Rare earth doped gadolinium-potassium fluoride nanometer material for magneto-optical double-module biological marker and preparation method thereof

A rare earth doping, gadolinium potassium fluoride technology, applied in nanotechnology, luminescent materials, chemical instruments and methods for materials and surface science, etc. The problem of unstable detection signal, etc., achieves the effect of low cost, high magnetic relaxation rate and narrow emission peak.

Active Publication Date: 2012-10-31
FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the application of this hybrid material in the field of biomarkers faces many difficulties, such as the magnetic induction effect of superparamagnetic iron oxide nanoparticles on normal tissue is not conducive to its magnetic resonance imaging detection in vivo; the photobleaching of organic dyes , emission peak width, and light chromaticity impurity lead to the instability of its detection signal; quantum dots are highly toxic and costly to prepare, so they are not suitable for in vivo imaging marker materials
In addition, combining two different particles tends to destroy their respective optical and magnetic properties, and inevitably increases the particle size, resulting in greatly reduced application effects

Method used

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  • Rare earth doped gadolinium-potassium fluoride nanometer material for magneto-optical double-module biological marker and preparation method thereof
  • Rare earth doped gadolinium-potassium fluoride nanometer material for magneto-optical double-module biological marker and preparation method thereof
  • Rare earth doped gadolinium-potassium fluoride nanometer material for magneto-optical double-module biological marker and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0023] Example 1: Take by weighing 0.0037 g europium chloride (EuCl 3 ·6H 2 O), 0.8 g potassium chloride (KCl) and 0.37 g gadolinium chloride (GdCl 3 ·6H 2 O) Dissolve completely in 12 mL of distilled water, then add 1 mL of ethanol, 20 mL of ethylene glycol, and 10 mL of polypropyleneimine solution, and stir to obtain a transparent solution A; in another beaker, dissolve an appropriate amount of ammonium fluoride in 0.5 mL of distilled water, then add 2.5 mL of ethanol, and stir to obtain a transparent solution B; under stirring, add solution A dropwise to solution B, continue stirring for ten minutes, transfer the solution into a hydrothermal tank, and heat it at 170 °C Heat treatment for 20 hours. After cooling, the supernatant liquid was removed, and the lower precipitate was washed with water and ethanol three times in turn, then dried, and then dried under vacuum at 60°C to obtain KGdF 4 :Eu 3+ nanocrystalline powder. The nanocrystalline powder was dissolved in di...

example 2

[0024] Example 2: Take by weighing 0.0037g terbium chloride (TbCl 3 ·6H 2 O), 1.8g potassium chloride (KCl) and 0.37g gadolinium chloride (GdCl 3 ·6H 2 O) Completely dissolve in 5mL of distilled water, then add 25mL of ethanol, 5mL of ethylene glycol and 5 mL of polypropyleneimine solution, and stir to obtain a transparent solution A; in another beaker, dissolve an appropriate amount of ammonium fluoride in 1mL of distilled water, then add 1mL of ethanol, stirred to obtain a transparent solution B; in the state of stirring, add solution A dropwise to solution B, continue stirring for ten minutes, transfer the solution into a hydrothermal tank, and hydrothermally treat it at 110 ℃ for 18 hours. After cooling, The supernatant liquid was removed, and the lower precipitate was washed with water and ethanol three times in turn, dried, and then dried under vacuum at 50°C to obtain KGdF 4 : Tb nanocrystalline powder. 2 mg KGdF 4 :Tb 3+ Dissolve the nanocrystalline powder in 20...

example 3

[0025] Example 3: Take by weighing 0.0037g dysprosium chloride (DyCl 3 ·6H 2 O), 1.8g potassium chloride (KCl) and 0.37g gadolinium chloride (GdCl3 ·6H 2 O) Completely dissolve in 2mL of distilled water, then add 28mL of ethylene glycol and 0.5 mL of polypropyleneimine solution, and stir to obtain a transparent solution A; in another beaker, dissolve an appropriate amount of ammonium fluoride in 5mL of distilled water, then add 1mL of ethanol, Stir to obtain a transparent solution B; under stirring, add solution A dropwise to solution B, continue stirring for ten minutes, transfer the solution into a hydrothermal tank, and perform hydrothermal treatment at 140 °C for 24 hours. After cooling, clear the upper layer The liquid was removed, and the lower precipitate was washed with water and ethanol three times in turn, dried, and then dried under vacuum at 65°C to obtain KGdF 4 : Dy 3+ nanocrystalline powder. 15 mg KGdF 4 : Dy nanocrystalline powder dissolved in 20mL of dis...

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Abstract

The invention relates to a rare earth doped gadolinium-potassium fluoride nanometer material for a magneto-optical double-module biological marker and a preparation method thereof. The preparation method comprises the following steps of: mixing gadolinium chloride, potassium chloride and ammonium fluoride in distilled water, ethanol and ethanediol by utilizing propylene imine as a surface active agent; carrying out hydro-thermal treatment at 50-230 DEG C for a period of time; washing, and drying to obtain a DGdF4:Ln nanometer crystal, wherein the commonest of the DGdF4:Ln nanometer crystal are as follows: xLn3+-(1-x)KGdF4 (Ln=Ce, Pr, Nd, Pm, Sm, Eu, Tb, Dy, Ho, Er, Tm, Yb; x=0-60 mol%). The rare earth doped DGdF4 nanometer fluorescence marker material prepared by adopting the method can not only control the size of nanometer granules at about 25 nanometers, but also has better water solubility, can utilize the amino on the surface to be connected with biological molecules; besides, the biological connection is subjected to hypersensitivity detection by realizing needed specific fluorescence emission in such a way that different rare earth ions are doped in the nanometer granules, namely the rare earth doped DGdF4 nanometer fluorescence marker material obtained through the preparation method has potential in being applied in the field of biological markers; and because gadolinium ions are contained in a matrix, the DGdF4 nanometer crystal can be further used as a T1 magnetic resonance imaging contrast agent.

Description

[0001] technical field [0002] The invention relates to a magneto-optical dual-mode biomarker material and a preparation method thereof, in particular to the preparation of a rare earth-doped gadolinium potassium fluoride nanometer material and its application in the field of magneto-optic dual-mode biomarkers. [0003] Background technique [0004] Multimodal biological detection has attracted more and more attention from the scientific community and society because of its ability to simultaneously realize imaging detection of multiple modes such as light, nuclear, magnetic and ultrasonic, among which magneto-optical dual-mode biomarkers are particularly attractive. Attention. This is because optical detection, which can provide the highest detection sensitivity among detection methods, is easily limited by the depth of detection. Although magnetic resonance imaging can perform three-dimensional detection, its wide application is limited due to low detection sensitivity a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/85A61K49/06G01N21/64B82Y30/00
Inventor 陈学元鞠强涂大涛李仁富朱浩淼
Owner FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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