CN104227013A - N-acetyl-L-cysteine-gold nanocluster fluorescent material and preparation method thereof - Google Patents
N-acetyl-L-cysteine-gold nanocluster fluorescent material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an N-acetyl-L-cysteine-gold nanocluster fluorescent material and a preparation method thereof. According to the N-acetyl-L-cysteine-gold nanocluster fluorescent material and the preparation method thereof, the gold nanocluster fluorescent material is synthesized in situ by taking N-acetyl-L-cysteine as a template, and the formation of a gold nanocluster is controlled by taking the N-acetyl-L-cysteine as a stabilizing agent and reducing agent. The invention relates to the preparation method for the novel gold nanocluster fluorescent material, and the preparation method has the advantages that preparation is simple and environmentally friendly, and the reducing agent is not needed; the prepared gold nanocluster has the characteristics of being strong in red fluorescence (the maximum emission wavelength is 650nm), long in fluorescence lifetime (765ns), high in stability (time, light, salt and oxidation stability) and larger in Stokes shift (300nm) and the like.
Description
Technical field
The present invention relates to N-acetyl-L-cysteine-fluorescent au nanocluster material and preparation method thereof, belong to field of nanometer technology.
Background technology
In recent years, fluorescence metal nanocluster receives much concern as a kind of novel fluorescent nano material.Metal nanometer cluster refers under certain molecular layer protective effect, by several molecule level aggregation formed to a hundreds of metallic atom.Due to the physics of its uniqueness, electricity and optical property, metal nanometer cluster demonstrates application prospect widely in unimolecule photoelectricity, catalysis, bio-imaging and sensor field.In all metal nanometer cluster materials, gold nano cluster (gold nanoclusters, AuNCs) has the advantage such as stable chemical nature and good biocompatibility because of it, is a kind of metal nanometer cluster material of current most study.Advantages such as comparing with fluorescin with small molecule fluorescent dyestuff, AuNCs is used as fluorescence probe and has that good water solubility, specific area are large, surface is easy to modify, anti-light bleaching power is strong and photoluminescent property is adjustable.Therefore, gold nano cluster is expected to the deficiency making up some poisonous small molecule fluorescent dyestuffs, even can replace the conventional fluorescent probe of some photostability difference.The synthetic route of fluorescent au nanocluster material is mainly divided into " from bottom to top " (bottom-up) and " from top to bottom " (top-down) two type.For the synthetic method of " from bottom to top ", gold ion (Au
3+or Au
+) being reduced to gold atom, then accumulation forms certain cluster.In contrast, for the synthetic method of " from top to bottom ", gold nano cluster etches the atom on larger golden nanometer particle surface by using suitable stabilizing agent to go and produce.
The present invention, without under the condition of adding any other reducing agent, take N-acetyl-L-cysteine as template fabricated in situ fluorescent au nanocluster material.N-acetyl-L-cysteine controls the formation of gold nano cluster as stabilizing agent and reducing agent.
Summary of the invention
The object of this invention is to provide one
n-acetyl-L-cysteine-fluorescent au nanocluster material andwithout under the condition of adding any other reducing agent, take N-acetyl-L-cysteine as template fabricated in situ fluorescent au nanocluster material
method.
To achieve these goals, the present invention is by the following technical solutions:
the preparation method of the fluorescent au nanocluster material of N-acetyl-L-cysteine protection of the present inventionit is characterized in that being made up of following reactions steps: it is in the chlorauric acid solution of 0.01 ~ 0.1 g/L that the sodium hydroxide solution of to be the N-acetyl-L-cysteine solution of 0.02 ~ 0.18 mol/L and concentration by concentration be 0.1 ~ 0.8 mol/L joins concentration, mixing, be placed in 20 ~ 70 ° of C constant temperature water bath reactions 0 ~ 3.5 hour, reaction terminate rear molecular cut off be 3500 bag filter dialysis purification process is carried out to reactant liquor, obtain the fluorescent au nanocluster material aqueous solution, after the freeze drying of the fluorescent au nanocluster material aqueous solution, fluorescent au nanocluster material powder can be obtained.
The present invention does not add any other reducing agent, and N-acetyl-L-cysteine controls the formation of gold nano cluster as stabilizing agent and reducing agent.
The volume ratio of described chlorauric acid solution, N-acetyl-L-cysteine solution and sodium hydroxide solution is 2:20:3, and three's cumulative volume is 5 mL.
The concentration of the chlorauric acid solution that step is used is 0.02 g/L, volume is 0.4 mL, the concentration of N-acetyl-L-cysteine solution and sodium hydroxide solution and volume are preferably 0.08 mol/L, 4 mL and 0.5 mol/L, 0.6 mL, reaction time is preferably 2.5 hours, and reaction temperature is 37 ° of C.
The gold nano cluster aqueous solution prepared by the present invention is colourless, ultraviolet-visible spectrum, without obvious absorption peaks, produces strong red fluorescence under ultra violet lamp, and maximum excitation wavelength and emission wavelength are respectively 355 nm and 650 nm, quantum yield is 1.1%, and fluorescence lifetime is 765 ns.
The gold nano cluster aqueous solution is placed in after 4 DEG C of dark places preserve one month, and relative intensity of fluorescence remains on more than 90%.
Under the gold nano cluster aqueous solution is placed in uviol lamp, Continuous irradiation is after one hour, and relative intensity of fluorescence remains on more than 90%.
The gold nano cluster aqueous solution is placed in after 2 mol/L sodium chloride solutions hatch 30 minutes, and relative intensity of fluorescence remains on more than 95%.
The gold nano cluster aqueous solution is placed in after 2 mol/L hydrogenperoxide steam generators hatch 30 minutes, and relative intensity of fluorescence remains on more than 95%.
The preparation of the fluorescent au nanocluster material that the present invention is concrete: all glasswares used in following process all soak through chloroazotic acid, and thoroughly clean with distilled water, dry.The preparation method of fluorescent au nanocluster material is as follows: it is in the N-acetyl-L-cysteine solution of 0.08 mol/L that the chlorauric acid solution of to be the sodium hydroxide solution of 0.5 mol/L and 0.4 mL concentration by 0.6 mL concentration be 0.02 g/L joins 4 mL concentration, mixing, be placed in 37 ° of C constant temperature water bath reactions 2.5 hours, reactant liquor is become colorless by light yellow.Reaction terminate rear molecular weight be 3500 bag filter dialysis purification process is carried out to reactant liquor.
Advantage of the present invention:
(1) the present invention is without under the condition of adding any other reducing agent, take N-acetyl-L-cysteine as template fabricated in situ fluorescent au nanocluster material.Preparation method's environmental protection, simple and efficient to handle, favorable reproducibility.
(2) gold nano cluster prepared by the present invention has strong red fluorescence (maximum emission wavelength is 650 nm), long fluorescence lifetime (765 ns), the features such as high stability (time, light, salt and oxidation stability) and larger Stokes shift (~ 300 nm).
Accompanying drawing explanation
Fig. 1 is the gold nano cluster fluorescent nano material outside drawing of (B) under visible ray (A) and uviol lamp respectively.
Fig. 2 is the uv-visible absorption spectra figure of gold nano cluster fluorescent nano material.
Fig. 3 is the fluorescence spectrum figure of gold nano cluster fluorescent nano material.
Fig. 4 is the effect diagram of N-acetyl-L-cysteine concentration to gold nano cluster fluorescence intensity.
Fig. 5 is the effect diagram of naoh concentration to gold nano cluster fluorescence intensity.
Fig. 6 is the effect diagram of reaction time to gold nano cluster fluorescence intensity.
Fig. 7 is the transmission electron microscope picture of gold nano cluster fluorescent nano material.
Fig. 8 is the SEAD figure of gold nano cluster fluorescent nano material.
Fig. 9 is the Energy Dispersive X energy spectrogram of gold nano cluster fluorescent nano material.
Figure 10 is the fluorescence lifetime figure of gold nano cluster fluorescent nano material.
Figure 11 is the x-ray photoelectron energy spectrogram of gold nano cluster fluorescent nano material.In figure: A is the 4f figure of gold, B is that the 2p of sulphur schemes.
Figure 12 is the infrared absorpting light spectra of gold nano cluster fluorescent nano material.In figure: A is gold nano cluster, B is N-acetyl-L-cysteine.
Figure 13 is the time stability figure of gold nano cluster.
Figure 14 is the photostability figure of gold nano cluster.
Figure 15 is the salt-stable figure of gold nano cluster.
Figure 16 is the oxidation stability figure of gold nano cluster.
Figure 17 is the emitted luminescence intensity value (F of gold nano cluster solution
650) and solution ph between linear relationship chart.
Detailed description of the invention
example 1:
It is in the N-acetyl-L-cysteine solution of 0.08 mol/L that the chlorauric acid solution of to be the sodium hydroxide solution of 0.5 mol/L and 0.4 mL concentration by 0.6 mL concentration be 0.02 g/L joins 4 mL concentration, mixing, is placed in 37 ° of C constant temperature water bath reactions 2.5 hours.Reaction terminate after reactant liquor molecular cut off be 3500 bag filter carry out dialysis purification process.Under the gold nano cluster solution visible ray obtained be colourless (A see in Fig. 1), strong red fluorescence (B see in Fig. 1) is produced under ultra violet lamp, ultraviolet-visible spectrum is without obvious absorption peaks (see figure 2), maximum excitation wavelength and emission wavelength are respectively 355 nm and 650 nm(are shown in Fig. 3), quantum yield is 1.1%.
example 2:
The chlorauric acid solution of to be the sodium hydroxide solution of 0.5 mol/L and 0.4 mL concentration by 0.6 mL concentration be 0.02 g/L joins in the N-acetyl-L-cysteine solution (0.02 ~ 0.18 mol/L) of 4 mL variable concentrations, mixing, is placed in 37 ° of C constant temperature water bath reactions 2.5 hours.Reaction terminate rear molecular cut off be 3500 bag filter dialysis purification process is carried out to reactant liquor.As shown in Figure 4, solution is at the fluorescence intensity level (F at 650 nm places
650) reach maximum when N-acetyl-L-cysteine solution concentration is 0.08 mol/L.
example 3:
It is in the N-acetyl-L-cysteine solution of 0.08 mol/L that the chlorauric acid solution being 0.02 g/L by the sodium hydroxide solution (0.1 ~ 0.8 mol/L) of 0.6 mL variable concentrations and 0.4 mL concentration joins 4 mL concentration, mixing, is placed in 37 ° of C constant temperature water bath reactions 2.5 hours.Reaction terminate rear molecular cut off be 3500 bag filter dialysis purification process is carried out to reactant liquor.As shown in Figure 5, solution is at the fluorescence intensity level (F at 650 nm places
650) reach maximum when concentration of sodium hydroxide solution is 0.5 mol/L.
example 4:
It is in the N-acetyl-L-cysteine solution of 0.08 mol/L that the chlorauric acid solution of to be the sodium hydroxide solution of 0.5 mol/L and 0.4 mL concentration by 0.6 mL concentration be 0.02 g/L joins 4 mL concentration, mixing, is placed in 37 ° of C constant temperature water bath reactions 0 ~ 3.5 hour.Reaction terminate rear molecular cut off be 3500 bag filter dialysis purification process is carried out to reactant liquor.As shown in Figure 6, solution is at the fluorescence intensity level (F at 650 nm places
650) be 2.5 littlely reach maximum constantly in the reaction time.
example 5:
It is in the N-acetyl-L-cysteine solution of 0.08 mol/L that the chlorauric acid solution of to be the sodium hydroxide solution of 0.5 mol/L and 0.4 mL concentration by 0.6 mL concentration be 0.02 g/L joins 4 mL concentration, mixing, is placed in 37 ° of C constant temperature water bath reactions 2.5 hours.Reaction terminate rear molecular cut off be 3500 bag filter dialysis purification process is carried out to reactant liquor.Gained solution is dripped and is coated on copper mesh.Transmission electron microscope analysis (see figure 7) shows that the particle diameter of gold nano cluster is about 2.4 nm.Energy Dispersive X energy spectrum analysis (see figure 8) shows that product contains gold.Selected area electron diffraction analysis (see figure 9) shows that the gold nano cluster prepared is polycrystalline.
example 6:
It is in the N-acetyl-L-cysteine solution of 0.08 mol/L that the chlorauric acid solution of to be the sodium hydroxide solution of 0.5 mol/L and 0.4 mL concentration by 0.6 mL concentration be 0.02 g/L joins 4 mL concentration, mixing, is placed in 37 ° of C constant temperature water bath reactions 2.5 hours.Reaction terminate rear molecular cut off be 3500 bag filter dialysis purification process is carried out to reactant liquor.The solution of gained is carried out fluorescence lifetime mensuration, and the fluorescence lifetime value recording gold nano cluster is that 765 nm(are shown in Figure 10).
example 7:
It is in the N-acetyl-L-cysteine solution of 0.08 mol/L that the chlorauric acid solution of to be the sodium hydroxide solution of 0.5 mol/L and 0.4 mL concentration by 0.6 mL concentration be 0.02 g/L joins 4 mL concentration, mixing, is placed in 37 ° of C constant temperature water bath reactions 2.5 hours.Reaction terminate rear molecular cut off be 3500 bag filter dialysis purification process is carried out to reactant liquor.Powder is obtained by after the freeze drying of gained solution, get gained powder and carry out x-ray photoelectron power spectrum mensuration, go out the 4f peak of cash at 84.5 eV and 88.3 eV places, occur the 2p peak (4f being gold see the A in Figure 11 schemes, and B is the 2p figure of sulphur) of sulphur at 162.9 eV and 164.0 eV places.
example 8:
It is in the N-acetyl-L-cysteine solution of 0.08 mol/L that the chlorauric acid solution of to be the sodium hydroxide solution of 0.5 mol/L and 0.4 mL concentration by 0.6 mL concentration be 0.02 g/L joins 4 mL concentration, mixing, is placed in 37 ° of C constant temperature water bath reactions 2.5 hours.Reaction terminate rear molecular cut off be 3500 bag filter dialysis purification process is carried out to reactant liquor.Obtain powder by after the freeze drying of gained solution, get gained powder and carry out infrared absorption spectrometry, 2547 cm
-1s-H RESONANCE ABSORPTION is obviously suppressed, and shows that N-acetyl-L-cysteine molecule and gold atom close (be gold nano cluster see the A in Figure 12, B is N-acetyl-L-cysteine) by Au-S bond.
example 9:
?it is in the N-acetyl-L-cysteine solution of 0.08 mol/L that the chlorauric acid solution of to be the sodium hydroxide solution of 0.5 mol/L and 0.4 mL concentration by 0.6 mL concentration be 0.02 g/L joins 4 mL concentration, mixing, is placed in 37 ° of C constant temperature water bath reactions 2.5 hours.Reaction terminate rear molecular cut off be 3500 bag filter dialysis purification process is carried out to reactant liquor.Be placed in by gained solution after 4 DEG C of dark places preserve one month, the relative intensity of fluorescence of gold nano cluster is 90.8%(Figure 13).
example 10:
?it is in the N-acetyl-L-cysteine solution of 0.08 mol/L that the chlorauric acid solution of to be the sodium hydroxide solution of 0.5 mol/L and 0.4 mL concentration by 0.6 mL concentration be 0.02 g/L joins 4 mL concentration, mixing, is placed in 37 ° of C constant temperature water bath reactions 2.5 hours.Reaction terminate rear molecular cut off be 3500 bag filter dialysis purification process is carried out to reactant liquor.Under gained solution being placed in uviol lamp, Continuous irradiation is after one hour, and the relative intensity of fluorescence of gold nano cluster is 91%(Figure 14).
example 11:
?it is in the N-acetyl-L-cysteine solution of 0.08 mol/L that the chlorauric acid solution of to be the sodium hydroxide solution of 0.5 mol/L and 0.4 mL concentration by 0.6 mL concentration be 0.02 g/L joins 4 mL concentration, mixing, is placed in 37 ° of C constant temperature water bath reactions 2.5 hours.Reaction terminate rear molecular cut off be 3500 bag filter dialysis purification process is carried out to reactant liquor.Be placed in by gained solution after 2 mol/L sodium chloride solutions hatch 30 minutes, the relative intensity of fluorescence of gold nano cluster is 97.5%(Figure 15).
example 12:
?it is in the N-acetyl-L-cysteine solution of 0.08 mol/L that the chlorauric acid solution of to be the sodium hydroxide solution of 0.5 mol/L and 0.4 mL concentration by 0.6 mL concentration be 0.02 g/L joins 4 mL concentration, mixing, is placed in 37 ° of C constant temperature water bath reactions 2.5 hours.Reaction terminate rear molecular cut off be 3500 bag filter dialysis purification process is carried out to reactant liquor.Be placed in by gained solution after 2 mol/L hydrogenperoxide steam generators hatch 30 minutes, the relative intensity of fluorescence of gold nano cluster is 99.9%(Figure 16).
example 13:
Add in the phosphate buffer (20 mmol/L) of 0.2 milliliter of different pH value (6.05 ~ 6.4) in the gold nano cluster that 0.2 milliliter of embodiment 1 is obtained, 25 ° of C react 10 minutes, measure solution emitted luminescence intensity value F
650.As shown in figure 17, F within the scope of 6.05 ~ 6.4pH value
650linear with solution ph, linear equation is F=17.53-2.73pH, r=0.998.Be 2.3% to the relative standard deviation of the solution parallel determination 6 times of pH=6.1.As can be seen here, the present invention may be used for measuring solution ph.
Claims (9)
1. one kind
the preparation method of the fluorescent au nanocluster material of N-acetyl-L-cysteine protectionit is characterized in that being made up of following reactions steps: it is in the chlorauric acid solution of 0.01 ~ 0.1 g/L that the sodium hydroxide solution of to be the N-acetyl-L-cysteine solution of 0.02 ~ 0.18 mol/L and concentration by concentration be 0.1 ~ 0.8 mol/L joins concentration, mixing, be placed in 20 ~ 70 ° of C constant temperature water bath reactions 0 ~ 3.5 hour, reaction terminate rear molecular cut off be 3500 bag filter dialysis purification process is carried out to reactant liquor, obtain the fluorescent au nanocluster material aqueous solution, after the freeze drying of the fluorescent au nanocluster material aqueous solution, fluorescent au nanocluster material powder can be obtained.
2. according to claim 1
the preparation method of the fluorescent au nanocluster material of N-acetyl-L-cysteine protection, it is characterized in that not adding any other reducing agent, N-acetyl-L-cysteine controls the formation of gold nano cluster as stabilizing agent and reducing agent.
3. according to claim 1
the preparation method of the fluorescent au nanocluster material of N-acetyl-L-cysteine protection, it is characterized in that the volume ratio of described chlorauric acid solution, N-acetyl-L-cysteine solution and sodium hydroxide solution is 2:20:3, three's cumulative volume is 5 mL.
4. according to claim 1 or 2 or 3
the preparation method of the fluorescent au nanocluster material of N-acetyl-L-cysteine protectionit is characterized in that the concentration of chlorauric acid solution used is 0.02 g/L, volume is 0.4 mL, the concentration of N-acetyl-L-cysteine solution and sodium hydroxide solution and volume are preferably 0.08 mol/L, 4 mL and 0.5 mol/L, 0.6 mL, reaction time is preferably 2.5 hours, and reaction temperature is 37 ° of C.
5. a claim 1-4 arbitrary described method is obtained
the gold nano cluster of N-acetyl-L-cysteine protection,it is characterized in that
the gold nano cluster of N-acetyl-L-cysteine protectionthe aqueous solution is colourless, and ultraviolet-visible spectrum, without obvious absorption peaks, produces strong red fluorescence under ultra violet lamp, and maximum excitation wavelength and emission wavelength are respectively 355 nm and 650 nm, and quantum yield is 1.1%, and fluorescence lifetime is 765 ns.
6. according to claim 5
the gold nano cluster of N-acetyl-L-cysteine protection, it is characterized in that
the gold nano cluster of N-acetyl-L-cysteine protectionthe aqueous solution is placed in after 4 DEG C of dark places preserve one month, and relative intensity of fluorescence remains on more than 90%.
7. according to claim 5
the gold nano cluster of N-acetyl-L-cysteine protection, it is characterized in that
the gold nano cluster of N-acetyl-L-cysteine protectionunder the aqueous solution is placed in uviol lamp, Continuous irradiation is after one hour, and relative intensity of fluorescence remains on more than 90%.
8. according to claim 5
the gold nano cluster of N-acetyl-L-cysteine protection, it is characterized in that
the gold nano cluster of N-acetyl-L-cysteine protectionthe aqueous solution is placed in after 2 mol/L sodium chloride solutions hatch 30 minutes, and relative intensity of fluorescence remains on more than 95%.
9. according to claim 5 or 6 or 7 or 8
the gold nano cluster of N-acetyl-L-cysteine protection, it is characterized in that
the gold nano cluster of N-acetyl-L-cysteine protectionthe aqueous solution is placed in after 2 mol/L hydrogenperoxide steam generators hatch 30 minutes, and relative intensity of fluorescence remains on more than 95%.
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