CN105798322B - The preparation method and applications of silver nanoclusters - Google Patents
The preparation method and applications of silver nanoclusters Download PDFInfo
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- CN105798322B CN105798322B CN201610152251.0A CN201610152251A CN105798322B CN 105798322 B CN105798322 B CN 105798322B CN 201610152251 A CN201610152251 A CN 201610152251A CN 105798322 B CN105798322 B CN 105798322B
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Abstract
The present invention provides a kind of preparation method of silver nanoclusters, the silver nanoclusters being prepared have high-purity, high fluorescent；The silver nanoclusters that are prepared are more uniform, favorable reproducibility；Preparation method is simple and practicable, and quickly, material source is cheap extensively, and preparation process is pollution-free, available for large-scale industrial production；Silver nanoclusters prepared by the present invention, strengthen to pH sensitive, with the increase fluorescence intensity of pH, show that silver nanoclusters can be as the change of pH in fluorescent switch directive system.
Description
Technical field
The present invention relates to silver nanoclusters synthetic technology, more particularly to a kind of preparation method and applications of silver nanoclusters.
Background technology
It is in recent years, water-soluble for Material synthesis with reagents such as various template molecules and stabilizer such as protein, DNA, mercaptan
The fluorescence metal nano-cluster of property becomes the hot spot of research.During synthesis, it is necessary to using substantial amounts of template molecule and surely
Determine agent, and these molecules are possible to that substance reactions can be analyzed with very much, so as to cause very big puzzlement to follow-up detection.And
The inner filtering effect of synthetic raw material can also reduce the fluorescence of synthesized cluster.So water-soluble nano cluster is purified to for current work
The emphasis of work.As far as we know, at present mainly using 3 kinds of methods come purifying nano cluster：Dialysis, ultrafiltration and chromatographic separation technology.
And comparatively these methods purify more complicated, time-consuming, refining effect is unsatisfactory.
The change of pH value is to weigh the important logo of living organism physiological change, with the science such as modern medicine, bioengineering
Research field is closely bound up.The method for measuring the change of pH value is very much, such as acidometer, fluorescent material etc..Fluorescence analysis uses
The change instruction pH value of fluorescence parameter, simplicity, quick, sensitivity is good, and exploitation is used to detect biosystem H+The pH fluorescence of change
Probe has broad application prospects in terms of biomedical research.In this patent, we are prepared for receiving the fluorescence of pH sensitivities
Rice cluster, and purify silver nanoclusters using a kind of simple method-precipitation method.
The content of the invention
The object of the present invention is to provide a kind of high-purity, the preparation method and applications of the silver nanoclusters of high fluorescent.
In order to achieve the above object, on the one hand, the present invention provides a kind of preparation method of silver nanoclusters, its feature exists
In：It comprises the following steps：
Step 1, the aqueous solution of bovine serum albumin(BSA) or lipoic acid is prepared；
Step 2, solvable silver salt is added in the aqueous solution of step 1, be uniformly mixed, then add solvable BH4 -Salting liquid, stirring
Silver nanoclusters stoste is made；
Step 3, acid solution is added in the silver nanoclusters stoste obtained to step 2, is 3-6 to pH value, obtains silver nanoclusters and sink
Form sediment；
Step 4, by silver nanoclusters that step 3 obtains precipitation through centrifuging, separate, wash, then it is 9- to be dispersed in pH value again
In 12 alkaline solution.
On the other hand, the silver nanoclusters being prepared using first aspect present invention the method, applied to detection biology
System H+The pH fluorescence probes of change.
The beneficial effects of the invention are as follows：The preparation method of silver nanoclusters provided by the present invention, the silver nanoparticle being prepared
Cluster has high-purity, high fluorescent；The silver nanoclusters that are prepared are more uniform, favorable reproducibility；Preparation method is simple and practicable, soon
Speed, material source is cheap extensively, and preparation process is pollution-free, available for large-scale industrial production；Yin Na prepared by the present invention
Rice cluster, strengthens to pH sensitive, with the increase fluorescence intensity of pH, shows that silver nanoclusters can be used as fluorescent switch directive system
The change of middle pH.
Embodiment
On the one hand, the present invention provides a kind of preparation method of silver nanoclusters, it is characterised in that：It comprises the following steps：
Step 1, the aqueous solution of bovine serum albumin(BSA) or lipoic acid is prepared；
Step 2, solvable silver salt is added in the aqueous solution of step 1, be uniformly mixed, then add solvable BH4 -Salting liquid, stirring
Silver nanoclusters stoste is made；
Step 3, acid solution is added in the silver nanoclusters stoste obtained to step 2, is 3-6 to pH value, obtains silver nanoclusters and sink
Form sediment；
Step 4, by silver nanoclusters that step 3 obtains precipitation through centrifuging, separate, wash, then it is 9- to be dispersed in pH value again
In 12 alkaline solution.
Preferably, in the step 1, the aqueous solution of lipoic acid is prepared, further includes step 5, will added in the dispersion liquid of step 4
Enter solvable BH4 -Salting liquid, stirs and silver nanoclusters is made.
Preferably, the aqueous solution of lipoic acid is prepared in the step 1, the Ag of every 1 molfraction in step 2+Corresponding addition
The BH of 4-6 molfractions4 -；Alternatively, the aqueous solution of bovine serum albumin(BSA) is prepared in step 1, the Ag of every 1 molfraction+Correspondence adds
Add the BH of 0.1-0.4 molfractions4 -。
Preferably, the aqueous solution of lipoic acid is prepared in the step 1, the Ag of every 1 molfraction in step 2+Corresponding addition
The lipoic acid of 12-16 molfractions；Alternatively, the aqueous solution of bovine serum albumin(BSA) is prepared in step 1, the Ag of every 1 mass fraction+It is right
The bovine serum albumin(BSA) of 26-34 mass fractions should be added.
Preferably, acid solution is HNO in the step 33Or HAc, concentration 0.1-1M.
Preferably, centrifugal speed turns/min for 10000-12000 in the step 4.
Preferably, the deionized water with 5-10mL is washed in the step 4, is cleaned 3-5 times.
Preferably, the step 2 and solvable BH in step 54 -Salt is NaBH4, concentration 1mM-1M.
Preferably, mixing time is 3-24h in the step 5.
On the other hand, the silver nanoclusters being prepared using first aspect present invention the method, applied to detection biology
System H+The pH fluorescence probes of change.
The preparation method of silver nanoclusters of the present invention is described further below in conjunction with specific embodiment.
Embodiment 1
(1) bovine serum albumin(BSA) dissolving is formed to the solution of clear in aqueous；
(2) by AgNO3Add in solution, be uniformly mixed, form mixed material, wherein, the Ag of every 1 mass fraction+Correspondence adds
Add the bovine serum albumin(BSA) of 30 mass fractions；
(3) under stirring, sodium hydroxide solution and sodium borohydride is slowly added dropwise, continues silver is made to receive when stirring 6 is small
Rice cluster stoste, wherein, the Ag of every 1 molfraction+The BH of 0.2 molfraction of corresponding addition4 -；
(4) 0.1M HAc are added in stoste, adjust the pH to 3-6 of silver nanoclusters stoste, promote silver nanoclusters precipitation
Generation；
(5) silver nanoclusters are deposited under 10000-12000 turns of rotating speed and centrifuged, separated, then will precipitated with 5-10mL's
Deionized water is cleaned 3 times；
(6) precipitation after cleaning is dispersed in the solution that clear is formed in alkaline solution again, alkaline solution
Silver nanoclusters are made in pH value between 9-12.
To the silver nanoclusters that are prepared at ambient temperature, it is glimmering using sepectrophotofluorometer test equipment test product
Quantum yield is 2.2%.
To the silver nanoclusters that are prepared at ambient temperature, it is front and rear using the purification of sepectrophotofluorometer test product
Fluorescence ratio, is 95%.
Embodiment 2
(1) bovine serum albumin(BSA) dissolving is formed to the solution of clear in aqueous；
(2) by AgNO3Add in solution, be uniformly mixed, form mixed material, wherein, the Ag of every 1 mass fraction+Correspondence adds
Add the bovine serum albumin(BSA) of 26 mass fractions；
(3) under stirring, sodium hydroxide solution and sodium borohydride is slowly added dropwise, continues silver is made to receive when stirring 6 is small
Rice cluster stoste, wherein, the Ag of every 1 molfraction+The BH of 0.1 molfraction of corresponding addition4 -；
(4) 0.5M HAc are added in stoste, adjust the pH to 3-6 of silver nanoclusters stoste, promote silver nanoclusters precipitation
Generation；
(5) silver nanoclusters are deposited under 10000-12000 turns of rotating speed and centrifuged, separated, then will precipitated with 5-10mL's
Deionized water is cleaned 3 times；
(6) precipitation after cleaning is dispersed in the solution that clear is formed in alkaline solution again, alkaline solution
Silver nanoclusters are made in pH value between 9-12.
To the silver nanoclusters that are prepared at ambient temperature, it is glimmering using sepectrophotofluorometer test equipment test product
Quantum yield is 2.0%.
To the silver nanoclusters that are prepared at ambient temperature, it is front and rear using the purification of sepectrophotofluorometer test product
Fluorescence ratio, is 90%.
Embodiment 3
(1) bovine serum albumin(BSA) dissolving is formed to the solution of clear in aqueous；
(2) by AgNO3Add in solution, be uniformly mixed, form mixed material, wherein, the Ag of every 1 mass fraction+Correspondence adds
Add the bovine serum albumin(BSA) of 34 mass fractions；
(3) under stirring, sodium hydroxide solution and sodium borohydride is slowly added dropwise, continues silver is made to receive when stirring 6 is small
Rice cluster stoste, wherein, the Ag of every 1 molfraction+The BH of 0.4 molfraction of corresponding addition4 -；
(4) 1M HAc are added in stoste, adjust the pH to 3-6 of silver nanoclusters stoste, promote the life of silver nanoclusters precipitation
Into；
(5) silver nanoclusters are deposited under 10000-12000 turns of rotating speed and centrifuged, separated, then will precipitated with 5-10mL's
Deionized water is cleaned 3 times；
(6) precipitation after cleaning is dispersed in the solution that clear is formed in alkaline solution again, alkaline solution
Silver nanoclusters are made in pH value between 9-12.
To the silver nanoclusters that are prepared at ambient temperature, it is glimmering using sepectrophotofluorometer test equipment test product
Quantum yield is 2.1%.
To the silver nanoclusters that are prepared at ambient temperature, it is front and rear using the purification of sepectrophotofluorometer test product
Fluorescence ratio, is 93%.
Embodiment 4
(1) lipoic acid is dissolved in the solution that clear is formed in alkaline aqueous solution；
(2) by AgNO3Add in solution, be uniformly mixed, form mixed material, wherein, the Ag of every 1 molfraction+Correspondence adds
Add the lipoic acid of 14 molfractions；
(3) under stirring, sodium borohydride solution is slowly added dropwise into mixed material, continues that silver is made when stirring 6 is small
Nano-cluster stoste, wherein, the Ag of every 1 molfraction+The BH of 5 molfractions of corresponding addition4 -；
(4) 0.1M HNO are added in stoste3, the pH to 3-6 of silver nanoclusters stoste is adjusted, promotes silver nanoclusters precipitation
Generation；
(5) silver nanoclusters are deposited under 10000-12000 turns of rotating speed and centrifuged, separated, then will precipitated with 5-10mL's
Deionized water is cleaned 4 times；
(6) precipitation after cleaning is dispersed in the solution that clear is formed in alkaline solution again, alkaline solution
PH value is between 9-12.
To the silver nanoclusters that are prepared at ambient temperature, it is glimmering using sepectrophotofluorometer test equipment test product
Quantum yield is 2.5%.
To the silver nanoclusters that are prepared at ambient temperature, it is front and rear using the purification of sepectrophotofluorometer test product
Fluorescence ratio, is 108%.
Embodiment 5
(1) lipoic acid is dissolved in the solution that clear is formed in alkaline aqueous solution；
(2) by AgNO3Add in solution, be uniformly mixed, form mixed material, wherein, the Ag of every 1 molfraction+Correspondence adds
Add the lipoic acid of 12 molfractions；
(3) under stirring, sodium borohydride solution is slowly added dropwise into mixed material, continues that silver is made when stirring 6 is small
Nano-cluster stoste, wherein, the Ag of every 1 molfraction+The BH of 4 molfractions of corresponding addition4 -；
(4) 0.5M HNO are added in stoste3, the pH to 3-6 of silver nanoclusters stoste is adjusted, promotes silver nanoclusters precipitation
Generation；
(5) silver nanoclusters are deposited under 10000-12000 turns of rotating speed and centrifuged, separated, then will precipitated with 5-10mL's
Deionized water is cleaned 4 times；
(6) precipitation after cleaning is dispersed in the solution that clear is formed in alkaline solution again, alkaline solution
PH value is between 9-12.
To the silver nanoclusters that are prepared at ambient temperature, it is glimmering using sepectrophotofluorometer test equipment test product
Quantum yield is 2.3%.
To the silver nanoclusters that are prepared at ambient temperature, it is front and rear using the purification of sepectrophotofluorometer test product
Fluorescence ratio, is 105%.
Embodiment 6
(1) lipoic acid is dissolved in the solution that clear is formed in alkaline aqueous solution；
(2) by AgNO3Add in solution, be uniformly mixed, form mixed material, wherein, the Ag of every 1 molfraction+Correspondence adds
Add the lipoic acid of 16 molfractions；
(3) under stirring, sodium borohydride solution is slowly added dropwise into mixed material, continues that silver is made when stirring 6 is small
Nano-cluster stoste, wherein, the Ag of every 1 molfraction+The BH of 6 molfractions of corresponding addition4 -；
(4) 1M HNO are added in stoste3, the pH to 3-6 of silver nanoclusters stoste is adjusted, promotes the life of silver nanoclusters precipitation
Into；
(5) silver nanoclusters are deposited under 10000-12000 turns of rotating speed and centrifuged, separated, then will precipitated with 5-10mL's
Deionized water is cleaned 4 times；
(6) precipitation after cleaning is dispersed in the solution that clear is formed in alkaline solution again, alkaline solution
PH value is between 9-12.
To the silver nanoclusters that are prepared at ambient temperature, it is glimmering using sepectrophotofluorometer test equipment test product
Quantum yield is 2.4%.
To the silver nanoclusters that are prepared at ambient temperature, it is front and rear using the purification of sepectrophotofluorometer test product
Fluorescence ratio, is 106%.
Embodiment 7
(1) lipoic acid is dissolved in the solution that clear is formed in alkaline aqueous solution；
(2) by AgNO3Add in solution, be uniformly mixed, form mixed material, wherein, the Ag of every 1 molfraction+Correspondence adds
Add the lipoic acid of 16 molfractions；
(3) under stirring, sodium borohydride solution is slowly added dropwise into mixed material, continues that silver is made when stirring 6 is small
Nano-cluster stoste, wherein, the Ag of every 1 molfraction+The BH of 6 molfractions of corresponding addition4 -；
(4) 0.1M HNO are added in stoste3, the pH to 3-6 of silver nanoclusters stoste is adjusted, promotes silver nanoclusters precipitation
Generation；
(5) silver nanoclusters are deposited under 10000-12000 turns of rotating speed and centrifuged, separated, then will precipitated with 5-10mL's
Deionized water is cleaned 5 times；
(6) precipitation after cleaning is dispersed in the solution that clear is formed in alkaline solution again, alkaline solution
PH value is between 9-12；
(7) toward addition 1mM-1M NaBH in above-mentioned solution4, stir 3-24h and silver nanoclusters be made.
To the silver nanoclusters that are prepared at ambient temperature, it is glimmering using sepectrophotofluorometer test equipment test product
Quantum yield is 2.1%.
To the silver nanoclusters that are prepared at ambient temperature, it is front and rear using the purification of sepectrophotofluorometer test product
Fluorescence ratio, is 110%.
The foregoing is merely the present invention better embodiment, not to limit invention, it is all the present invention spirit and
Within principle, any modification, equivalent substitution, improvement and etc. done should all be included in the protection scope of the present invention.
Claims (9)
- A kind of 1. preparation method of silver nanoclusters, it is characterised in that：It comprises the following steps：Step 1, the aqueous solution of lipoic acid is prepared；Step 2, solvable silver salt is added in the aqueous solution of step 1, be uniformly mixed, then add solvable BH4 -Salting liquid, stirring system Obtain silver nanoclusters stoste；Step 3, acid solution is added in the silver nanoclusters stoste obtained to step 2, is 3-6 to pH values, obtains silver nanoclusters and sink Form sediment；Step 4, by silver nanoclusters that step 3 obtains precipitation through centrifuging, separate, wash, then it is 9-12 to be dispersed in pH values again Alkaline solution in；Step 5 is further included, solvable BH will be added in the dispersion liquid of step 44 -Salting liquid, stirs and silver nanoclusters is made.
- 2. the preparation method of the silver nanoclusters as described in claim 1, it is characterised in that：Every 1 molar part in the step 2 Several Ag+The BH of corresponding addition 4-6 molfractions4 -。
- 3. the preparation method of the silver nanoclusters as described in claim 1, it is characterised in that：Every 1 molar part in the step 2 Several Ag+The lipoic acid of corresponding addition 12-16 molfractions.
- 4. the preparation method of the silver nanoclusters as described in claim 1, it is characterised in that：Acid solution is HNO in the step 33Or HAc, concentration 0.1-1M.
- 5. the preparation method of the silver nanoclusters as described in claim 1, it is characterised in that：Centrifugal speed is in the step 4 10000-12000 turns/min.
- 6. the preparation method of the silver nanoclusters as described in claim 1, it is characterised in that：Washing 5-10 in the step 4 The deionized water of mL, is cleaned 3-5 times.
- 7. the preparation method of the silver nanoclusters as described in claim 1, it is characterised in that：The step 2 with it is solvable in step 5 BH4 -Salt is NaBH4, concentration 1mM-1M.
- 8. the preparation method of the silver nanoclusters as described in claim 1, it is characterised in that：Mixing time is in the step 5 3-24h。
- 9. the silver nanoclusters being prepared using claim 1 the method, applied to detection biosystem H+The pH of change is glimmering Light probe.
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| CN106984826B (en) * | 2016-11-17 | 2019-05-17 | 湖南科技大学 | A kind of method for the silver nanoclusters that there is hyperfluorescence to emit for the preparation of pH regulation |
| CN106891016A (en) * | 2017-01-10 | 2017-06-27 | 青岛科技大学 | A kind of preparation of fluorescence silver nanoclusters and its method for manifesting latent fingerprint |
| CN107018991B (en) * | 2017-04-26 | 2020-05-08 | 江南大学 | Antibacterial film modified by silver-lysozyme nanoclusters |
| CN107011527A (en) * | 2017-05-04 | 2017-08-04 | 长春工业大学 | A kind of preparation method and application of the silver nanoclusters of temperature-responsive/polyalcohol hydrogel composite |
| CN109001281B (en) * | 2018-09-03 | 2020-06-30 | 湖北大学 | Molecular imprinting photoelectrochemical sensor based on organic-inorganic quantum dot P-N heterostructure and preparation method and application thereof |
| CN111208099B (en) * | 2020-01-08 | 2021-07-23 | 同济大学 | Silver nano-cluster fluorescent probe, preparation method thereof and application thereof in detection of active oxygen species |
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| US20110207232A1 (en) * | 2009-05-13 | 2011-08-25 | University Of Utah Research Foundation | Water soluble ph responsive fluorescent nanoparticles |
| CN102516997A (en) * | 2011-12-09 | 2012-06-27 | 吉林大学 | Silver nano-cluster fluorescent probe for detecting trace mercury ion in water with high sensitivity and high selectivity |
| CN105092551B (en) * | 2015-08-14 | 2017-10-10 | 上海交通大学 | Nitric oxide production method is detected based on the fluorescence noble-metal nanoclusters that bovine serum albumin is modified |
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| CN1354748A (en) * | 1999-08-14 | 2002-06-19 | Skw特罗斯特贝格股份公司 | Method for production of solvent-free alpha-liponic acid |
| CN101137642A (en) * | 2005-03-22 | 2008-03-05 | 国际化学实验室有限公司 | Process for purifying thioctic acid in water |
| CN102127428A (en) * | 2010-12-14 | 2011-07-20 | 中国科学院苏州纳米技术与纳米仿生研究所 | Fluorescent silver cluster, and preparation method and application thereof |
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