Carboxyl functionalized micro-scale rod-like upconversion fluorescence material and preparation method thereof

A carboxyl-functionalized, fluorescent material technology, applied in luminescent materials, chemical instruments and methods, etc., can solve the application of micron-scale rod-shaped up-conversion fluorescent materials in the field of biological detection, the leakage of encoded microsphere fluorescent particles, and the fluorescence intensity of microspheres. Differences and other problems, to avoid spectral overlap, the preparation process is simple and easy, and the fluorescence is stable.

Active Publication Date: 2015-09-09
天津渤化讯创科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] However, there are still some unavoidable problems in the up-conversion encoded microspheres: the process of up-converting the encoded microspheres by using high temperature swelling technology is complicated and time-consuming; During the use of microspheres, there may be leakage of internal fluorescent particles
However, there is currently no micron-scale rod-shaped upconversion fluorescent material functionalized with carboxyl groups in the field of biological detection.

Method used

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  • Carboxyl functionalized micro-scale rod-like upconversion fluorescence material and preparation method thereof
  • Carboxyl functionalized micro-scale rod-like upconversion fluorescence material and preparation method thereof
  • Carboxyl functionalized micro-scale rod-like upconversion fluorescence material and preparation method thereof

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Embodiment 1

[0037] 1) Add an aqueous solution containing 4.5 mg of NaOH and a salt solution containing 12 mmol of rare earth elements in sequence to 25 mL of a mixed solution of ethanol and oleic acid (volume ratio = 1:1). Among them, the molar ratio of rare earth elements is Y 3+ : Yb 3+ : Tm 3+ =80:27:0.3.

[0038] 2) Add 1.85mg NH 4 For the aqueous solution of F, the mixed solution was stirred evenly and then transferred to a high-temperature reaction kettle, and kept at 180° C. for 12 hours;

[0039] 3) After the reaction is completed, the obtained white precipitate is washed with ethanol, dispersed in hydrochloric acid solution (2M) and ultrasonically washed for 3 minutes, and then cleaned again to obtain a pure micron-scale rod-shaped up-conversion fluorescent material with good dispersibility.

[0040]4) The obtained up-conversion material was added to a mixed solution of 25mL CTAB solution (5%), 0.33mL sodium hydroxide solution (2M) and 0.33mL TEOS, reacted at 80°C for 30min a...

Embodiment 2

[0045] 1) Add an aqueous solution containing 4.5 mg of NaOH and a salt solution containing 12 mmol of rare earth elements in sequence to 25 mL of a mixed solution of ethanol and oleic acid (volume ratio = 1:1). Among them, the proportion of rare earth elements is Y 3+ : Yb 3+ :Er 3+ =80:20:1.

[0046] 2) Add 1.85mg NH 4 For the aqueous solution of F, stir the mixture for 30 minutes, transfer it to a high-temperature reaction kettle, and keep it at 180°C for 12 hours;

[0047] 3) After the reaction is completed, the obtained white precipitate is washed with ethanol, dispersed in hydrochloric acid solution (2M) and ultrasonically washed for 3 minutes, and then cleaned again to obtain a pure micron-scale rod-shaped up-conversion fluorescent material with good dispersibility.

[0048] 4) The obtained up-converting material was added to a mixed solution of 18.75mL CTAB solution (5%), 0.25mL sodium hydroxide solution (2M) and 0.25mL TEOS, reacted at 60°C for 30min and then centr...

Embodiment 3

[0052] 1) Into 25mL of a mixed solution of ethanol and oleic acid (volume ratio = 1:1), sequentially add an aqueous solution of 3.75mg of NaOH and a salt solution containing 8mmol of rare earth elements. Among them, the molar ratio of rare earth elements is Y3+: Yb 3+ :Er 3+ =80:80:0.08.

[0053] 2) Plus contains 1.48mg NH 4 For the aqueous solution of F, the mixed solution was stirred evenly and then transferred to a high-temperature reaction kettle, and kept at 200° C. for 8 hours;

[0054] 3) After the reaction is completed, the obtained white precipitate is washed with ethanol, dispersed in hydrochloric acid solution (2M) and ultrasonically washed for 3 minutes, and then cleaned again to obtain a pure micron-scale rod-shaped up-conversion fluorescent material with good dispersibility.

[0055] 4) The obtained up-conversion material was added to a mixed solution of 12mL CTAB solution (5%), 0.16mL sodium hydroxide solution (2M) and 0.16mL TEOS, reacted at 70°C for 30min a...

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Abstract

The present invention relates to a carboxyl functionalized micro-scale rod-like upconversion fluorescence material and a preparation method thereof, wherein a micro-scale upconversion fluorescence material is subjected to one-step synthesis through a hydrothermal method, different colors of the upconversion fluorescence materials having a length of about 1-2 [mu]m can be prepared, and the preparation process is simple and convenient. According to the present invention, during the synthesis process, the required raw materials are added to a mixed solvent of oleic acid and ethanol according to a certain ratio, reaction is performed for 8-12 h at a temperature of 180-200 DEG C, and the product is subjected to centrifugal washing so as to obtain the purified upconversion micrometer rod; the amino can be introduced onto the upconversion material surface through the classical method and the carboxyl functionalization is successfully achieved by adding PAA through the amide bond coupling so as to enhance the dispersity in the aqueous solution and provide a large number of the reactive sites for coupling biomolecules; and the prepared material has characteristics of low production cost, good fluorescence stability and easy surface modification, can be used for detection of biological macromolecules, and can further be widely used for rapid detection of antigens, nucleic acids and the like.

Description

technical field [0001] The invention relates to a carboxyl-functionalized micron-scale rod-shaped up-conversion fluorescent material and a preparation method thereof. Background technique [0002] Bioanalysis, disease diagnosis, and monitoring of disease treatment all require real-time acquisition of relevant information on various target substances (proteins or nucleic acids, etc.). The rapid development of multifunctional suspension array technology (usually also called "liquid chip" technology) has made the high-throughput, rapid and accurate detection of target substances a reality. [0003] Fluorescence-encoded microspheres are the most commonly used technology in liquid chips. The fluorescence of the front-end microspheres and the reporter fluorescence of the target are encoded simultaneously, and the information of the two kinds of fluorescence is obtained through dual-light excitation to complete the detection of the target object. Fluorescence-encoded microspheres...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/85C09K11/02
Inventor 常津苏琳王汉杰郑学荣王生张莹侯贝贝窦妍张健
Owner 天津渤化讯创科技有限公司
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