CN107243629A - A kind of new type structure of hud nano-particle and preparation method thereof - Google Patents
A kind of new type structure of hud nano-particle and preparation method thereof Download PDFInfo
- Publication number
- CN107243629A CN107243629A CN201710434566.9A CN201710434566A CN107243629A CN 107243629 A CN107243629 A CN 107243629A CN 201710434566 A CN201710434566 A CN 201710434566A CN 107243629 A CN107243629 A CN 107243629A
- Authority
- CN
- China
- Prior art keywords
- solution
- nanometer gold
- gold bar
- dna
- adds
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
- B22F1/102—Metallic powder coated with organic material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention discloses a kind of new type structure of hud nano-particle, preparation method is:(1) CTAB solution is added in container, adds HAuCl4Solution, adds NaBH4Solution, obtains crystal seed;CTAB solution is added in another container, HAuCl is sequentially added4Nanometer gold bar is made in solution, silver nitrate solution, L AA solution, crystal seed;(2) DNA modification of nanometer gold bar, obtains the nanometer gold bar of the stable protections of sulfhydrylation DNA;(3) nanometer gold bar is centrifuged, be dissolved in CTAB solution, sequentially add SDS solution, silver nitrate solution, L AA solution, standing is produced.The nano-particle of the present invention, with extraordinary stability, the silver covering at core shell structure two ends is very thin, the connected single-stranded meeting major parts of DNA are exposed outside, tip portion has higher surface plasma bulk effect, has huge application value in fields such as bio-light electronics, biological nano detections.
Description
Technical field
The present invention relates to a kind of new type structure of hud nano-particle and preparation method thereof, belong to nanobiology and nanometer medicine
Thing field.
Background technology
Gold is extracted first as heavy metal material in B.C. 5th century, when gold is divided into less than 100nm sizes
Golden nanometer particle becomes more precious when golden.Golden nanometer particle (gold nanoparticle) is the molecule for referring to gold, and its is straight
Footpath is in 1~100nm, and golden nanometer particle has higher cloud density, dielectric property and catalytic action, with good biology
Compatibility, can be combined, and do not influence its bioactivity with a variety of large biological molecules.Diameter Nano grade golden nanometer particle,
Elementary cell is all the particle of microsize, and with the golden unexistent physical characteristic of many macroscopic views, such as optical effect, surface are imitated
Should, small-size effect, Dielectric confinement effect, macro quanta tunnel effect and some other special effectses.Golden nanometer particle
Special effects cause golden nanometer particle to be widely used in the research fields such as material, medical test, disease treatment.
Golden nanometer particle is deep to be had deep love for by researcher because of its excellent all manifold effect, and research is most sufficiently nanometer at present
Gold goal and nanometer gold bar.Nanogold is bored as a kind of new golden nanometer particle, and early stage is not very due to its synthesis preparation method
Maturation, therefore the property research of nanogold cone much also rests on theoretical research stage.Current researcher utilizes seed mediated growth method,
By controlling the temperature factor in building-up process, the extraordinary dispersed nano gold cone particle of homogeneity is obtained, has been nanogold
Quickly propelling for cone research is laid a good foundation.
The plasma model of metal nanoparticle depends on shape, size, composition and the local environment of nano-particle.Stretching
Nano-particle be optical research preferable nano-particle, its spectrum is adjusted by changing the draw ratio of particle.With nanogold
Rod is compared, and the tip portion at two ends of nanogold cone has bigger curvature, and the field enhancing of tip portion is bigger, and nanogold cone is gathered around
There are the plasma properties for surmounting nanometer gold bar.Nanogold cone is first by it has been found that be the by-product that is synthesized as nanometer gold bar
What thing was present, researcher shows that the surface plasma volume property of nanogold cone is higher than using the calculating research of FDTD scheduling theories and received
The surface plasma volume property of the golden rod of rice.Theoretical calculation shows nanogold cone in necks such as surface plasma body resonant vibration, Raman enhancings
Domain has great researching value, huge promotion will be played to the application in terms of bio-imaging, electrooptical device, treatment of cancer
Effect.
What current Raman enhancing mechanism was generally accepted mainly has both of which:Physics enhancement mode and Chemical enhancement pattern.
Physics enhancement mode is also known as surface plasma body resonant vibration model;Chemical enhancement pattern is mainly based upon technical face binding molecule
The Raman enhancing of chemical property and molecule and the environment on surface.Physics strengthens both model and Chemical enhancement model and had any different,
It is complementary to one another again simultaneously, typically in Raman enhancing, the two exists simultaneously.People under the enhanced mechanism guiding of research Raman,
Synthesize the Nano sol of various forms, such as nanometer rods, nano wire, nano flower, triangle and square.Core-shell type nano structure
Turn into study hotspot, gold and silver core shell structure is research and applies more core shell structures, and it combines the particle diameter of aurosol
Uniformly, stably, good biocompatibility the characteristics of, while possess the high Raman enhancement effect of silver again, therefore silver nucleocapsid knot covered with gold leaf
Structure has very big researching value.
What silver-colored gold filled core shell structure research was hotter at present is concentrated mainly on spherical and bar-shaped core shell structure, similar to nanometer
Golden taper and starlike core shell structure are relatively fewer.The gold and silver core shell structure surface that current method is prepared is by a thin layer of
Silver covering, can exist on some follow-up bio-modifications influences.
The content of the invention
For above-mentioned prior art, the invention provides a kind of new type structure of hud nano-particle and preparation method thereof.This
The new type structure of hud nano-particle of invention, profile is similar to the structure that nanogold is bored, common with extremely strong surface plasma
Shake effect;Body structure surface covers one layer of silver-colored film, with the Raman enhancing effect that Nano silver grain is extremely strong;For ease of modification
Gold and silver core shell structure, is easy to follow-up application study;For the nano-particle of special sex modification, the spy of 1-dimention nano particle is realized
Different in nature end modification, is the head to head configuration (head-to-head) of excellent performance.The method of the present invention utilizes the DNA with sulfydryl
The nanometer gold bar of single-stranded protection is as core, under certain environment, and silver bag is prepared using reducing agent L-AA reduction silver nitrate growths
Golden core-shell nano, the core shell structure profile is bored similar to nanogold, and the core shell structure whole body is protected by the DNA ends of the naked leakage in part
Shield, two ends silver nanoparticle layer covering is relatively thin, and most of naked leakage outside, can both play a protective role, base complementrity can be utilized again
The preparation of special construction is realized in pairing, and core shell structure property is stable, is had in fields such as bio-light electronics, biological nano detections huge
Big application value.
The present invention is achieved by the following technical solutions:
A kind of new type structure of hud nano-particle, is prepared by the following method and obtains:
(1) preparation of nanometer gold bar:At room temperature, by 10~15ml 0.1molL-1CTAB solution be added to reaction hold
In device (20ml round-bottomed flasks), 50~80ul 50mmolL is added-1HAuCl4Solution, quick stirring 1 minute;Then
It is rapidly added 0.6~1.0ml 10mmolL-1NaBH4Solution, quick stirring 1 minute, obtains crystal seed;
By 30~40ml 0.1molL-1CTAB solution be added in another reaction vessel (50ml round-bottomed flasks), fit
When (being added while stirring, with well mixed) under speed stirring, 230~250ul 50mmolL is added-1HAuCl4Solution,
Then 230~250ul 10mmolL is added-1Silver nitrate solution, add 150~180ul 0.1molL-1L-
AA solution (ascorbic acid solution), now solution become colorless by light yellow, be eventually adding 90ul crystal seeds, stir 1 minute, stand
4 hours, solution colour was changed into taupe from colourless, and nanometer gold bar is made;
The NaBH4Solution, need to use to be placed in after preceding preparation, preparation in -20 DEG C of refrigerators and place 10 minutes, stand-by;
(2) DNA modification of nanometer gold bar:At room temperature, 8000~10000rpm of nanometer gold bar of above-mentioned preparation is centrifuged 10
~20mins, reject supernatant is dissolved in 0.2% (mass percent) SDS solution, with hydrochloric acid conditioning solution pH to 3 ± 0.5,
Add 5 × tbe buffer liquid so that its final concentration of 1 × TBE, then add NaCl solution to the final concentration of 500mmol of NaCl
L-1, it is eventually adding sulfhydrylation DNA, the weight ratio of sulfhydrylation DNA and nanometer gold bar is 500~10000:1, mix, stand 5 points
Clock, obtains the nanometer gold bar of the stable protections of sulfhydrylation DNA;
The sequence of the sulfhydrylation DNA is that (5 ' ends are sulfydryl to 5 ' SH-AAA AAA AAA AAA AAA, and nucleotide sequence is such as
Shown in SEQ ID NO.1);
Sulfhydrylation DNA used (sulfhydrylation DNA sequence dna is 5 ' SH-AAA AAA AAA AAA AAA) of the invention, entrusts Shanghai
Sheng Gong bioengineering limited company synthesizes, and is purified through HPLC, is to be dissolved in ultra-pure water before freeze-dried powder, use, standby;
(3) 8000~10000rpm of the nanometer gold bar centrifugations 10 stably protected sulfhydrylation DNA obtained above~
20mins, to remove unnecessary discrete sulfhydrylation DNA in solution, is dissolved in 0.05M CTAB solution, and adding 1%SDS solution makes
SDS final concentration of 0.05~0.1% (mass fraction), adding silver nitrate solution, (mol ratio of gold, silver is 1:0.8~1:
1.5), being eventually adding reducing agent L-AA solution, (silver and L-AA mol ratio are 1:12~1:18), mix, stand 3 hours, produce
New type structure of hud nano-particle --- silver-colored gold-covered nano core-shell structure nanometer particle.
The new type structure of hud nano-particle of the present invention, with extraordinary stability, adds NaCl, concentration in the solution
When reaching 1 mole every liter, still keep being stabilized, do not occur aggregate and precipitate, be easy to follow-up correlative study.Au-Ag nucleocapsid knots
The transmission electron microscope of structure is as shown in Fig. 2 the silver covering at core shell structure two ends is very thin, therefore is connected as the nanometer gold bar of core
The single-stranded meeting major parts of DNA are exposed outside, on the one hand as blocking group, make core shell structure property stable, on the other hand can profit
With the base pairing principle of DNA double helical structure, the terminal modified one-dimensional of core shell structure two is realized.Different from general Jenner
The nano-particles such as rice grain, gold and silver core shell structure, because its modification is non-directional, it is impossible to realize special sex modification, it is difficult to realize class
It is similar to head to head (head-to-head) this structure.Researcher calculates research using FDTD scheduling theories and found, sharp receives
Rice corpuscles surface electronic is concentrated, and surface plasma body resonant vibration effect is better than the slow blunt region of nano-particle.Head to head nanostructured
It is the close structure of two nano-particle sharp parts, stronger nanoparticle surface plasma resonance can be realized.This hair
Bright new type structure of hud nano-particle, research shows that nano-particle tip portion has higher surface plasma bulk effect,
Therefore the directed modification of nano-particle has huge application value in fields such as bio-light electronics, biological nano detections.
Brief description of the drawings
Fig. 1:Core shell structure prepares simplified schematic diagram.
Fig. 2:Au-Ag core shell structures project electron microscope.
Embodiment
With reference to embodiment, the present invention is further illustrated.
Involved instrument, reagent, material etc. in following embodiments, are existing in the prior art unless otherwise noted
Conventional instrument, reagent, material etc., can be obtained by regular commercial sources.Involved experimental method in following embodiments, inspection
Survey method etc., is existing normal experiment method in the prior art, detection method etc. unless otherwise noted.
Embodiment 1 prepares new type structure of hud nano-particle
Preparation process is as shown in figure 1, step is as follows:
(1) preparation of nanometer gold bar:At room temperature, by 10ml 0.1molL-1CTAB solution be added to container (20ml
Round-bottomed flask) in, add 50ul 50mmolL-1HAuCl4Solution, quick stirring 1 minute;Then it is rapidly added
0.6ml 10mmolL-1NaBH4Solution, quick stirring 1 minute, obtains crystal seed;
By 30ml 0.1molL-1CTAB solution be added in another container (50ml round-bottomed flasks), appropriate speed is stirred
Mix down and (add while stirring, with well mixed), add 234ul 50mmolL-1HAuCl4Solution, then adds 234ul
10mmolL-1Silver nitrate solution, add 150ul 0.1molL-1L-AA solution (ascorbic acid solution), this
When solution become colorless by light yellow, be eventually adding 90ul crystal seeds, stir 1 minute, stand 4 hours, solution colour is by without discoloration
For taupe, nanometer gold bar is made;
The NaBH4Solution, is prepared using preceding, is placed in -20 DEG C of refrigerators and places 10 minutes after preparation, stand-by;
(2) DNA modification of nanometer gold bar:At room temperature, the nanometer gold bar 8000rpm of above-mentioned preparation is centrifuged into 15min, reject
Supernatant, is dissolved in 0.2% (mass percent) SDS solution, with hydrochloric acid conditioning solution pH to 3, adds 5 × tbe buffer liquid, makes
Its final concentration of 1 × TBE is obtained, NaCl solution is then added to the final concentration of 500mmolL of NaCl-1, it is eventually adding sulfhydrylation
(the weight ratio of sulfhydrylation DNA and nanometer gold bar is 2000 to DNA:1), mix, stand 5 minutes, obtain the stable protections of sulfhydrylation DNA
Nanometer gold bar;
Sulfhydrylation DNA used of the invention, sequence is 5 ' SH-AAA AAA AAA AAA AAA, the biological work of commission Shanghai life work
Journey limited company synthesizes, and is purified through HPLC, is to be dissolved in ultra-pure water before freeze-dried powder, use, standby;
The synthesis of Shanghai Sheng Gong bioengineering limited company is entrusted, is purified through HPLC, is to be dissolved in before freeze-dried powder, use
It is standby in ultra-pure water;
(3) the nanometer gold bar 8000rpm of the stable protections of sulfhydrylation DNA obtained above is centrifuged 15min to remove solution
In unnecessary discrete dna, be dissolved in 0.05M CTAB solution, adding 1%SDS solution makes the (quality point of SDS final concentration of 0.05%
Number), adding silver nitrate solution, (mol ratio of gold, silver is 1:1), being eventually adding reducing agent L-AA solution, (silver rubs with L-AA's
You are than being 1:15), mix, stand 3 hours, produce new type structure of hud nano-particle --- silver-colored gold-covered nano nuclear shell structure nano
Particle.
The new type structure of hud nano-particle of the present invention, with extraordinary stability, adds NaCl, concentration in the solution
When reaching 1 mole every liter, still keep being stabilized, do not occur aggregate and precipitate, be easy to follow-up correlative study.Au-Ag nucleocapsid knots
The transmission electron microscope of structure is as shown in Fig. 2 the silver covering at core shell structure two ends is very thin, therefore is connected as the nanometer gold bar of core
The single-stranded meeting major parts of DNA are exposed outside, on the one hand as blocking group, make core shell structure property stable, on the other hand can profit
With the base pairing principle of DNA double helical structure, the terminal modified one-dimensional of core shell structure two is realized.Different from general Jenner
The nano-particles such as rice grain, gold and silver core shell structure, because its modification is non-directional, it is impossible to realize special sex modification, it is difficult to realize class
It is similar to head to head (head-to-head) this structure.Researcher calculates research using FDTD scheduling theories and found, sharp receives
Rice corpuscles surface electronic is concentrated, and surface plasma body resonant vibration effect is better than the slow blunt region of nano-particle.Head to head nanostructured
It is the close structure of two nano-particle sharp parts, stronger nanoparticle surface plasma resonance can be realized.This hair
Bright new type structure of hud nano-particle, research shows that nano-particle tip portion has higher surface plasma bulk effect,
Therefore the directed modification of nano-particle has huge application value in fields such as bio-light electronics, biological nano detections.
Embodiment 2 prepares new type structure of hud nano-particle
Step is as follows:
(1) preparation of nanometer gold bar:At room temperature, by 15ml 0.1molL-1CTAB solution be added to reaction vessel
In (20ml round-bottomed flasks), 80ul 50mmolL is added-1HAuCl4Solution, quick stirring 1 minute;Then it is rapid to add
Enter 1.0ml 10mmolL-1NaBH4Solution, quick stirring 1 minute, obtains crystal seed;
By 40ml 0.1molL-1CTAB solution be added in another reaction vessel (50ml round-bottomed flasks), appropriate speed
(added while stirring, with well mixed) under degree stirring, add 250ul 50mmolL-1HAuCl4Solution, is then added
250ul 10mmolL-1Silver nitrate solution, add 180ul 0.1molL-1L-AA solution (ascorbic acid is molten
Liquid), now solution is become colorless by light yellow, is eventually adding 90ul crystal seeds, is stirred 1 minute, stands 4 hours, solution colour by
It is colourless to be changed into taupe, nanometer gold bar is made;
The NaBH4Solution, need to use to be placed in after preceding preparation, preparation in -20 DEG C of refrigerators and place 10 minutes, stand-by;
(2) DNA modification of nanometer gold bar:At room temperature, the nanometer gold bar 10000rpm of above-mentioned preparation is centrifuged into 20mins, abandoned
Except supernatant, it is dissolved in 0.2% (mass percent) SDS solution, with hydrochloric acid conditioning solution pH to 3, adds 5 × tbe buffer liquid,
So that its final concentration of 1 × TBE, then adds NaCl solution to the final concentration of 500mmolL of NaCl-1, it is eventually adding sulfhydrylation
The weight ratio of DNA, sulfhydrylation DNA and nanometer gold bar is 10000:1, mix, stand 5 minutes, obtain the stable protections of sulfhydrylation DNA
Nanometer gold bar;
(3) the nanometer gold bar 10000rpm by the stable protections of sulfhydrylation DNA obtained above centrifuges 20mins, molten to remove
Unnecessary discrete sulfhydrylation DNA, is dissolved in 0.05M CTAB solution in liquid, and adding 1%SDS solution makes SDS final concentration of 0.1%
(mass fraction), adding silver nitrate solution, (mol ratio of gold, silver is 1:1.5), be eventually adding reducing agent L-AA solution (silver with
L-AA mol ratio is 1:18), mix, stand 3 hours, produce new type structure of hud nano-particle --- silver-colored gold-covered nano nucleocapsid
Structure nano particle.
Embodiment 3 prepares new type structure of hud nano-particle
Step is as follows:
(1) preparation of nanometer gold bar:At room temperature, by 12ml 0.1molL-1CTAB solution be added to reaction vessel
In (20ml round-bottomed flasks), 60ul 50mmolL is added-1HAuCl4Solution, quick stirring 1 minute;Then it is rapid to add
Enter 0.8ml 10mmolL-1NaBH4Solution, quick stirring 1 minute, obtains crystal seed;
By 35ml 0.1molL-1CTAB solution be added in another reaction vessel (50ml round-bottomed flasks), appropriate speed
(added while stirring, with well mixed) under degree stirring, add 240ul 50mmolL-1HAuCl4Solution, is then added
240ul 10mmolL-1Silver nitrate solution, add 170ul 0.1molL-1L-AA solution (ascorbic acid is molten
Liquid), now solution is become colorless by light yellow, is eventually adding 90ul crystal seeds, is stirred 1 minute, stands 4 hours, solution colour by
It is colourless to be changed into taupe, nanometer gold bar is made;
The NaBH4Solution, need to use to be placed in after preceding preparation, preparation in -20 DEG C of refrigerators and place 10 minutes, stand-by;
(3) DNA modification of nanometer gold bar:At room temperature, the nanometer gold bar 8000rpm of above-mentioned preparation is centrifuged into 20mins, abandoned
Except supernatant, it is dissolved in 0.2% (mass percent) SDS solution, with hydrochloric acid conditioning solution pH to 3, adds 5 × tbe buffer liquid,
So that its final concentration of 1 × TBE, then adds NaCl solution to the final concentration of 500mmolL of NaCl-1, it is eventually adding sulfhydrylation
The weight ratio of DNA, sulfhydrylation DNA and nanometer gold bar is 5000:1, mix, stand 5 minutes, obtain the stable protections of sulfhydrylation DNA
Nanometer gold bar;
(3) the nanometer gold bar 8000rpm by the stable protections of sulfhydrylation DNA obtained above centrifuges 20mins, molten to remove
Unnecessary discrete sulfhydrylation DNA, is dissolved in 0.05M CTAB solution in liquid, and adding 1%SDS solution makes SDS final concentration of
0.08% (mass fraction), adding silver nitrate solution, (mol ratio of gold, silver is 1:0.8), it is eventually adding reducing agent L-AA molten
(silver and L-AA mol ratio are 1 to liquid:12), mixing, stand 3 hours, produce new type structure of hud nano-particle --- silver is covered with gold leaf
Nano-core-shell structure nano-particle.
Claims (6)
1. a kind of new type structure of hud nano-particle, it is characterised in that:It is prepared by the following method and obtains:
(1) preparation of nanometer gold bar:At room temperature, by 10~15ml 0.1molL-1CTAB solution be added to reaction vessel
In, add 50~80ul 50mmolL-1HAuCl4Solution, is stirred 1 minute;Then add 0.6~1.0ml's
10mmol·L-1NaBH4Solution, stirs 1 minute, obtains crystal seed;
By 30~40ml 0.1molL-1CTAB solution be added in another reaction vessel, under stirring, add 230~
250ul 50mmolL-1HAuCl4Solution, then adds 230~250ul 10mmolL-1Silver nitrate solution, then add
Enter 150~180ul 0.1molL-1L-AA solution, be eventually adding 90ul crystal seeds, stir 1 minute, stand 4 hours, be made
Nanometer gold bar;
(2) DNA modification of nanometer gold bar:At room temperature, by 8000~10000rpm of nanometer gold bar of above-mentioned preparation centrifugation 10~
20mins, reject supernatant is dissolved in 0.2%SDS solution, with hydrochloric acid conditioning solution pH to 3 ± 0.5, adds tbe buffer liquid,
So that its final concentration of 1 × TBE, then adds NaCl solution to the final concentration of 500mmolL of NaCl-1, it is eventually adding sulfhydrylation
The weight ratio of DNA, sulfhydrylation DNA and nanometer gold bar is 500~10000:1, mix, stand 5 minutes, obtain sulfhydrylation DNA steady
Surely the nanometer gold bar protected;
(3) 8000~10000rpm of nanometer gold bar by the stable protections of sulfhydrylation DNA obtained above centrifuges 10~20mins, molten
Solution is in 0.05M CTAB solution, and adding SDS solution makes SDS final concentration of 0.05~0.1%, adds silver nitrate solution, gold,
The mol ratio of silver is 1:0.8~1:1.5, reducing agent L-AA solution is eventually adding, the silver-colored mol ratio with L-AA is 1:12~1:18,
Mix, stand 3 hours, produce.
2. new type structure of hud nano-particle according to claim 1, it is characterised in that:The sequence of the sulfhydrylation DNA
For 5 ' SH-AAA AAA AAA AAA AAA.
3. new type structure of hud nano-particle according to claim 1 or 2, it is characterised in that:Step is as follows:
(1) preparation of nanometer gold bar:At room temperature, by 10ml 0.1molL-1CTAB solution be added in container, add
50ul 50mmolL-1HAuCl4Solution, quick stirring 1 minute;Then it is rapidly added 0.6ml 10mmolL-1NaBH4
Solution, quick stirring 1 minute, obtains crystal seed;
By 30ml 0.1molL-1CTAB solution be added in another container, under stirring, add 234ul 50mmolL-1
HAuCl4Solution, then adds 234ul 10mmolL-1Silver nitrate solution, add 150ul 0.1molL-1's
L-AA solution, is eventually adding 90ul crystal seeds, stirs 1 minute, stands 4 hours, and nanometer gold bar is made;
The NaBH4Solution, is prepared using preceding, is placed in -20 DEG C of refrigerators and places 10 minutes after preparation, stand-by;
(2) DNA modification of nanometer gold bar:At room temperature, the nanometer gold bar 8000rpm of above-mentioned preparation is centrifuged into 15min, reject supernatant
Liquid, is dissolved in 0.2%SDS solution, with hydrochloric acid conditioning solution pH to 3, adds 5 × tbe buffer liquid so that its final concentration of 1 ×
TBE, then adds NaCl solution to the final concentration of 500mmolL of NaCl-1, sulfhydrylation DNA is eventually adding, sulfhydrylation DNA is with receiving
The weight ratio of the golden rod of rice is 2000:1, mix, stand 5 minutes, obtain the nanometer gold bar of the stable protections of sulfhydrylation DNA;
(3) it is the nanometer gold bar 8000rpm centrifugations 15min of the stable protections of sulfhydrylation DNA obtained above is more in solution to remove
Remaining discrete dna, is dissolved in 0.05M CTAB solution, and adding 1%SDS solution makes SDS final concentration of 0.05%, adds nitric acid
Silver-colored solution, the mol ratio of gold, silver is 1:1, reducing agent L-AA solution is eventually adding, the silver-colored mol ratio with L-AA is 1:15, mix,
3 hours are stood, is produced.
4. a kind of preparation method of new type structure of hud nano-particle, it is characterised in that:Comprise the following steps:
(1) preparation of nanometer gold bar:At room temperature, by 10~15ml 0.1molL-1CTAB solution be added to reaction vessel
In, add 50~80ul 50mmolL-1HAuCl4Solution, is stirred 1 minute;Then add 0.6~1.0ml's
10mmol·L-1NaBH4Solution, stirs 1 minute, obtains crystal seed;
By 30~40ml 0.1molL-1CTAB solution be added in another reaction vessel, under stirring, add 230~
250ul 50mmolL-1HAuCl4Solution, then adds 230~250ul 10mmolL-1Silver nitrate solution, then add
Enter 150~180ul 0.1molL-1L-AA solution, be eventually adding 90ul crystal seeds, stir 1 minute, stand 4 hours, be made
Nanometer gold bar;
(2) DNA modification of nanometer gold bar:At room temperature, by 8000~10000rpm of nanometer gold bar of above-mentioned preparation centrifugation 10~
20mins, reject supernatant is dissolved in 0.2%SDS solution, with hydrochloric acid conditioning solution pH to 3 ± 0.5, adds tbe buffer liquid,
So that its final concentration of 1 × TBE, then adds NaCl solution to the final concentration of 500mmolL of NaCl-1, it is eventually adding sulfhydrylation
The weight ratio of DNA, sulfhydrylation DNA and nanometer gold bar is 500~10000:1, mix, stand 5 minutes, obtain sulfhydrylation DNA steady
Surely the nanometer gold bar protected;
(3) 8000~10000rpm of nanometer gold bar by the stable protections of sulfhydrylation DNA obtained above centrifuges 10~20mins, molten
Solution is in 0.05M CTAB solution, and adding SDS solution makes SDS final concentration of 0.05~0.1%, adds silver nitrate solution, gold,
The mol ratio of silver is 1:0.8~1:1.5, reducing agent L-AA solution is eventually adding, the silver-colored mol ratio with L-AA is 1:12~1:18,
Mix, stand 3 hours, produce.
5. the preparation method of new type structure of hud nano-particle according to claim 3, it is characterised in that:The sulfhydrylation
DNA sequence is 5 ' SH-AAA AAA AAA AAA AAA.
6. the preparation method of the new type structure of hud nano-particle according to claim 4 or 5, it is characterised in that:Step is such as
Under:
(1) preparation of nanometer gold bar:At room temperature, by 10ml 0.1molL-1CTAB solution be added in container, add
50ul 50mmolL-1HAuCl4Solution, quick stirring 1 minute;Then it is rapidly added 0.6ml 10mmolL-1NaBH4
Solution, quick stirring 1 minute, obtains crystal seed;
By 30ml 0.1molL-1CTAB solution be added in another container, under stirring, add 234ul 50mmolL-1
HAuCl4Solution, then adds 234ul 10mmolL-1Silver nitrate solution, add 150ul 0.1molL-1's
L-AA solution, is eventually adding 90ul crystal seeds, stirs 1 minute, stands 4 hours, and nanometer gold bar is made;
The NaBH4Solution, is prepared using preceding, is placed in -20 DEG C of refrigerators and places 10 minutes after preparation, stand-by;
(2) DNA modification of nanometer gold bar:At room temperature, the nanometer gold bar 8000rpm of above-mentioned preparation is centrifuged into 15min, reject supernatant
Liquid, is dissolved in 0.2%SDS solution, with hydrochloric acid conditioning solution pH to 3, adds 5 × tbe buffer liquid so that its final concentration of 1 ×
TBE, then adds NaCl solution to the final concentration of 500mmolL of NaCl-1, sulfhydrylation DNA is eventually adding, sulfhydrylation DNA is with receiving
The weight ratio of the golden rod of rice is 2000:1, mix, stand 5 minutes, obtain the nanometer gold bar of the stable protections of sulfhydrylation DNA;
(3) it is the nanometer gold bar 8000rpm centrifugations 15min of the stable protections of sulfhydrylation DNA obtained above is more in solution to remove
Remaining discrete dna, is dissolved in 0.05M CTAB solution, and adding 1%SDS solution makes SDS final concentration of 0.05%, adds nitric acid
Silver-colored solution, the mol ratio of gold, silver is 1:1, reducing agent L-AA solution is eventually adding, the silver-colored mol ratio with L-AA is 1:15, mix,
3 hours are stood, is produced.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201710434566.9A CN107243629B (en) | 2017-06-09 | 2017-06-09 | A kind of core-shell structure nanometer particle and preparation method thereof |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201710434566.9A CN107243629B (en) | 2017-06-09 | 2017-06-09 | A kind of core-shell structure nanometer particle and preparation method thereof |
Publications (2)
Publication Number | Publication Date |
---|---|
CN107243629A true CN107243629A (en) | 2017-10-13 |
CN107243629B CN107243629B (en) | 2019-01-22 |
Family
ID=60018017
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201710434566.9A Active CN107243629B (en) | 2017-06-09 | 2017-06-09 | A kind of core-shell structure nanometer particle and preparation method thereof |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN107243629B (en) |
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107916263A (en) * | 2017-11-10 | 2018-04-17 | 刁晓荃 | The preservation particulate and long-term preservation method of inhereditary material |
CN108048906A (en) * | 2017-12-08 | 2018-05-18 | 中山大学 | A kind of DNA is oriented to gold nano-crystal and preparation method and application |
CN108145176A (en) * | 2018-01-10 | 2018-06-12 | 云南大学 | A kind of autoreduction preparation method of gold nano ball-bar polymer |
CN110625138A (en) * | 2019-10-30 | 2019-12-31 | 中山大学 | DNA-oriented gold-silver bimetallic nanoparticle and preparation method and application thereof |
CN111408732A (en) * | 2020-04-23 | 2020-07-14 | 江南大学 | Method for synthesizing chiral nano material by utilizing DNA induction and chiral light auxiliary growth |
Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102382815A (en) * | 2011-09-15 | 2012-03-21 | 王利兵 | Binary plasma nanoparticle site singularity self-assembly method |
CN102825261A (en) * | 2012-09-29 | 2012-12-19 | 江南大学 | Binary plasma nanoparticle site specificity self-assembling method |
CN102908633A (en) * | 2012-07-31 | 2013-02-06 | 南京大学 | Multifunctional gold and silver core-shell nanoparticles and preparation method |
WO2013069732A1 (en) * | 2011-11-08 | 2013-05-16 | 財団法人神奈川科学技術アカデミー | Magnetic nanoparticles |
CN103776772A (en) * | 2014-02-14 | 2014-05-07 | 国家纳米科学中心 | Method for detecting DNA (deoxyribonucleic acid) on basis of gold nanocone accumulated circular dichroism signal |
CN104985176A (en) * | 2015-06-11 | 2015-10-21 | 江南大学 | Preparation method of silver-wrapped gold nanorod dimer with controllable chiral signals |
CN106729710A (en) * | 2016-12-20 | 2017-05-31 | 上海纳米技术及应用国家工程研究中心有限公司 | A kind of thermochemotherapy Integral rice grain and preparation and application |
-
2017
- 2017-06-09 CN CN201710434566.9A patent/CN107243629B/en active Active
Patent Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102382815A (en) * | 2011-09-15 | 2012-03-21 | 王利兵 | Binary plasma nanoparticle site singularity self-assembly method |
WO2013069732A1 (en) * | 2011-11-08 | 2013-05-16 | 財団法人神奈川科学技術アカデミー | Magnetic nanoparticles |
CN102908633A (en) * | 2012-07-31 | 2013-02-06 | 南京大学 | Multifunctional gold and silver core-shell nanoparticles and preparation method |
CN102825261A (en) * | 2012-09-29 | 2012-12-19 | 江南大学 | Binary plasma nanoparticle site specificity self-assembling method |
CN103776772A (en) * | 2014-02-14 | 2014-05-07 | 国家纳米科学中心 | Method for detecting DNA (deoxyribonucleic acid) on basis of gold nanocone accumulated circular dichroism signal |
CN104985176A (en) * | 2015-06-11 | 2015-10-21 | 江南大学 | Preparation method of silver-wrapped gold nanorod dimer with controllable chiral signals |
CN106729710A (en) * | 2016-12-20 | 2017-05-31 | 上海纳米技术及应用国家工程研究中心有限公司 | A kind of thermochemotherapy Integral rice grain and preparation and application |
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107916263A (en) * | 2017-11-10 | 2018-04-17 | 刁晓荃 | The preservation particulate and long-term preservation method of inhereditary material |
CN108048906A (en) * | 2017-12-08 | 2018-05-18 | 中山大学 | A kind of DNA is oriented to gold nano-crystal and preparation method and application |
CN108145176A (en) * | 2018-01-10 | 2018-06-12 | 云南大学 | A kind of autoreduction preparation method of gold nano ball-bar polymer |
CN110625138A (en) * | 2019-10-30 | 2019-12-31 | 中山大学 | DNA-oriented gold-silver bimetallic nanoparticle and preparation method and application thereof |
CN110625138B (en) * | 2019-10-30 | 2022-07-22 | 中山大学 | DNA-oriented gold-silver bimetallic nanoparticle and preparation method and application thereof |
CN111408732A (en) * | 2020-04-23 | 2020-07-14 | 江南大学 | Method for synthesizing chiral nano material by utilizing DNA induction and chiral light auxiliary growth |
Also Published As
Publication number | Publication date |
---|---|
CN107243629B (en) | 2019-01-22 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN107243629B (en) | A kind of core-shell structure nanometer particle and preparation method thereof | |
Zhan et al. | A study of mesoporous silica-encapsulated gold nanorods as enhanced light scattering probes for cancer cell imaging | |
Ratto et al. | Size and shape control in the overgrowth of gold nanorods | |
Zhang et al. | Synthesis of size-tunable chitosan encapsulated gold–silver nanoflowers and their application in SERS imaging of living cells | |
CN105036070B (en) | Gold nanorod-silicon dioxide core-shell structure nanometer material, preparation method and application | |
CN107849726A (en) | The bicone template of single dispersing noble metal nano crystal is combined to | |
CN105832699B (en) | A kind of Fe3O4@SiO2The preparation method and application of yolk-eggshell structure hollow complex microsphere | |
Liu et al. | Plasmonic property and stability of core-shell Au@ SiO 2 nanostructures | |
US20170219572A1 (en) | Lspr-based high sensitivity aptamer sensor using intercalation agent | |
CN107418554B (en) | A kind of gold nanorods and upper conversion nano crystalline substance composite nano materials and preparation method thereof | |
CN108723385A (en) | A kind of monocrystalline silver nanoparticle ball aqueous phase preparation method | |
CN113770372B (en) | Preparation method of gold nanoparticle aggregate material | |
CN109596822A (en) | A kind of gold core silver shell nanocomposite and preparation method thereof | |
CN109128210A (en) | A kind of dumbbell shaped gold nano bipyramid/argentum nano composite material and preparation method thereof | |
CN104384523B (en) | Preparing method of three-dimensional chiral silver nanometer material | |
Liu et al. | Aptamer-modified selenium nanoparticles for dark-field microscopy imaging of nucleolin | |
CN103923656A (en) | Preparation method of gadolinium oxide-coated ferroferric oxide magnetic fluorescent nano hollow spheres | |
CN106887295A (en) | A kind of structure and preparation method of magnetic honeysuckle flower nano particle | |
Yang et al. | The early life of gold nanorods: temporal separation of anisotropic and isotropic growth modes | |
CN105149613A (en) | Preparation method for flaky silver nanometer materials | |
Xu et al. | Synthesis and characterisation of a pH-sensitive magnetic nanocomposite for controlled delivery of doxorubicin | |
CN111718705A (en) | One-dimensional core-shell structure nano material with optimized metal fluorescence enhancement effect and preparation method thereof | |
CN106141172B (en) | Three-dimensional " photo frame and photograph " structure nano gold material, its synthetic method and application | |
Zeng et al. | Up-down conversion luminescence and drug-loading capability of novel MoO3-x based carriers | |
Nafisah et al. | Synthesis of gold nanorices on ITO substrate using silver seed-mediated growth method |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
GR01 | Patent grant | ||
GR01 | Patent grant |