Near infrared fluorescent probe substrate material of rare earth ion nano alkali metal rare earth fluoride and preparation method of near infrared fluorescent probe substrate material

A technology of rare earth fluoride and rare earth ions, which is applied in the field of biomedical materials and optical functional materials, can solve the problems of poor stability and low efficiency of near-infrared fluorescent probes, and achieve good photostability and chemical stability, multiple excitation bands, Easy to manipulate effects

Inactive Publication Date: 2013-02-13
KUNMING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The purpose of the present invention is to overcome the shortcomings of low efficiency and poor stability of existing near-infrared fluorescent probes, to provide a near-

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] (1) According to the molar ratio of Na ion: Y ion: Er ion: Nd ion: Yb ion: F = 1: 0.997: 0.001: 0.001: 0.001: 4, weigh YbNO 3 , YNO 3 , NdNO 3 , ErNO 3 Dissolved in water to prepare a solution with a total rare earth ion concentration of 0.01mol / L;

[0026] (2) Add polyvinylpyrrolidone to the solution in step (1) according to 1% of the total mass of rare earth nitrate, and adjust the pH of the solution to 2 with ammonia water;

[0027] (3) Weigh and dissolve sodium nitrate in ethanol according to the chemical composition to prepare a 0.1mol / L solution; then add sodium fluoride into the solution according to the molar ratio of F ions to alkali metal ions is 1:1 ， In a stirring state, add to the solution obtained in step (2), and stir for 0.5 hours to obtain a mixture;

[0028] (4) Place the mixture obtained in step (3) in a closed high-pressure hydrothermal reactor with polytetrafluoroethylene, and keep it warm for 48 hours at a temperature of 100°C and a volume rati...

Embodiment 2

[0030] (1) According to the molar ratio of Na ion: Gd ion: Tm ion: Nd ion: Yb ion: F = 1: 0.975: 0.01: 0.005: 0.01: 4, weigh GdNO 3 , YbNO 3 , NdNO 3 , TmNO 3 Dissolved in ethylene glycol to prepare a solution with a total rare earth ion concentration of 0.02mol / L;

[0031] (2) Add polyethylene glycol to the solution in step (1) according to 10% of the total mass of rare earth nitrate, and adjust the pH of the solution to 5 with sodium hydroxide;

[0032] (3) Weigh and dissolve sodium nitrate in methanol according to the chemical composition to prepare a 0.2mol / L solution; then add sodium fluoride into the solution according to the molar ratio of F ions to alkali metal ions is 2:1 ， Stirring for 0.5 hours under stirring, adding to the solution obtained in step (2) to obtain a mixture;

[0033] (4) Place the mixture obtained in step (3) in a closed high-pressure hydrothermal reactor with polytetrafluoroethylene, and keep it warm for 24 hours at a temperature of 120°C and a ...

Embodiment 3

[0035] (1) According to the molar ratio of K ions: (Lu+Gd) ions: Tb ions: Nd ions: Yb ions: F = 1: (0.5+0.42): 0.03: 0.01: 0.04: 4, weigh the rare earth ions Nitrate GdNO 3 , YbNO 3 , NdNO 3 、LuNO 3 , TbNO 3 Dissolve in propanol, and prepare a solution with a total rare earth ion concentration of 0.05mol / L;

[0036] (2) Add sodium oleate to the solution in step (1) according to 50% of the total mass of rare earth nitrate, and adjust the pH of the solution to 8 with ammonia water;

[0037] (3) Dissolve potassium nitrate in a mixed solution of ethanol and water according to the chemical composition to prepare a 0.1mol / L solution; Add to solution to dissolve ， In a stirring state, add to the solution obtained in step (2), and stir for 0.2 hours to obtain a mixture;

[0038] (4) Place the mixture obtained in step (3) in a closed high-pressure hydrothermal reactor with polytetrafluoroethylene, and keep it warm for 12 hours at a temperature of 140°C and a volume ratio of 0.5;...

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Abstract

The invention provides a near infrared fluorescent probe substrate material of rare earth ion nano alkali metal rare earth fluoride and a preparation method of the near infrared fluorescent probe substrate material. The chemical formula of the material is MRe (1-x-y) Rm (x) YbyNdzF4, wherein the M is one or more of Li, Na and K, the Re is one or more of Gd, La, Y and Lu, and the Rm is one or more of Er, Tm, Tb and Ho. The material is prepared through a solvothermal method and a hydro-thermal method, efficient near infrared light of 980 nm of a wave band can be obtained under the excitement of infrared light of 730 nm and 800 nm of wave bands, and upconversion fluorescence visible to near infrared light wave bands can be obtained under the excitement of infrared light of 980 nm and 800 nm of wave bands. Therefore, the material can serve as an upconversion fluorescence probe and a downconversion fluorescence probe for fluorescence imaging after being packed and subjected to surface decoration, and the material can serve as magnetic resonance imaging when a substrate contains magnetic element Gd.

Description

technical field [0001] The invention relates to the technical field of biomedical materials and optical functional materials, in particular to a near-infrared fluorescent probe matrix material of rare earth ion nano-alkali metal rare earth fluoride and a preparation method thereof. Background technique [0002] Due to its high sensitivity, easy operation, and large amount of information, fluorescence technology has been widely used in research in the field of life in recent years, such as DNA sequencing, protein analysis, clinical diagnosis, and biological imaging. For example, biological probes are the most effective means of biological staining and diagnosis. At present, there are two main types of bioluminescent probes, one is organic fluorescent molecules, such as rhodamine and fluorescein. However, the fatal disadvantage of these organic molecules is photofading, that is, their fluorescence intensity decreases rapidly with time; the other type is a new type of semicond...

Claims

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Application Information

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IPC IPC(8): C09K11/85
Inventor 宋志国王雪李臣李永进邱建备杨正文尹兆益周大成余雪杨勇
Owner KUNMING UNIV OF SCI & TECH
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