Composite microsphere marker for conducting fluorescent marking on rear earth and preparation method of composite microsphere marker

A rare earth fluorescence, composite microsphere technology, applied in the preparation of microspheres, microcapsule preparations, chemical instruments and methods, etc., can solve the problems of short fluorescence lifetime and low sensitivity, achieve long fluorescence lifetime, improve resolution, and enhance specificity. Effects of Sex and Sensitivity

Inactive Publication Date: 2016-06-01
JIANGSU YINUOWAN CELL CLINIC CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Among the existing rare earth fluorescent complex markers, commonly used fluorescent markers, such as fluorescein isothiocyanate (FITC), rhodamine-6-G (R-6-G), etc., have relatively short fluorescence lifetimes. , long-term use is difficult to overcome the interference of background fluorescence, and the sensitivity is usually low in its detection; the rare earth ions are mainly Eu 3+ 、Sm 3+ 、Dy 3+ and Tb 3+ The complexes formed with some organic complexes such as β-diketone compounds, o-phenanthroline compounds, salicylic acid compounds, bipyridine compounds, etc., have been used to varying degrees, but it is difficult to meet the requirements simultaneously. The following requirements: (1), strong fluorescence; (2), good stability: including thermodynamic stability and resistance to photobleaching, etc.; (3), easy to cross-link with biological macromolecules such as antibodies and nucleic acids, and can be maintained at the same time after cross-linking The high fluorescence intensity of the marker and the biological activity of the marker; (4) easy to synthesize

Method used

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  • Composite microsphere marker for conducting fluorescent marking on rear earth and preparation method of composite microsphere marker
  • Composite microsphere marker for conducting fluorescent marking on rear earth and preparation method of composite microsphere marker
  • Composite microsphere marker for conducting fluorescent marking on rear earth and preparation method of composite microsphere marker

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Experimental program
Comparison scheme
Effect test

specific Embodiment 1

[0040] Specific embodiment 1 prepares BHHCT-Eu 3+ Fluorescent Nanospheres:

[0041] (1), raw material preparation:

[0042] Prepare raw materials by weight: 15g polyvinylpyrrolidone (PVP), 0.03g potassium persulfate (KPS), 8g styrene (St), 80ml ethanol or water and 4,4,-bis(1,1,1,2,2 ,3,3-Heptafluoro-4,6-hexanedionyl)chlorosulfo-o-terphenyl (BHHCT);

[0043] (2), preparation of composite microspheres:

[0044] 4,4,-Bis(1,1,1,2,2,3,3-heptafluoro-4,6-hexanedionyl)chlorosulfo-o-terphenyl (BHHCT) is a trilobal β-diketone compounds can form stable complexes with Eu3+, and can emit strong fluorescence under the excitation of ultraviolet light; BHHCT has poor water solubility, good solubility in ethanol, and its own -SOCl2 group Groups can react with amino groups to form covalent bonds; use materials such as styrene preparation to prepare polystyrene nano-microsphere cores, and use aminosilane to introduce amino groups on the surface of microspheres, and BHHCT-Eu3+ can be marked ...

specific Embodiment 2

[0051] Specific embodiment 2 prepares BHHCT-Eu 3+ Fluorescent Nanospheres:

[0052] (1), raw material preparation:

[0053] Prepare raw materials by weight: 30g polyvinylpyrrolidone (PVP), 0.10g potassium persulfate (KPS), 12g styrene (St), 120ml ethanol or water and 4,4,-bis(1,1,1,2,2 ,3,3-Heptafluoro-4,6-hexanedionyl)chlorosulfo-o-terphenyl (BHHCT);

[0054] (2), preparation of composite microspheres:

[0055] 1), preparation of aminated nanospheres:

[0056] Dissolve 30g of polyvinylpyrrolidone (PVP), 0.10g of potassium persulfate (KPS), 12g of styrene (St), 120ml of ethanol or water medium and place it in an ultrasonic reactor, pass nitrogen gas to remove the oxygen in the system, and turn on the ultrasonic wave The generator performs a polymerization reaction, and obtains a polystyrene nanosphere dispersion after 10 hours of reaction;

[0057] Collect polystyrene nanospheres by centrifugation, suspend them with 5 mL of absolute ethanol, add 5 μL of aminosilane, stir ...

specific Embodiment 3

[0061] Specific embodiment 3 prepares BHHCT-Eu 3+ Fluorescent Nanospheres:

[0062] (1), raw material preparation:

[0063] Prepare raw materials by weight: 25g polyvinylpyrrolidone (PVP), 0.06g potassium persulfate (KPS), 10g styrene (St), 100ml ethanol or water and 4,4,-bis(1,1,1,2,2 ,3,3-Heptafluoro-4,6-hexanedionyl)chlorosulfo-o-terphenyl (BHHCT);

[0064] (2), preparation of composite microspheres:

[0065] 1), preparation of aminated nanospheres:

[0066] Add 25g of polyvinylpyrrolidone, 0.06g of potassium persulfate, and 10g of styrene into 100mL of ethanol or water medium to dissolve and place them in an ultrasonic reactor, pass nitrogen to remove the oxygen in the system, and turn on the ultrasonic generator for polymerization. After 8 hours, polystyrene nanosphere dispersion liquid was obtained;

[0067] Collect polystyrene nanospheres by centrifugation, suspend them with 5 mL of absolute ethanol, add 5 μL of aminosilane, stir and react at room temperature for 1...

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Abstract

The invention provides a composite microsphere marker for conducting fluorescent marking on rear earth and a preparation method of the composite microsphere marker and relates to the technical field of functional polymer biomaterials. The preparation method includes the steps that polyvinylpyrrolidone, potassium persulfate / persulphate and styrene are added to an ethyl alcohol medium or a water medium to be dissolved and then placed into an ultrasonic-wave reactor, a polymerization reaction is generated under protection of nitrogen gas, and polystyrene nanometer microsphere dispersion liquid is obtained; then rare earth fluorescence complex 4, 7-dichloro sulfo benzene-1, 10 phenanthroline-2, 9 dicarboxylic acid-europium or 4, 4-di (1, 1, 1, 2, 2, 3, 3, -heptafluoride-4,6,-adipic ketone group) chlorine sulfo-adjacent-terphenyl- europium is fixed to the surface of a silicon dioxide microsphere in a chemical bonding mode, and finally the composite microsphere marker for conducting fluorescent marking on rear earth is prepared. The composite microsphere marker has the advantages of being long in fluorescent lifetime, good in stability, easy to synthesize, low in cost and easy to mark.

Description

technical field [0001] The invention relates to the technical field of functional polymer biomaterials, in particular to a rare earth fluorescent-labeled composite microsphere marker and a preparation method thereof. As a fluorescent material with excellent performance, rare earth fluorescent microsphere markers can be widely used in the medical field. Background technique [0002] In the prior art, there have been many reports on rare earth ions or rare earth complexes and silicon dioxide-doped luminescent materials, such as Cannasa (Cannasa.C, etal, Mat.Res.Soc.Symp.Proc.676(Y3)18.1 -18.6, 2001) described the preparation of directly doped europium (Eu 3+ ) Y2O3-SiO2 nanoluminescent material; Moran et al. (C.E.Moranetal, Langmuir2001, 17, 8376-8379) synthesized silicon nanoparticles doped with Pr3+ and Er3+; Cheng Yanling et al. , 1217-1220) with polyvinylpyrrolidone as a stabilizer, the monomer styrene was dispersed and polymerized by ultrasonic irradiation to prepare po...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/06C09K11/02B01J13/02
CPCB01J13/02C09K11/02C09K11/06C09K2211/1007C09K2211/1029C09K2211/182
Inventor 曾骥孟胡鹏唐振洲蒙明慧林辉暖
Owner JIANGSU YINUOWAN CELL CLINIC CO LTD
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