CN110144207A - A kind of method and application of photoinduction synthesis red fluorescence gold nanoclusters - Google Patents
A kind of method and application of photoinduction synthesis red fluorescence gold nanoclusters Download PDFInfo
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- CN110144207A CN110144207A CN201910338231.6A CN201910338231A CN110144207A CN 110144207 A CN110144207 A CN 110144207A CN 201910338231 A CN201910338231 A CN 201910338231A CN 110144207 A CN110144207 A CN 110144207A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- C—CHEMISTRY; METALLURGY
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/58—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing copper, silver or gold
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- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
- G01N21/643—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes" non-biological material
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N2021/6417—Spectrofluorimetric devices
Abstract
The invention discloses a kind of method and its application of photoinduction synthesis red fluorescence gold nanoclusters, belong to fluorescence gold nanoclusters technical field.At room temperature, single (6- sulfydryl -6- the deoxidation)-beta-cyclodextrin of general is added in gold chloride and reacts in the case where stirring rate is 550~600rmp to solution is colourless obtains solution A to the present invention；It is slowly added to silver nitrate in solution A and reacts 9~10min in the case where stirring rate is 550~600rmp, then it adds lipoic acid to obtain mixed system B and react 9~10min in the case where stirring rate is 550~600rmp, the pH of hydrochloric acid conditioning solution is then used to obtain solution B for 3.5~4.5；Solution B is placed under LED lamplight and reacts 85~90min and obtains yellow solution to get to red fluorescence gold nano cluster Au (0)@Au (I) -6-SH- β-CD.The present invention synthesizes gold nanoclusters by coating agent of sulfydryl-beta cyclodextrin using photoreduction met hod, and synthetic method is simple, can be applied to selective enumeration method silver ion.
Description
Technical field
The present invention relates to the methods and application of a kind of photoinduction synthesis red fluorescence gold nanoclusters, belong to red fluorescence Jenner
Rice cluster technical field.
Background technique
It is excellent that gold nanoclusters have good light stability, fluorescence spectrum is adjustable, good biocompatibility, Stokes shift are big etc.
Point, before making it that there is wide application in fields such as biosensor, environmental monitoring, cell imaging, disease detection, drug deliveries
Scape.
There are many synthetic methods of reported in literature synthesis gold nanoclusters at present: one is " etching " methods, i.e., by " carving
Erosion " reagent or " etching " technology keep the bulky grain nanoparticle wrapped up broken or dissolution, the partial size of nanoparticle are made to become smaller,
To prepare the gold nanoclusters for the different light that set out；Another kind is chemical reduction method, that is, selects specific coating agent or template molecule,
Metal ion is wrapped up, then restores gold ion, prepares luminous gold nanoclusters.The synthesis of gold nanoclusters is to template molecule
Screening it is particularly significant, different template molecule is different as the gold nanoclusters property that coating agent synthesizes.Common synthesis Jenner
The template molecule of rice cluster has sulfhydryl compound, protein, polypeptide, DNA and organic polymer etc., wherein with DNA and protein
It is the most universal as template molecule synthesis gold nanoclusters.Other than template molecule, synthetic method also has the synthesis of gold nanoclusters
Great influence selects different synthetic methods to will affect the property of aggregate velocity and gold nanoclusters.
In the prior art the shortcomings that gold nanoclusters:
(1) method for synthesizing gold nanoclusters has very much, such as common etching method, chemical reduction method, ligand exchange method, aggregation
The above-mentioned synthetic method such as induced luminescence is only applicable to specific nano-cluster, is not particularly suited for owning, and some of them are gone back while being generated
Bigger nano particle is without generating fluorescence, it is therefore desirable to cumbersome purification step；
(2) be coated in the stabilizer on metal nanometre cluster surface property the photoluminescent property of metal nanometre cluster is also played it is very heavy
The effect wanted, currently used stabilizer have oligonucleotide, peptide and protein, thiol class substance etc., these substances are often
Without selectivity, to be applied to certain restrictions.
Summary of the invention
The technical issues of for gold nanoclusters in the prior art, the present invention provide a kind of photoinduction synthesis red fluorescence Jenner
The method and its application of rice cluster, the present invention synthesize gold nanoclusters, synthesis by coating agent of sulfydryl-beta cyclodextrin using photoreduction met hod
Method is simple, can be applied to selective enumeration method silver ion.
A kind of method of photoinduction synthesis red fluorescence gold nanoclusters, the specific steps are as follows:
(1) at room temperature, single (6- sulfydryl -6- deoxidation)-beta-cyclodextrin is added in gold chloride and in stirring speed
Rate is to react under 550~600rmp to solution is colourless to obtain solution A；
(2) be slowly added in the solution A of step (1) silver nitrate obtain mixed system A and stirring rate be 550~
9~10min is reacted under 600rmp, is then added lipoic acid and is obtained mixed system B and in the case where stirring rate is 550~600rmp
9~10min is reacted, the pH of hydrochloric acid conditioning solution is then used to obtain solution B for 3.5~4.5；
(3) solution B of step (2) is placed under LED lamplight and reacts 85~90min and obtains yellow solution to get to red
Color fluorescence gold nano cluster Au (0) Au (I) -6-SH- β-CD.
Gold chloride concentration is 0.9~1.2 μm of ol/L, gold chloride and single (6- sulfydryl -6- deoxidation)-β-in the step (1)
The molar ratio of cyclodextrin is 1:3.5~1:4.5.
Silver nitrate concentration is 20~400 μm of ol/L in step (2) the mixed system A.
The concentration of lipoic acid is 9~12mmol/L in the mixed system B.
The wavelength of LED lamplight is 350~370nm in the step (3), and intensity of illumination is 7~9W.
Red fluorescence gold nanoclusters Au (0)@Au (the I) -6-SH- β-CD, be by 0 valence golden metal core Au (0) and+
Shell Au (the I) -6-SH- β-CD of 1 valence is constituted.
The maximum excitation wavelength of gold nanoclusters Au (0)@Au (the I) -6-SH- β-CD is at 380nm, maximum emission wavelength
At 584nm.
Red fluorescence gold nanoclusters prepared by the method for photoinduction synthesis red fluorescence gold nanoclusters of the present invention are answered
Detection for silver ion.
The present invention is in red fluorescence gold nanoclusters Au (0)@Au (I) -6-SH- β-CD synthesis, different concentration of silver ions
The fluorescence emission wavelengths of the gold nanoclusters of synthesis and intensity are all influenced, the fluorescence hair of Au (0) Au (I) -6-SH- β-CD
The intensity for penetrating peak is changed to 117 by 30, and the position of fluorescence emission peak is by 560nm to 600nm；The fluorescence color of reaction system also with
The change of concentration of silver ions and change, by Exocarpium Citri Rubrum to red, silver ion in 22-156 μM of concentration range linearly detection and it is glimmering
Light emitting peak is linearly increased in 566-594nm.
Beneficial effects of the present invention:
The present invention synthesizes gold nanoclusters by coating agent of sulfydryl-beta cyclodextrin using photoreduction met hod, and synthetic method is simple, can
Applied to selective enumeration method silver ion；
Detailed description of the invention
Fig. 1 is the fluorescence excitation-emission spectrogram of 1 gold nanoclusters of embodiment；
Fig. 2 is the UV-vis abosrption spectrogram of 1 gold nanoclusters of embodiment；
Fig. 3 is that the TEM of 1 gold nanoclusters of embodiment schemes；
Fig. 4 is the x-ray photoelectron spectroscopy figure of 1 gold nanoclusters of embodiment；
Fig. 5 is the fluorescent emission spectrogram of Examples 1 to 10 gold nanoclusters；
Fig. 6 is the fluorescent emission spectrogram of 11~12 gold nanoclusters of embodiment；
Fig. 7 is the fluorescent emission spectrogram of 13~14 gold nanoclusters of embodiment；
Fig. 8 is the fluorescent emission spectrogram of 15 gold nanoclusters of embodiment；
Fig. 9 is the fluorescent emission spectrogram of 16 gold nanoclusters of embodiment；
Figure 10 is the fluorescent emission spectrogram of 17 gold nanoclusters of embodiment；
Figure 11 is the fluorescent emission spectrogram of 18 gold nanoclusters of embodiment；
Figure 12 is the fluorescent emission spectrogram of 19 gold nanoclusters of embodiment；
Figure 13 is the fluorescent emission spectrogram of 20 gold nanoclusters of embodiment；
Figure 14 is the fluorescent emission intensity linear graph of 0 gold nanoclusters of Examples 1 to 2；
Figure 15 is the wavelength location figure of the fluorescence emission peak of 0 gold nanoclusters of Examples 1 to 2；
Figure 16 is the compound histogram that 1 different metal ions of embodiment participate in synthesis.
Specific embodiment
Invention is further described in detail With reference to embodiment, but protection scope of the present invention and unlimited
In the content.
A kind of embodiment 1: method of photoinduction synthesis red fluorescence gold nanoclusters, the specific steps are as follows:
(1) at room temperature, single (6- sulfydryl -6- deoxidation)-beta-cyclodextrin is added to gold chloride (HAuCl4) in simultaneously
In the case where stirring rate is 550rmp, reaction obtains solution A to solution is colourless；Wherein gold chloride and single (6- sulfydryl -6- deoxidation)-β -
The 1:3.5 of cyclodextrin, gold chloride concentration are 1.10 μm of ol/L；
(2) silver nitrate is slowly added in the solution A of step (1) to obtain mixed system A and be 600rmp in stirring rate
Then lower reaction 10min adds lipoic acid and obtains mixed system B and react 10min in the case where stirring rate is 600rmp, then
The pH of hydrochloric acid conditioning solution is used to obtain solution B for 4；Wherein silver nitrate concentration is 22 μm of ol/L, mixed system in mixed system A
The concentration of lipoic acid is 10mmol/L in mixed system B in B；
(3) solution B of step (2) is placed under the LED lamplight that intensity of illumination that wavelength is 365nm is 9W and reacts 90min
Yellow solution is obtained to get red fluorescence gold nano cluster Au (0)@Au (I) -6-SH- β-CD is arrived；
The fluorescence excitation-emission spectrograms of the present embodiment gold nanoclusters as shown in Figure 1, as can be known from Fig. 1, gold nanoclusters
Maximum excitation wavelength is at 380nm, and maximum emission wavelength is at 584nm；
The UV-vis abosrption spectrograms of the present embodiment gold nanoclusters is as shown in Fig. 2, as can be known from Fig. 2, ultraviolet absorption curve
500nm does not nearby have an absorption peak, therefore gold nanoclusters rather than gold nanoparticle, presents under the ultraviolet light irradiation of 365nm red
Color fluorescence；
The TEM of the present embodiment gold nanoclusters schemes as shown in figure 3, as can be known from Fig. 3, the partial size of gold nanoclusters be about 2nm and
In monodisperse status；
The present embodiment gold nanoclusters are colourless under natural light, are Chinese red under the ultraviolet lamp of 365nm；
The x-ray photoelectron spectroscopy figures of the present embodiment gold nanoclusters is as shown in figure 4, as can be known from Fig. 4, the knot of gold nanoclusters
Closing can be Au (0) 4f5/2 at the fitting peak at 87.99eV, in conjunction with that can be Au (0) 4f7/2 at the fitting peak at 84.36eV, tie
Close can fitting peak 88.87eV at be Au (I) 4f5/2, in conjunction with can the fitting peak at 85.26eV be Au (I) 4f7/2, because
The valence state of this gold is Au (0) or Au (I)；
The present embodiment different metal ions participate in synthesis compound histogram see Figure 16, as can be seen from Figure 16, only silver from
The compound that son participates in synthesis has fluorescent red-orange.
A kind of embodiment 2: method of photoinduction synthesis red fluorescence gold nanoclusters, the specific steps are as follows:
(1) at room temperature, single (6- sulfydryl -6- deoxidation)-beta-cyclodextrin is added in gold chloride and in stirring speed
Rate is to react under 580rmp to solution is colourless to obtain solution A；Wherein gold chloride and single (6- sulfydryl -6- deoxidation)-beta-cyclodextrin
Molar ratio is 1:4, and gold chloride concentration is 1.15 μm of ol/L；
(2) silver nitrate is slowly added in the solution A of step (1) to obtain mixed system A and be 600rmp in stirring rate
Then lower reaction 10min adds lipoic acid and obtains mixed system B and react 9.5min then in the case where stirring rate is 600rmp
The pH of hydrochloric acid conditioning solution is used to obtain solution B for 4；Wherein silver nitrate concentration is 44 μm of ol/L, mixed system in mixed system A
The concentration of lipoic acid is 9mmol/L in B；
(3) solution B of step (2) is placed under the LED lamplight that intensity of illumination that wavelength is 365nm is 9W and reacts 85min
Yellow solution is obtained to get red fluorescence gold nano cluster Au (0)@Au (I) -6-SH- β-CD is arrived.
A kind of embodiment 3: method of photoinduction synthesis red fluorescence gold nanoclusters, the specific steps are as follows:
(1) at room temperature, single (6- sulfydryl -6- deoxidation)-beta-cyclodextrin is added in gold chloride and in stirring speed
Rate is to react under 600rmp to solution is colourless to obtain solution A；Wherein gold chloride and single (6- sulfydryl -6- deoxidation)-beta-cyclodextrin
Molar ratio is 1:4.5, and gold chloride concentration is 1.20 μm of ol/L；
(2) silver nitrate is slowly added in the solution A of step (1) to obtain mixed system A and be 600rmp in stirring rate
Then lower reaction 9.8min adds lipoic acid and obtains mixed system B and react 9.8min in the case where stirring rate is 600rmp, so
The pH of hydrochloric acid conditioning solution is used to obtain solution B for 4 afterwards；Wherein silver nitrate concentration is 67 μm of ol/L, mixture in mixed system A
The concentration for being lipoic acid in B is 12mmol/L；
(3) solution B of step (2) is placed under the LED lamplight that intensity of illumination that wavelength is 365nm is 9W and reacts 90min
Yellow solution is obtained to get red fluorescence gold nano cluster Au (0)@Au (I) -6-SH- β-CD is arrived.
A kind of embodiment 4: method of photoinduction synthesis red fluorescence gold nanoclusters, the specific steps are as follows:
(1) at room temperature, single (6- sulfydryl -6- deoxidation)-beta-cyclodextrin is added in gold chloride and in stirring speed
Rate is to react under 600rmp to solution is colourless to obtain solution A；Wherein gold chloride and single (6- sulfydryl -6- deoxidation)-beta-cyclodextrin
Molar ratio is 1:4, and gold chloride concentration is 1.0 μm of ol/L；
(2) silver nitrate is slowly added in the solution A of step (1) to obtain mixed system A and be 600rmp in stirring rate
Then lower reaction 9.5min adds lipoic acid and obtains mixed system B and react 10min in the case where stirring rate is 600rmp, so
The pH of hydrochloric acid conditioning solution is used to obtain solution B for 4 afterwards；Wherein silver nitrate concentration is 89 μm of ol/L, mixture in mixed system A
The concentration for being lipoic acid in B is 11mmol/L；
(3) solution B of step (2) is placed under the LED lamplight that intensity of illumination that wavelength is 350nm is 9W and reacts 88min
Yellow solution is obtained to get red fluorescence gold nano cluster Au (0)@Au (I) -6-SH- β-CD is arrived；
A kind of embodiment 5: method of photoinduction synthesis red fluorescence gold nanoclusters, the specific steps are as follows:
(1) at room temperature, single (6- sulfydryl -6- deoxidation)-beta-cyclodextrin is added in gold chloride and in stirring speed
Rate is to react under 600rmp to solution is colourless to obtain solution A；Wherein gold chloride and single (6- sulfydryl -6- deoxidation)-beta-cyclodextrin
Molar ratio is 1:4, and gold chloride concentration is 0.9 μm of ol/L；
(2) silver nitrate is slowly added in the solution A of step (1) to obtain mixed system A and be 600rmp in stirring rate
Then lower reaction 9min adds lipoic acid and obtains mixed system B and react 10min in the case where stirring rate is 600rmp, then
The pH of hydrochloric acid conditioning solution is used to obtain solution B for 4；Wherein silver nitrate concentration is 111 μm of ol/L, mixture in mixed system A
The concentration for being lipoic acid in B is 10.5mmol/L；
(3) solution B of step (2) is placed under the LED lamplight that intensity of illumination that wavelength is 370nm is 7W and reacts 90min
Yellow solution is obtained to get red fluorescence gold nano cluster Au (0)@Au (I) -6-SH- β-CD is arrived；
A kind of embodiment 6: method of photoinduction synthesis red fluorescence gold nanoclusters, the specific steps are as follows:
(1) at room temperature, single (6- sulfydryl -6- deoxidation)-beta-cyclodextrin is added in gold chloride and in stirring speed
Rate is to react under 600rmp to solution is colourless to obtain solution A；Wherein gold chloride and single (6- sulfydryl -6- deoxidation)-beta-cyclodextrin
Molar ratio is 1:4, and gold chloride concentration is 0.95 μm of ol/L；
(2) silver nitrate is slowly added in the solution A of step (1) to obtain mixed system A and be 600rmp in stirring rate
Then lower reaction 10min adds lipoic acid and obtains mixed system B and react 9min in the case where stirring rate is 600rmp, then
The pH of hydrochloric acid conditioning solution is used to obtain solution B for 4；Wherein silver nitrate concentration is 133 μm of ol/L, mixture in mixed system A
The concentration for being lipoic acid in B is 10mmol/L；
(3) solution B of step (2) is placed under the LED lamplight that intensity of illumination that wavelength is 365nm is 9W and reacts 90min
Yellow solution is obtained to get red fluorescence gold nano cluster Au (0)@Au (I) -6-SH- β-CD is arrived；
A kind of embodiment 7: method of photoinduction synthesis red fluorescence gold nanoclusters, the specific steps are as follows:
(1) at room temperature, single (6- sulfydryl -6- deoxidation)-beta-cyclodextrin is added in gold chloride and in stirring speed
Rate is to react under 600rmp to solution is colourless to obtain solution A；Wherein gold chloride and single (6- sulfydryl -6- deoxidation)-beta-cyclodextrin
Molar ratio is 1:4, and gold chloride concentration is 1.10 μm of ol/L；
(2) silver nitrate is slowly added in the solution A of step (1) to obtain mixed system A and be 600rmp in stirring rate
Then lower reaction 10min adds lipoic acid and obtains mixed system B and react 10min in the case where stirring rate is 600rmp, then
The pH of hydrochloric acid conditioning solution is used to obtain solution B for 4；Wherein silver nitrate concentration is 156 μm of ol/L, mixture in mixed system A
The concentration for being lipoic acid in B is 10mmol/L；
(3) solution B of step (2) is placed under the LED lamplight that intensity of illumination that wavelength is 365nm is 8W and reacts 90min
Yellow solution is obtained to get red fluorescence gold nano cluster Au (0)@Au (I) -6-SH- β-CD is arrived.
A kind of embodiment 8: method of photoinduction synthesis red fluorescence gold nanoclusters, the specific steps are as follows:
(1) at room temperature, single (6- sulfydryl -6- deoxidation)-beta-cyclodextrin is added in gold chloride and in stirring speed
Rate is to react under 600rmp to solution is colourless to obtain solution A；Wherein gold chloride and single (6- sulfydryl -6- deoxidation)-beta-cyclodextrin
Molar ratio is 1:4, and gold chloride concentration is 1.10 μm of ol/L；
(2) silver nitrate is slowly added in the solution A of step (1) to obtain mixed system A and be 600rmp in stirring rate
Then lower reaction 10min adds lipoic acid and obtains mixed system B and react 10min in the case where stirring rate is 600rmp, then
The pH of hydrochloric acid conditioning solution is used to obtain solution B for 4；Wherein, silver nitrate concentration is 178 μm of ol/L, mixture in mixed system A
The concentration for being lipoic acid in B is 10mmol/L；
(3) solution B of step (2) is placed under the LED lamplight that intensity of illumination that wavelength is 365nm is 9W and reacts 90min
Yellow solution is obtained to get red fluorescence gold nano cluster Au (0)@Au (I) -6-SH- β-CD is arrived.
A kind of embodiment 9: method of photoinduction synthesis red fluorescence gold nanoclusters, the specific steps are as follows:
(1) at room temperature, single (6- sulfydryl -6- deoxidation)-beta-cyclodextrin is added in gold chloride and in stirring speed
Rate is to react under 600rmp to solution is colourless to obtain solution A；Wherein gold chloride and single (6- sulfydryl -6- deoxidation)-beta-cyclodextrin
Molar ratio is 1:4, and gold chloride concentration is 1.10 μm of ol/L；
(2) silver nitrate is slowly added in the solution A of step (1) to obtain mixed system A and be 600rmp in stirring rate
Then lower reaction 10min adds lipoic acid and obtains mixed system B and react 10min in the case where stirring rate is 600rmp, then
The pH of hydrochloric acid conditioning solution is used to obtain solution B for 4；Wherein silver nitrate concentration is 200 μm of ol/L, mixture in mixed system A
The concentration for being lipoic acid in B is 10mmol/L；
(3) solution B of step (2) is placed under the LED lamplight that intensity of illumination that wavelength is 365nm is 9W and reacts 90min
Yellow solution is obtained to get red fluorescence gold nano cluster Au (0)@Au (I) -6-SH- β-CD is arrived.
A kind of embodiment 10: method of photoinduction synthesis red fluorescence gold nanoclusters, the specific steps are as follows:
(1) at room temperature, single (6- sulfydryl -6- deoxidation)-beta-cyclodextrin is added in gold chloride and in stirring speed
Rate is to react under 600rmp to solution is colourless to obtain solution A；Wherein gold chloride and single (6- sulfydryl -6- deoxidation)-beta-cyclodextrin
Molar ratio is 1:4, and gold chloride concentration is 1.10 μm of ol/L；
(2) silver nitrate is slowly added in the solution A of step (1) to obtain mixed system A and be 600rmp in stirring rate
Then lower reaction 10min adds lipoic acid and obtains mixed system B and react 10min in the case where stirring rate is 600rmp, then
The pH of hydrochloric acid conditioning solution is used to obtain solution B for 4；Wherein silver nitrate concentration is 222 μm of ol/L, mixture in mixed system A
The concentration for being lipoic acid in B is 10mmol/L；
(3) solution B of step (2) is placed under the LED lamplight that intensity of illumination that wavelength is 365nm is 9W and reacts 90min
Yellow solution is obtained to get red fluorescence gold nano cluster Au (0)@Au (I) -6-SH- β-CD is arrived.
A kind of embodiment 11: method of photoinduction synthesis red fluorescence gold nanoclusters, the specific steps are as follows:
(1) at room temperature, single (6- sulfydryl -6- deoxidation)-beta-cyclodextrin is added in gold chloride and in stirring speed
Rate is to react under 600rmp to solution is colourless to obtain solution A；Wherein gold chloride and single (6- sulfydryl -6- deoxidation)-beta-cyclodextrin
Molar ratio is 1:4, and gold chloride concentration is 1.10 μm of ol/L；
(2) silver nitrate is slowly added in the solution A of step (1) to obtain mixed system A and be 600rmp in stirring rate
Then lower reaction 10min adds lipoic acid and obtains mixed system B and react 10min in the case where stirring rate is 600rmp, then
The pH of hydrochloric acid conditioning solution is used to obtain solution B for 4；Wherein silver nitrate concentration is 244 μm of ol/L, mixture in mixed system A
The concentration for being lipoic acid in B is 10mmol/L；
(3) solution B of step (2) is placed under the LED lamplight that intensity of illumination that wavelength is 365nm is 9W and reacts 90min
Yellow solution is obtained to get red fluorescence gold nano cluster Au (0)@Au (I) -6-SH- β-CD is arrived.
A kind of embodiment 12: method of photoinduction synthesis red fluorescence gold nanoclusters, the specific steps are as follows:
(1) at room temperature, single (6- sulfydryl -6- deoxidation)-beta-cyclodextrin is added in gold chloride and in stirring speed
Rate is to react under 600rmp to solution is colourless to obtain solution A；Wherein gold chloride and single (6- sulfydryl -6- deoxidation)-beta-cyclodextrin
Molar ratio is 1:4, and gold chloride concentration is 1.10 μm of ol/L；
(2) silver nitrate is slowly added in the solution A of step (1) to obtain mixed system A and be 600rmp in stirring rate
Then lower reaction 10min adds lipoic acid and obtains mixed system B and react 10min in the case where stirring rate is 600rmp, then
The pH of hydrochloric acid conditioning solution is used to obtain solution B for 4；Wherein silver nitrate concentration is 267 μm of ol/L, mixture in mixed system A
The concentration for being lipoic acid in B is 10mmol/L；
(3) solution B of step (2) is placed under the LED lamplight that intensity of illumination that wavelength is 365nm is 9W and reacts 90min
Yellow solution is obtained to get red fluorescence gold nano cluster Au (0)@Au (I) -6-SH- β-CD is arrived.
A kind of embodiment 13: method of photoinduction synthesis red fluorescence gold nanoclusters, the specific steps are as follows:
(1) at room temperature, single (6- sulfydryl -6- deoxidation)-beta-cyclodextrin is added in gold chloride and in stirring speed
Rate is to react under 600rmp to solution is colourless to obtain solution A；Wherein gold chloride and single (6- sulfydryl -6- deoxidation)-beta-cyclodextrin
Molar ratio is 1:4, and gold chloride concentration is 1.10 μm of ol/L；
(2) silver nitrate is slowly added in the solution A of step (1) to obtain mixed system A and be 600rmp in stirring rate
Then lower reaction 10min adds lipoic acid and obtains mixed system B and react 10min in the case where stirring rate is 600rmp, then
The pH of hydrochloric acid conditioning solution is used to obtain solution B for 4；Wherein silver nitrate concentration is 289 μm of ol/L, mixture in mixed system A
The concentration for being lipoic acid in B is 10mmol/L；
(3) solution B of step (2) is placed under the LED lamplight that intensity of illumination that wavelength is 365nm is 9W and reacts 90min
Yellow solution is obtained to get red fluorescence gold nano cluster Au (0)@Au (I) -6-SH- β-CD is arrived.
A kind of embodiment 14: method of photoinduction synthesis red fluorescence gold nanoclusters, the specific steps are as follows:
(1) at room temperature, single (6- sulfydryl -6- deoxidation)-beta-cyclodextrin is added in gold chloride and in stirring speed
Rate is to react under 600rmp to solution is colourless to obtain solution A；Wherein gold chloride and single (6- sulfydryl -6- deoxidation)-beta-cyclodextrin
Molar ratio is 1:4, and gold chloride concentration is 1.10 μm of ol/L；
(2) silver nitrate is slowly added in the solution A of step (1) to obtain mixed system A and be 600rmp in stirring rate
Then lower reaction 10min adds lipoic acid and obtains mixed system B and react 10min in the case where stirring rate is 600rmp, then
The pH of hydrochloric acid conditioning solution is used to obtain solution B for 4；Wherein silver nitrate concentration is 311 μm of ol/L, mixture in mixed system A
The concentration for being lipoic acid in B is 10mmol/L；
(3) solution B of step (2) is placed under the LED lamplight that intensity of illumination that wavelength is 365nm is 9W and reacts 90min
Yellow solution is obtained to get red fluorescence gold nano cluster Au (0)@Au (I) -6-SH- β-CD is arrived.
A kind of embodiment 15: method of photoinduction synthesis red fluorescence gold nanoclusters, the specific steps are as follows:
(1) at room temperature, single (6- sulfydryl -6- deoxidation)-beta-cyclodextrin is added in gold chloride and in stirring speed
Rate is to react under 600rmp to solution is colourless to obtain solution A；Wherein gold chloride and single (6- sulfydryl -6- deoxidation)-beta-cyclodextrin
Molar ratio is 1:4, and gold chloride concentration is 1.10 μm of ol/L；
(2) silver nitrate is slowly added in the solution A of step (1) to obtain mixed system A and be 600rmp in stirring rate
Then lower reaction 10min adds lipoic acid and obtains mixed system B and react 10min in the case where stirring rate is 600rmp, then
The pH of hydrochloric acid conditioning solution is used to obtain solution B for 4；Wherein silver nitrate concentration is 333 μm of ol/L, mixture in mixed system A
The concentration for being lipoic acid in B is 10mmol/L；
(3) solution B of step (2) is placed under the LED lamplight that intensity of illumination that wavelength is 365nm is 9W and reacts 90min
Yellow solution is obtained to get red fluorescence gold nano cluster Au (0)@Au (I) -6-SH- β-CD is arrived.
A kind of embodiment 16: method of photoinduction synthesis red fluorescence gold nanoclusters, the specific steps are as follows:
(1) at room temperature, single (6- sulfydryl -6- deoxidation)-beta-cyclodextrin is added in gold chloride and in stirring speed
Rate is to react under 600rmp to solution is colourless to obtain solution A；Wherein gold chloride and single (6- sulfydryl -6- deoxidation)-beta-cyclodextrin
Molar ratio is 1:4, and gold chloride concentration is 1.10 μm of ol/L；
(2) silver nitrate is slowly added in the solution A of step (1) to obtain mixed system A and be 600rmp in stirring rate
Then lower reaction 10min adds lipoic acid and obtains mixed system B and react 10min in the case where stirring rate is 600rmp, then
The pH of hydrochloric acid conditioning solution is used to obtain solution B for 4；Wherein silver nitrate concentration is 356 μm of ol/L, mixture in mixed system A
The concentration for being lipoic acid in B is 10mmol/L；
(3) solution B of step (2) is placed under the LED lamplight that intensity of illumination that wavelength is 365nm is 9W and reacts 90min
Yellow solution is obtained to get red fluorescence gold nano cluster Au (0)@Au (I) -6-SH- β-CD is arrived.
A kind of embodiment 17: method of photoinduction synthesis red fluorescence gold nanoclusters, the specific steps are as follows:
(1) at room temperature, single (6- sulfydryl -6- deoxidation)-beta-cyclodextrin is added in gold chloride and in stirring speed
Rate is to react under 600rmp to solution is colourless to obtain solution A；Wherein gold chloride and single (6- sulfydryl -6- deoxidation)-beta-cyclodextrin
Molar ratio is 1:4, and gold chloride concentration is 1.10 μm of ol/L；
(2) silver nitrate is slowly added in the solution A of step (1) to obtain mixed system A and be 600rmp in stirring rate
Then lower reaction 10min adds lipoic acid and obtains mixed system B and react 10min in the case where stirring rate is 600rmp, then
The pH of hydrochloric acid conditioning solution is used to obtain solution B for 4；Wherein silver nitrate concentration is 378 μm of ol/L, mixture in mixed system A
The concentration for being lipoic acid in B is 10mmol/L；
(3) solution B of step (2) is placed under the LED lamplight that intensity of illumination that wavelength is 365nm is 9W and reacts 90min
Yellow solution is obtained to get red fluorescence gold nano cluster Au (0)@Au (I) -6-SH- β-CD is arrived.
A kind of embodiment 18: method of photoinduction synthesis red fluorescence gold nanoclusters, the specific steps are as follows:
(1) at room temperature, single (6- sulfydryl -6- deoxidation)-beta-cyclodextrin is added in gold chloride and in stirring speed
Rate is to react under 600rmp to solution is colourless to obtain solution A；Wherein gold chloride and single (6- sulfydryl -6- deoxidation)-beta-cyclodextrin
Molar ratio is 1:4, and gold chloride concentration is 1.10 μm of ol/L；
(2) silver nitrate is slowly added in the solution A of step (1) to obtain mixed system A and be 600rmp in stirring rate
Then lower reaction 10min adds lipoic acid and obtains mixed system B and react 10min in the case where stirring rate is 600rmp, then
The pH of hydrochloric acid conditioning solution is used to obtain solution B for 4；Wherein silver nitrate concentration is 400 μm of ol/L, mixture in mixed system A
The concentration for being lipoic acid in B is 10mmol/L；
(3) solution B of step (2) is placed under the LED lamplight that intensity of illumination that wavelength is 365nm is 9W and reacts 90min
Yellow solution is obtained to get red fluorescence gold nano cluster Au (0)@Au (I) -6-SH- β-CD is arrived.
A kind of embodiment 19: method of photoinduction synthesis red fluorescence gold nanoclusters, the specific steps are as follows:
(1) at room temperature, single (6- sulfydryl -6- deoxidation)-beta-cyclodextrin is added in gold chloride and in stirring speed
Rate is to react under 600rmp to solution is colourless to obtain solution A；Wherein gold chloride and single (6- sulfydryl -6- deoxidation)-beta-cyclodextrin
Molar ratio is 1:4, and gold chloride concentration is 1.10 μm of ol/L；
(2) silver nitrate is slowly added in the solution A of step (1) to obtain mixed system A and be 600rmp in stirring rate
Then lower reaction 10min adds lipoic acid and obtains mixed system B and react 10min in the case where stirring rate is 600rmp, then
The pH of hydrochloric acid conditioning solution is used to obtain solution B for 4；Wherein silver nitrate concentration is 422 μm of ol/L, mixture in mixed system A
The concentration for being lipoic acid in B is 10mmol/L；
(3) solution B of step (2) is placed under the LED lamplight that intensity of illumination that wavelength is 365nm is 9W and reacts 90min
Yellow solution is obtained to get red fluorescence gold nano cluster Au (0)@Au (I) -6-SH- β-CD is arrived.
A kind of embodiment 20: method of photoinduction synthesis red fluorescence gold nanoclusters, the specific steps are as follows:
(1) at room temperature, single (6- sulfydryl -6- deoxidation)-beta-cyclodextrin is added in gold chloride and in stirring speed
Rate is to react under 600rmp to solution is colourless to obtain solution A；Wherein gold chloride and single (6- sulfydryl -6- deoxidation)-beta-cyclodextrin
Molar ratio is 1:4, and gold chloride concentration is 1.10 μm of ol/L；
(2) silver nitrate is slowly added in the solution A of step (1) to obtain mixed system A and be 600rmp in stirring rate
Then lower reaction 10min adds lipoic acid and obtains mixed system B and react 10min in the case where stirring rate is 600rmp, then
The pH of hydrochloric acid conditioning solution is used to obtain solution B for 4；Wherein silver nitrate concentration is 444 μm of ol/L, mixture in mixed system A
The concentration for being lipoic acid in B is 10mmol/L；
(3) solution B of step (2) is placed under the LED lamplight that intensity of illumination that wavelength is 365nm is 9W and reacts 90min
Yellow solution is obtained to get red fluorescence gold nano cluster Au (0)@Au (I) -6-SH- β-CD is arrived.
The fluorescent emission spectrogram of Examples 1 to 10 gold nanoclusters is shown in Fig. 5, the fluorescent emission of 11~12 gold nanoclusters of embodiment
Spectrogram is shown in Fig. 6, and the fluorescent emission spectrogram of 13~14 gold nanoclusters of embodiment is shown in Fig. 7, the fluorescent emission of 15 gold nanoclusters of embodiment
Spectrogram is shown in Fig. 8, and the fluorescent emission spectrogram of 16 gold nanoclusters of embodiment is shown in Fig. 9, the fluorescent emission spectrogram of 17 gold nanoclusters of embodiment
See Figure 10, the fluorescent emission spectrogram of 18 gold nanoclusters of embodiment is shown in Figure 11, and the fluorescent emission spectrogram of 19 gold nanoclusters of embodiment is shown in
The fluorescent emission spectrogram of Figure 12,20 gold nanoclusters of embodiment are shown in Figure 13, from Fig. 5~13 it is found that with concentration of silver ions increase,
The fluorescent emission intensity of gold nanoclusters is by 30 enhancings to 117；In addition, the fluorescent emission displacement of gold nanoclusters is changed to by 560nm
600nm。
The fluorescent emission intensity linear graph of 0 gold nanoclusters of Examples 1 to 2 is shown in Figure 14, and as can be seen from Figure 14, concentration of silver ions exists
Within the scope of 22-156 μm of ol/L, the fluorescent emission intensity of gold nanoclusters is linearly increased；
The wavelength location figure of the fluorescence emission peak of 0 gold nanoclusters of Examples 1 to 2 is shown in Figure 15, from figure 15, it can be known that silver ion is dense
Within the scope of 50-289 μm of ol/L, fluorescence emission peak linearly increases degree in 566-594nm.
Claims (6)
1. a kind of method of photoinduction synthesis red fluorescence gold nanoclusters, which is characterized in that specific step is as follows:
(1) at room temperature, single (6- sulfydryl -6- deoxidation)-beta-cyclodextrin is added in gold chloride and is in stirring rate
Reaction obtains solution A to solution is colourless under 550~600rmp；
(2) silver nitrate is slowly added in the solution A of step (1) to obtain mixed system A and be 550~600rmp in stirring rate
Then 9~10min of lower reaction adds lipoic acid and obtains mixed system B and react 9 in the case where stirring rate is 550~600rmp
Then~10min uses the pH of hydrochloric acid conditioning solution to obtain solution B for 3.5~4.5；
(3) solution B of step (2) is placed in 85~90min of reaction under LED lamplight and obtains yellow solution to get glimmering to red
Light gold nano cluster Au (0)@Au (I) -6-SH- β-CD.
2. the method for photoinduction synthesis red fluorescence gold nanoclusters according to claim 1, it is characterised in that: in step (1)
Gold chloride concentration is 0.9~1.2 μm of ol/L, and gold chloride and the singly molar ratio of (6- sulfydryl -6- deoxidation)-beta-cyclodextrin are 1:3.5
~1:4.5.
3. the method for photoinduction synthesis red fluorescence gold nanoclusters according to claim 1, it is characterised in that: step (2) is mixed
Silver nitrate concentration is 20~400 μm of ol/L in zoarium system A.
4. the method for photoinduction synthesis red fluorescence gold nanoclusters according to claim 1, it is characterised in that: step (2) is mixed
The concentration of lipoic acid is 9~12mmol/L in zoarium system B.
5. the method for photoinduction synthesis red fluorescence gold nanoclusters according to claim 1, it is characterised in that: in step (3)
The wavelength of LED lamplight is 350~370nm, and intensity of illumination is 7~9W.
6. red fluorescence gold nanoclusters prepared by the method for the synthesis red fluorescence gold nanoclusters of photoinduction described in claim 1 are answered
Detection for silver ion.
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