CN106001606A - Preparing method capable of adjusting particle size of gold nanoparticles based on sodium citrate reduction method - Google Patents
Preparing method capable of adjusting particle size of gold nanoparticles based on sodium citrate reduction method Download PDFInfo
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- CN106001606A CN106001606A CN201610517781.0A CN201610517781A CN106001606A CN 106001606 A CN106001606 A CN 106001606A CN 201610517781 A CN201610517781 A CN 201610517781A CN 106001606 A CN106001606 A CN 106001606A
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- 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
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- 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
Abstract
The invention relates to a preparing method capable of adjusting the particle size of gold nanoparticles based on a sodium citrate reduction method. Sodium citrate serves as a reducing agent to reduce chloroauric acid, nucleation is controlled to prepare gold nanoparticles with different particle diameters, the influence of the particle size of the gold nanoparticles on the gold nanoparticles in the immunolabelling field is researched, and the nano gold marking efficiency is improved; and the method has the beneficial effects that compared with other methods, the method for using the sodium citrate for reducing the chloroauric acid to prepare the gold nanoparticles with different particle sizes has the obvious advantages in controllability, and the prepared gold nanoparticles are uniform in dispersion. Only through control over nucleation, that is, only through control over the frequency of adding of sodium citrate and chloroauric acid, the gold nanoparticles with different particle sizes can be prepared, and the particle size ranges from 16.6 nm to 64.7 nm.
Description
Technical field
The present invention relates to technical field of nanometer material preparation, regulate gold nano more particularly to one based on reduction of sodium citrate method
The preparation method of particle granules size.
Background technology
Square being directly proportional of the surface area of spheroidal particle and diameter, cube being directly proportional of its volume and diameter, therefore its specific surface area
(surface area/volume) and diameter are inversely proportional to.Along with particle diameter diminishes, specific surface area will significantly increase, and illustrates that surface is former
Percent shared by son will significantly increase.Negligible to the diameter particle surface effect more than 0.1 micron, work as size
During less than 0.1 micron, its surface atom percent swashs the length that increases severely, and the even summation of 1 gram of ultramicro powder surface area may be up to 100
Square metre, skin effect at this moment is by non-negligible.Along with the reduction of nano material particle diameter, surface atom number increases sharply.Example
As when particle diameter is 10nm, surface atom number is the 20% of full die total atom number；And particle diameter is when being 1nm, its surface is former
Sub-percent increases to 99%；All about 30 the atom almost all now forming this nanocrystal are distributed in surface.Due to
Lack adjacent atom around surface atom: have many dangling bonds, there is unsaturation, easily combine with other atoms and stablize
Get off, therefore show the highest chemism.Along with the reduction of particle diameter, the surface area of nano material, surface energy and surface combine
Can increase the most rapidly, therefore nano material has that particle size is little, specific surface area big, surface can high, surface atom proportion
The feature such as big.Therefore the size inquiring into nanoparticle has directive significance for preferably application nanoparticle.
Nanometer gold i.e. refers to the molecule of gold, and its diameter, 1～100nm, has high electron density, dielectric property and catalysis and makees
With, can be combined with multiple biomacromolecule, and not affect its biological activity.Can be prepared easily by reducing process by gold chloride
The nanometer gold of various different-grain diameters, its color takes on a red color to purple according to diameter.As one of modern four big labelling techniques
Nano gold mark technology (nanogold labelling techique), substantially the macromolecule such as protein is adsorbed to nanogold particle
Surface be coated process.Adsorption mechanism is probably nanogold particle surface negative charge, inhales because of electrostatic with the positive charge group of protein
Attached and form strong bonded, and biomolecule degeneration will not be made after adsorbing, owing to gold grain has the characteristic of high electron density,
At gold mark protein binding, visible pitchy granule under the microscope, when these labels are assembled at corresponding part in a large number
Time, naked eyes red color visible or pink speckle, thus in qualitative or semiquantitative tachysynthesis detection method.Due to spherical
Nano Au particle protein is had the strongest adsorption function, can with staphylococcal protein A, immunoglobulin, toxin,
The Non-covalent binding such as glycoprotein, enzyme, antibiotic, hormone, bovine serum albumin, thus become non-in basic research and experiment
The instrument of Chang Youyong.So the present invention intends developing a kind of preparation based on reduction of sodium citrate method regulation golden nanometer particle particle size
Method, sets about improving the efficiency of nano gold mark technology, thus is mark diagnostic disease on the horizon from the skin effect of nanometer
Revolution is provided fundamental basis.
Summary of the invention
In view of golden nanometer particle unique advantage in terms of immunolabelling technique, nano-particles size are for nanoparticle physical chemistry
The tremendous influence of performance.We will utilize sodium citrate as reducing agent, reduce gold chloride, and by controlling nucleation preparation difference
The golden nanometer particle of particle diameter, research gold nanometer particle grain size size for the golden nanometer particle impact in immune labeled field,
Improve nano gold mark efficiency.
Technical scheme is as follows:
A kind of preparation method based on reduction of sodium citrate method regulation golden nanometer particle particle size；Its step is as follows:
(1) sodium citrate solution is joined reactor, under the conditions of magnetic agitation, be heated to boiling, add gold chloride molten
Liquid, solution stops heating after becoming lightpink, and solution cools to 90～95 DEG C, adds the reaction of equivalent chlorauric acid solution
20～30min, again add the reaction of equivalent chlorauric acid solution and obtain gold kind solution；
(2) gold is planted solution and the sodium citrate solution mixing growth-promoting media as reaction, and growth-promoting media is heated to 90～95 DEG C of additions
React 20～30min with the chlorauric acid solution of step (1) equivalent, again add equivalent chlorauric acid solution and obtain next step reaction
Gold plants solution；
(3) step (2) repeats 1～5 time, prepares the golden nanometer particle of different-grain diameter.
Described step (1) and (2) gold chloride are four hydration gold chlorides.
The mol ratio of described step (1) gold chloride and sodium citrate is 1:10～20.
Described step (2) gold kind solution: gold chloride: sodium citrate mol ratio is 1:1:10～20.
Described step (3) regulation number of repetition, i.e. can get the golden nanometer particle of different-grain diameter, and number of repetition is the most, Jenner
Rice corpuscles particle diameter is the biggest.
The golden nanometer particle that the present invention obtains as can be seen from Figure 1 is spherical nanoparticle, and golden nanometer particle size exists
Between 16.6～64.7nm, and it is uniformly dispersed.From the granularity data of Fig. 2 golden nanometer particle it can also be seen that granularity data is with electric
Mirror photo coincide.Fig. 3 ultra-violet absorption spectrum display golden nanometer particle of preparing of the present invention launch wavelength 520nm～550nm it
Between, show that the gold nano grain of different-grain diameter is the most successfully prepared.
The golden nanometer particle advantage of different-grain diameter prepared by the present invention is:
The most only by controlling nucleation, the number of times i.e. adding sodium citrate and gold chloride can prepare the golden nanometer particle of different-grain diameter,
Grain size is between 16.6～64.7nm, and is uniformly dispersed.
2. can optimize the optimum mark particle diameter of nanometer gold by the immune labeled experiment of golden nanometer particle of different-grain diameter, optimize labelling
Efficiency, improves the sensitivity of detection.
3. the method that the golden nanometer particle of different-grain diameter prepared by the present invention uses reduction of sodium citrate gold chloride, controllability is than it
He has a clear superiority at method, and the golden nanometer particle dispersion of preparation is homogeneous.
Accompanying drawing explanation
The electromicroscopic photograph of different-grain diameter golden nanometer particle prepared by Fig. 1 present invention, 16.6nm (a)；21.0nm(b)；26.6nm(c)；
35.5nm(d)；41.2nm(e)；48.6nm(f)；54.4nm(g)；64.7nm(h).
The ultra-violet absorption spectrum of different-grain diameter golden nanometer particle prepared by Fig. 2 present invention, be followed successively by from left to right 16.6nm,
21.0nm, 26.6nm, 35.5nm, 41.2nm, 48.6nm, 54.4nm and 4.7nm.
The granularity data of different-grain diameter golden nanometer particle prepared by Fig. 3 present invention, 16.6nm (a)；21.0nm(b)；26.6nm(c)；
35.5nm(d)；41.2nm(e)；48.6nm(f)；54.4nm(g)；64.7nm(h).
Different-grain diameter golden nanometer particle immune labeled Experimental comparison figure prepared by Fig. 4 present invention.
Detailed description of the invention
In following case study on implementation, the invention will be further elaborated, but the invention is not restricted to this.
Embodiment 1:
(1) 150mL 2.2mM sodium citrate solution is joined reactor, under the conditions of magnetic agitation, be heated to boiling, add
Entering 1mL 24mM chlorauric acid solution, solution stops heating after becoming lightpink, and solution cools to 90 DEG C, adds 1mL
24mM chlorauric acid solution reaction 30min, again adds the reaction of 1mL 24mM chlorauric acid solution and obtains gold kind solution；
(2) above-mentioned 55mL gold kind solution and 2mL 60mM sodium citrate solution and 53mL pure water are mixed as next
The growth-promoting media of step reaction, growth-promoting media adds 1mL24mM chlorauric acid solution reaction 30min, again addition etc. after being heated to 90 DEG C
Amount chlorauric acid solution obtains the gold of next step reaction and plants solution；
(3) step (2) is repeated 1 times, and obtains solution of gold nanoparticles.
As Fig. 1 (a) and 3 (a) understand, step (1) gained gold nanometer particle grain size is 16.6nm；Fig. 2 (a) understands
Golden nanometer particle has the strongest uv absorption at 520nm, corresponding with its grain size.
As Fig. 1 (d) and 3 (d) understand, gained (3) gold nanometer particle grain size is 35.5nm；Fig. 2 (d) understands Jenner
Rice corpuscles has the strongest uv absorption at 531nm, corresponding with its grain size.
Embodiment 2:
(1) 150mL 2.2mM sodium citrate solution is joined reactor, under the conditions of magnetic agitation, be heated to boiling, add
Entering 1mL 24mM chlorauric acid solution, solution stops heating after becoming lightpink, and solution cools to 90 DEG C, adds 1mL
24mM chlorauric acid solution reaction 30min, again adds the reaction of 1mL 24mM chlorauric acid solution and obtains gold kind solution；
(2) above-mentioned 55mL gold kind solution and 2mL 60mM sodium citrate solution and 53mL pure water are mixed as next
The growth-promoting media of step reaction, growth-promoting media adds 1mL24mM chlorauric acid solution reaction 30min, again addition etc. after being heated to 90 DEG C
Amount chlorauric acid solution obtains the gold of next step reaction and plants solution；
(3) step (2) is repeated 2 times, and obtains solution of gold nanoparticles.
As Fig. 1 (e) and 3 (e) understand, step (3) gained gold nanometer particle grain size is 41.2nm；Fig. 2 (e) understands
Golden nanometer particle has the strongest uv absorption at 535nm, corresponding with its grain size.
Embodiment 3
(1) 150mL 2.2mM sodium citrate solution is joined reactor, under the conditions of magnetic agitation, be heated to boiling, add
Entering 1mL 24mM chlorauric acid solution, solution stops heating after becoming lightpink, and solution cools to 90 DEG C, adds 1mL
24mM chlorauric acid solution reaction 30min, again adds the reaction of 1mL 24mM chlorauric acid solution and obtains gold kind solution；
(2) above-mentioned 55mL gold kind solution and 2mL 60mM sodium citrate solution and 53mL pure water are mixed as next
The growth-promoting media of step reaction, growth-promoting media adds 1mL24mM chlorauric acid solution reaction 30min, again addition etc. after being heated to 90 DEG C
Amount chlorauric acid solution obtains the gold of next step reaction and plants solution；
(3) step (2) is repeated 3 times, and obtains solution of gold nanoparticles.
As Fig. 1 (f) and 3 (f) understand, step (3) gained gold nanometer particle grain size is 48.6nm；Fig. 2 (f) understands gold
Nanoparticle has the strongest uv absorption at 537nm, corresponding with its grain size.
Embodiment 4:
(1) 150mL 2.2mM sodium citrate solution is joined reactor, under the conditions of magnetic agitation, be heated to boiling, add
Entering 1mL 24mM chlorauric acid solution, solution stops heating after becoming lightpink, and solution cools to 90 DEG C, adds 1mL
24mM chlorauric acid solution reaction 30min, again adds the reaction of 1mL 24mM chlorauric acid solution and obtains gold kind solution；
(2) above-mentioned 55mL gold kind solution and 2mL 60mM sodium citrate solution and 53mL pure water are mixed as next
The growth-promoting media of step reaction, growth-promoting media adds 1mL24mM chlorauric acid solution reaction 30min, again addition etc. after being heated to 90 DEG C
Amount chlorauric acid solution obtains the gold of next step reaction and plants solution；
(3) step (2) is repeated 4 times, and obtains solution of gold nanoparticles.
As Fig. 1 (g) and 3 (g) understand, step (3) gained gold nanometer particle grain size is 54.4nm；Fig. 2 (g) understands
Golden nanometer particle has the strongest uv absorption at 543nm, corresponding with its grain size.
Embodiment 5:
(1) 150mL 2.2mM sodium citrate solution is joined reactor, under the conditions of magnetic agitation, be heated to boiling, add
Entering 1mL 24mM chlorauric acid solution, solution stops heating after becoming lightpink, and solution cools to 90 DEG C, adds 1mL
24mM chlorauric acid solution reaction 30min, again adds the reaction of 1mL 24mM chlorauric acid solution and obtains gold kind solution；
(2) above-mentioned 55mL gold kind solution and 2mL 60mM sodium citrate solution and 53mL pure water are mixed as next
The growth-promoting media of step reaction, growth-promoting media adds 1mL24mM chlorauric acid solution reaction 30min, again addition etc. after being heated to 90 DEG C
Amount chlorauric acid solution obtains the gold of next step reaction and plants solution；
(3) step (2) is repeated 5 times, and obtains solution of gold nanoparticles.
As Fig. 1 (h) and 3 (h) understand, step (3) gained gold nanometer particle grain size is 64.7nm；Fig. 2 (h) understands
Golden nanometer particle has the strongest uv absorption at 550nm, corresponding with its grain size.
Embodiment 6:
(1) 150mL 1.6mM sodium citrate solution is joined reactor, under the conditions of magnetic agitation, be heated to boiling, add
Entering 1mL 24mM chlorauric acid solution, solution stops heating after becoming lightpink, and solution cools to 93 DEG C, adds 1mL
24mM chlorauric acid solution reaction 25min, again adds the reaction of 1mL 24mM chlorauric acid solution and obtains gold kind solution；
(2) using above-mentioned 55mL gold kind solution and 1.45mL 60mM sodium citrate solution and the mixing of 53mL pure water as under
The growth-promoting media of single step reaction, growth-promoting media adds 1mL24mM chlorauric acid solution reaction 25min, again adds after being heated to 93 DEG C
Equivalent chlorauric acid solution obtains the gold of next step reaction and plants solution；
(3) step (2) is repeated 1 times, and obtains solution of gold nanoparticles.
As Fig. 1 (b) and 3 (b) understand, step (3) gained gold nanometer particle grain size is 21.0nm；Fig. 2 (b) understands
Golden nanometer particle has the strongest uv absorption at 522nm, corresponding with its grain size.
Embodiment 7:
(1) 150mL 2.4mM sodium citrate solution is joined reactor, under the conditions of magnetic agitation, be heated to boiling, add
Entering 1mL 24mM chlorauric acid solution, solution stops heating after becoming lightpink, and solution cools to 95 DEG C, adds 1mL
24mM chlorauric acid solution reaction 20min, again adds the reaction of 1mL 24mM chlorauric acid solution and obtains gold kind solution；
(2) using above-mentioned 55mL gold kind solution and 2.9mL 60mM sodium citrate solution and the mixing of 53mL pure water as under
The growth-promoting media of single step reaction, growth-promoting media adds 1mL24mM chlorauric acid solution reaction 20min, again adds after being heated to 95 DEG C
Equivalent chlorauric acid solution obtains the gold of next step reaction and plants solution；
(3) step (2) is repeated 1 times, and obtains solution of gold nanoparticles.
As Fig. 1 (c) and 3 (c) understand, gained gold nanometer particle grain size is 26.6nm；Fig. 2 (c) understands golden nanometer particle
The strongest uv absorption is had at 528nm, corresponding with its grain size.
Embodiment 8:
(1) 150mL 2.4mM sodium citrate solution is joined reactor, under the conditions of magnetic agitation, be heated to boiling, add
Entering 1mL 24mM chlorauric acid solution, solution stops heating after becoming lightpink, and solution cools to 95 DEG C, adds 1mL
24mM chlorauric acid solution reaction 20min, again adds the reaction of 1mL 24mM chlorauric acid solution and obtains gold kind solution；
(2) above-mentioned 55mL gold kind solution and 2mL 60mM sodium citrate solution and 53mL pure water are mixed as next
The growth-promoting media of step reaction, growth-promoting media adds 1mL24mM chlorauric acid solution reaction 20min, again addition etc. after being heated to 95 DEG C
Amount chlorauric acid solution obtains the gold of next step reaction and plants solution；
(3) step (2) is repeated 2 times, and obtains solution of gold nanoparticles.By gained golden nanometer particle conjugate enzyme molecule and antibody
Molecule, prepares the immune labeled probe of golden nanometer particle.
Different-grain diameter golden nanometer particle conjugate enzyme molecule and antibody molecule show as shown in Figure 4, experimental group 1ng/mL AFP and right
According to group 0ng/mLAFP fluorescence difference comparsion, when gold goal particle diameter is at 41.2nm, immune effect is optimal, and 41.2nm gold goal is described
Labeling effciency is the highest.
Claims (5)
1. a preparation method based on reduction of sodium citrate method regulation golden nanometer particle particle size；Its step is such as
Under:
(1) sodium citrate solution is joined reactor, under the conditions of magnetic agitation, be heated to boiling, add
Chlorauric acid solution, solution stops heating after becoming lightpink, and solution cools to 90～95 DEG C, adds equivalent chlorine
Auric acid solution reaction 20～30min, again adds the reaction of equivalent chlorauric acid solution and obtains gold kind solution；
(2) gold is planted solution and the sodium citrate solution mixing growth-promoting media as reaction, and growth-promoting media is heated to
90～95 DEG C of chlorauric acid solutions added with step (1) equivalent react 20～30min, again add equivalent chlorine gold
Acid solution obtains the gold of next step reaction and plants solution；
(3) step (2) repeats 1～5 time, prepares the golden nanometer particle of different-grain diameter.
2. the method for claim 1, is characterized in that described gold chloride is four hydration gold chlorides.
3. the method for claim 1, is characterized in that the mol ratio of described gold chloride and sodium citrate is 1:
10～20.
4. the method for claim 1, it is characterized in that gold plant solution: gold chloride: sodium citrate mol ratio
For 1:1:10～20.
5. the method for claim 1, is characterized in that regulating number of repetition, obtains the gold nano of different-grain diameter
Particle, number of repetition is the most, and gold nanometer particle grain size is the biggest.
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| CN108405875A (en) * | 2018-03-15 | 2018-08-17 | 山东豪迈化工技术有限公司 | It is used to prepare the method and device of gold nanoparticle |
| CN109604634A (en) * | 2019-01-31 | 2019-04-12 | 云南师范大学 | A kind of preparation method of different-grain diameter size nanogold particle |
| CN111085692A (en) * | 2019-12-27 | 2020-05-01 | 季华实验室 | Irregular alloy nano material synthesis method based on high-temperature water phase reaction |
| CN111940754A (en) * | 2019-05-17 | 2020-11-17 | 西北民族大学 | Nano gold particles with uniform particle size extracted based on sodium citrate reduction method and preparation method thereof |
| CN115575623A (en) * | 2022-12-06 | 2023-01-06 | 深圳市卓润生物科技有限公司 | Colloidal gold and preparation method and application thereof |
| CN116660517A (en) * | 2023-07-31 | 2023-08-29 | 山东康华生物医疗科技股份有限公司 | Colloidal gold preparation method for gastric helicobacter pylori IgG antibody detection test strip and test strip preparation method |
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Cited By (7)
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| CN111940754A (en) * | 2019-05-17 | 2020-11-17 | 西北民族大学 | Nano gold particles with uniform particle size extracted based on sodium citrate reduction method and preparation method thereof |
| CN111085692A (en) * | 2019-12-27 | 2020-05-01 | 季华实验室 | Irregular alloy nano material synthesis method based on high-temperature water phase reaction |
| CN115575623A (en) * | 2022-12-06 | 2023-01-06 | 深圳市卓润生物科技有限公司 | Colloidal gold and preparation method and application thereof |
| CN116660517A (en) * | 2023-07-31 | 2023-08-29 | 山东康华生物医疗科技股份有限公司 | Colloidal gold preparation method for gastric helicobacter pylori IgG antibody detection test strip and test strip preparation method |
| CN116660517B (en) * | 2023-07-31 | 2023-10-20 | 山东康华生物医疗科技股份有限公司 | Colloidal gold preparation method for gastric helicobacter pylori IgG antibody detection test strip and test strip preparation method |
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