Water-soluble rare earth doped gadolinium sodium tetrafluoride fluorescent marked nano-crystal, and preparation method thereof

A technique for doping sodium tetrafluorogadolinium and rare earth, which is applied in chemical instruments and methods, pharmaceutical formulations, luminescent materials, etc. It can solve the problems of poor monodispersity of solvents, poor particle crystallization, and low biocompatibility, and achieve phase Uniformity, high reaction efficiency, and stable thermodynamic properties

Inactive Publication Date: 2012-10-03
JILIN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The technical problem to be solved in the present invention is to provide a well-dispersed, highly water-soluble rare earth-doped tetrafluorogadolinium sodium multifunctional up-conversion fluorescent label nanocrystal and its microwave synthesis preparation method, which can solve the problems existing in the background technology. In the existing preparation method, the particle crystallization is not good, the fluorescence intensity is weak, the monodispersity in the solvent is poor, and the biocompatibility is low.

Method used

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  • Water-soluble rare earth doped gadolinium sodium tetrafluoride fluorescent marked nano-crystal, and preparation method thereof
  • Water-soluble rare earth doped gadolinium sodium tetrafluoride fluorescent marked nano-crystal, and preparation method thereof
  • Water-soluble rare earth doped gadolinium sodium tetrafluoride fluorescent marked nano-crystal, and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0044] ①Mix 2.4mmol ammonium fluoride and 6mL ethylene glycol in a weighing bottle, stir at room temperature for 2h until uniform, and obtain NH 4 F / EG mixed solution.

[0045] ②Weigh 0.15g polyethyleneimine into another weighing bottle first, then add sodium chloride, gadolinium trichloride, ytterbium trichloride hexahydrate, erbium trichloride hexahydrate in proportion; gadolinium trichloride and Polyethyleneimine is calculated at a molar ratio of 1:6, and the molar ratio of erbium trichloride hexahydrate, ytterbium trichloride hexahydrate and gadolinium trichloride is 2%: 20% to 70%: 28% to 78% The ratio calculation; The total amount of rare earth salt is 0.6mmol, and the molar ratio of sodium chloride and the total amount of rare earth salt is 1:1. In the same weighing bottle, inject 9 mL of ethylene glycol.

[0046] ③ When the solution is mixed to a uniform solution, quickly inject the prepared ethylene glycol solution of ammonium fluoride, stir for about 10 minutes, pu...

Embodiment 2

[0050] ①Mix 4.8mmol ammonium fluoride and 6mL ethylene glycol in a weighing bottle, stir at room temperature for 2h until uniform, and obtain NH 4 F / EG mixed solution.

[0051] ②Weigh 0.24g polyethyleneimine into another weighing bottle. Then add sodium chloride, gadolinium trichloride, ytterbium trichloride hexahydrate, erbium trichloride hexahydrate in proportion; The molar ratio of erbium trichloride, ytterbium trichloride hexahydrate and gadolinium trichloride is 2%: 20% ~ 70%: 28% ~ 78%, the total amount of rare earth salt is 0.6mmol, sodium chloride and rare earth salt The molar ratio of the total amount is 1:1. In the same weighing bottle, inject 9 mL of ethylene glycol.

[0052] ③When it is mixed to a uniform solution, quickly inject the prepared ethylene glycol solution of ammonium fluoride, stir for about 10 minutes, put the solution into the microwave reactor lining, put it in a microwave reactor at 200°C, react for 10 minutes, and cool to room temperature.

[...

Embodiment 3

[0056] ① Mix 6.0mmol ammonium fluoride and 6mL ethylene glycol in a weighing bottle, stir at room temperature for 2 hours until uniform, and obtain NH 4 F / EG mixed solution.

[0057] ② Weigh 0.30g polyethyleneimine into another weighing bottle. Then add sodium chloride, gadolinium trichloride, ytterbium trichloride hexahydrate, erbium trichloride hexahydrate in proportion; The molar ratio of erbium chloride, ytterbium trichloride hexahydrate and gadolinium trichloride is 2%: 20% ~ 70%: 28% ~ 78%, the total amount of rare earth salt is 0.6mmol, the total amount of sodium chloride and rare earth salt The molar ratio of the amounts is 1:1. In the same weighing bottle, inject 9 mL of ethylene glycol.

[0058] ③When it is mixed to a uniform solution, quickly inject the prepared ethylene glycol solution of ammonium fluoride, stir for about 10 minutes, put the solution into the microwave reactor lining, put it in a microwave reactor at 200°C, react for 10 minutes, and cool to roo...

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Abstract

The invention provides a water-soluble rare earth doped gadolinium sodium tetrafluoride fluorescent marked nano-crystal and a preparation method thereof, and belongs to the technical field of chemical synthesis of microwave polyalcohol. The rare earth fluorescent nano-crystal is divided into two forms of dual-dope and tri-dope, wherein the dual-dope refers to dope ytterbium and one rare earth selected from erbium, thulium and holmium in gadolinium sodium tetrafluoride, and tri-dope refers to dope ytterbium thulium and holmium in gadolinium sodium tetrafluoride. The preparation method comprises the steps of using ammonium fluoride as a fluorine source, sodium chloride as a sodium source, and rare earth chloride as a rare ion source, using polyethyleneimine as surface modification macromolecules, and reacting in a microwave reactor with polytetrafluoroethylene lining. With the adoption of the method, the reaction efficiency is high, the operation is convenient and fast, the environmental pollution is avoided, the product yield is high, and the process repeatability is high; the gadolinium sodium tetrafluoride nano-crystal substrate with stable thermodynamic property, even material phase, good diffusion, high water-soluble ability, and high fluorescence luminous efficiency is obtained by adjusting the ratio of gadolinium ions and fluorine ions; and the product is suitable for multicolor biomarkers.

Description

technical field [0001] The invention belongs to the field of microwave polyol chemical synthesis technology, in particular to a rare earth-doped sodium tetrafluorogadolinium tetrafluorogadolinium multifunctional up-conversion fluorescent label nanocrystal and a preparation method thereof. Background technique [0002] The up-conversion material [CN101550593A, CN101100604A] is a luminescent material that is excited by a long wavelength and emits short-wavelength light, that is, a material that converts low-energy photons into high-energy photons. Up-conversion luminescence imaging uses near-infrared (such as 980nm) continuous laser excitation, which has relatively low tissue absorption and scattering, and the endogenous fluorescent substances and down-conversion luminescence probes in the organism cannot be excited by 980nm continuous laser light. Upconversion luminescence imaging can completely eliminate biological background fluorescence, and the upconversion luminescence i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/85C09K11/02A61K49/00A61K49/06
Inventor 施展李菲菲李春光冯守华
Owner JILIN UNIV
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