CN105328203B - 1 H, 1,2,4 triazoles, 3 mercaptan bovine serum albumin(BSA) fluorescent au nanocluster material and preparation method thereof - Google Patents
1 H, 1,2,4 triazoles, 3 mercaptan bovine serum albumin(BSA) fluorescent au nanocluster material and preparation method thereof Download PDFInfo
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- CN105328203B CN105328203B CN201510622104.0A CN201510622104A CN105328203B CN 105328203 B CN105328203 B CN 105328203B CN 201510622104 A CN201510622104 A CN 201510622104A CN 105328203 B CN105328203 B CN 105328203B
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
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Abstract
The present invention discloses 1 H 1 of one kind, 2,4 triazole, 3 mercaptan bovine serum albumin(BSA) fluorescent au nanocluster material and preparation method thereof, with gold chloride, 1 H 1,2,4 triazole, 3 mercaptan, bovine serum albumin(BSA) are raw material one-step synthesis water-soluble gold nano cluster fluorescent material.The present invention is a kind of preparation method of new fluorescent au nanocluster material, has the advantages that to prepare quick, simple and environmentally-friendly.Synthesized 1 H, 1,2,4 triazoles, 3 mercaptan bovine serum albumin(BSA) gold nano cluster shows strong rose fluorescence（Maximum emission wavelength is 650 nm）, Stokes shift is big（245 nm）, good water solubility, has the advantages that higher stability.
Description
Technical field
The present invention relates to the system of 1-H-1,2,4- triazoles -3- mercaptan-bovine serum albumin(BSA)-fluorescent au nanocluster material
Preparation Method, belongs to field of nanometer technology.
Background technology
In recent years, application of the fluorescent nano material as fluorescent marker in biology receives much concern.So far, grind
Study carefully personnel and have been developed for a variety of different types of fluorescence such as semiconductor-quantum-point, dyestuff dopen Nano particle, carbon nano dot
Nano material.Fluorescence gold nano cluster（gold nanoclusters, AuNCs）The fluorescent nano material new as one kind,
Have the advantages that photophysical property is good, specific surface area is big, surface is easy to modification and photoluminescent property is adjustable.Gold nano cluster be by
The stable aggregate of several to tens gold atom compositions, diameter are typically smaller than 2 nm, between monatomic and nano-particle or big
Between the metal of volume.Since it is closely sized to Fermi's wavelength in electronics, continuous energy state property is split into discrete energy state,
And the size for similar molecule occur relies on effect.In compound test, bio-sensing and imaging, photoelectronics and nanosecond medical science etc.
Field has a wide range of applications.
The technology of preparing of fluorescent au nanocluster material mainly includes chemical reduction method, reverse microemulsion process, templated synthesis
Method monolayer protection technique and ligand etching method etc..Wherein monolayer protection technique is a kind of cluster synthesis of Simple temperature sum
Method, by the use of the small molecule containing certain functional group as protection group, forms protective layer, so as to stablize gold nano group on cluster surface
Cluster, makes it be not easy to reunite.In recent decades, researchers both domestic and external propose a variety of different methods and prepare high fluorescent quantum
The adjustable gold nano cluster of yield, good water solubility, glow color.
The present invention is water-soluble as raw material one-step synthesis using gold chloride, 1-H-1,2,4- triazole -3- mercaptan, bovine serum albumin(BSA)
Property fluorescent au nanocluster material.Bovine serum albumin(BSA) is as stabilizer, 1-H-1,2,4- triazole -3- mercaptan for reducing agent and
Dressing agent controls the formation of gold nano cluster.Prepared 1-H-1,2,4- triazoles -3- mercaptan-bovine serum albumin(BSA)-gold
Nanocluster has strong rose fluorescence, and Stokes shift is big, good water solubility.
The content of the invention
The object of the present invention is to provide a kind of 1-H-1,2,4- triazoles -3- mercaptan-bovine serum albumin(BSA)-gold nano cluster
Fluorescent material and its with 1-H-1,2,4- triazole -3- mercaptan are reducing agent and dressing agent, using bovine serum albumin(BSA) as stabilizer
The method of one-step synthesis fluorescent au nanocluster material.
To achieve these goals, the present invention uses following technical scheme：1-H-1,2,4- triazoles of the present invention-
The preparation method of 3- mercaptan-bovine serum albumin(BSA)-fluorescent au nanocluster material, it is characterized in that it is made of following steps：Ox
Serum albumin solution is uniformly mixed with chlorauric acid solution, then adds 1-H-1,2,4- triazole -3- thiol solutions, and shaking mixes
Even, reaction certain time obtains 1-H-1,2,4- triazole -3- mercaptan-bovine serum albumin(BSA)-gold nano cluster, gold nano cluster
Fluorescent au nanocluster material powder is can obtain after the freeze-drying of fluorescent material aqueous solution.
The preparation side of the 1-H-1,2,4- triazoles -3- mercaptan-bovine serum albumin(BSA)-fluorescent au nanocluster material
Method, it is characterized in that using bovine serum albumin(BSA) as stabilizer, 1-H-1,2,4- triazole -3- mercaptan are reducing agent and dressing agent control
The formation of gold nano cluster processed.
The volume of the chlorauric acid solution, bovine serum albumin solution and 1-H-1,2,4- triazole -3- thiol solutions
Than for 5：3：2.
The concentration of chlorauric acid solution used can be 1 ~ 100 mmol/L, and most preferable concentrations are 10 mmol/L, cow's serum
Albumin solution can be 5 ~ 500 mg/mL, and most preferable concentrations are 50 mg/mL, 1-H-1,2,4- triazole -3- thiol solutions
Concentration can be 0.01 ~ 1 mol/L, most preferable concentrations are 0.1 mol/L, wherein dissolved with most preferable concentrations be 0.1
The sodium hydroxide of mol/L.
The chlorauric acid solution, bovine serum albumin solution and 1-H-1,2,4- triazole -3- thiol solutions mix postposition
When 4 DEG C of reactions 0.5 ~ 2 are small, most preferably 1 h.
Obtained gold nano cluster material aqueous solution is colourless, and uv-vis spectra is at 520 nm without absworption peak.
Strong rose fluorescence is produced under ultra violet lamp, maximum excitation wavelength and launch wavelength are respectively 405 nm and 650 nm.
The preparation method of the optimal fluorescent au nanocluster material of the present invention is as follows：
All glasswares used in procedure below are soaked by chloroazotic acid, and are thoroughly cleaned with distilled water, are dried.Gold
Preparing for nanocluster fluorescent material is as follows：The bovine serum albumin(BSA) that 0.75 mL concentration is 50 mg/mL is with 1.25 mL concentration
The chlorauric acid solution of 10 mmol/L is uniformly mixed, and adds 1-H-1,2,4- triazole -3- that 0.5 mL concentration is 0.1 mol/L
Thiol solution（Containing 0.1 mol/L sodium hydroxides）, shake and mix, react 1 h at 4 DEG C, obtain 1-H-1,2,4- triazole -3- sulphur
Alcohol-bovine serum albumin(BSA)-gold nano cluster.The gold nano cluster of gained be rufous liquid, ultraviolet lamp（365 nm）Irradiation
Under have strong rose fluorescence.
1-H-1,2,4- triazoles -3- mercaptan-bovine serum albumin(BSA)-gold nano made from the above-mentioned preparation method of the present invention
Cluster, it is characterized in that soluble easily in water, aqueous solution is rufous, and strong rose fluorescence is produced under ultra violet lamp, maximum
Excitation wavelength and launch wavelength are respectively 405 nm and 650 nm.
The gold nano cluster average grain diameter is 2 nm.
The 1-H-1,2,4- triazole -3- mercaptan-bovine serum albumin(BSA)-gold nano cluster, it is characterized in that aqueous solution
Place under 4 DEG C of dark places 2 months and occur without sediment, fluorescence intensity and maximum emission peak position remain unchanged.
The 1-H-1,2,4- triazole -3- mercaptan-bovine serum albumin(BSA)-gold nano cluster, it is characterized in that with chlorine gold
Acid is Jin Yuan, 1-H-1,2, and 4- triazole -3- mercaptan is reducing agent and dressing agent, and bovine serum albumin(BSA) is prepared for stabilizer.
Advantages of the present invention：
（1）For the present invention with 1-H-1,2,4- triazole -3- mercaptan are reducing agent and dressing agent, are existed in bovine serum albumin(BSA)
Under conditions of one-step synthesis water-soluble gold nano cluster fluorescent material, have the advantages that to prepare quick, simple and environmentally-friendly.
（2）Gold nano cluster prepared by the present invention has strong rose fluorescence（Maximum emission wavelength is 650
nm）, larger Stokes shift（245 nm）The features such as.
Brief description of the drawings
Fig. 1 is gold nano cluster fluorescent nano material in visible ray（A）Under ultraviolet lamp（B）Outside drawing.
Fig. 2 is the UV-visible absorption spectrum of gold nano cluster fluorescent nano material.
Fig. 3 is the excitation and emission spectra figure of gold nano cluster fluorescent nano material.
Fig. 4 is the Energy Dispersive X energy spectrum diagram of gold nano cluster fluorescent nano material.
Fig. 5 is the transmission electron microscope picture of gold nano cluster fluorescent nano material.
Fig. 6 is the x-ray photoelectron spectroscopy figure of gold nano cluster fluorescent nano material.
Embodiment
Example 1：
The bovine serum albumin(BSA) that 0.75 mL concentration is 50 mg/mL and the gold chloride that 1.25 mL concentration are 10 mmol/L are molten
Liquid is uniformly mixed, and adds the 1-H-1 that 0.5 mL concentration is 0.1 mol/L, 2,4- triazole -3- thiol solutions（Containing 0.1 mol/L
Sodium hydroxide）, shake and mix, react 1 h at 4 DEG C, obtain 1-H-1,2,4- triazole -3- mercaptan-bovine serum albumin(BSA)-Jenner
Rice cluster.The gold nano cluster of gained is the liquid of rufous（See Figure 1A）, it is glimmering that strong rose is produced under ultra violet lamp
Light（See Figure 1B）.
Example 2：
The bovine serum albumin(BSA) that 0.75 mL concentration is 50 mg/mL and the gold chloride that 1.25 mL concentration are 10 mmol/L are molten
Liquid is uniformly mixed, and adds the 1-H-1 that 0.5 mL concentration is 0.1 mol/L, 2,4- triazole -3- thiol solutions（Containing 0.1 mol/L
Sodium hydroxide）, shake and mix, react 1 h at 4 DEG C, obtain 1-H-1,2,4- triazole -3- mercaptan-bovine serum albumin(BSA)-Jenner
Rice cluster.Obtained gold nano cluster solution carries out ultraviolet-visible spectrum scanning, obtains it at 520 nm wavelength without gold nano
Particle characteristics absworption peak（See Fig. 2）.
Example 3：
The bovine serum albumin(BSA) that 0.75 mL concentration is 50 mg/mL and the gold chloride that 1.25 mL concentration are 10 mmol/L are molten
Liquid is uniformly mixed, and adds the 1-H-1 that 0.5 mL concentration is 0.1 mol/L, 2,4- triazole -3- thiol solutions（Containing 0.1 mol/L
Sodium hydroxide）, shake and mix, react 1 h at 4 DEG C, obtain 1-H-1,2,4- triazole -3- mercaptan-bovine serum albumin(BSA)-Jenner
Rice cluster.Obtained gold nano cluster solution carries out fluorescence spectrum scanning, obtains its maximum excitation wavelength and launch wavelength difference
For 405 nm and 650 nm（See Fig. 3）.
Example 4：
The bovine serum albumin(BSA) that 0.75 mL concentration is 50 mg/mL and the gold chloride that 1.25 mL concentration are 10 mmol/L are molten
Liquid is uniformly mixed, and adds the 1-H-1 that 0.5 mL concentration is 0.1 mol/L, 2,4- triazole -3- thiol solutions（Containing 0.1 mol/L
Sodium hydroxide）, shake and mix, react 1 h at 4 DEG C, obtain 1-H-1,2,4- triazole -3- mercaptan-bovine serum albumin(BSA)-Jenner
Rice cluster.Obtained gold nano cluster solution drop coating is on copper mesh.Energy Dispersive X energy spectrum analysis（See Fig. 4）Show to produce
Thing contains gold element.
Example 5：
The bovine serum albumin(BSA) that 0.75 mL concentration is 50 mg/mL and the gold chloride that 1.25 mL concentration are 10 mmol/L are molten
Liquid is uniformly mixed, and adds the 1-H-1 that 0.5 mL concentration is 0.1 mol/L, 2,4- triazole -3- thiol solutions（Containing 0.1 mol/L
Sodium hydroxide）, shake and mix, react 1 h at 4 DEG C, obtain 1-H-1,2,4- triazole -3- mercaptan-bovine serum albumin(BSA)-Jenner
Rice cluster.Obtained gold nano cluster solution carries out the measure of transmission electron microscope, and the average grain diameter for measuring gold nano cluster is 2
nm（See Fig. 5）.
Example 6：
The bovine serum albumin(BSA) that 0.75 mL concentration is 50 mg/mL and the gold chloride that 1.25 mL concentration are 10 mmol/L are molten
Liquid is uniformly mixed, and adds the 1-H-1 that 0.5 mL concentration is 0.1 mol/L, 2,4- triazole -3- thiol solutions（Containing 0.1 mol/L
Sodium hydroxide）, shake and mix, react 1 h at 4 DEG C, obtain 1-H-1,2,4- triazole -3- mercaptan-bovine serum albumin(BSA)-Jenner
Rice cluster.Powder is obtained after obtained gold nano cluster solution freeze-drying, takes gained powder to carry out x-ray photoelectron spectroscopy
Measure, the 4f of XPS Au (4f) display gold7/2Peak and 4f5/2Peak is located at 84.5 eV and 88.2 eV respectively, shows gold nano cluster
Middle golden valence state is coexisted in a manner of 0 valency and+1 valency（See Fig. 6）.
Claims (4)
1. a kind of 1-H-1, the preparation method of 2,4- triazole -3- mercaptan-bovine serum albumin(BSA)-fluorescent au nanocluster material,
Comprise the following steps：The chlorine that the bovine serum albumin(BSA) and 1.25 mL concentration that 0.75 mL concentration is 50 mg/mL are 10 mmol/L
Auric acid solution is uniformly mixed, and adds the 1-H-1 wherein containing 0.1 mol/L sodium hydroxides that 0.5 mL concentration is 0.1 mol/L,
2,4- triazole -3- thiol solutions, shaking mix, and when reaction 1 is small at 4 DEG C, obtain 1-H-1,2,4- triazole -3- mercaptan-ox
Seralbumin-gold nano cluster, obtained gold nano cluster material aqueous solution is rufous, and uv-vis spectra is 520
Without absworption peak at nm, strong rose fluorescence, maximum excitation wavelength and launch wavelength are produced under 365 nm ultra violet lamps
Respectively 405 nm and 650 nm.
2. 1-H-1,2,4- triazoles -3- mercaptan-bovine serum albumin(BSA)-gold nano cluster fluorescence according to claim 1
The preparation method of material, it is characterized in that using bovine serum albumin(BSA) as stabilizer, 1-H-1,2,4- triazole -3- mercaptan are reduction
Agent and the formation of dressing agent control gold nano cluster.
3. 1-H-1,2,4- triazoles -3- mercaptan-bovine serum albumin(BSA)-gold nano cluster fluorescence according to claim 1
The preparation method of material, it is characterized in that gold nano cluster average grain diameter is 2 nm.
4. 1-H-1,2,4- triazoles -3- mercaptan-bovine serum albumin(BSA)-gold nano cluster fluorescence according to claim 1
The preparation method of material, occurs, fluorescence intensity and maximum it is characterized in that aqueous solution is placed 2 months under 4 DEG C of dark places without sediment
Emission peak positions remain unchanged.
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| CN105860959B (en) * | 2016-04-16 | 2018-05-18 | 福建医科大学 | Arginine/6- azepines -2- thio-thymines-gold nano cluster and preparation method thereof |
| CN105860963B (en) * | 2016-04-16 | 2018-06-22 | 福建医科大学 | Guanidine hydrochloride/6- azepines -2- thio-thymines-gold nano cluster and preparation method thereof |
| CN105689735B (en) * | 2016-04-20 | 2017-10-17 | 中国科学院新疆理化技术研究所 | A kind of preparation method and application of the gold nanoclusters of fluorescence and size adjustable |
| CN106353290B (en) * | 2016-09-28 | 2019-03-26 | 西华师范大学 | The fluorescence gold nanoclusters synthetic method and lemon yellow measuring method of triazole package |
| CN106984827B (en) * | 2017-03-08 | 2019-08-16 | 吉林大学 | It is a kind of using dithiothreitol (DTT) synthesis gold nano-material, preparation method and application |
| CN110079299B (en) * | 2019-05-08 | 2022-01-04 | 桂林理工大学 | Preparation method of sulfur quantum dot coated bovine serum albumin fluorescent composite nanospheres |
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