CN109014240A - The preparation method of the gold nano cluster of energy efficient transmission short wavelength-NIR light - Google Patents
The preparation method of the gold nano cluster of energy efficient transmission short wavelength-NIR light Download PDFInfo
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Abstract
The preparation method of the gold nano cluster of energy efficient transmission short wavelength-NIR light of the present invention; using beta-cyclodextrin as reducing agent and protective agent; three hydration tetra chlorauric acids are reacted in alkaline solution to the gold nano cluster for generating the sulfenyl beta-cyclodextrin modified of energy efficient transmission short wavelength-NIR light with beta-cyclodextrin; its specific steps has: (1) raw material weighing, reaction solution configuration；(2) heat；(3) filter；(4) refrigerate；Obtain the gold nano cluster, molecular structural formula are as follows:Wherein,It is near-infrared luminous that gold nano cluster prepared by the present invention can generate 795nm under 450nm light source activation, the transmitting section can further decrease the noise of biological context in modern imaging techniques, it is more accurately imaged, has huge application prospect in bio-imaging field.
Description
Technical field
The invention belongs to technical field of organic luminescence materials, and in particular to one kind is capable of efficient transmission short wavelength-NIR light
The preparation method of gold nano cluster.
Background technique
Early in late 1960s, fluorescence gold nano cluster (Au nanoclusters, AuNCs) has been ground by science
The person's of studying carefully discovery, however due to dispersion performance difference etc. in fluorescence volume production lower (generally less than 0.1%), aqueous solution, always not
As scientific research hot spot.In the past 10 years, as the field, the preparation method of fluorescence gold nano cluster is added in more and more scientists
It is strong with its low toxicity, easily preparation, fluorescence volume production height, optical stability as a kind of novel metal nano material by gradual perfection
And the concern that the advantages that excellent biocompatibility is concentrated.Gold nano cluster size is less than 3nm, the diameter and electronics
Fermi's wavelength it is close, so that it is had the characteristic of class molecule.With the gold nano grain (Au known to researcher
Nanoparticles, AuNPs) it is different, the gold nano cluster of super-small will not show the surface ion in visible light region
RESONANCE ABSORPTION (SPR), but possess the fluorescent emission of visible region and near infrared region.Based on the above good characteristic, gold nano group
Cluster is widely used in the fields such as photoelectronics, bio-imaging, medicament transport and release, photodynamic therapy.It is worth mentioning
It is to possess the gold nano cluster of near infrared emission in transmitting light section, it is wide due to possessing stronger tissue transmission capacity
The general in-vivo imaging that is applied to detects.And short wavelength-NIR (SWIR) within the scope of 780-1100nm it is visible with tradition-infrared imaging
It compares, biological tissue's ambient noise can be further decreased, simultaneously as beta-cyclodextrin (β-CD) is nontoxic, water-soluble, environment is friendly
It good, bio-compatible and does not need covalent combination reaction and can form the advantages such as host-guest interaction, make beta-cyclodextrin functionalization
Nano material has obtained extensive attention.Currently, cyclodextrin (CD) modification gold nano cluster usually requires more complex surface and changes
Property or need the booster action of reducing agent, and the gold nano cluster (AuNCs@CD) for using one-step synthesis method cyclodextrin modified
Article is also few.In addition, cyclodextrin modified gold nano cluster generates green fluorescence mostly.Therefore, it is synthesized using beta-cyclodextrin
The gold nano cluster of transmitting short wavelength-NIR light seems and is highly desirable.
Summary of the invention
It is an object of the invention to overcome the deficiencies in the prior art and on the basis of existing research achievement, a kind of energy is provided
The preparation method of the gold nano cluster of efficient transmission short wavelength-NIR light, the near-infrared luminous sulfenyl beta-cyclodextrin modified
Gold nano cluster (AuNCs@β-SH-CD) be with mercapto-modified beta-cyclodextrin (β-SH-CD) be reducing agent and protective agent, adopt
With one-step synthesis method, the preparation method is easy, and raw material is simple and easy to get, not only overcomes existing cyclodextrin (CD) modification gold nano
The disadvantage of cluster (AuNCs CD) process complexity, moreover it is possible to solve the problems, such as that cyclodextrin modified AuNCs generates green fluorescence mostly；
The good luminescence property of the gold nano cluster of preparation can promote the progress of luminescent material.
To achieve the above object, this invention takes following technical schemes.
The preparation method of the gold nano cluster of energy efficient transmission short wavelength-NIR light, which is characterized in that be with beta-cyclodextrin
Reducing agent and protective agent are hydrated tetra chlorauric acid (HAuCl for three4·3H2O it) is reacted in alkaline solution with beta-cyclodextrin and generates energy
The gold nano cluster (AuNCs@β-SH-CD) of the sulfenyl beta-cyclodextrin modified of efficient transmission short wavelength-NIR light, specific steps
It is as follows:
(1) raw material weighing, reaction solution configuration
Under room temperature, the mercapto-modified β-ring of macrocyclic host-is added in the alkaline aqueous solution of three hydration tetra chlorauric acids
Dextrin alkaline reaction liquid, wherein the alkaline aqueous solution and mercapto-modified beta-cyclodextrin alkaline reaction liquid of three hydration tetra chlorauric acids
Proportion be 2~1, stirred 1~5 minute under 200~400 revs/min of revolving speed using magnetic stirring apparatus, make mixed solution face
Color is changed into colourless by yellow；
(2) it heats
The mixed solution that step (1) obtains is transferred in 60~90 DEG C of oil bath pan, in 200~400 revs/min turn
Speed lower stirring 6~72 hours；Mixed solution color gradually becomes pink colour from colourless, when becoming light brown again later, closes stirring,
Stop heating reaction；
(3) it filters
Mixed solution after step (2) heating reaction is restored to 25 DEG C of room temperatures, it is molten using the needle tubing sucking gained of 10mL
Liquid installs the water phase filtering head of 200 mesh on injector head, squeezes needle tubing by hand, solution is leached into the vial of 10ml
In, obtain light brown aqueous solution；
(4) it refrigerates
The light brown aqueous solution being placed in vial that step (3) obtains is saved in 0~5 DEG C of condition, obtains mesh
Mark product --- gold nano cluster (the AuNCs@β-SH- of the sulfenyl beta-cyclodextrin modified of energy efficient transmission short wavelength-NIR light
CD)；
The molecular structural formula of the gold nano cluster of the sulfenyl beta-cyclodextrin modified of energy efficient transmission short wavelength-NIR light are as follows:
Wherein,
Further, the macrocyclic host in step (1) must be with mercapto-modified beta-cyclodextrin (β-SH-CD), and reaction
Solution is alkalinity.
The positive effect of the present invention are as follows:
(1) due to using using mercapto-modified beta-cyclodextrin as reducing agent and protective agent, one-step synthesis method Jenner can be used
Rice cluster overcomes cyclodextrin modified gold nano cluster to usually require more complex surface modification or reducing agent is needed to play auxiliary work
Deficiency.
(2) with the growth in reaction time, the illumination effect of AuNCs@β-SH-CD is better, and intensity is higher, it is important that
Only alkaline preparation condition can produce the AuNCs@β-SH-CD of short wavelength-NIR transmitting.
(3) it is near-infrared luminous to generate 795nm under 450nm light source activation for gold nano cluster prepared by the present invention --- place
In the transmitting section of 780~1100nm of short wavelength-NIR, the transmitting section in modern imaging techniques relative to it is traditional it is visible-
Near infrared imaging can further decrease the interference of biological context noise, be more accurately imaged, and have in bio-imaging field
Huge application prospect.
Detailed description of the invention
Fig. 1 is the flow diagram of the preparation method of the gold nano cluster of present invention energy efficient transmission short wavelength-NIR light.
Fig. 2 is the transient optical state service life spectrogram of AuNCs β-SH-CD.
Fig. 3 is the spectrogram for the AuNCs@β-SH-CD that different preparation times obtain.
Fig. 4 is the variation trends for the AuNCs@β-SH-CD that different preparation times obtain.
The UV-visible absorption spectrum and correspond under daylight that Fig. 5 is the AuNCs@β-SH-CD that different preparation times obtain
Solution figure.
Fig. 6 is the normalized wavelength graph of AuNCs@β-SH-CD.
Fig. 7 is the transmitting spectrogram through AuNCs β-SH-CD that is acid, neutral, obtaining after alkaline condition preparation in 795nm.
Specific embodiment
The preparation method of the gold nano cluster of present invention energy efficient transmission short wavelength-NIR light is introduced below in conjunction with attached drawing
Specific embodiment provides 3 embodiments.It should be noted that implementation of the invention embodiment not limited to the following.
Embodiment 1
A kind of preparation method of the gold nano cluster of energy efficient transmission short wavelength-NIR light, specific step is as follows (referring to
Fig. 1):
(1) raw material weighing, reaction solution configuration
Weigh 200.00mg (2.38mmol) sodium bicarbonate (NaHCO3) be dissolved in the water of 25.0mL, preparation concentration is about
The alkaline reaction liquid of 0.1M；It takes the beta-cyclodextrin of 69.04mg (0.06mmol) to be dissolved in 0.6mL alkaline reaction liquid, prepares concentration
For by the beta-cyclodextrin alkaline reaction liquid of 0.1M；By the NaHCO of the three hydration tetra chlorauric acids of 2.0mL (5.00mM)3Aqueous solution adds
Enter in the round-bottomed flask of 25mL, the beta-cyclodextrin alkaline reaction liquid and 1.04mL of 1.8mL are added under 25 DEG C of room temperature environments
NaHCO3Aqueous solution is stirred 1 minute under 300 revs/min of revolving speeds using magnetic stirring apparatus, turns mixed solution color by yellow
It becomes colorless.
(2) it heats
The colourless mixed solution that step (1) obtains is transferred in 70 DEG C of oil bath pan, is stirred under 300 revs/min of revolving speeds
It mixes, heat reaction 72 hours；Mixed solution color gradually becomes pink colour from colourless, when becoming light brown again later, closes stirring,
Stop heating reaction.
(3) it filters
Mixed solution after step (2) heating reaction is restored to 25 DEG C of room temperatures, it (can with the filtering of 200 mesh water phase filtering heads
Acquired solution is sucked using the needle tubing of 10mL, the water phase filtering head of 200 mesh is installed on injector head, needle tubing is squeezed by hand,
Solution is leached into the vial of 10ml), obtain light brown aqueous solution.
(4) it refrigerates
(being placed in vial) light brown aqueous solution that step (3) obtains is stored in 0 DEG C of condition, target production is obtained
Object --- the gold nano cluster (AuNCs@β-SH-CD) of the sulfenyl beta-cyclodextrin modified of energy efficient transmission short wavelength-NIR light.
It is described can the molecular structural formula of AuNCs@β-SH-CD of efficient transmission short wavelength-NIR light be,
Wherein,
The wavelength of the normalization standard of the AuNCs@β-SH-CD of energy efficient transmission short wavelength-NIR light prepared by embodiment 1
Scheme (referring to Fig. 6).The transient optical state service life spectrogram (referring to fig. 2) of the AuNCs β-SH-CD.
Embodiment 2
A kind of preparation method of the gold nano cluster of energy efficient transmission short wavelength-NIR light, the specific steps of which are as follows:
(1) raw material weighing, reaction solution configuration
Raw material weighing, reaction solution are configured with embodiment 1；1 is stirred under 400 revs/min of revolving speed using magnetic stirring apparatus
Minute, it is changed into mixed solution color by yellow colourless.
(2) it heats
The colourless mixed solution that step (1) obtains is transferred in 60 DEG C of oil bath pan, under 400 revs/min of revolving speed
Stirring, heating reaction, time are respectively set as 6 hours, 12 hours or 24 hours；Mixed solution color gradually becomes powder from colourless
Color when becoming light brown again later, closes stirring, stops heating reaction.
(3) (with embodiment 1) is filtered.
(4) it refrigerates
(being placed in vial) light brown aqueous solution that step (3) obtains is stored in 0 DEG C of condition, target production is obtained
Object --- the AuNCs@β-SH-CD of energy efficient transmission short wavelength-NIR light.
Products therefrom is subjected to luminescent properties test respectively, obtains result are as follows: the AuNCs@β-that different preparation times obtain
SH-CD spectrum (referring to Fig. 3)；The variation trends (referring to fig. 4) for the AuNCs@β-SH-CD that different preparation times obtain；No
Solution under the UV-visible absorption spectrum of the AuNCs@β-SH-CD obtained with preparation time and corresponding daylight is (referring to figure
5)。
With the available more AuNCs@β-SH-CD with short wavelength-NIR transmitting of the growth of time.Work as reaction
After duration extends to 72h by 6h, about 10 times of luminous intensity generation is substantially improved, while absorption intensity also obviously rises.
The normalized wave of AuNCs@β-SH-CD for the energy efficient transmission short wavelength-NIR light that the peak optimization reaction time is 72 hours
Long figure (referring to Fig. 6).The transient optical state service life spectrogram (referring to fig. 2) of the AuNCs β-SH-CD.
Embodiment 3
A kind of preparation method of the gold nano cluster of energy efficient transmission short wavelength-NIR light, the specific steps of which are as follows:
(1) raw material weighing, reaction solution configuration
1. measuring 35% concentrated hydrochloric acid of 7.0 μ L with liquid-transfering gun, it is dissolved in the beaker for having 25mL water, is then transferred to
In 100mL volumetric flask, water supplement to volumetric flask 100mL graduation mark, the acid reaction liquid (PH < 7) that preparation concentration is about 0.8mM.
2. the ultrapure water of 25mL is measured, as neutral reaction liquid (PH=7).
3. weighing 200.00mg (2.38mmol) sodium bicarbonate (NaHCO3) to be dissolved in the water of 25.0mL, preparation concentration is about
The alkaline reaction liquid (PH > 7) of 0.1M.
The beta-cyclodextrin of 69.04mg (0.06mmol) is taken to be dissolved in 0.6mL acidity or neutral or alkaline reaction liquid respectively, point
Beta-cyclodextrin alkalinity that concentration is 0.1M or neutral or acid reaction liquid are not prepared for future use；By the three of 2.0mL (5.00mM)
It is hydrated the NaHCO of tetra chlorauric acid3Aqueous solution is added in the round-bottomed flask of 25mL, and the β-of 1.6mL is added under 25 DEG C of room temperature environments
The NaHCO of cyclodextrin reaction solution and 1.0mL3Aqueous solution stirs 5 points using magnetic stirring apparatus under 200 revs/min of revolving speed
Clock is changed into mixed solution color by yellow colourless.
(2) it heats
The colourless mixed solution that step (1) obtains is transferred in 90 DEG C of oil bath pan, under 200 revs/min of revolving speed
Stirring, heating reaction, time are respectively set as 48 hours or 72 hours；Mixed solution color gradually becomes pink colour from colourless, it
When becoming light brown again afterwards, stirring is closed, stops heating reaction.
(3) (with embodiment 1) is filtered
(4) it refrigerates
The light brown aqueous solution that step (3) obtains is stored in 5 DEG C of conditions, target product is obtained --- it can efficient transmission
The AuNCs@β-SH-CD of short wavelength-NIR light, carries out luminescent properties test for products therefrom respectively.It obtains through acid, neutral, alkali
Property condition preparation after obtained AuNCs β-SH-CD 795nm transmitting spectrogram (referring to Fig. 7).
To the test knot of the AuNCs@β-SH-CD of the energy efficient transmission short wavelength-NIR light of 1-3 of embodiment of the present invention preparation
Fruit (see Fig. 2~6) is analyzed:
(1) variation trends of the gold nano cluster of the sulfenyl beta-cyclodextrin modified obtained under different preparation times
(see Fig. 4) is as can be seen that with the available more AuNCs@β-SH- with short wavelength-NIR transmitting of the growth of time
CD: after length extends to 72h by 6h when reacted, about 10 times of luminous intensity generation is substantially improved, while absorption intensity is also obvious
Rise.
(2) what is obtained under different acid-base property reaction solution preparation conditions prepares through acid, neutral, alkaline condition
Transmitting spectrogram (see Fig. 7) of the AuNCs β-SH-CD in 795nm can significantly be found out: prepare under acid and neutrallty condition
Gold nano cluster spectrogram at 759nm does not occur peak value close to straight line, this explanation: both gold nano clusters are that do not have
There is short wavelength-NIR fluorescent emission, and the gold nano cluster prepared under alkaline condition can see obviously peak shape,
Intensity is up to 7 × 10-5, this proof: the AuNCs@β-SH- with short wavelength-NIR fluorescent emission can be prepared under alkaline condition
CD.UV-visible absorption spectrum (see Fig. 5) display: the AuNCs@β-SH-CD only generated under alkaline preparation condition is water-soluble
Liquid begins with heaving slightly at 470nm, corresponding with the color of solution (referring to Fig. 7).
(3) test result more than passing through it can be seen that with the reaction time growth, AuNCs@β-SH-CD's shines
Effect is better, and intensity is higher, it is important that only alkaline preparation condition can produce the AuNCs@β-SH- of short wavelength-NIR transmitting
CD.The gold nano cluster of sulfenyl beta-cyclodextrin modified prepared by the present invention can generate 795nm near-infrared under 450nm light source activation
It shines, overcomes the deficiency that previous cyclodextrin modified gold nano cluster generates green fluorescence mostly completely；Also, it is described
The light of the 795nm of the transmitting of AuNCs β-SH-CD is in the transmitting section (780~1100nm) of short wavelength-NIR, the emitter region
Section can further decrease the interference of biological context noise in modern imaging techniques relative to traditional Visible-to-Near InfaRed imaging,
It is more accurately imaged, has huge application prospect in bio-imaging field.
Claims (2)
1. the preparation method of the gold nano cluster of energy efficient transmission short wavelength-NIR light, which is characterized in that with beta-cyclodextrin for also
Former agent and protective agent are hydrated tetra chlorauric acid (HAuCl for three4·3H2O) reacting generation in alkaline solution with beta-cyclodextrin can be high
The gold nano cluster (AuNCs@β-SH-CD) of the sulfenyl beta-cyclodextrin modified of effect transmitting short wavelength-NIR light, specific steps are such as
Under:
(1) raw material weighing, reaction solution configuration
Under room temperature, the mercapto-modified beta-cyclodextrin of macrocyclic host-is added in the alkaline aqueous solution of three hydration tetra chlorauric acids
Alkaline reaction liquid, wherein the three hydration alkaline aqueous solutions of tetra chlorauric acid and matching for mercapto-modified beta-cyclodextrin alkaline reaction liquid
Than being 2~1, stirred 1~5 minute under 200~400 revs/min of revolving speed using magnetic stirring apparatus, make mixed solution color by
Yellow is changed into colourless；
(2) it heats
The mixed solution that step (1) obtains is transferred in 60~90 DEG C of oil bath pan, under 200~400 revs/min of revolving speed
Stirring 6~72 hours；Mixed solution color gradually becomes pink colour from colourless, when becoming light brown again later, closes stirring, stops
Heating reaction；
(3) it filters
Mixed solution after step (2) heating reaction is restored to 25 DEG C of room temperatures, sucks acquired solution using the needle tubing of 10mL,
The water phase filtering head that 200 mesh are installed on injector head squeezes needle tubing by hand, solution is leached into the vial of 10ml, is obtained
To light brown aqueous solution；
(4) it refrigerates
The light brown aqueous solution being placed in vial that step (3) obtains is saved in 0~5 DEG C of condition, obtains target production
Object --- the gold nano cluster (AuNCs@β-SH-CD) of the sulfenyl beta-cyclodextrin modified of energy efficient transmission short wavelength-NIR light；
The molecular structural formula of the gold nano cluster of the sulfenyl beta-cyclodextrin modified of energy efficient transmission short wavelength-NIR light are as follows:
Wherein,
2. the preparation method of the gold nano cluster of energy efficient transmission short wavelength-NIR light according to claim 1, feature
It is, the macrocyclic host in step (1) must be with mercapto-modified beta-cyclodextrin (β-SH-CD), and reaction solution is alkalinity.
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Application publication date: 20181218 |