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Rare-earth-doped calcium phosphate fluorescent nanoparticles, and preparation method and application thereof

A technology of rare earth doping and fluorescent nanotechnology, applied in biochemical equipment and methods, fluorescence/phosphorescence, chemical instruments and methods, etc., can solve problems such as difficult element ratio, uneven distribution of doped elements, and easy powder agglomeration. Achieve the effects of low synthesis temperature, high fluorescence intensity, and reduced agglomeration

Active Publication Date: 2015-11-04
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the particles prepared by the precipitation method have the disadvantages of easy powder agglomeration, difficult precise control of element ratio, and uneven distribution of doping elements.

Method used

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  • Rare-earth-doped calcium phosphate fluorescent nanoparticles, and preparation method and application thereof
  • Rare-earth-doped calcium phosphate fluorescent nanoparticles, and preparation method and application thereof
  • Rare-earth-doped calcium phosphate fluorescent nanoparticles, and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] First, configure Ca(NO 3 ) 3 , Eu(NO 3 ) 3 and Gd(NO 3 ) 3 50ml of mixed solution, control Ca 2+ 、Eu 3+ and Gd 3+ The total concentration of is 0.0334mol / L, wherein (Eu+Gd) / (Eu+Gd+Ca) molar percentage is 4%, and the Eu / Gd molar ratio is Eu:Gd=2:2. According to the concentration of PAA after adding is 0.5mg / ml, accurately weigh 25mg of PAA, add to Ca(NO 3 ) 3 , Eu(NO 3 ) 3 and Gd(NO 3 ) 3 The mixed solution was sonicated with a high-energy ultrasonic probe for 4 minutes to obtain a colloidal solution. Then, configure (NH 4 ) 2 HPO 4 Aqueous solution 50ml, control PO 4 3- The concentration is 0.02mol / L. According to the molar ratio (Ca+Eu+Gd) / P=1.67, 50mL (NH 4 ) 2 HPO 4 Quickly pour the aqueous solution into the colloidal solution obtained above, stir and mix evenly, add dilute nitric acid to adjust the pH value to 3, and evaporate the obtained colloidal solution in a water bath at 80°C until its volume is reduced to 25ml to obtain a gel. Finally, ...

Embodiment 2

[0036] First, configure Ca(NO 3 ) 3 , Eu(NO 3 ) 3 and Tb(NO 3 ) 3 50ml of mixed solution, control Ca 2+ 、Eu 3+ and Tb 3+The total concentration is 0.1002mol / L, the molar percentage of (Eu+Tb) / (Eu+Tb+Ca) is 4%, and the molar ratio of Eu / Tb is Eu:Tb=2:2. According to the concentration after the addition of PAA is 0.3 mg / ml, 15 mg of PAA was quantitatively weighed, added to the mixed solution obtained above at room temperature, and sonicated with a high-energy ultrasonic probe for 4 minutes to obtain a colloidal solution. Then, configure (NH 4 ) 2 HPO 4 Aqueous solution, control PO 4 3- The molar concentration is 0.0668mo1 / L. According to the molar ratio (Ca+Eu+Tb) / P=1.5, 50mL (NH 4 ) 2 HPO 4 Quickly pour the aqueous solution into 50 mL of the colloidal solution obtained above, stir and mix evenly, add dilute nitric acid to adjust the pH value to 3, and evaporate water from the aforementioned colloidal solution until its volume shrinks to about 20 ml in a water ba...

Embodiment 3

[0038] First, configure Ca(NO 3 ) 3 , Eu(NO 3 ) 3 and Gd(NO 3 ) 3 50ml of mixed solution, control Ca 2+ 、Eu 3+ and Gd 3+ The total concentration is 0.0334mol / L, wherein (Eu+Gd) / (Eu+Gd+Ca) molar percentage is 3.5%, and the Eu / Gd molar ratio is Eu:Gd=2:1.5. According to the concentration of PAA after adding is 0.7mg / ml, accurately weigh 35mg of PAA, add to Ca(NO 3 ) 3 , Eu(NO 3 ) 3 and Gd(NO 3 ) 3 The mixed solution was sonicated with a high-energy ultrasonic probe for 4 minutes to obtain a colloidal solution. Then, configure (NH 4 ) 2 HPO 4 Aqueous solution 50ml, control PO 4 3- The concentration is 0.02mol / L. According to the molar ratio, 50mL (NH 4 ) 2 HPO 4 Quickly pour the aqueous solution into the colloidal solution obtained above, stir and mix evenly, add dilute nitric acid to adjust the pH value to 3, and evaporate the obtained colloidal solution in a water bath at 80°C until its volume is reduced to 25ml to obtain a gel. Finally, the obtained gel ...

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Abstract

The invention relates to rare-earth-doped calcium phosphate fluorescent nanoparticles, and a preparation method and an application thereof. The method comprises the following steps: (1) a mixed solution of calcium nitrate and rare earth nitrate is prepared; (2) a chelating agent polyacrylic acid is added into the mixed solution; with ultrasonic treatment with a high-energy ultrasonic probe, a colloidal solution is obtained; (2) a diammonium hydrogen phosphate water solution is prepared; under room temperature, the diammonium hydrogen phosphate water solution is quickly poured into the colloidal solution obtained in the step (2); the mixture is well mixed by stirring; the pH value is regulated with dilute nitric acid; water in the solution is evaporated under a temperature of 60-80 DEG C, such that a gel is obtained; and (4) the gel is calcined, and the temperature is maintained, such that the rare-earth-doped calcium phosphate fluorescent nano-grade powder is obtained. The rare-earth-doped calcium phosphate fluorescent nanoparticles prepared with the method provided by the invention have the advantages of low synthesis temperature and nanoscale dimensions. With the sol-gel method, a particle agglomeration phenomenon is effectively reduced.

Description

technical field [0001] The invention relates to a rare earth-doped calcium phosphate fluorescent nanoparticle and a preparation method thereof. The prepared fluorescent nanoparticle can be used for cell fluorescence labeling and detection. Background technique [0002] With the development of nanotechnology, various new nanomaterials have shown obvious advantages in the early diagnosis and treatment of tumors. After labeling tumor cells with fluorescent probes, early diagnosis of cancer can be realized, which has attracted widespread attention. Compared with organic fluorescent dyes, inorganic nanofluorescent probe materials exhibit unique properties, such as good optical stability, long life, and multicolor labeling. At present, inorganic fluorescent probe materials mainly include quantum dots, metal nanoparticles, rare earth luminescent nanoparticles, etc., but these materials have certain cytotoxicity. [0003] Calcium phosphate, such as hydroxyapatite and β-tricalcium ...

Claims

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Application Information

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IPC IPC(8): C09K11/71C12Q1/02G01N21/64
Inventor 韩颖超谢云飞李芳王欣宇戴红莲李世普
Owner WUHAN UNIV OF TECH
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