50w ultrasonic treatment, At the same time, alkali solution is added to adjust the pH value to 10 to form a suspension system II of nano-hydroxyapatite sol;

[0028] D. Place the suspension system II obtained in step C at 20°C for aging in an autoclave for 24 hours, then wash and dry to obtain the chemical composition formula Ca 0.99 Eu 0.01 (PO 4 ) 0.6 (OH) 0.2 Fluorescently labeled hydroxyapatite powder;

[0029] E. The fluorescently labeled hydroxyapatite...

Embodiment 2

[0033] A. According to the molar ratio of (Er ion + Ho ion) to Ca ion is 0.1︰0.9, take Er(NO 3 ) 3 、Ho(NO 3 ) 3 and a calcium nitrate solution with a concentration of 0.2mol / L, Er(NO 3 ) 3 、Ho(NO 3 ) 3 dissolved in calcium nitrate solution to obtain solution I;

[0034] B. The preparation concentration is the diammonium hydrogen phosphate solution of 0.133mol / L;

[0035] C. According to (Er ion+Ho ion), the molar ratio of Ca ion and phosphate ion is 0.1︰0.9︰0.6, get the solution I obtained in step A and the phosphate solution obtained in step B, and combine the solution I and the phosphate solution in Mix under 20w ultrasonic treatment, and add ammonia water to adjust the pH value to 10.5 at the same time, forming the suspension system II of nano-hydroxyapatite sol;

[0036] D. Place the suspension II obtained in step C in an ultrasonic field for 30 hours at 160°C, and then wash and dry to obtain the chemical composition formula Ca 0.9 Er0.05 Ho 0.05 (PO 4 ) 0....

Embodiment 3

[0041] A. According to the molar ratio of (Sm ion + Tm ion + Tb ion) to Ca ion is 0.09︰0.91, take Sm(NO 3 ) 3 , Tm(NO 3 ) 3 , Tb(NO 3 ) 3 and a calcium nitrate solution with a concentration of 3mol / L, the Sm(NO 3 ) 3 , Tm(NO 3 ) 3 , Tb(NO 3 ) 3 dissolved in calcium nitrate solution to obtain solution I;

[0042] B. Prepare a disodium hydrogen phosphate solution with a concentration of 3mol / L;

[0043] C. According to (Sm ion+Tm ion+Tb ion), the molar ratio of Ca ion and phosphate ion is 0.09︰0.91︰0.6, take the solution I obtained in step A and the disodium hydrogen phosphate solution obtained in step B, and mix the obtained solution I with phosphoric acid The disodium hydrogen solution was mixed under 80w ultrasonic treatment, and ammonia water was added to adjust the pH value to 11 at the same time to form a suspension system II of nano-hydroxyapatite sol;

[0044] D. Put the suspension system II obtained in step C at 80°C in a magnetic field to age for 36 hou...

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Abstract

The invention discloses a fluorescently-labeled hydroxyapatite hollow microsphere and a preparation method thereof. The fluorescently-labeled hydroxyapatite hollow microsphere has a chemical formula of Ca (1-x) Rex (PO4) 0.6 (OH)0.2, wherein x is 0.005-1 and RE is one or several of Eu, Er, Ho, Pr, Tm, Sm and Tb; the outside diameter of the microsphere is 100-600mu m; and the wall thickness of the microsphere is 30-100mum. The preparation method comprises the following steps: preparing a mixed solution of calcium salts and RE (NO3)3 and phosphate solution or phosphoric acid; then fully mixing the mixed solution and the phosphate solution or phosphoric acid under ultrasonic treatment; adding an aqueous water of sodium carboxymethylcellulose; impregnating a styrene microsphere; and carrying out drying, thermal treatment and sintering to obtain the fluorescently-labeled hydroxyapatite hollow microsphere. According to the fluorescently-labeled hydroxyapatite hollow microsphere, the luminous colors and strength adjustment of the microsphere can be realized, so that the fluorescently-labeled hydroxyapatite hollow microsphere has higher application flexibility; according to the preparation method, due to the selection of hydroxyapatite and rare earth ions which have relative-favorable biocompatibility, the problems of fluorescence decay and the like caused by change of an organic structure are solved while environment pollution or physiology toxicity can be avoided.

Description

technical field [0001] The invention relates to a fluorescent-labeled hydroxyapatite hollow microsphere and a preparation method thereof, belonging to the technical fields of biomedical materials and photofunctional materials. Background technique [0002] Due to the characteristics of large specific surface area, strong adsorption, large agglutination and strong surface reaction ability, functional microspheres have been widely studied and applied, and people have given them various characteristics according to different uses, such as biospecific binding, Magnetic properties have been extensively studied. As one of them, fluorescent microspheres refer to solid particles with diameters ranging from nanometers to micrometers, loaded with fluorescent substances, and capable of emitting fluorescence when excited by external energy. Compared with ordinary fluorescent compounds, they have a relatively uniform shape and size, and their luminescent properties are relatively stable...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K9/00
Inventor 宋志国邱建备尹兆益杨正文周大成
Owner KUNMING UNIV OF SCI & TECH
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