CN105328203A - 1-H-1,2,4-triazole-3-thiol-bovine serum albumin-gold nanocluster fluorescent material and preparation method thereof - Google Patents
1-H-1,2,4-triazole-3-thiol-bovine serum albumin-gold nanocluster fluorescent material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a 1-H-1,2,4-triazole-3-thiol-bovine serum albumin-gold nanocluster fluorescent material and a preparation method thereof. Chloroauric acid, 1-H-1,2,4-triazole-3-thiol and bovine serum albumin are used as raw materials, so that the water-soluble gold nanocluster fluorescent material is synthesized through one step. The preparation method of the novel gold nanocluster fluorescent material has the beneficial effects of being fast, simple and environment-friendly in preparation process. The synthesized 1-H-1,2,4-triazole-3-thiol-bovine serum albumin-gold nanocluster presents strong rose red fluorescence with the maximum transmitting wavelength being 650 nm, is large in Stokes shift (245 nm) and good in water solubility and has the beneficial effects of being higher in stability and the like.
Description
Technical field
The present invention relates to 1-H-1, the preparation method of 2,4-triazole-3-mercaptan-bovine serum albumin(BSA)-fluorescent au nanocluster material, belongs to field of nanometer technology.
Background technology
In recent years, fluorescent nano material receives much concern as the application of fluorescent marker in biology.So far, researcher have developed the fluorescent nano material of the number of different types such as semiconductor-quantum-point, dye adulterated nano particle, carbon nano dot.Fluorogold nanocluster (goldnanoclusters, AuNCs), as the novel fluorescent nano material of a class, has that photophysical property is good, specific area large, surface is easy to modify and the advantage such as photoluminescent property is adjustable.Gold nano cluster is by several stable aggregate formed to tens gold atoms, and diameter is less than 2nm usually, between the monatomic and metal of nano particle or large volume.Because its size is close to Fermi's wavelength of electronics, continuous print energy state character is split into discrete energy state, and occurs the Size dependence effect of similar molecule.Have a wide range of applications in fields such as compound test, bio-sensing and imaging, photoelectronics and nanosecond medical sciences.
The technology of preparing of fluorescent au nanocluster material mainly comprises chemical reduction method, reverse microemulsion process, template synthesis method monolayer resist technology and part etching method etc.Wherein monolayer resist technology be a kind of Simple temperature and cluster synthetic method, utilize containing the Small molecular of certain functional group as protecting group, form protective layer on cluster surface, thus stablize gold nano cluster, make it not easily reunite.In recent decades, researchers both domestic and external propose multiple diverse ways and prepare high-fluorescence quantum yield, good water solubility, gold nano cluster that glow color is adjustable.
The present invention is with gold chloride, 1-H-1, and 2,4-triazole-3-mercaptan, bovine serum albumin(BSA) are raw material one-step synthesis water-soluble gold nano cluster fluorescent material.Bovine serum albumin(BSA) is as stabilizing agent, and 1-H-1,2,4-triazole-3-mercaptan is the formation that reducing agent and dressing agent control gold nano cluster.Prepared 1-H-1,2,4-triazole-3-mercaptan-bovine serum albumin(BSA)-gold nano cluster has strong rose fluorescence, and Stokes shift is large, good water solubility.
Summary of the invention
The object of this invention is to provide a kind of 1-H-1,2,4-triazole-3-mercaptan-bovine serum albumin(BSA)-fluorescent au nanocluster material and with 1-H-1,2,4-triazole-3-mercaptan is reducing agent and dressing agent, take bovine serum albumin(BSA) as the method for stabilizing agent one-step synthesis fluorescent au nanocluster material.
To achieve these goals, the present invention by the following technical solutions: of the present invention
the preparation method of 1-H-1,2,4-triazole-3-mercaptan-bovine serum albumin(BSA)-fluorescent au nanocluster material,it is characterized in that it is made up of following steps: bovine serum albumin solution mixes with chlorauric acid solution, then 1-H-1 is added, 2,4-triazole-3-thiol solution, jolting mixes, and reaction certain hour obtains 1-H-1,2,4-triazole-3-mercaptan-bovine serum albumin(BSA)-gold nano cluster, can obtain fluorescent au nanocluster material powder after the freeze drying of the fluorescent au nanocluster material aqueous solution.
Described
the preparation method of 1-H-1,2,4-triazole-3-mercaptan-bovine serum albumin(BSA)-fluorescent au nanocluster material,it is characterized in that using bovine serum albumin(BSA) as stabilizing agent, 1-H-1,2,4-triazole-3-mercaptan is the formation that reducing agent and dressing agent control gold nano cluster.
Described chlorauric acid solution, bovine serum albumin solution and 1-H-1, the volume ratio of 2,4-triazole-3-thiol solution is 5:3:2.
The concentration of chlorauric acid solution used can be 1 ~ 100mmol/L, most preferable concentrations is 10mmol/L, bovine serum albumin solution can be 5 ~ 500mg/mL, most preferable concentrations is 50mg/mL, the concentration of 1-H-1,2,4-triazole-3-thiol solution can be 0.01 ~ 1mol/L, most preferable concentrations is 0.1mol/L, is wherein dissolved with the NaOH that most preferable concentrations is 0.1mol/L.
Described chlorauric acid solution, bovine serum albumin solution and 1-H-1, the mixing of 2,4-triazole-3-thiol solution is placed on 4 DEG C of reactions 0.5 ~ 2 hour, most preferably 1h.
Obtained gold nano cluster material water solution is colourless, uv-vis spectra at 520nm place without absworption peak.Under ultra violet lamp, produce strong rose fluorescence, maximum excitation wavelength and emission wavelength are respectively 405nm and 650nm.
The preparation method of the fluorescent au nanocluster material of the best of the present invention is as follows:
The all glasswares used in following process all soak through chloroazotic acid, and thoroughly clean with distilled water, dry.Being prepared as follows of fluorescent au nanocluster material: 0.75mL concentration is that the chlorauric acid solution that bovine serum albumin(BSA) and the 1.25mL concentration of 50mg/mL is 10mmol/L mixes, add the 1-H-1 that 0.5mL concentration is 0.1mol/L, 2,4-triazole-3-thiol solution (containing 0.1mol/L NaOH), jolting mixes, and reacts 1h, obtain 1-H-1 at 4 DEG C, 2,4-triazole-3-mercaptan-bovine serum albumin(BSA)-gold nano cluster.The gold nano cluster of gained is the liquid of rufous, and uviol lamp (365nm) has strong rose fluorescence under irradiating.
The above-mentioned preparation method of the present invention obtains
1-H-1,2,4-triazole-3-mercaptan-bovine serum albumin(BSA)-gold nano cluster,it is characterized in that soluble in water, the aqueous solution is rufous, and under ultra violet lamp, produce strong rose fluorescence, maximum excitation wavelength and emission wavelength are respectively 405nm and 650nm.
Described gold nano cluster average grain diameter is 2nm.
Described
1-H-1,2,4-triazole-3-mercaptan-bovine serum albumin(BSA)-gold nano cluster,it is characterized in that the aqueous solution is placed under 4 DEG C of dark places to occur without precipitum for 2 months, fluorescence intensity and emission maximum peak position remain unchanged.
Described
1-H-1,2,4-triazole-3-mercaptan-bovine serum albumin(BSA)-gold nano cluster,it is characterized in that taking gold chloride as Jin Yuan, 1-H-1,2,4-triazole-3-mercaptan is reducing agent and dressing agent, and bovine serum albumin(BSA) is stabilizing agent preparation.
advantage of the present invention:
(1) the present invention is with 1-H-1, and 2,4-triazole-3-mercaptan is reducing agent and dressing agent, in next step synthesizing water-solubility fluorescent au nanocluster material of bovine serum albumin(BSA) existent condition, has and prepares advantage that is quick, simple, environmental protection.
(2) gold nano cluster prepared by the present invention has strong rose fluorescence (maximum emission wavelength is 650nm), the features such as larger Stokes shift (245nm).
Accompanying drawing explanation
Fig. 1 is gold nano cluster fluorescent nano material outside drawing of (B) under visible ray (A) and uviol lamp.
Fig. 2 is the uv-visible absorption spectra figure 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 spectrogram 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 energy spectrogram of gold nano cluster fluorescent nano material.
Detailed description of the invention
example 1:
0.75mL concentration is that the chlorauric acid solution that bovine serum albumin(BSA) and the 1.25mL concentration of 50mg/mL is 10mmol/L mixes, add the 1-H-1 that 0.5mL concentration is 0.1mol/L, 2,4-triazole-3-thiol solution (containing 0.1mol/L NaOH), jolting mixes, and reacts 1h, obtain 1-H-1 at 4 DEG C, 2,4-triazole-3-mercaptan-bovine serum albumin(BSA)-gold nano cluster.The gold nano cluster of gained is the liquid (see Figure 1A) of rufous, produces strong rose fluorescence (see Figure 1B) under ultra violet lamp.
example 2:
0.75mL concentration is that the chlorauric acid solution that bovine serum albumin(BSA) and the 1.25mL concentration of 50mg/mL is 10mmol/L mixes, add the 1-H-1 that 0.5mL concentration is 0.1mol/L, 2,4-triazole-3-thiol solution (containing 0.1mol/L NaOH), jolting mixes, and reacts 1h, obtain 1-H-1 at 4 DEG C, 2,4-triazole-3-mercaptan-bovine serum albumin(BSA)-gold nano cluster.The gold nano cluster solution obtained carries out ultraviolet-visible spectrum scanning, obtains it at 520nm wavelength place without golden nanometer particle characteristic absorption peak (see figure 2).
example 3:
0.75mL concentration is that the chlorauric acid solution that bovine serum albumin(BSA) and the 1.25mL concentration of 50mg/mL is 10mmol/L mixes, add the 1-H-1 that 0.5mL concentration is 0.1mol/L, 2,4-triazole-3-thiol solution (containing 0.1mol/L NaOH), jolting mixes, and reacts 1h, obtain 1-H-1 at 4 DEG C, 2,4-triazole-3-mercaptan-bovine serum albumin(BSA)-gold nano cluster.The gold nano cluster solution obtained carries out fluorescence spectrum scanning, obtains its maximum excitation wavelength and emission wavelength and is respectively 405nm and 650nm(and sees Fig. 3).
example 4:
0.75mL concentration is that the chlorauric acid solution that bovine serum albumin(BSA) and the 1.25mL concentration of 50mg/mL is 10mmol/L mixes, add the 1-H-1 that 0.5mL concentration is 0.1mol/L, 2,4-triazole-3-thiol solution (containing 0.1mol/L NaOH), jolting mixes, and reacts 1h, obtain 1-H-1 at 4 DEG C, 2,4-triazole-3-mercaptan-bovine serum albumin(BSA)-gold nano cluster.The gold nano cluster solution obtained drips and is coated on copper mesh.Energy Dispersive X energy spectrum analysis (see figure 4) shows that product contains gold element.
example 5:
0.75mL concentration is that the chlorauric acid solution that bovine serum albumin(BSA) and the 1.25mL concentration of 50mg/mL is 10mmol/L mixes, add the 1-H-1 that 0.5mL concentration is 0.1mol/L, 2,4-triazole-3-thiol solution (containing 0.1mol/L NaOH), jolting mixes, and reacts 1h, obtain 1-H-1 at 4 DEG C, 2,4-triazole-3-mercaptan-bovine serum albumin(BSA)-gold nano cluster.The gold nano cluster solution obtained carries out the mensuration of transmission electron microscope, and the average grain diameter recording gold nano cluster is that 2nm(is shown in Fig. 5).
example 6:
0.75mL concentration is that the chlorauric acid solution that bovine serum albumin(BSA) and the 1.25mL concentration of 50mg/mL is 10mmol/L mixes, add the 1-H-1 that 0.5mL concentration is 0.1mol/L, 2,4-triazole-3-thiol solution (containing 0.1mol/L NaOH), jolting mixes, and reacts 1h, obtain 1-H-1 at 4 DEG C, 2,4-triazole-3-mercaptan-bovine serum albumin(BSA)-gold nano cluster.Obtain powder after the gold nano cluster solution freeze drying obtained, get gained powder and carry out x-ray photoelectron power spectrum mensuration, the 4f of XPSAu (4f) display gold
7/2peak and 4f
5/2peak lays respectively at 84.5eV and 88.2eV, to show in gold nano cluster that the valence state of gold to coexist (see figure 6) with 0 valency and+1 valency mode.
Claims (10)
1. one kind
the preparation method of 1-H-1,2,4-triazole-3-mercaptan-bovine serum albumin(BSA)-fluorescent au nanocluster material,it is characterized in that it is made up of following steps: bovine serum albumin solution mixes with chlorauric acid solution, then 1-H-1 is added, 2,4-triazole-3-thiol solution, jolting mixes, and reaction certain hour obtains 1-H-1,2,4-triazole-3-mercaptan-bovine serum albumin(BSA)-gold nano cluster, can obtain fluorescent au nanocluster material powder after the freeze drying of the fluorescent au nanocluster material aqueous solution.
2. according to claim 1
the preparation method of 1-H-1,2,4-triazole-3-mercaptan-bovine serum albumin(BSA)-fluorescent au nanocluster material,it is characterized in that using bovine serum albumin(BSA) as stabilizing agent, 1-H-1,2,4-triazole-3-mercaptan is the formation that reducing agent and dressing agent control gold nano cluster.
3. according to claim 1
the preparation method of 1-H-1,2,4-triazole-3-mercaptan-bovine serum albumin(BSA)-fluorescent au nanocluster material,it is characterized in that chlorauric acid solution, bovine serum albumin solution and 1-H-1, the volume ratio of 2,4-triazole-3-thiol solution is 5:3:2.
4. according to claim 1 or 3
the preparation method of 1-H-1,2,4-triazole-3-mercaptan-bovine serum albumin(BSA)-fluorescent au nanocluster material,it is characterized in that the concentration of chlorauric acid solution used is 10mmol/L, bovine serum albumin solution is 50mg/mL, 1-H-1, and the concentration of 2,4-triazole-3-thiol solution is 0.1mol/L, is wherein dissolved with 0.1mol/L NaOH.
5. according to claim 1 or 3
the preparation method of 1-H-1,2,4-triazole-3-mercaptan-bovine serum albumin(BSA)-fluorescent au nanocluster material,it is characterized in that chlorauric acid solution, bovine serum albumin solution and 1-H-1, the mixing of 2,4-triazole-3-thiol solution is placed on 4 DEG C of reaction 1h.
6. according to claim 1 or 3
the preparation method of 1-H-1,2,4-triazole-3-mercaptan-bovine serum albumin(BSA)-fluorescent au nanocluster material,it is characterized in that the chlorauric acid solution that 0.75mL concentration be bovine serum albumin(BSA) and the 1.25mL concentration of 50mg/mL is 10mmol/L mixes, add the 1-H-1 wherein containing 0.1mol/L NaOH that 0.5mL concentration is 0.1mol/L, 2, 4-triazole-3-thiol solution, jolting mixes, react at 4 DEG C, obtain 1-H-1, 2, 4-triazole-3-mercaptan-bovine serum albumin(BSA)-gold nano cluster, obtained gold nano cluster material water solution is colourless, uv-vis spectra at 520nm place without absworption peak, strong rose fluorescence is produced under 365nm ultra violet lamp, maximum excitation wavelength and emission wavelength are respectively 405nm and 650nm.
7. the arbitrary described preparation method of claim 1-6 obtains
1-H-1,2,4-triazole-3-mercaptan-bovine serum albumin(BSA)-gold nano cluster,it is characterized in that soluble in water, the aqueous solution is rufous, and under ultra violet lamp, produce strong rose fluorescence, maximum excitation wavelength and emission wavelength are respectively 405nm and 650nm.
8. according to claim 7
1-H-1,2,4-triazole-3-mercaptan-bovine serum albumin(BSA)-gold nano cluster,it is characterized in that gold nano cluster average grain diameter is 2nm.
9. according to claim 7 or 8
1-H-1,2,4-triazole-3-mercaptan-bovine serum albumin(BSA)-gold nano cluster,it is characterized in that the aqueous solution is placed under 4 DEG C of dark places to occur without precipitum for 2 months, fluorescence intensity and emission maximum peak position remain unchanged.
10. according to claim 7 or 8
1-H-1,2,4-triazole-3-mercaptan-bovine serum albumin(BSA)-gold nano cluster,it is characterized in that taking gold chloride as Jin Yuan, 1-H-1,2,4-triazole-3-mercaptan is reducing agent and dressing agent, and bovine serum albumin(BSA) is stabilizing agent preparation.
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| CN105860963A (en) * | 2016-04-16 | 2016-08-17 | 福建医科大学 | Guanidine hydrochloride/6-aza-2-sulfo-thymine-gold nano cluster and preparation method thereof |
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| CN106353290A (en) * | 2016-09-28 | 2017-01-25 | 西华师范大学 | Synthesis method of fluorescent gold nanocluster coated with triazole and lemon yellow detection method |
| CN106984827A (en) * | 2017-03-08 | 2017-07-28 | 吉林大学 | A kind of gold nano-material of utilization dithiothreitol (DTT) synthesis, preparation method and application |
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| CN105860963A (en) * | 2016-04-16 | 2016-08-17 | 福建医科大学 | Guanidine hydrochloride/6-aza-2-sulfo-thymine-gold nano cluster and preparation method thereof |
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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 |
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| CN106353290A (en) * | 2016-09-28 | 2017-01-25 | 西华师范大学 | Synthesis method of fluorescent gold nanocluster coated with triazole and lemon yellow detection method |
| 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 |
| CN106984827A (en) * | 2017-03-08 | 2017-07-28 | 吉林大学 | A kind of gold nano-material of utilization dithiothreitol (DTT) synthesis, preparation method and application |
| 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 |
| CN110079299A (en) * | 2019-05-08 | 2019-08-02 | 桂林理工大学 | The preparation method of the bovine serum albumin(BSA) fluorescence composite Nano ball of sulphur quantum dot cladding |
| 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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