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Method for preparing fluorescent rare earth complex compound silicon nano particles

A technology of silicon nanoparticles and complexes, which is applied in the field of preparation of fluorescent silicon nanoparticles, to achieve the effect of improving fluorescence intensity, easy realization, and good stability

Inactive Publication Date: 2008-07-23
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Chinese patent CN1298807C discloses a preparation method similar to the above-mentioned patent, but only uses physical doping to dope fluorescent rare earth complexes into silicon nanoparticles
[0013] The preparation methods disclosed in the above patent applications all dope the fluorescent rare earth complexes inside the carrier nanoparticles, and bond the fluorescent rare earth complexes to the surface of the silicon nanoparticle carrier, especially through cyclic grafting. The method of layer modification to bond rare earth complexes to the surface of silicon nanoparticles has not been reported yet.

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  • Method for preparing fluorescent rare earth complex compound silicon nano particles

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Embodiment 1: Preparation of BHHCT-Eu silicon nanoparticles

[0044] This example describes the preparation of silicon nanoparticle carriers by the inverse microemulsion method, using APTMS to modify amino groups on the surface of the particles, using BHHCT with sulfonyl chloride groups as the bonded rare earth ligands, and using Eu 3+ Preparation process of fluorescent rare earth complex silicon nanoparticles for rare earth ions.

[0045] (1) Preparation of silicon nanoparticle carrier: Take 30mL of cyclohexane, 10mL of Tx-100, and 10mL of n-hexanol into the Erlenmeyer flask, place it on a magnetic particle stirrer and stir, after stirring evenly, add 2mL of ultrapure water and 300μL of ammonia water in turn , 800μLTEOS, after stirring for 24 hours, add an equal volume of acetone, mix well, centrifuge to separate the particles, then wash the particles several times with ultrapure water and absolute ethanol to remove surfactants and other unreacted reagents, and finally...

Embodiment 2

[0051] Embodiment 2: Preparation of BC-EDTA-Eu silicon nanoparticles

[0052] This example describes the preparation of silicon nanoparticle carriers by the inverse microemulsion method, using APTMS to modify the amino group on the surface of the particles, using BC-EDTA as the bonding rare earth ligand, and using Eu 3+ Preparation process of fluorescent rare earth complex silicon nanoparticles for rare earth ions.

[0053] (1) Preparation of silicon nanoparticle carrier: Same as Example 1.

[0054] (2) Amination of the surface of silicon nanoparticles: same as in Example 1.

[0055] (3) Chemical bonding of fluorescent rare earth complexes: take 1 mL of silicon nanoparticles modified with amino groups on the surface, the concentration is 15 mg / mL, wash twice with 0.05 mol / L phosphate buffer saline (PBS), pH=6.8 , ultrasonically suspended in 1 mL of 0.05 mol / L PBS. Take another 3.4mg BC-EDTA (2,9-bis[N,N-bis(carboxymethyl)aminomethyl]-4,7-diphenyl-1,10-phenanthroline), 0.4mg...

Embodiment 3

[0059] Embodiment 3: Preparation of BBCAP-Eu silicon nanoparticles

[0060] This example describes the preparation of silicon nanoparticle carriers by the inverse microemulsion method, using APTMS to modify the amino groups on the surface of the particles, using BBCAP as a bonded rare earth ligand, and using Eu 3+ Preparation process of fluorescent rare earth complex silicon nanoparticles for rare earth ions.

[0061] (1) Preparation of silicon nanoparticle carrier: Same as Example 1.

[0062] (2) Amination of the surface of silicon nanoparticles: same as in Example 1.

[0063] (3) Chemical bonding of fluorescent rare earth complexes: Take 1 mL of silicon nanoparticles modified with amino groups on the surface, the concentration is 15 mg / mL, wash with 0.05 mol / L carbonate buffer (CB), pH=9.5, wash twice Repeatedly, ultrasonically suspend in 1 mL of 0.05 mol / L CB. Take another 2.6mg BBCAP (2,9-bis[N,N-bis(carboxymethyl)aminomethyl]-1,10-phenanthroline), 0.4mg NHS, 3.9mg EDC,...

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Abstract

The invention relates to a preparation method of a fluorescent silicon nano-grain of rare-earth complex, belonging to the preparation method of fluorescent silicon nano-grain, in particular to a preparation method which enables the rare-earth complex to circularly link on the surface of the silicon nano-grain to make the fluorescent silicon nano-grain of rare-earth complex. The fluorescent silicon nano-grain of rare-earth complex has the advantages of good control performance, easy achievement, even made grain and strong fluorescence intensity. The preparation method adopts the tactics for multi-layer to modify, namely the fluorescent rare-earth complex is linked on the surface of the silicon nano-grain and circularly grafted by silane, which can make the quantity of the complexes linked on the surface of the silicon nano-grain to maximum and then obtains the fluorescent silicon nano-grain of rare-earth complex with strong fluorescence intensity, good stability and easy marking performance. The fluorescent silicon nano-grain of rare-earth complex adopts the preparation method that the nano-grain is surface functionalized after preparing the carrier of the nano-grain, then the surface radical of the grain is grafted after chemically linking the fluorescent rare-earth complex, finally the fluorescent silicon nano-grain is surface functionalized again after circularly grafting and multi-layer modifying.

Description

technical field [0001] The invention relates to the preparation of fluorescent silicon nanoparticles, in particular to a method for preparing fluorescent rare earth complex silicon nanoparticles by cyclically bonding rare earth complexes on the surface of silicon nanoparticles. Background technique [0002] Commonly used fluorescent markers have a short fluorescence lifetime, which makes it difficult to overcome the interference of background fluorescence and low detection sensitivity. Using rare earth complexes with long-lived fluorescence as markers and time-resolved detection technology can eliminate the interference of background fluorescence and improve sensitivity by several orders of magnitude. This technology called time-resolved fluorescence detection has become the current biomedical Promising ultratrace analytical method in research and clinical biochemical assays. [0003] The existing fluorescent rare earth complex markers, the rare earth ions are mainly Eu 3+...

Claims

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Application Information

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IPC IPC(8): C09K11/77
Inventor 李庆阁许晔
Owner XIAMEN UNIV
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