CN109399627A - Quantum dot-graphene oxide composite material preparation method of DNA guidance - Google Patents
Quantum dot-graphene oxide composite material preparation method of DNA guidance Download PDFInfo
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Abstract
The present invention relates to a kind of quantum dot-graphene oxide composite material preparation methods of DNA guidance, its specifically: the DNA for crossing sulfydryl modification is added in graphene oxide solution, it is stirred at room temperature, stands 10 hours and obtain mixed solution, it is dialysed in distilled water with dialysis membrane 10 hours and removes free DNA, DNA- graphene oxide complex solution is made；Cadmium ion precursor solution and chalcogen precursor solution are added in DNA-graphene oxide complex solution, in the environment of pH is 9.0~11.0, it is heated to 50~90 DEG C, isothermal reaction obtains QDs-DNA-graphene oxide complex solution after 2~8 hours, after dehydrated alcohol washing, centrifugation, quantum dot-graphene oxide composite material of DNA guidance is made.The shortcomings that product property that the present invention successfully overcomes the prior art is unstable, complex steps, composite properties obtained are stablized.
Description
Technical field
The invention belongs to technical field of composite materials, specifically, being related to a kind of quantum dot-graphene oxide of DNA guidance
The preparation method of composite material.
Background technique
Graphene oxide is a kind of derivative of graphene, is by carbon atom with sp2Hybridized orbit composition hexangle type be in
The two-dimensional slice structure nano material of honeycomb lattice.The hydroxyl of surface random distribution, the carboxyl of epoxy group and edge distribution, carbonyl
Base makes graphene oxide thin slice that hydrophilic to hydrophobic property distribution be presented from edge to center.Meanwhile depositing because of oxygen-containing group
Graphene oxide thin slice is easier to surface-functionalized.A series of this unique feature of graphene oxide are metallic nanoparticle
The fixation and growth of son and inorganic nanoparticles, provide medium and platform.
In recent years, lot of domestic and foreign study group reports the nano material compound based on graphene and its derivative
Synthesis and application study.Cao etc., which reports to utilize, is dissolved in graphene oxide synthesis CdS QDs and graphite in dimethyl sulfoxide
The method of the compound (CdS QDs-G) of alkene (graphene)." a pot method " for the research synthesizes, and realizes graphene oxide also
Original settles synthesis with CdS QDs on the surface of graphene and carries out simultaneously, and the single-layer graphene oxide of high stability in solution
In the presence of ensure that single layer, the laminated structure of CdS QDs-G compound, so that it be made to possess excellent photoelectric properties.Tan et al.
The bracket grown using the effect of the pi-pi accumulation of dsDNA and GO and dsDNA as metal nanoparticle, proposes a kind of synthesis Ag-
The universal synthesis method of GO, Au-GO, Cu-GO, Pt-GO and Au/Cu/Pt-GO composite material.Ag-GO nanostructure is used for simultaneously
The detection of dopamine shows excellent detection performance.
Quantum dot-graphene oxide is as a kind of novel nanocomposite materials, because it combines graphene oxide specific surface
It the advantages that product is big, conductive speed is fast and quantum dot size relies on optical property and high-luminous-efficiency, in solar battery, passes
The fields such as sensor, photoelectric material have broad application prospects.However, existing hydro-thermal method, solvent-thermal method, electrochemistry etc. synthesize
Method, technique is harsh, it is cumbersome, do not have versatility.Therefore, exploitation has versatility, the simple synthetic method of synthesis technology,
Quantum dot-the graphene oxide composite material for synthesizing high quality has the research and application that push such composite material important
Meaning.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of quantum dot-graphene oxide composite material of DNA guidance
The shortcomings that preparation method, the product property for successfully overcoming the prior art is unstable, complex steps, composite properties obtained
Stablize, overcomes the shortcomings that can not determining quantum dot sites and distribution in existing synthesis technology.
The present invention is implemented as follows:
A kind of quantum dot-graphene oxide composite material preparation method of DNA guidance comprising following steps:
S1, design single stranded DNA:
For single stranded DNA since 5 ends, the P=O key in chain structure in phosphoric acid backbone is successively modified to the single stranded DNA of P=S key,
Obtain mercapto-modified single stranded DNA；
S2, preparation DNA- graphene oxide compound:
The DNA that sulfydryl modification is crossed is added in graphene oxide solution, is stirred at room temperature, stands 10 hours and mixed
Solution is closed, is dialysed in distilled water with dialysis membrane 10 hours and removes free DNA, it is molten that DNA- graphene oxide compound is made
Liquid；
S3, the quantum dot-graphene oxide composite material for preparing DNA guidance:
It is compound that DNA-graphene oxide that step S2 is obtained is added in cadmium ion precursor solution and chalcogen precursor solution
In object solution, in the environment of pH is 9.0~11.0,50~90 DEG C are heated to, isothermal reaction obtained QDs-after 2~8 hours
Quantum dot-graphene oxide of DNA guidance is made after dehydrated alcohol washing, centrifugation in DNA-graphene oxide complex solution
Composite material.
Preferably, the modification quantity of sulfydryl is 5~10 in step S1.
Preferably, the mass concentration ratio for the DNA that graphene oxide and sulfydryl modification are crossed in step S2 is 4~1:1.
Preferably, in step S3, oxygen group elements include sulphur, selenium and tellurium.
Preferably, the molar ratio of the cadmium ion precursor solution and chalcogen precursor solution is 4~1:1.
Preferably, the volume of the DNA- graphene oxide complex solution and cadmium ion and chalcogen precursor mixed solution
Than for 1:99.
Preferably, quantum dot obtained in step S3 is one of CdTe, CdSe, CdS, CdTeSe.
Compared with prior art, the invention has the following advantages:
(1) quantum dot produced by the present invention-graphene oxide composite material property is stablized, moreover, guiding quantum using DNA
The synthesis of point-graphene oxide composite material, which overcomes, can not determine lacking for quantum dot sites and distribution in existing synthesis technology
Point.
(2) raw material that the present invention uses is environmental-friendly, reaction condition is mild, need to only change the molar ratio of each material in synthesis
Rate can be obtained quantum dot-graphene oxide composite material of different-grain diameter quantum dot distribution.
(3) present invention synthesizes quantum dot-graphene oxide composite material in an aqueous medium, improves the biofacies of material
Capacitive.
Detailed description of the invention
Fig. 1 is the flow chart for quantum dot-graphene oxide composite material preparation method that DNA of the invention is guided；
Fig. 2 a is the UV-visible spectrum of CdS-GO made from embodiment 1；
Fig. 2 b is the UV-visible spectrum of CdSe-GO made from embodiment 2；
Fig. 2 c is the UV-visible spectrum of CdTe-GO made from embodiment 3；
Fig. 2 d is the UV-visible spectrum of CdTeSe-GO made from embodiment 4；
Fig. 3 a is the transmission electron microscope picture of CdS-GO made from embodiment 1；
Fig. 3 b is the transmission electron microscope picture of CdSe-GO made from embodiment 2；
Fig. 3 c is the transmission electron microscope picture of CdTe-GO made from embodiment 3；
Fig. 3 d is the transmission electron microscope picture of CdTeSe-GO made from embodiment 4.
Specific embodiment
Below with reference to the attached drawing exemplary embodiment that the present invention will be described in detail, feature and aspect of performance.It is identical in attached drawing
Appended drawing reference indicate element functionally identical or similar.Although the various aspects of embodiment are shown in the attached drawings, remove
It non-specifically points out, it is not necessary to attached drawing drawn to scale.
As shown in Figure 1, a kind of quantum dot-graphene oxide composite material preparation method of DNA guidance comprising following
Step:
S1, design single stranded DNA:
For single stranded DNA since 5 ends, the P=O key in chain structure in phosphoric acid backbone is successively modified to the single stranded DNA of P=S key,
Obtain mercapto-modified single stranded DNA；
S2, preparation DNA- graphene oxide compound:
The DNA that sulfydryl modification is crossed is added in graphene oxide solution, is stirred at room temperature, stands 10 hours and mixed
Solution is closed, is dialysed in distilled water with dialysis membrane 10 hours and removes free DNA, it is molten that DNA- graphene oxide compound is made
Liquid；
S3, the quantum dot-graphene oxide composite material for preparing DNA guidance:
It is compound that DNA-graphene oxide that step S2 is obtained is added in cadmium ion precursor solution and chalcogen precursor solution
In object solution, in the environment of pH is 9.0~11.0,50~90 DEG C are heated to, isothermal reaction obtained QDs-after 2~8 hours
Quantum dot-graphene oxide of DNA guidance is made after dehydrated alcohol washing, centrifugation in DNA-graphene oxide complex solution
Composite material.
Preferably, the modification quantity of sulfydryl is 5~10 in step S1.
Preferably, the mass concentration ratio for the DNA that graphene oxide and sulfydryl modification are crossed in step S2 is 4~1:1.
Preferably, in step S3, oxygen group elements include sulphur, selenium and tellurium.
Preferably, the molar ratio of cadmium ion precursor solution and chalcogen precursor solution is 4~1:1.
Preferably, DNA- graphene oxide complex solution and the volume ratio of cadmium ion and chalcogen precursor mixed solution are
1:99。
Preferably, quantum dot obtained in step S3 is one of CdTe, CdSe, CdS, CdTeSe.
Embodiment 1
S1, design single stranded DNA:
For single stranded DNA since 5 ends, the P=O key in chain structure in phosphoric acid backbone is successively modified to the single stranded DNA of P=S key,
Mercapto-modified single stranded DNA is obtained, sulfydryl modification quantity is 5；
S2, preparation DNA- graphene oxide compound:
The ratio for being 4:1 in graphene oxide and DNA mass concentration ratio, by 16 μ L (1.0mg/mL) GO solution and 8 μ L
DNA that (0.5mg/mL) sulfydryl modification is crossed is added in the centrifuge tube of 0.5mL, is stirred at room temperature, stands 10 hours and mixed
Solution is closed, 10 hours of being dialysed in distilled water with dialysis membrane remove free DNA, and DNA-GO complex solution (concentration is made
About 0.8mg/mL)；
S3, the quantum dot-graphene oxide composite material for preparing DNA guidance:
By the anhydrous caddy of 0.0183g (0.1mmol), 8.70 μ L (0.1mmol) MPA, 0.0060g (0.025mmol) nine
Hydrated sodium sulfide, 25mL distilled water are added in three-necked flask, adjust pH to 9.0 with NaOH (1M) after mixing evenly, and forerunner is made
Body mixed solution (Cd:S molar ratio is 4:1)；
10 μ LDNA-GO complex solutions are mixed with 990 μ L precursor mixed solutions, 8 hour systems are heated at 50 DEG C
Obtain QDs-DNA-GO complex solution；Quantum dot-graphene oxide that DNA guidance is made after dehydrated alcohol washing separation is compound
Object.
As shown in Figure 2 a, the ultraviolet absorption peak of the aqueous solution of CdS-GO obtained is near 337nm, rule of thumb formula D
=(- 6.6521 × 10-8)λ3+(1.9557×10-4)λ2-(9.2352×10-2) λ+(13.29), calculate to obtain graphene oxide table
The CdS QDs partial size in face is 1.83nm, consistent with result is observed in the transmission electron microscope picture of Fig. 3 a.
Embodiment 2
S1, design single stranded DNA:
For single stranded DNA since 5 ends, the P=O key in chain structure in phosphoric acid backbone is successively modified to the single stranded DNA of P=S key,
Mercapto-modified single stranded DNA is obtained, sulfydryl modification quantity is 6；
S2, preparation DNA- graphene oxide compound:
The ratio for being 3:1 in graphene oxide and DNA mass concentration ratio, by 12 μ L (1.0mg/mL) GO solution and 8 μ L
(0.5mg/mL) DNA is added in the centrifuge tube of 0.5mL, is stirred at room temperature, stands 10 hours and obtain mixed solution, with dialysis
Dialyse in distilled water 10 hours of film remove free DNA, are made DNA-GO complex solution (concentration is about 0.8mg/mL)；
S3, the quantum dot-graphene oxide composite material for preparing DNA guidance:
By the anhydrous caddy of 0.0183g (0.1mmol), 8.70 μ L (0.1mmol) MPA, 0.0040g (0.05mmol) Se
Powder, 0.0378g (0.1mmol) sodium borohydride, 25mL distilled water are added in three-necked flask, are adjusted after mixing evenly with NaOH (1M)
Precursor mixed solution is made in pH to 10.0 (Cd:Se molar ratio is 2:1).
10 μ LDNA-GO composite solutions are mixed with 990 μ L precursor mixed solutions, it is obtained that 2 hours are heated at 70 DEG C
QDs-DNA-GO complex solution；Quantum dot-graphene oxide that DNA guidance is made after dehydrated alcohol washing separation is compound
Object.
As shown in Figure 2 b, the ultraviolet absorption peak of the aqueous solution of CdSe-GO obtained is near 472nm, rule of thumb formula D
=(1.6122 × 10-9)λ4-(2.6575×10-6)λ3+(1.6242×10-3)λ2(0.4277) λ+(41.57), calculate to obtain oxygen
The CdSe QDs partial size on graphite alkene surface is 2.11nm, consistent with result is observed in the transmission electron microscope picture of Fig. 3 b.
Embodiment 3
S1, design single stranded DNA:
For single stranded DNA since 5 ends, the P=O key in chain structure in phosphoric acid backbone is successively modified to the single stranded DNA of P=S key,
Mercapto-modified single stranded DNA is obtained, sulfydryl modification quantity is 8；
S2, preparation DNA- graphene oxide compound:
The ratio for being 2:1 in graphene oxide and DNA mass concentration ratio, by 8 μ L (1.0mg/mL) GO solution and 8 μ L
(0.5mg/mL) DNA is added in the centrifuge tube of 0.5mL, is stirred at room temperature, stands 10 hours and obtain mixed solution, with dialysis
Dialyse in distilled water 10 hours of film remove free DNA, are made DNA-GO complex solution (concentration is about 0.8mg/mL)；
S3, the quantum dot-graphene oxide composite material for preparing DNA guidance:
The anhydrous caddy of 0.0183g (0.1mmol), 8.70 μ L (0.1mmol) MPA, 0.0074g (0.033mmol) are sub-
Llurate and 0.0249g (0.66mmol) sodium borohydride, 25mL distilled water are added in three-necked flask, use NaOH after mixing evenly
(1M) adjusts pH to 9.0, and precursor mixed solution is made (Cd:Te molar ratio is 3:1).
10 μ LDNA-GO composite solutions are mixed with 990 μ L precursor mixed solutions, it is obtained that 3 hours are heated at 80 DEG C
QDs-DNA-GO complex solution；Quantum dot-graphene oxide that DNA guidance is made after dehydrated alcohol washing separation is compound
Object.
As shown in Figure 2 c, the ultraviolet absorption peak of the aqueous solution of CdTe-GO obtained is near 485nm, rule of thumb formula D
=(9.8127 × 10-7)λ3-(1.7147×10-3)λ2+ (1.0064) λ-(194.84) calculates to obtain surface of graphene oxide
CdTe QDs partial size is 1.87nm, consistent with result is observed in the transmission electron microscope picture of Fig. 3 c.
Embodiment 4
S1, design single stranded DNA:
For single stranded DNA since 5 ends, the P=O key in chain structure in phosphoric acid backbone is successively modified to the single stranded DNA of P=S key,
Mercapto-modified single stranded DNA is obtained, sulfydryl modification quantity is 10；
S2, preparation DNA- graphene oxide compound:
The ratio for being 2:1 in graphene oxide and DNA mass concentration ratio, by 8 μ L (1.0mg/mL) GO solution and 8 μ L
(0.5mg/mL) DNA is added in the centrifuge tube of 0.5mL, is stirred at room temperature, stands 10 hours and obtain mixed solution, with dialysis
Dialyse in distilled water 10 hours of film remove free DNA, are made DNA-GO complex solution (concentration is about 0.8mg/mL)；
S3, the quantum dot-graphene oxide composite material for preparing DNA guidance:
By the anhydrous caddy of 0.0183g (0.1mmol), 8.70 μ L (0.1mmol) MPA, 0.0040g (0.05mmol) Se
Three mouthfuls of burnings are added in powder, 0.0023g (0.01mmol) sodium tellurite and 0.0113g (0.30mmol) sodium borohydride, 25mL distilled water
In bottle, pH to 11.0 is adjusted with NaOH (1M) after mixing evenly, is made precursor mixed solution (Cd:Te:Se 8:4:3)；
10 μ LDNA-GO composite solutions are mixed with 990 μ L precursor mixed solutions, it is obtained that 2 hours are heated at 90 DEG C
QDs-DNA-GO complex solution；Quantum dot-graphene oxide that DNA guidance is made after dehydrated alcohol washing separation is compound
Object.
As shown in Figure 2 d, the ultraviolet absorption peak of the aqueous solution of CdTeSe-GO obtained is near 499nm, because of CdTeSe
Main body is CdTe quantum, so being D=(9.8127 × 10 according to CdTe quantum empirical equation approximate calculation-7)λ3-
(1.7147×10-3)λ2+ (1.0064) λ-(194.84), calculate its partial size be 2.31nm, with the transmission electron microscope picture of Fig. 3 d in
It is consistent to observe result.
To sum up, the invention has the following advantages that
(1) quantum dot produced by the present invention-graphene oxide composite material property is stablized, moreover, guiding quantum using DNA
The synthesis of point-graphene oxide composite material, which overcomes, can not determine lacking for quantum dot sites and distribution in existing synthesis technology
Point.
(2) raw material that the present invention uses is environmental-friendly, reaction condition is mild, need to only change the molar ratio of each material in synthesis
Rate can be obtained quantum dot-graphene oxide composite material of different-grain diameter quantum dot distribution.
(3) present invention synthesizes quantum dot-graphene oxide composite material in an aqueous medium, improves the biofacies of material
Capacitive.
Finally, it should be noted that above-described each embodiment is merely to illustrate technical solution of the present invention, rather than it is limited
System；Although the present invention is described in detail referring to the foregoing embodiments, those skilled in the art should understand that: its
It can still modify to technical solution documented by previous embodiment, or part of or all technical features are carried out
Equivalent replacement；And these modifications or substitutions, technical solution of various embodiments of the present invention that it does not separate the essence of the corresponding technical solution
Range.
Claims (7)
1. a kind of quantum dot-graphene oxide composite material preparation method of DNA guidance, it is characterised in that: it includes following
Step:
S1, design single stranded DNA:
For single stranded DNA since 5 ends, the P=O key in chain structure in phosphoric acid backbone is successively modified to the single stranded DNA of P=S key, obtains
Mercapto-modified single stranded DNA；
S2, preparation DNA- graphene oxide compound:
The DNA that sulfydryl modification is crossed is added in graphene oxide solution, be stirred at room temperature, stand 10 hours obtain mixing it is molten
Liquid is dialysed 10 hours in distilled water with dialysis membrane and removes free DNA, DNA- graphene oxide complex solution is made；
S3, the quantum dot-graphene oxide composite material for preparing DNA guidance:
It is molten that DNA-graphene oxide compound that step S2 is obtained is added in cadmium ion precursor solution and chalcogen precursor solution
In liquid, in the environment of pH is 9.0~11.0,50~90 DEG C are heated to, isothermal reaction obtains QDs-DNA-oxygen after 2~8 hours
Quantum dot-graphene oxide composite wood of DNA guidance is made after dehydrated alcohol washing, centrifugation in graphite alkene complex solution
Material.
2. quantum dot-graphene oxide composite material preparation method of DNA guidance according to claim 1, feature
Be: the modification quantity of sulfydryl is 5~10 in step S1.
3. quantum dot-graphene oxide composite material preparation method of DNA guidance according to claim 1, feature
Be: the mass concentration ratio for the DNA that graphene oxide and sulfydryl modification are crossed in step S2 is 4~1:1.
4. quantum dot-graphene oxide composite material preparation method of DNA guidance according to claim 1, feature
Be: in step S3, oxygen group elements include sulphur, selenium and tellurium.
5. quantum dot-graphene oxide composite material preparation method of DNA guidance according to claim 4, feature
Be: the molar ratio of the cadmium ion precursor solution and chalcogen precursor solution is 4~1:1.
6. quantum dot-graphene oxide composite material preparation method of DNA guidance according to claim 5, feature
Be: the volume ratio of the DNA- graphene oxide complex solution and cadmium ion and chalcogen precursor mixed solution is 1:99.
7. quantum dot-graphene oxide composite material preparation method of -6 any DNA guidance according to claim 1,
It is characterized by: quantum dot obtained in step S3 is one of CdTe, CdSe, CdS, CdTeSe.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111948186A (en) * | 2020-08-31 | 2020-11-17 | 燕山大学 | Preparation method of fluorescent sensor |
| CN113651317A (en) * | 2021-07-29 | 2021-11-16 | 南昌大学 | Method for preparing graphene foam film capable of shielding terahertz waves by polystyrene microspheres |
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2018
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111948186A (en) * | 2020-08-31 | 2020-11-17 | 燕山大学 | Preparation method of fluorescent sensor |
| CN111948186B (en) * | 2020-08-31 | 2022-05-10 | 燕山大学 | Preparation method of fluorescent sensor |
| CN113651317A (en) * | 2021-07-29 | 2021-11-16 | 南昌大学 | Method for preparing graphene foam film capable of shielding terahertz waves by polystyrene microspheres |
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