CN1332775C - Gold nanometer particle grain size control method based on glutathione - Google Patents
Gold nanometer particle grain size control method based on glutathione Download PDFInfo
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- CN1332775C CN1332775C CNB2005100275715A CN200510027571A CN1332775C CN 1332775 C CN1332775 C CN 1332775C CN B2005100275715 A CNB2005100275715 A CN B2005100275715A CN 200510027571 A CN200510027571 A CN 200510027571A CN 1332775 C CN1332775 C CN 1332775C
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Abstract
The present invention relates to a control method for the particle sizes of gold nano-particles on the basis of glutathione, which belongs to the field of nanotechnology. The method comprises the following concrete steps: a. a sodium citrate solution and a glutathione solution are mixed; b. a solution obtained in step a and a chloroauric acid solution are respectively heated and then mixed; c. after a solution obtained in step b discolors, the solution is heated until the solution boils so that the solution thoroughly reacts, and then the solution is cooled to obtain the sol solution of the gold nano-particles. The method provided by the present invention has the characteristics of convenience, high efficiency, convenient and adjustable particle sizes, good bio-compatibility, etc.; the obtained nano-particles have good dispersivity and uniform particle sizes, and the particle sizes can be controlled within the range of 8 to 40 nm. The gold nano-particles prepared by the method can be applied to the technical field of DNA detection, biology, medicine, etc., and is convenient for popularization and application.
Description
Technical field
What the present invention relates to is a kind of method of field of nanometer technology, particularly a kind of based on the control method of glutathione to gold nanometer particle grain size.
Background technology
In recent years, along with the rise of nanosecond science and technology, the gold grain of nanoscale shows potential using value in a lot of fields with its unique optics, electrical properties, has caused the research interest that people are dense.The particle diameter of nano Au particle and size affect its potential application at aspects such as chemistry, biology, electronic devices strongly.When particle during less than 100nm, its optics, electricity and magnetism characteristic rely on particle size strongly, therefore by the particle diameter of control golden nanometer particle can be indirect obtain desired physical property.The control method of gold nanometer particle grain size has multiple, as liquid-phase extraction method, crystal seed method, electrochemical process etc.But the common operating procedure complexity of these methods, condition is wayward, the particle diameter wider distribution.
Find through literature search prior art, people such as calendar year 2001 Gen T are at " Japanese applicating physical magazine " (Jpn.J.Appl.Phys., 2001,40 (1) 346-349) delivered the article of " Well-size-controlledColloidal Gold Nanoparticles Dispersed in Organic Solvents " (being dispersed in the golden nanometer particle of controllable size in the organic solvent) on, this article adopts in the process of preparation aurosol and adds tannic acid, obtain the method for the gold nano grain of different-grain diameter by changing the volume that adds tannic acid, and will dissolve in the multiple organic solvent behind the aurosol solution centrifugal.This method is simple to operate, and the size that can control golden nanometer particle is between the 5-18 nanometer.But the prepared golden nanometer particle bio-compatibility of this method is relatively low, and the controlled dimensions scope of golden nanometer particle is narrower.
Summary of the invention
The objective of the invention is at deficiency of the prior art, provide a kind of based on the control method of glutathione to gold nanometer particle grain size, make it pass through the adding of glutathione, directly obtain the glutathione gold nano-particles modified, method is simple, practical, good, the uniform particle diameter of gained nanoparticulate dispersed, particle diameter can be controlled in the 8-40nm scope.
The present invention is achieved by the following technical solutions, and concrete steps of the present invention are as follows:
A. citric acid three sodium solution and glutathione solution are mixed.
B. solution and the chlorauric acid solution with gained among the step a heats respectively, mixes then.
C. after treating the solution changes color of gained among the step b, solution is heated to boiling, reacts fully, then the solution cooling is obtained the golden nanometer particle sol solution.
In step a, glutathione used in the present invention is oxidized form of glutathione or reduced glutathione.The mass ratio of glutathione and gold chloride is controlled to be (0.01-2): 1, because the glutathione of minute quantity is less to the influence of gold nanometer particle grain size, and after glutathione surpasses certain proportion, the gold chloride reduction rate slows down, grain diameter influence's effect to gold particle weakens, so the optimum quality ratio of glutathione and gold chloride is (0.1-0.8): 1.
In step b, in order to make the gold chloride Restore All, need to add excessive trisodium citrate, therefore the mass ratio of controlling trisodium citrate and gold chloride is greater than 1: 1, preferred proportion (3-4): 1, heating and temperature control is between 50-75 ℃.
In step c, the ebuillition of heated time is 5~20 minutes, is evenly distributed in order to make particle diameter, and sufficient reacting reduces the reunion of golden nanometer particle simultaneously, and Best Times is 8-15 minute, and the particle diameter of gained golden nanometer particle is 8-40nm.
The present invention utilizes trisodium citrate reduction gold chloride to obtain gold particle, in preparation process, directly add glutathione simultaneously, utilize the coating effect of glutathione, the particle diameter of control golden nanometer particle, and form modification and the dispersion of glutathione to the golden nanometer particle surface.
The present invention's employing adds glutathione and prepares the controlled golden nanometer particle of particle diameter in the golden nanometer particle preparation process.Can realize the modification of glutathione easily owing in course of reaction, directly add glutathione to golden nanometer particle.Method provided by the present invention has simple, efficient height, characteristics such as particle size is convenient adjustable, and bio-compatibility is good.The golden nanometer particle that makes thus can be applicable to DNA detection, biology and medicine and other fields, is easy to be extended and applied.
The specific embodiment
Provide following examples in conjunction with content of the present invention:
Embodiment 1
1ml 1% (w/v) chlorauric acid solution is joined (a solution) in the 79ml ultra-pure water.Get citric acid three sodium solution and oxidized form of glutathione solution, add ultra-pure water to 20ml (b solution), the mass ratio of control glutathione and gold chloride is 0.1: 1, the mass ratio of trisodium citrate and gold chloride 3: 1.A, b solution all are heated to 60 ℃, b solution are poured in a solution fast mixed then.After the mixed solution variable color, solution is heated to boiling.Keep boiling 15 minutes, react fully, then the solution cooling is obtained 38nm golden nanometer particle sol solution, volume distributed median 91.6%.
Embodiment 2
The 1ml chlorauric acid solution is joined (a solution) in the 79ml ultra-pure water.Get citric acid three sodium solution and reduced glutathione solution, add ultra-pure water to 20ml (b solution), the mass ratio of control glutathione and gold chloride is 0.5: 1, the mass ratio of trisodium citrate and gold chloride 4: 1.A, b solution all are heated to 75 ℃, b solution are poured in a solution fast mixed then.After the mixed solution variable color, solution is heated to boiling.Keep boiling 5 minutes, react fully, then the solution cooling is obtained 8 nm of gold nanoparticle sol solution, volume distributed median 97.6%.
Embodiment 3
The 1ml chlorauric acid solution is joined (a solution) in the 79ml ultra-pure water.Get citric acid three sodium solution and oxidized form of glutathione solution, add ultra-pure water to 20ml (b solution), the mass ratio of control glutathione and gold chloride is 0.8: 1, the mass ratio of trisodium citrate and gold chloride 4: 1.A, b solution all are heated to 50 ℃, b solution are poured in a solution fast mixed then.After the mixed solution variable color, solution is heated to boiling.Keep about 8 minutes of boiling, react fully, then the solution cooling is obtained 15 nm of gold nanoparticle sol solution, volume distributed median 99.2%.
Embodiment 4
The 1ml chlorauric acid solution is joined (a solution) in the 79ml ultra-pure water.Get citric acid three sodium solution and oxidized form of glutathione solution, add ultra-pure water to 20ml (b solution), the mass ratio of control glutathione and gold chloride is 2: 1, the mass ratio of trisodium citrate and gold chloride 4: 1.A, b solution all are heated to 60 ℃, b solution are poured in a solution fast mixed then.After the mixed solution variable color, solution is heated to boiling.Keep boiling 20 minutes, react fully, then the solution cooling is obtained 13 nm of gold nanoparticle sol solution, volume distributed median 92.8%.
Embodiment 5
The 1ml chlorauric acid solution is joined (a solution) in the 79ml ultra-pure water.Get citric acid three sodium solution and reduced glutathione solution, add ultra-pure water to 20ml (b solution), the mass ratio of control glutathione and gold chloride is 0.01: 1, the mass ratio of trisodium citrate and gold chloride 4: 1.A, b solution all are heated to 55 ℃, b solution are poured in a solution fast mixed then.After the mixed solution variable color, solution is heated to boiling.Keep about 10 minutes of boiling, react fully, then the solution cooling is obtained 25 nm of gold nanoparticle sol solution, volume distributed median 97.1%.
Claims (8)
1, a kind of based on the control method of glutathione to gold nanometer particle grain size, it is characterized in that concrete steps are as follows:
A. citric acid three sodium solution and glutathione solution are mixed;
B. solution and the chlorauric acid solution with gained among the step a heats respectively, mixes then;
C. after treating the solution changes color of gained among the step b, solution is heated to boiling, reacts fully, then the solution cooling is obtained the golden nanometer particle sol solution.
2, according to claim 1ly it is characterized in that based on the control method of glutathione in step a, employed glutathione is oxidized form of glutathione or reduced glutathione to gold nanometer particle grain size.
3, according to claim 1ly it is characterized in that based on the control method of glutathione the mass ratio of glutathione and gold chloride is 0.01-2: 1 to gold nanometer particle grain size.
4, according to claim 3ly it is characterized in that based on the control method of glutathione the mass ratio of described glutathione and gold chloride is 0.1-0.8: 1 to gold nanometer particle grain size.
5, according to claim 1ly it is characterized in that based on the control method of glutathione in step b, the mass ratio of trisodium citrate and gold chloride was greater than 1: 1 to gold nanometer particle grain size.
6, according to claim 5ly it is characterized in that based on the control method of glutathione the mass ratio of described trisodium citrate and gold chloride is 3-4: 1 to gold nanometer particle grain size.
7, according to claim 1ly it is characterized in that based on the control method of glutathione to gold nanometer particle grain size in step c, the ebuillition of heated time is 5~20 minutes, the particle diameter of gained golden nanometer particle is 8-40nm.
8, according to claim 7ly it is characterized in that based on the control method of glutathione the described ebuillition of heated time is 8-15 minute to gold nanometer particle grain size.
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CN100531972C (en) * | 2008-02-20 | 2009-08-26 | 厦门大学 | Method of manufacturing light sensitive metal nanometer material |
CN101875132B (en) * | 2010-05-31 | 2012-01-11 | 武汉大学 | Method for bionically preparing water-soluble gold nanoclusters |
CN101987364B (en) * | 2010-09-14 | 2012-06-20 | 江南大学 | Method for preparing functional gold nanoparticles with high stability |
CN103128309B (en) * | 2013-03-14 | 2015-03-11 | 山东大学 | Synthetic method of water-solubility biocompatibility monodisperse spherical gold nanometer crystals |
CN103143722B (en) * | 2013-03-21 | 2014-12-17 | 江西农业大学 | Method for preparing multipod-like gold nanoparticles by chemical method |
CN103212056B (en) * | 2013-05-07 | 2015-07-08 | 东南大学 | Preparation based on gold, silver, gold-silver mixture and glutathione/chitosan, and application of preparation |
CN106984828B (en) * | 2017-03-28 | 2019-03-12 | 东南大学 | A kind of fluorescence gold nanoclusters fast synthesis method based on chemical etching |
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JPH07204493A (en) * | 1994-01-18 | 1995-08-08 | Kanebo Ltd | Gold colloid solution |
WO2004012855A2 (en) * | 2002-08-01 | 2004-02-12 | E.I. Du Pont De Nemours And Company | Ethylene glycol monolayer protected nanoparticles |
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Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
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JPH07204493A (en) * | 1994-01-18 | 1995-08-08 | Kanebo Ltd | Gold colloid solution |
WO2004012855A2 (en) * | 2002-08-01 | 2004-02-12 | E.I. Du Pont De Nemours And Company | Ethylene glycol monolayer protected nanoparticles |
Non-Patent Citations (3)
Title |
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Controlled Nucleation for the Regulation of the Particle SizeinMonodisperse Gold Suspensions Frens G,Nature Physical Science,Vol.241 No.105 1973 * |
Controlled Nucleation for the Regulation of the Particle SizeinMonodisperse Gold Suspensions Frens G,Nature Physical Science,Vol.241 No.105 1973;Well-size-controlled Colloidal Gold NanoparticlesDispersedinOrganic Solvents Gen Tsutsui et al,Japanese Journal of Applied Physics,Vol.40 No.1 2001 * |
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