CN108414486A - A kind of preparation method and application of water soluble fluorescence palladium nanocluster - Google Patents
A kind of preparation method and application of water soluble fluorescence palladium nanocluster Download PDFInfo
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Abstract
The invention discloses a kind of preparation method and applications of water soluble fluorescence palladium nanocluster, this method is metal precursor using tetrachloro-palladium acid ammonium, methionine is stabilizer, and ascorbic acid is reducing agent, passes through water-soluble palladium nanocluster of the water bath heating synthesis with blue-green fluorescent.Stabilizer used in the present invention, reducing agent are the indispensable nutrient of human body, and nontoxic, environmentally protective, preparation condition is mild, easy to control.The fluorescence palladium nanocluster of the present invention has that size is small, distribution is uniform, has good stability, the characteristic that strong antijamming capability, surface topography are consistent, the fluorescence palladium nanocluster has excellent capabilities of fluorescence detection, it is very sensitive to the hemoglobin of low concentration, it can be in 0.25~3.5 μm of ol/L to its linear response, reach 50 μM by detection limit known to three times signal-to-noise ratio computation, there is potential application prospect in biomolecule detection field.
Description
Technical field
The invention belongs to technical field of nano material, and in particular to a kind of preparation method of water soluble fluorescence palladium nanocluster
And water soluble fluorescence palladium nanocluster is in the application in fluoroscopic examination field.
Background technology
Metal nanometer cluster is one kind by several novel fluorescence nano materials formed to hundreds of metallic atoms, size
Close to Fermi's wavelength of electronics, specific energy level separation can be generated, and emit fluorescence under the excitation of certain wavelength light, had
There are some to be similar to the property of molecule, also have the feature that nano material often has, but is not the simple linear of the two property
Interpolation or extension.Compared to fluorescent nano probes such as organic dye molecule, fluorescin, nano particle, semiconductor-quantum-points
Speech, metal nanometer cluster show the properties such as different physics, optics, electricity due to its unique electronic structure, it are made to receive
It is concerned in rice investigation of materials.Various metal nanometer clusters are synthesized by changing ligand or biological support, in biochemical sensitive, life
The fields such as substance markers, fluorescence imaging, catalysis and unimolecule photoelectric device have a wide range of applications.
Super-small (grain size is less than 2nm) preparation of luminescent metal cluster is always a very attractive research class
Topic.Researchers prepare gold nano cluster and silver with different IPs size under conditions of different ligands and reducing agent,
Copper, platinum nanoclusters, and ripe is gradually tended to the research of such nanocluster, and about the synthesis of fluorescence palladium nanocluster and
Property Quality Research report it is relatively fewer.And the preparation of traditional palladium nanocluster has qualitatively difficult a, organic reagent used
With certain toxicity, there is different degrees of stimulation to human eye, skin and respiratory tract.
Invention content
In view of the deficienciess of the prior art, that the technical problem to be solved in the present invention is to provide a kind of preparation conditions is mild,
Easily-controlled operation, the preparation method of environmentally protective water soluble fluorescence palladium nanocluster and water soluble fluorescence palladium nanocluster
Application in fluoroscopic examination field.
To achieve the goals above, the present invention is to realize by the following technical solutions：A kind of water soluble fluorescence palladium is received
Rice cluster preparation method, includes the following steps：
A. tetrachloro-palladium acid ammonium-methionine solution is prepared；
B. it is added sodium hydroxide solution into step a acquired solutions, mixing is to get to metal-stabilizer under water bath condition
The mixed solution of compound；
C. it is added reducing agent in step b acquired solutions, continues water-bath to get to fluorescence palladium nanocluster；
Preferably, the preparation method of tetrachloro-palladium acid ammonium-methionine solution described in step a is：By tetrachloro-palladium acid ammonium salt solution
It is uniformly mixed with methionine solution；
It is furthermore preferred that a concentration of 2.5mmol/L of tetrachloro-palladium acid ammonium salt solution in step a, dosage 12mL；Methionine solution
A concentration of 0.06~0.14mol/L, dosage 24mL；
Preferably, in step b sodium hydrate aqueous solution a concentration of 0.4~0.8mol/L；
It is furthermore preferred that in the step b sodium hydrate aqueous solution a concentration of 0.6mol/L, dosage 3.6mL；
Preferably, the time that water-bath described in step b mixes is 30min, and temperature is 40~70 DEG C；
Preferably, reducing agent described in step c is ascorbic acid, a concentration of 0~0.2mol/L；
It is furthermore preferred that in the step c ascorbic acid a concentration of 0.14mol/L, dosage 9mL；
Preferably, in step c, water-bath temperature is 40~70 DEG C, and the time is 4~10h.
Further, the water soluble fluorescence palladium nanocluster that prepared by the present invention is in fluoroscopic examination low concentration hemoglobin
Using.
Benefit of the present invention
The present invention is used as metal precursor using water-soluble good tetrachloro-palladium acid ammonium, low using toxicity, with good
The formic acid propylhomoserin of good biocompatibility is stabilizer, uses more mild, environmental protection ascorbic acid for reducing agent.
Preparation process of the present invention is simple, easy to control.
Water soluble fluorescence Metal Palladium nanocluster size produced by the present invention is small, distribution is uniform, can be in 365nm ultraviolet lamps
Under send out blue-green fluorescent, quantum yield is about 5.47%.
Palladium nanocluster size distribution produced by the present invention is uniform, and stability is good.
Palladium nanocluster strong antijamming capability produced by the present invention, possesses excellent capabilities of fluorescence detection, to biomolecule
The hemoglobin of low concentration is very sensitive, it is made to be had potential application in biomolecule detection field.
Description of the drawings
Fig. 1 is the fluorescence excitation spectrum and emission spectra of the embodiment of the present invention 5；
Fig. 2 is the high-resolution-ration transmission electric-lens figure of the embodiment of the present invention 5；
Fig. 3 is the atomic force microscopy diagram of the embodiment of the present invention 5；
Fig. 4 is response of the palladium nanocluster fluorescent emission intensity of the embodiment of the present invention 10 to various concentration hemoglobin
Figure；
Fig. 5 is linear response section of the palladium nanocluster fluorescent emission intensity to hemoglobin of the embodiment of the present invention 10
Fitted figure.
Specific implementation mode
Following embodiment is only being expanded on further and illustrate to the present invention, rather than limiting the scope of the invention.Under
Face is further elaborated on the present invention with reference to embodiment, it should be appreciated to those skilled in the art that the present invention is not limited to this
A little embodiments and the preparation method used.Moreover, those skilled in the art's description according to the present invention can to the present invention into
Row equivalent replacement, combination, improvement or modification, but these are intended to be included in the scope of the present invention
Embodiment 1
Figure is please referred to, the present invention provides a kind of technical solution：A kind of preparation method of water soluble fluorescence palladium nanocluster,
It is characterized in that, preparation method includes the following steps：
A. by 12mL, the tetrachloro-palladium acid ammonium salt solution and 24mL of 2.5mmol/L, the methionine solution mixing of 0.07mol/L
Uniformly；
B. 3.6mL, 0.4mol/L sodium hydroxide solutions, under 40 DEG C of water bath condition are added into step a acquired solutions
Mix 30min, you can obtain the mixed solution of metal-stabilizer compound；
C. 9mL distilled water is added in step b acquired solutions, continuation reacts 8h in 40 DEG C of water-baths, obtains achromaticity and clarification
Solution.
Embodiment 2
A. by 12mL, the tetrachloro-palladium acid ammonium salt solution and 24mL of 2.5mmol/L, the methionine solution mixing of 0.07mol/L
Uniformly；
B. 3.6mL, 0.4mol/L sodium hydroxide solutions, under 40 DEG C of water bath condition are added into step a acquired solutions
Mix 30min, you can obtain the mixed solution of metal-stabilizer compound；
C. 9mL is added in step b acquired solutions, 0.14mol/L ascorbic acid reducing agents continue anti-in 40 DEG C of water-baths
8h is answered, the clear water soluble fluorescence palladium nanocluster of yellow is obtained.
Embodiment 3
A. by 12mL, the tetrachloro-palladium acid ammonium salt solution and 24mL of 2.5mmol/L, the methionine solution mixing of 0.07mol/L
Uniformly；
B. 3.6mL, 0.4mol/L sodium hydroxide solutions, under 40 DEG C of water bath condition are added into step a acquired solutions
Mix 30min, you can obtain the mixed solution of metal-stabilizer compound；
C. 9mL is added in step b acquired solutions, 0.2mol/L ascorbic acid reducing agents continue anti-in 40 DEG C of water-baths
8h is answered, the clear water soluble fluorescence palladium nanocluster of yellow is obtained.
Embodiment 4
A. by 12mL, the methionine solution mixing of the tetrachloro-palladium acid ammonium salt solution and 24mL of 2.5mmol/L, 0.1mol/L is equal
It is even；
B. 3.6mL, 0.6mol/L sodium hydroxide solutions, under 60 DEG C of water bath condition are added into step a acquired solutions
Mix 30min, you can obtain the mixed solution of metal-stabilizer compound；
C. 9mL distilled water is added in step b acquired solutions, continuation is reacted 5.5h in 60 DEG C of water-baths, obtained colourless clear
Clear solution.
Embodiment 5
A. by 12mL, the methionine solution mixing of the tetrachloro-palladium acid ammonium salt solution and 24mL of 2.5mmol/L, 0.1mol/L is equal
It is even；
B. 3.6mL, 0.6mol/L sodium hydroxide solutions, under 60 DEG C of water bath condition are added into step a acquired solutions
Mix 30min, you can obtain the mixed solution of metal-stabilizer compound；
C. 9mL is added in step b acquired solutions, 0.14mol/L ascorbic acid reducing agents continue anti-in 60 DEG C of water-baths
5.5h is answered, the clear water soluble fluorescence palladium nanocluster of yellow is obtained.
Fluorescence excitation spectrum and emission spectra test are carried out to water soluble fluorescence palladium nanocluster obtained by the present embodiment, as a result as schemed
Shown in 1.
As shown in Figure 1, the excitation peak of palladium nanocluster is located at 420nm or so, and emission peak is located at 500nm or so, thus demonstrate,proves
Bright, transmitting is blue-green fluorescent and Stokes shift is only 80nm, in metal nanometer cluster, is less than this of 150nm
The luminescence generated by light of lentor displacement generally results from the band-to-band transition of electronics, according to formulaPalladium can be calculated
The quantum yield of nanocluster is about 5.47%.
Wherein A is the absorbance in excitation wave strong point metal cluster；
ArFor in the absorbance of excitation wave strong point reference substance；
I is the integrated fluorescence intensities of metal cluster；
IrFor the integrated fluorescence intensities of reference substance；
N is the solvent refractive index of metal cluster；
nrFor the solvent refractive index of reference substance；
Q is the photoluminescence quantum yield of metal cluster；
QrFor the photoluminescence quantum yield of reference substance；
The reference substance of the present invention is Rhodamine 101.
High-resolution-ration transmission electric-lens test is carried out to the water soluble fluorescence palladium nanocluster obtained by the present embodiment, as a result such as Fig. 2
It is shown.
As shown in Figure 2, the water soluble fluorescence palladium nanocluster grain size that prepared by the present invention is small and is evenly distributed, and average diameter is about
For 1.91nm, random spherical shape is showed, apparent clustering phenomena does not occur.Thus it proves, fluorescence palladium of the invention is received
Rice cluster has good dispersion performance.
Atomic force microscope test equally is carried out to the present embodiment, the results are shown in Figure 3.
From the figure 3, it may be seen that water soluble fluorescence palladium nanocluster typical case's Terrain Elevation is less than 2.5nm, and it is evenly distributed, thus demonstrate,proves
Bright, the present invention has successfully prepared the fluorescence palladium nanocluster of super-small.
Embodiment 6
A. by 12mL, the methionine solution mixing of the tetrachloro-palladium acid ammonium salt solution and 24mL of 2.5mmol/L, 0.1mol/L is equal
It is even；
B. 3.6mL, 0.6mol/L sodium hydroxide solutions, under 70 DEG C of water bath condition are added into step a acquired solutions
Mix 30min, you can obtain the mixed solution of metal-stabilizer compound；
C. 9mL is added in step b acquired solutions, 0.2mol/L ascorbic acid reducing agents continue anti-in 70 DEG C of water-baths
4.5h is answered, the clear water soluble fluorescence palladium nanocluster of yellow is obtained.
Embodiment 7
A. by 12mL, the tetrachloro-palladium acid ammonium salt solution and 24mL of 2.5mmol/L, the methionine solution mixing of 0.12mol/L
Uniformly；
B. 3.6mL, 0.8mol/L sodium hydroxide solutions, under 70 DEG C of water bath condition are added into step a acquired solutions
Mix 30min, you can obtain the mixed solution of metal-stabilizer compound；
C. 9mL distilled water is added in step b acquired solutions, continuation is reacted 4.5h in 70 DEG C of water-baths, obtained colourless clear
Clear solution.
Embodiment 8
A. by 12mL, the tetrachloro-palladium acid ammonium salt solution and 24mL of 2.5mmol/L, the methionine solution mixing of 0.12mol/L
Uniformly；
B. 3.6mL, 0.8mol/L sodium hydroxide solutions, under 70 DEG C of water bath condition are added into step a acquired solutions
Mix 30min, you can obtain the mixed solution of metal-stabilizer compound；
C. 9mL is added in step b acquired solutions, 0.14mol/L ascorbic acid reducing agents continue anti-in 70 DEG C of water-baths
4.5h is answered, the clear water soluble fluorescence palladium nanocluster of yellow is obtained.
Embodiment 9
A. by 12mL, the tetrachloro-palladium acid ammonium salt solution and 24mL of 2.5mmol/L, the methionine solution mixing of 0.12mol/L
Uniformly；
B. 3.6mL, 0.8mol/L sodium hydroxide solutions, under 70 DEG C of water bath condition are added into step a acquired solutions
Mix 30min, you can obtain the mixed solution of metal-stabilizer compound；
C. 9mL is added in step b acquired solutions, 0.2mol/L ascorbic acid reducing agents continue anti-in 70 DEG C of water-baths
4.5h is answered, the clear water soluble fluorescence palladium nanocluster of yellow is obtained.
Embodiment 10
The haemoglobin aqueous solution of one group of various concentration is prepared respectively, prepares solution concentration range in 0.1~200 μm of ol/L
Between
The palladium nanocluster for taking one group of 1.9mL institutes the present embodiment 5 to prepare, the hemoglobin for being separately added into various concentration are water-soluble
100 μ L of liquid test response of the palladium nanocluster fluorescent emission intensity to various concentration hemoglobin, as a result such as by fluorescence spectrum
Shown in Fig. 4；And it finds the fluorescent emission intensity of palladium nanocluster there are linear response section, warps with the concentration that is added hemoglobin
Fitting, the results are shown in Figure 5.
As shown in Figure 4, the fluorescent emission intensity of gradually increasing with hemoglobin concentration, palladium nanocluster gradually subtracts
It is weak.Thus illustrate, fluorescence palladium nanocluster of the invention possesses excellent capabilities of fluorescence detection, to the hemoglobin ten of low concentration
Divide sensitivity, may be used as the fluorescence probe of detection hemoglobin.
As shown in Figure 5, when testing result shows that the concentration range of hemoglobin is 0.25~3.5 μm of ol/L, fluorescence palladium is received
The fluorescence of rice cluster reduces degree and shows certain linear relationship with hemoglobin concentration, obtained coefficient R2For
0.9915.Thus it proves, in relatively low and wider concentration range, fluorescence palladium nanocluster of the invention has hemoglobin
Good detection performance.
The above shows and describes the basic principles and main features of the present invention and the advantages of the present invention, for this field skill
For art personnel, it is clear that invention is not limited to the details of the above exemplary embodiments, and without departing substantially from the present invention spirit or
In the case of essential characteristic, the present invention can be realized in other specific forms.Therefore, in all respects, should all incite somebody to action
Embodiment regards exemplary as, and is non-limiting, the scope of the present invention by appended claims rather than on state
Bright restriction, it is intended that including all changes that come within the meaning and range of equivalency of the claims in the present invention
It is interior.Any reference signs in the claims should not be construed as limiting the involved claims.
In addition, it should be understood that although this specification is described in terms of embodiments, but not each embodiment is only wrapped
Containing an independent technical solution, this description of the specification is merely for the sake of clarity, and those skilled in the art should
It considers the specification as a whole, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art
The other embodiment being appreciated that.
Claims (10)
1. a kind of preparation method of water soluble fluorescence palladium nanocluster, which is characterized in that include the following steps：
A. tetrachloro-palladium acid ammonium-methionine solution is prepared；
B. sodium hydroxide solution is added into step a acquired solutions, mixing is to get compound to metal-stabilizer under water bath condition
The mixed solution of object；
C. it is added reducing agent in step b acquired solutions, continues water-bath to get to fluorescence palladium nanocluster.
2. the preparation method of fluorescence palladium nanocluster according to claim 1, which is characterized in that tetrachloro palladium described in step a
The preparation method of sour ammonium-methionine solution is：Tetrachloro-palladium acid ammonium salt solution is uniformly mixed with methionine solution.
3. the preparation method of fluorescence palladium nanocluster according to claim 2, which is characterized in that tetrachloro-palladium acid in step a
Ammonium salt solution a concentration of 2.5mmol/L, dosage 12mL；A concentration of 0.06~0.14mol/L of methionine solution, dosage are
24mL。
4. the preparation method of fluorescence palladium nanocluster according to claim 1, which is characterized in that sodium hydroxide in step b
A concentration of 0.4~0.8mol/L of aqueous solution.
5. the preparation method of fluorescence palladium nanocluster according to claim 4, which is characterized in that hydrogen-oxygen in the step b
Change a concentration of 0.6mol/L, dosage 3.6mL of sodium water solution.
6. the preparation method of fluorescence palladium nanocluster according to claim 1, which is characterized in that water-bath described in step b is mixed
The time of conjunction is 30min, and temperature is 40~70 DEG C.
7. the preparation method of fluorescence palladium nanocluster according to claim 1, which is characterized in that reducing agent described in step c
For ascorbic acid, wherein a concentration of 0~0.2mol/L of ascorbic acid.
8. the preparation method of fluorescence palladium nanocluster according to claim 7, which is characterized in that the ascorbic acid it is dense
Degree is 0.14mol/L, dosage 9mL.
9. the preparation method of fluorescence palladium nanocluster according to claim 1, which is characterized in that in step c, water-bath
Temperature is 40~70 DEG C, and the time is 4~10h.
10. application of the fluorescence palladium nanocluster made from claim 1~9 in fluoroscopic examination low concentration hemoglobin.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110508828A (en) * | 2019-08-28 | 2019-11-29 | 淮北师范大学 | The preparation method of fluorescent red-orange copper nanocluster based on l-methionine |
| CN110976906A (en) * | 2019-12-04 | 2020-04-10 | 山西大学 | Fluorescent palladium nanocluster and synthesis method and application thereof |
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| CN101279375A (en) * | 2008-01-16 | 2008-10-08 | 南京大学 | Preparation of Pd nano particle |
| CN103611946A (en) * | 2013-12-08 | 2014-03-05 | 福建医科大学 | Preparation method of gold nanocluster fluorescent materials protected by methionine |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110508828A (en) * | 2019-08-28 | 2019-11-29 | 淮北师范大学 | The preparation method of fluorescent red-orange copper nanocluster based on l-methionine |
| CN110976906A (en) * | 2019-12-04 | 2020-04-10 | 山西大学 | Fluorescent palladium nanocluster and synthesis method and application thereof |
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Application publication date: 20180817 |