CN1699443A - Polymer microsphere encoded by nano-gold and method for preparing same - Google Patents
Polymer microsphere encoded by nano-gold and method for preparing same Download PDFInfo
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- CN1699443A CN1699443A CN 200510040518 CN200510040518A CN1699443A CN 1699443 A CN1699443 A CN 1699443A CN 200510040518 CN200510040518 CN 200510040518 CN 200510040518 A CN200510040518 A CN 200510040518A CN 1699443 A CN1699443 A CN 1699443A
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Abstract
The invention discloses a polymer microsphere encoded by nano-gold and method for preparation, which comprises nano gold particles and ethylene polymer, the ethylene polymer can be polyphenylacetylene, or polymethyl methacryate, of polyacrylonitrile, or polyethylene, or polypropylene, or polyethyl acrylate. The preparation method comprises dissolving the ethylene polymer in organic solvent, forming ethylene polymer solution, dropping into polyvinyl alcohol solution through a droplet formation apparatus, finally volatilizing the organic solvent to obtain the polymer microballoon.
Description
Technical field
The present invention relates to a kind of polymer microballoon that can be used as the high-throughput carrier of multiple bioanalysis and protein, gene, drug screening, relate in particular to a kind of polymer microballoon that nanometer gold encodes and preparation method thereof that utilizes.
Background technology
After human genomic sequence was decoded, the interaction between the function of gene and the protein of genes encoding became the focus of research, and the mankind have entered the genome times afterwards comprehensively.The distinguishing feature of genome times afterwards comprehensively is exactly will study between a large amount of albumen and nucleic acid, between the protein-protein and the interaction between protein and the medicine, these Study of Interaction almost are impossible adopting traditional test method, therefore need a kind of high-throughout test platform.High-throughout test platform has then required high-throughout molecular vehicle, identifies the difference interaction that different molecules takes place, promptly so-called cataloged procedure.Array biochip utilize molecule institute fixed different positions just coordinate distinguish different biomolecules as coding, but because the coordinate of array biochip can only be to be fixed in the two-dimensional space, therefore limited the speed and the application thereof of reaction.Novel in recent years code carrier occurs in succession.The making of polymer microballoon and application have had the history of decades, and its size expands to Nano grade from micron level always.But as a kind of solid phase code carrier and mark, microballoon becomes the focus that fields such as high flux screening and combinatorial chemistry are paid close attention to.
With respect to other forms of solid phase carrier, microballoon has significant advantage: the first, and the specific surface area of microballoon is big, can increase the effecting reaction surface to volume ratio, and the chemical reaction on surface is carried out in littler volume; The second, adopt microballoon can utilize some other supplementary meanss to realize a kind of reaction system between solid-liquid reaction and liquid-liquid reaction, thereby accelerate the speed of response of system as stir, liquid washes away etc. as carrier; The 3rd, microsphere surface bonded molecule can be separated from solution after reaction is finished easily; The 4th, along with the change of microsphere surface functionalization group, can expand the purposes of microballoon.
The code carrier of microballoon mainly contains fluorescence-encoded micro-beads, quantum point coding microball, nano strip font code coding microball, combinatorial chemistry coding microball, photonic crystal coding particle, colloid bar coding etc. at present.Fluorescence-encoded micro-beads is that two kinds of different fluorescence dyes are mixed in the micro polymer bulb matrix according to accurate ratio, according to the difference of the ratio of these two kinds of fluorescence dyes in the microballoon microballoon is divided into not of the same race, thereby realize the coding of microballoon.Quantum point coding microball then is to utilize the different fluorescence of semiconductor nanocrystal luminescent quantum dot to encode with different fluorescence intensities.The preparation relative complex of these coded systems and volume carrier, and decode procedure needs laser excitation, therefore cause the complexity and the cost of test set to raise, in addition, adopts and fluorescence-encodedly also exist photofading, radiative emission peak is difficult to problems such as differentiation and biocompatibility.The employing inorganic dyestuff then can be simplified the process of making coding microball, and the cost that reduces Code And Decode, and does not have the problems such as photofading of the used color of encoding.
Polymer microballoon is by the Vanderhoff of U.S. Lehigh University and Brodford professor synthetic the earliest, up to the present, synthetic and application multi-functional, the high-performance polymer microballoon is a focus of studying both at home and abroad always, and has penetrated in the research of numerous related disciplines.Method for preparing polymer micro commonly used has emulsion polymerization, dispersion copolymerization method, seeding polymerization method, suspension polymerization and microsuspension method etc., but the microspherulite diameter of this method preparation is in nanometer and sub-micrometer range, and the difficulty that certain particle is coated in the polymkeric substance is very big.And prepare hundreds of micron a method spray-drying process and template etc. are arranged, but have problems such as the inhomogeneous and making equipment requirement height of particle diameter, cost of manufacture height to several millimeters particle diameter polymer microballoons.
Nanometer gold is meant particle diameter or length gold ball or the rod-shpaed particle between 1～100nm.Absorb the light of specific wavelength in visible light and near infrared range, the absorption of the gold nano grain team light of different-grain diameter size or long-width ratio is different with reflecting properties, therefore can present not distinct colors.Nm gold particles is fast light, heat-resisting, corrosion-resistant, have a good film forming characteristics, therefore be widely used in optics, conduction and coloured material.The present invention prepares nano gold sol about nm gold particles is distributed to exactly in the polymers soln, prepared the method for the polymer microballoon of encoded by nano-gold then by nano gold sol.
Summary of the invention
Technical problem: what the purpose of this invention is to provide a kind of uniform particle diameter utilizes polymer microballoon of encoded by nano-gold and preparation method thereof, this polyalcohol microspherulite diameter scope at 200 μ m between the 6mm, can be used as the carrier of high flux screening and multiple bioanalysis and detection, its coded system and preparation method are simply efficient, can reduce the complexity of test set and detect cost.
Technical scheme: the present invention is that the nm gold particles with required color evenly spreads to and obtains nano gold sol in the polymers soln, by the drop of a drop generating apparatus generation different colours, polymkeric substance just solidifies the polymer microballoon that obtains with the nm gold particles coding after the droplet drying.
This microballoon is made up of ethene polymers and nm gold particles, and wherein by weight, the content of nm gold particles is 1.42～33.3 ‰ in the polymer microballoon, ethene polymers is a polystyrene, or polymethylmethacrylate, or polyacrylonitrile, or polyethylene, or polypropylene, or polyethyl acrylate.
The preparation method may further comprise the steps:
Ethene polymers is dissolved in forms vinyl polymer solution in the organic solvent, wherein, the concentration of ethene polymers in solution is 3%～7%g/ml, and organic solvent is a benzene, or the mixing solutions of ethylene dichloride or benzene and ethylene dichloride;
The ratio of nm gold particles with 0.1～1.0mg/ml is added in the vinyl polymer solution, and stirs;
In the drop generating apparatus, inject 3%～10% polyvinyl alcohol solution by interface;
The vinyl polymer solution that contains nm gold particles is injected in the polyvinyl alcohol solution in the device by tip glass tube, makes vinyl polymer solution by glass point mouth in polyvinyl alcohol solution, be dispersed into one by one spherical droplets;
The bore that tip glass tube point mouth is set is 200 μ m～500 μ m, by regulating the injection speed of vinyl polymer solution and polyvinyl alcohol solution, and the grass tube upper end is to the distance between the tip glass tube point mouth (4), obtain the spherical droplets of required size, collect the ethene polymers drop that comprises nm gold particles with flask;
Flask 30 ℃～70 ℃ slow rotary evaporations on Rotary Evaporators, to accelerate the volatilization of organic solvent in the vinyl polymer solution, treat that volatilization finishes, droplet solidification becomes the polymer microballoon of the nm gold particles coding of dry, hard.
The principle of the structure of drop generating apparatus and polymer microballoon preparation is: the drop generating apparatus is by the syringe pump interface, the electromagnetic pump interface, and glass infuser, tip glass tube, grass tube is collected flask and is constituted; The glass infuser internal fixing has the Glass tubing with sharp mouth, and at the bottom of grass tube passed tin, upper port faced tip glass tube, and glass infuser is connected with the electromagnetic pump interface, and the syringe pump interface is connected the glass infuser upper end.Polymers soln is injected into the interior tip glass tube of tube by the syringe pump interface; Polyvinyl alcohol solution injects in the glass infuser by the electromagnetic pump interface; When polymers soln was flowed through tip glass tube, because the induced effect of action of gravity and mobile polyvinyl alcohol solution, polymers soln was separated into small droplets one by one; Small droplets falls and falls into the collection flask by grass tube; After the organic solvent of polymers soln finished through rotary evaporation, small droplets just became hard polymer globules; The size of microballoon can be passed through the flow velocity of concentration, polymers soln and the polyvinyl alcohol solution of telomerized polymer solution, and the bore of glass point mouth and grass tube port are controlled to the distance of glass point mouth; Can prepare size polymer micro balls with uniform by this method from 200 μ m to 6mm.
Technique effect: utilize the nm gold particles material of encoding according to the present invention, and use the polymer coating nm gold particles, make the microballoon of different coding, have the following advantages with the drop generating apparatus:
(1) adopt nm gold particles simply effective as the coding material, with low cost: according to the size of nm gold particles, 20 kinds of colors can be arranged in visible-range, every kind of color can have 10 kinds of weights simultaneously, therefore can produce hundreds of coding, and the cost of nm gold particles is very low, and joint has reduced application cost greatly;
(2) coding/decoding method of polymer microballoon is simple, owing to encode with color rather than with fluorescence or other modes, therefore decoding need not excitation light source or other devices, can directly distinguish with spectrum, microscope even naked eyes;
(3) preparation facilities of polymer microballoon is simple, utilizes drop generating apparatus of the present invention can be easy to make versicolor coding microball, control easily, and cost of manufacture is cheap, and is simple efficient;
(4) the code used good stability of polymer microballoon, the nm gold particles acid-fast alkali-proof, high temperature resistant, anti-all kinds of SOLVENTS is difficult to variable color, therefore can not have phenomenons such as the photobleaching of high-visibility pigment and optical quenching, remains stable coding in application process;
(5) applied range, can be in the process of preparation polystyrene the various functional groups of polymerization, realize the functionalization of polystyrene microsphere, thereby provide and the fixed molecular chemistry link coupled condition of wanting.
Description of drawings
Fig. 1 is the synoptic diagram that the present invention prepares the used drop generating apparatus of coding microball, and syringe pump interface 1 is wherein arranged, electromagnetic pump interface 2, and glass infuser 3, tip glass tube 4, grass tube 5 is collected flask 6.
Embodiment
This microballoon is made up of ethene polymers and nm gold particles, and wherein: the content of nm gold particles is 1.42～33.3 ‰ in the polymer microballoon, and ethene polymers is a polystyrene, or polymethylmethacrylate, or polyacrylonitrile, or polyethylene, or polypropylene, or polyethyl acrylate
Embodiment one: the preparation of green pearly lustre pigment coded carboxyl modified polystyrene microsphere
1. carboxyl modified polystyrene solid is dissolved in the mixed solvent of ethylene dichloride and benzene with 7% concentration, the blending ratio of ethylene dichloride and benzene is 1: 1;
2. the ratio with 0.1mg nm gold particles/ml polymers soln adds the red nano gold grain in polystyrene solution, and stirs;
The bore that 3. tip glass tube 4 sharp mouths are set is 200 μ m, and grass tube 5 upper port are 1mm to the distance between the tip glass tube point mouth;
4. inject 5% polyvinyl alcohol solution by electromagnetic pump interface 2 in glass infuser, after filling with glass infuser 3 polyvinyl alcohol solutions, control polyvinyl alcohol solution injection speed is 25ml/min;
5. inject the polystyrene solution that contains green pearly pigment by syringe pump interface 1, regulating flow velocity is 10 μ l/min;
6. collect the polystyrene drop that comprises pearly pigment with flask, be put into the 30 ℃ of rotary evaporations of speed that change with per minute two on the Rotary Evaporators,
7. evaporate to filter and obtain the green polystyrene microsphere that particle diameter is 300 μ m.
Embodiment two: the preparation of the pearly lustre pigment coded poly (methyl methacrylate) micro-sphere of purple
1. polymethylmethacrylate is dissolved in the mixed solvent of ethylene dichloride and benzene with 5% concentration, the blending ratio of ethylene dichloride and benzene is 2: 3;
2. in polystyrene solution, add green pearly pigment with the ratio of 0.5mg pearly pigment/ml polymers soln and be added to, and stir;
The bore that 3. tip glass tube 4 sharp mouths are set is 200 μ m, and grass tube 5 upper port are 1.5mm to the distance between the tip glass tube point mouth;
4. inject 5% polyvinyl alcohol solution by electromagnetic pump interface 2 in glass infuser, after filling with glass infuser (3) polyvinyl alcohol solution, control polyvinyl alcohol solution injection speed is 20ml/min;
5. inject the polystyrene solution that contains the purple pearly pigment by syringe pump interface 1, regulating flow velocity is 20 μ l/min;
6. collect the polystyrene drop that comprises pearly pigment with flask, be put into the 30 ℃ of rotary evaporations of speed that change with per minute two on the Rotary Evaporators,
7. evaporate to filter and obtain the purple poly (methyl methacrylate) micro-sphere of uniform size that particle diameter is 500 μ m.
Claims (2)
1. the polymer microballoon of nm gold particles coding, it is characterized in that this microballoon is made up of ethene polymers and nm gold particles, wherein calculate by weight, the content of nm gold particles is 1.42～33.3 ‰ in the polymer microballoon, and ethene polymers is a polystyrene, or polymethylmethacrylate, or polyacrylonitrile, or polyethylene, or polypropylene, or polyethyl acrylate.
2. the preparation method of the polymer microballoon of a nm gold particles as claimed in claim 1 coding,
It is characterized in that the preparation method may further comprise the steps:
1. ethene polymers is dissolved in and forms vinyl polymer solution in the organic solvent, wherein, the concentration of ethene polymers in solution is 3%～7%mg/ml, and organic solvent is a benzene, or the mixing solutions of ethylene dichloride or benzene and ethylene dichloride;
2. the ratio of nm gold particles with 0.1～1.0mg/ml is added in the vinyl polymer solution, and stirs;
3. in the glass infuser (3) of drop generating apparatus, inject 3%～10% polyvinyl alcohol solution by electromagnetic pump interface (2);
4. the vinyl polymer solution that contains nm gold particles is injected in the polyvinyl alcohol solution in the glass infuser (3) by tip glass tube (4), makes vinyl polymer solution by glass point mouth (4) in polyvinyl alcohol solution, be dispersed into one by one spherical droplets;
The bore that the sharp mouth of tip glass tube (4) 5. is set is 200 μ m～500 μ m, by regulating the injection speed of vinyl polymer solution and polyvinyl alcohol solution, and grass tube (5) upper end is to the distance between the tip glass tube point mouth (4), obtain the spherical droplets of required size, collect the ethene polymers drop that comprises nm gold particles with flask;
6. flask 30 ℃～70 ℃ slow rotary evaporations on Rotary Evaporators, to accelerate the volatilization of organic solvent in the vinyl polymer solution, treat that volatilization finishes, droplet solidification becomes the polymer microballoon of the nm gold particles coding of dry, hard.
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| CN 200510040518 CN1280340C (en) | 2005-06-15 | 2005-06-15 | Polymer microsphere encoded by nano-gold and method for preparing same |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102230896A (en) * | 2011-04-11 | 2011-11-02 | 西安交通大学 | Method for quantitative detection of ultramicro-protein based on principle of biomineralization |
| CN103159969A (en) * | 2013-03-13 | 2013-06-19 | 哈尔滨工业大学 | Preparation method and self-repair method of self-repairable polymethylmethacrylate resin film |
| CN107305776A (en) * | 2016-04-18 | 2017-10-31 | 中国科学院化学研究所 | A kind of information recording method and information transmitting methods using photonic crystal as carrier |
-
2005
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102230896A (en) * | 2011-04-11 | 2011-11-02 | 西安交通大学 | Method for quantitative detection of ultramicro-protein based on principle of biomineralization |
| CN102230896B (en) * | 2011-04-11 | 2013-07-10 | 西安交通大学 | Method for quantitative detection of ultramicro-protein based on principle of biomineralization |
| CN103159969A (en) * | 2013-03-13 | 2013-06-19 | 哈尔滨工业大学 | Preparation method and self-repair method of self-repairable polymethylmethacrylate resin film |
| CN107305776A (en) * | 2016-04-18 | 2017-10-31 | 中国科学院化学研究所 | A kind of information recording method and information transmitting methods using photonic crystal as carrier |
| CN107305776B (en) * | 2016-04-18 | 2019-12-10 | 中国科学院化学研究所 | Information recording method and information transmission method using photonic crystal as carrier |
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