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Ultra-small-size fluorescent mesoporous organic silicon oxide probe and preparation method and application

An organic silicon oxide and mesoporous technology, applied in the field of nanomaterials, to achieve the effect of expanding performance and application, good biocompatibility, and good polar solvent dispersion performance

Inactive Publication Date: 2019-02-01
NANJING UNIV OF POSTS & TELECOMM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, ultra-small fluorescent mesoporous organosilica probes have not been reported yet.

Method used

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  • Ultra-small-size fluorescent mesoporous organic silicon oxide probe and preparation method and application
  • Ultra-small-size fluorescent mesoporous organic silicon oxide probe and preparation method and application
  • Ultra-small-size fluorescent mesoporous organic silicon oxide probe and preparation method and application

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preparation example Construction

[0049] A method for preparing an ultra-small fluorescent mesoporous organic silicon oxide probe, comprising the following steps:

[0050] Step (1): Dissolve an appropriate amount of surfactant in an ammonia solution or a solution of triethylamine, and then add 1,4-bis[γ(triethoxy Mixtures of silyl)propyl]tetrasulfide with tetramethylorthosilicate or 1,4-bis[γ(triethoxysilyl)propyl]tetrasulfide with tetraethylorthosilicate, Reaction 2~24h;

[0051] Step (2), add polyethylene glycol-silane to the solution obtained in step (1), the molecular weight of polyethylene glycol-silane is 500-700g / moL, and react under heating and stirring at 30-60°C for 24-48h ;

[0052] Step (3), heating up the solution obtained in step (2), and reacting for 24-48 hours under the condition of heating and stirring at 70-90°C;

[0053] Step (4), transfer the product obtained after the reaction in step (3) to a dialysis bag for dialysis. The dialysate is a mixed solution of deionized water, ethanol and ...

Embodiment 1

[0063] A method for preparing an ultra-small fluorescent mesoporous organic silicon oxide probe, comprising the following steps:

[0064] Step (1), 29 μL concentrated ammonia water (the NH contained in the concentrated ammonia water 3 The mass percentage concentration is 25%) mixed with 80mL deionized water to obtain a weakly alkaline ammonia solution, then 0.8379g cetyltrimethylammonium bromide was dissolved in the mixed solution, stirred for 30min, and finally 540μL Add a mixture of tetramethyl orthosilicate and 100 μL of 1,4-bis[γ(triethoxysilyl)propyl]tetrasulfide to the solution obtained in step (1), heat and stir at 30°C and 500 rpm Continue to stir for 24 h;

[0065] Step (2), add 1 mL of polyethylene glycol-silane to the reaction solution obtained in step (1), and stir for 24 hours at 30°C and 500 rpm with heating and stirring;

[0066] Step (3), raise the reaction temperature of step (2) to 80°C, and continue to stir for 48h under the condition of heating and stirri...

Embodiment 2

[0073] A method for preparing an ultra-small fluorescent mesoporous organic silicon oxide probe, comprising the following steps:

[0074] Step (1), under the conditions of 20°C and 500rpm, 290 μL of concentrated ammonia water (the NH 3 The mass percent concentration is 25%) mixed with 80 mL of water, then 0.8379g of cetyltrimethylammonium bromide was dissolved in the mixed solution, and stirred for 30min. Finally, add 540 μL of methyl orthosilicate and 100 μL of a mixture of 1,4-bis[γ(triethoxysilyl)propyl]tetrasulfide to the solution obtained in step (1), at 30°C, 500 Continue to stir for 24h under the rpm condition;

[0075] Step (2), add 1 mL of polyethylene glycol-silane to the reaction product obtained in step (1), and stir at 20°C and 500 rpm for 24 h;

[0076] Step (3), raise the reaction temperature of step (2) to 90°C, and continue stirring at 500 rpm for 48h;

[0077] Step (4), dialyze the reaction product obtained in step (3), the volume ratio of deionized water:...

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Abstract

The invention discloses an ultra-small-size fluorescent mesoporous organic silicon oxide probe and a preparation method and application. The probe is an irregular ball, a framework is doped with a thioether group, polyethylene glycol is modified on the surface of the probe, and the probe has a mesoporous duct. The preparation method of the probe comprises the following steps: dissolving a surfactant in a solution which contains a catalyst, adding 1,4-bis[gamma(triethoxy silicon group) propyl] tetrasulfide, tetramethyl silicate or tetraethoxysilane while heating and stirring, after reacting fora period of time, adding polyethylene glycol-silane in a reaction solution, keeping reacting for a period time, then increasing a reaction temperature, keeping reacting while stirring, then dialyzingthe obtained reaction product to ensure that the surfactant is removed thoroughly, and finally connecting dyestuff by a click chemistry method so as to obtain the ultra-small-size fluorescent mesoporous organic silicon oxide probe. The preparation process is simple, and the prepared probe has huge application potentiality in the fields of drug delivery, medical image and the like.

Description

technical field [0001] The invention belongs to the technical field of nanomaterials, and in particular relates to an ultra-small fluorescent mesoporous organic silicon oxide probe, a preparation method and an application. Background technique [0002] Mesoporous organosilica nanoparticles (MONs) have uniformly distributed organic groups, rich and uniform pores, high specific surface area and good stability, and can be used in drugs, gene delivery and biosensing, etc., in the field of tumor treatment Show great advantages and broad prospects. Mesoporous nanoparticles have modifiable inner and outer surfaces. However, the silica framework has low chemical stability in aqueous solution and humid environment, and silanol can induce red blood cell hemolysis. Current research mainly overcomes the defects of oxidized frameworks through organic functionalization. However, the uneven distribution of organic groups on the mesoporous surface and adverse side reactions are unavoidab...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/06C09K11/02B82Y20/00B82Y30/00B82Y40/00G01N21/64
CPCB82Y20/00B82Y30/00B82Y40/00C09K11/025C09K11/06G01N21/64G01N21/6428G01N21/6456G01N2021/6417G01N2021/6439G01N2021/6497
Inventor 滕兆刚张俊杰汪联辉苏晓丹
Owner NANJING UNIV OF POSTS & TELECOMM