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Rare earth-doped upconversion nanometer crystal-based fluorescent coding microspheres and preparation method thereof

A technology of nanocrystals and fluorescent coding, which is applied in the field of fluorescent coding microspheres and its preparation, can solve the problems of large deviation of the design value of the fluorescent coding value, interference with test results, and decreased accuracy, so as to improve sensitivity and detection quantity, and broaden Application prospects, phototoxicity reduction effect

Active Publication Date: 2011-09-28
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, the workload of the preparation process is very huge, and there are often deviations during the embedding process, which leads to a large deviation between the fluorescence encoding value of the final product and the original design value
Since the fluorescence emission peaks of organic fluorescent dyes and quantum dots are broad and overlap each other seriously, the accuracy begins to decline as the number of samples increases.
In addition, in the multiple detection process, in addition to fluorescently encoded microspheres, fluorescent reporter molecules are also required to identify the detection substances. Most of the reporter molecules also use organic fluorescent dyes, and the emission peaks of organic reporter molecules in the detection process. If the emission peaks of the coded microspheres overlap, it will greatly interfere with the test results

Method used

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  • Rare earth-doped upconversion nanometer crystal-based fluorescent coding microspheres and preparation method thereof
  • Rare earth-doped upconversion nanometer crystal-based fluorescent coding microspheres and preparation method thereof
  • Rare earth-doped upconversion nanometer crystal-based fluorescent coding microspheres and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Example 1: NaYF 4 : Preparation of 0.2 mol % Yb / 0.2 mol % Ho / 0.2 mol % Tm up-conversion nanocrystals. Specific steps are as follows:

[0023] (1) Take a 50 mL three-neck round bottom flask as the reaction vessel, first add 1 mmol CF 3 COONa, 0.4mmol Y(CF 3 COO) 3 , 0.14mmol Yb (CF 3 COO) 3 , 0.011mmol Ho(CF 3 COO) 3 and 0.011mmol Tm(CF 3 COO) 3 ; followed by the addition of 10 g of tri-n-octylphosphine oxide (TOPO).

[0024] (2) Stir and heat the reactants in step (1) to 120 o C. Vacuum dehydration and deoxygenation for 30 minutes, and finally obtain a transparent mixed solution.

[0025] (3) Under the protection of high-purity argon, the reactants were heated at 10 oC / min speed up to 340 oC After incubation, the reaction was carried out for 1 hour.

[0026] (4) Cool the reactants to 50 oC Afterwards, ethanol is added to precipitate the product from the solution, followed by centrifugation, and repeated washing with absolute ethanol for 3-5 times to o...

Embodiment 2

[0028] Example 2: NaYF 4 : Preparation of 0.2 mol % Yb / 0.2 mol % Er / 0.2 mol % Tm upconversion nanocrystals. Specific steps are as follows:

[0029] (1) Take a 50 mL three-neck round bottom flask as the reaction vessel, first add 0.4 mmol YCl 3 , 0.14mmol YbCl 3 , 0.011mmol ErCl 3 and 0.011 mmol TmCl 3 ; followed by the addition of 10g oleic acid (OA), 10g octadecene (ODE).

[0030] (2) Stir and heat the reactants in step (1) to 120 o C. Vacuum dehydration and deoxygenation for 30 minutes, and finally obtain a transparent mixed solution.

[0031] (3) Add 2.25 mmol NH 4 F was dissolved in 5 mL of methanol solution, mixed and injected into the above reaction solution for reaction. After continuous stirring for 20 minutes, the reactant was heated under the protection of high-purity argon for 10 oC / min speed up to 340 oC After incubation, the reaction was carried out for 1 hour.

[0032] (4) Cool the reactants to 50 oC Afterwards, ethanol is added to precipitate the...

Embodiment 3

[0034] Example 3: Y 2 o 3 : Preparation of 0.2 mol % Yb / 0.2 mol % Er / 0.2 mol % Tm up-conversion nanocrystals. Specific steps are as follows:

[0035] (1) Take a 50 mL three-neck round bottom flask as the reaction vessel, first add 0.4 mmol Y(Ac) 3 , 0.14mmol Yb(Ac) 3 , 0.011mmol Er(Ac) 3 and 0.011mmol Tm(Ac) 3 ; followed by the addition of 10g oleic acid (OA), 10g octadecene (ODE).

[0036] (2) Stir and heat the reactants in step (1) to 120 o C. Vacuum dehydration and deoxygenation for 30 minutes, and finally obtain a transparent mixed solution.

[0037] (3) Under the protection of high-purity argon, the reactants were heated at 10 oC / min speed up to 340 oC After incubation, the reaction was carried out for 1 hour.

[0038] (4) Cool the reactants to 50 oC Afterwards, ethanol is added to precipitate the product from the solution, followed by centrifugation, and repeated washing with absolute ethanol for 3-5 times to obtain the product.

[0039] In addition, the ...

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Abstract

The invention belongs to the technical field of nanometer biological materials, and particularly relates to rare earth-doped upconversion nanometer crystal-based fluorescent coding microspheres and a preparation method thereof. According to the principle that an upconversion material doped by different rare earth ions emits fluorescent light with different wavelengths under the excitation of an infrared light source, in the rare earth-doped upconversion nanometer crystal-based fluorescent coding microspheres, a strength ratio of the emitted fluorescent light with different wavelengths is usedas fluorescent codes, namely the number of the fluorescent codes is changed by changing the doping varieties and doping content of the rare earth ions in the process of synthesizing nanometer crystals or the fluorescent codes are regulated by controlling ratios of upconversion nanometer crystals of different varieties in a microsphere carrier material. By the fluorescent coding microspheres, the sensitivity and number of detection can be improved further, and a plurality of fluorescent report molecules with different colors can be used simultaneously. The coding microspheres has the wide application prospects in aspects of gene expression, mutual effect among proteins, the high-flux screening of biological samples, the detection of multichannel biological science, disease diagnosis, combined chemistry and the like.

Description

technical field [0001] The invention belongs to the technical field of nano-biological materials, and in particular relates to a fluorescent coded microsphere based on infrared up-conversion nano-crystals and a preparation method thereof. Background technique [0002] Since the decoding of the human genome, researchers have been expecting to obtain more information from biological samples in various complex biological systems, so as to provide more scientific basis for the diagnosis and treatment of diseases. The fields of bioanalysis, disease diagnosis, and biomedical research require more information on protein and gene target identification. Multiplex detection enables rapid signal identification of nucleic acids and proteins. However, the multiple detection methods currently used are all multiple detection based on multi-well plate technology. Although this technology has been widely used, the increasing demand for high-throughput detection requires more advanced multi...

Claims

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Application Information

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IPC IPC(8): C09K11/85C09K11/78C09K11/84
Inventor 张凡
Owner FUDAN UNIV
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