CN113181906A - Pt @ CDs composite nano material and preparation method thereof - Google Patents
Pt @ CDs composite nano material and preparation method thereof Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
- B01J23/42—Platinum
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K33/00—Medicinal preparations containing inorganic active ingredients
- A61K33/24—Heavy metals; Compounds thereof
- A61K33/243—Platinum; Compounds thereof
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K33/00—Medicinal preparations containing inorganic active ingredients
- A61K33/44—Elemental carbon, e.g. charcoal, carbon black
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
- A61K47/50—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient the non-active ingredient being chemically bound to the active ingredient, e.g. polymer-drug conjugates
- A61K47/51—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient the non-active ingredient being chemically bound to the active ingredient, e.g. polymer-drug conjugates the non-active ingredient being a modifying agent
- A61K47/52—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient the non-active ingredient being chemically bound to the active ingredient, e.g. polymer-drug conjugates the non-active ingredient being a modifying agent the modifying agent being an inorganic compound, e.g. an inorganic ion that is complexed with the active ingredient
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P39/00—General protective or antinoxious agents
- A61P39/06—Free radical scavengers or antioxidants
-
- B01J35/40—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/65—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing carbon
Abstract
The invention provides a Pt @ CDs complexThe nanometer material and its preparation process includes the following steps: step 1, the concentration is 0.5mg mL‑1And 10mM H2PtCl6Uniformly mixing the solution according to the volume ratio of 4:1 to obtain a mixed solution; step 2, preparing the obtained mixed solution into an alkaline solution; step 3, adding NaBH with the concentration of 10mg mL-1 into the alkaline solution4The solution is stirred uniformly, kept stand and subjected to impurity removal in sequence to obtain a Pt @ CDs solution; the invention has the characteristics of simple synthesis steps, environmental protection, small material size, stable dispersibility and the like, and has wide prospects in practical applications of oxidative damage protection, anti-inflammatory treatment and the like.
Description
Technical Field
The invention belongs to the research field of nano-enzyme, mimic enzyme and catalytic nano-material, and particularly relates to a Pt @ CDs composite nano-material and a preparation method thereof.
Background
The nano enzyme is a nano material with enzymatic characteristics, can catalyze a substrate of the enzyme to generate a catalytic reaction similar to that of natural enzyme, has the characteristics of enzymatic reaction kinetics and the like, and belongs to a novel mimic enzyme. Since the first report in 2007, nanoenzyme has become a research hotspot with multidisciplinary intersection, and the application research of nanoenzyme relates to a plurality of fields such as medicine, environment, agriculture, national defense safety and the like.
The hydrogen peroxide nanoenzyme and the superoxide dismutase nanoenzyme are two types of nanoenzymes with antioxidant effect, can effectively remove active oxygen clusters to maintain the redox balance of the cell microenvironment, and play an important role in antioxidant treatment. Most of the materials with the two types of nano-enzyme activities discovered at present are metal oxides or noble metal nano-materials, the synthesis process is complex, the yield is low, mass production is not facilitated, the nano-enzyme activity is low and the stability is insufficient, the nano-enzyme is difficult to degrade when applied to biomedicine such as living body imaging, cell protection, disease diagnosis and treatment and the like, and metal ions are possibly released to generate toxicity, so that the potential biological safety problem exists. Therefore, the development of a novel antioxidant nanoenzyme with low toxicity, good biocompatibility and high enzyme activity is needed.
Disclosure of Invention
The invention aims to provide a Pt @ CDs composite nano material and a preparation method thereof, and overcomes the defects in the prior art.
In order to achieve the purpose, the invention adopts the technical scheme that:
the invention provides a preparation method of a Pt @ CDs composite nano material, which comprises the following steps:
step 2, preparing the obtained mixed solution into an alkaline solution;
step 3, adding NaBH with the concentration of 10mg mL-1 into the alkaline solution4And (3) stirring the solution uniformly, standing and removing impurities in sequence to obtain the Pt @ CDs solution.
Preferably, in step 1, the preparation method of the CDs solution is as follows:
adding activated carbon into mixed acid, and preparing by oxidation reflux method to obtain 10-17ug mL-1The mixed solution of (1); purifying the obtained mixed solution to obtain a CDs solution;
preferably, the mixed acid comprises H2SO4Solution and HNO3Solution of, wherein H2SO4Solution and HNO3The solutions were mixed in a volume ratio of 1: 1.
Preferably, the specific method for purifying the obtained mixed solution is as follows:
adding NaHCO into the mixed solution3Carrying out neutralization;
and sequentially filtering, dialyzing, filtering and ultrafiltering the neutralized mixed solution to obtain a CDs solution with the molecular interception amount of less than 100 kDa.
Preferably, in step 1, the molecular cut-off of the CDs solution is less than 100 kDa.
Preferably, in step 3, NaBH4Solution and H2PtCl6The volume ratio of the solution was 2: 15.
Preferably, in step 3, the molecular cut-off of the Pt @ CDs solution is less than 100 kDa.
Preferably, in step 3, the process conditions for removing impurities are as follows:
and adjusting the pH value of the solution after standing to be neutral, and then sequentially filtering, dialyzing, filtering and ultrafiltering to obtain a Pt @ CDs solution with the molecular interception amount of less than 100 kDa.
A Pt @ CDs composite nanomaterial prepared based on the method for preparing a Pt @ CDs composite nanomaterial recited in any one of claims 1 to 8.
Compared with the prior art, the invention has the beneficial effects that:
the invention provides a preparation method of Pt @ CDs composite nano-materials, which aims to solve the technical problems mentioned in the background technology, prepares a Pt @ CDs nano-material with activities of hydrogen peroxide nanoenzyme and superoxide dismutase nanoenzyme by taking carbon points with low toxicity, good biocompatibility and strong stability as raw materials, and adopts an in-situ synthesis strategy to obtain a batch of Pt @ CDs composite nano-materials with multi-enzyme catalytic activity and hydroxyl radical scavenging property by introducing platinum atoms in situ on the surfaces of the carbon points; research results show that the carbon dots are loaded on the surface of the platinum nano-particles, so that the stability of the platinum nano-particles can be improved, the activity of hydrogen peroxide nano-particles of the platinum nano-particles is enhanced, and the activity of superoxide dismutase nano-particles is improved under the synergistic effect with nano-platinum.
The Pt @ CDs composite nano material prepared by the invention has high-efficiency antioxidant enzyme catalytic activity for the first time, and provides material basis and technical support for an antioxidant treatment platform; meanwhile, the Pt @ CDs composite nano material shows ultrahigh catalytic activity of superoxide dismutase and catalase and hydroxyl radical scavenging property in a physiological environment.
Drawings
FIG. 1 is a TEM and HRTEM image of the product obtained in example 1;
FIG. 2 is a graph of the excitation-dependent emitted fluorescence spectrum of the product obtained in example 1;
FIG. 3 shows the superoxide dismutase activity of various products of example 2;
FIG. 4 shows the catalase activity of different products in example 3;
FIG. 5 shows hydroxyl radical scavenging properties of various products of example 4;
FIG. 6 is a graph of the total antioxidant capacity of the different products of example 5.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings.
The invention aims to provide a Pt @ CDs composite nano material and a preparation method thereof, and the application value of nano enzyme in the fields of oxidative damage protection and anti-inflammatory treatment is improved by utilizing the high-efficiency antioxidant activity and hydroxyl radical scavenging property of superoxide dismutase and catalase.
The invention provides a preparation method of a Pt @ CDs composite nano material, which comprises the following steps:
preparation of CDs solution: adding activated carbon into mixed acid (H) by using an oxidation reflux method2SO4/HNO31:1), boiling the mixed solution until the activated carbon is completely oxidized to obtain a brown yellow liquid, then cooling the brown yellow liquid at room temperature, and collecting the obtained CDs solution, wherein the concentration of the mixed solution is 10-17ug mL-1(ii) a Since the brown yellow liquid obtained above is in a strong acid environment, for further purification NaHCO is used3Carrying out neutralization; filtering the neutralized mixed solution with 0.22 μm BIOSHARPP filter membrane, transferring into a dialysis bag with molecular cut-off of 3500Dalton, and dialyzing for 5-7 d; filtering the dialyzed CDs solution with 0.22 μm BIOSHARPP membrane again to remove a small amount of insoluble substances, ultrafiltering the obtained filtrate with ultrafiltration tube with molecular cut-off of 100kDa, and separating to obtain CDs solution with molecular cut-off of less than 100 kDa.
Preparation of Pt @ CDs: 0.5mg mL of each of the solutions was added in a volume ratio of 4:1-1CDs solution and 10mM H2PtCl6Placing the solution in a 20mL scintillation bottle, and magnetically stirring for 30min to obtain a mixed solution; to enable more efficient reduction of the Pt atoms, the pH was adjusted to 12 with NaOH solution. According to the addition of H2PtCl6The content of the solution is 10mg mL-1NaBH dropwise added according to the volume ratio of 2:154The solution was magnetically stirred for 3h, then left to stand at room temperature for 24h, and adjusted to neutral pH with HCl solution. The resulting solution was first filtered through a 0.22 μm BIOSHARPP membrane filter and transferred to a dialysis bag with a molecular cut-off of 3500Dalton for dialysis for 3 d. Filtering the dialyzed solution with 0.22 μm BIOSHARPP membrane to remove a small amount of insoluble substances, ultrafiltering the obtained filtrate with ultrafiltration tube with molecular cut-off of 100kDa, and separating to obtainPt @ CDs solution with molecular cut-off less than 100 kDa.
Superoxide dismutase activity of Pt @ CDs: the superoxide dismutase activity of Pt @ CDs was detected using a superoxide dismutase detection kit (WST-8).
Catalase activity of Pt @ CDs: detection kit and detection H adopting catalase2O2In A240Two methods to verify the catalase activity of Pt @ CDs.
Hydroxyl radical scavenging properties of Pt @ CDs: the hydroxyl radical can discolor Methylene Blue (MB), and the detection of MB at A is carried out by means of UV-Vis675The characteristic absorption peak of (a), and the hydroxyl radical scavenging property of Pt @ CDs is verified.
Total antioxidant capacity of Pt @ CDs: and (3) detecting the total antioxidant capacity level of the Pt @ CDs by using a total antioxidant capacity detection kit (ABTS method).
The invention has the advantages of novelty and remarkable characteristics
(1) The Pt @ CDs nanoenzyme not only introduces the catalase activity and the hydroxyl radical scavenging characteristic with high activity by doping platinum atoms on the surface of the carbon point in situ, but also has stronger activity of the original superoxide dismutase of the carbon point, and plays a role in the catalytic performance of cascade amplification.
(2) By controlling the content of CDs in the in-situ synthesis process, the evidence obtained by the invention shows that the CDs not only can obviously enhance the activity of superoxide dismutase, but also play a role in stabilizing Pt atoms in the Pt @ CDs composite nano material.
(3) The Pt @ CDs nanoenzyme has the characteristics of simple synthesis steps, greenness, small material size, stable dispersibility and the like, and is beneficial to improving the foundation of a catalyst and a substrate, so that a better catalytic effect can be obtained by adding a small amount of the Pt @ CDs nanoenzyme in the reaction process.
Example 1
Preparation of CDs: adding activated carbon to mixed acid (H) using a convenient oxidative reflux process2SO4/HNO31:1), boiling the mixed solution until the activated carbon is completely oxidized to obtain a brown yellow liquid, then cooling at room temperature, and collecting to obtain a CDs solution, wherein the mixed solution is preparedThe concentration of the mixed solution is 10ug mL-1(ii) a Since the brown yellow liquid obtained above is in a strong acid environment, for further purification NaHCO is used3Carrying out neutralization; filtering the obtained neutralized CDs solution through a 0.22 μm BIOSHARPP membrane filter, transferring into a dialysis bag with molecular cut-off of 3500Dalton, and dialyzing for 5 d; filtering the CDs solution after dialysis with 0.22 μm BIOSHARPP membrane again to remove a small amount of insoluble substances, ultrafiltering the obtained filtrate with ultrafiltration tube with molecular cut-off of 100kDa, and separating to obtain CDs solution with molecular cut-off of less than 100 kDa.
Preparation of Pt @ CDs: 0.5mg mL of each of the solutions was added in a volume ratio of 4:1-1CDs solution and 10mM H2PtCl6Placing the solution in a 20mL scintillation bottle, and magnetically stirring for 30min to obtain a mixed solution; to enable more efficient reduction of the Pt atoms, the pH was adjusted to 12 with NaOH solution. According to the addition of H2PtCl6The content of the solution is 10mg mL-1NaBH dropwise added according to the volume ratio of 2:154The solution was magnetically stirred for 3h, then left to stand at room temperature for 24h, and the pH was adjusted to neutral with HCl solution. The resulting solution was first filtered through a 0.22 μm BIOSHARPP membrane filter and transferred to a dialysis bag with a molecular cut-off of 3500Dalton for dialysis for 3 d. The solution after dialysis was again filtered through a 0.22 μm BIOSHARPP membrane to remove a small amount of insoluble matter, the obtained filtrate was ultrafiltered through an ultrafiltration tube having a molecular cut-off of 100kDa, and after separation, a Pt @ CDs solution having a molecular cut-off of less than 100kDa was obtained.
The particle size of CDs is shown in figure 1 to be about 1.5nm, whereas Pt @ CDs particle size is about 4nm, and by measuring its lattice size, CDs (100) is found to be present, d ═ 0.21 nm; pt @ CDs (111), d ═ 0.23 nm. The above results indicate the successful incorporation of Pt.
It is shown in fig. 2 that doping of Pt atoms does not change the excitation dependent emission photoluminescence properties of CDs.
Detecting the activity of the superoxide dismutase by adopting a superoxide dismutase detection kit (WST-8). WST-8 superoxide anion (O) generated by xanthine oxidase2.-) The reaction generates water-soluble formazan dye, and superoxide dismutase can catalyze superoxide anionThe ions are subjected to disproportionation, so that the reaction step can be inhibited by the superoxide dismutase, and the activity of the superoxide dismutase is in negative correlation with the generation amount of the formazan dye, so that the enzyme activity of the superoxide dismutase can be calculated by colorimetric analysis of a WST-8 product. The absorbance was measured at 450 nm. Plotting the inhibition rate (%) that the unit of the activity of the superoxide dismutase enzyme in the sample to be tested is 50%/(1-50%) units is 1unit when the inhibition percentage is 50%; when the percentage of inhibition is 60%, the unit of activity of superoxide dismutase enzyme in the sample to be tested is 60%/(1-60%) units is 1.5 units. The final concentration of the sample used was 50ug mL-1。
FIG. 3 shows that CDs and Pt @ CDs have significantly higher superoxide dismutase activity than Pt NPs, and the superoxide dismutase activity of Pt @ CDs is significantly higher than that of CDs and SOD Norm (SOD Norm: standard, 30U, inhibition rate is about 50%) at the same concentration. Indicating that the Pt @ CDs have ultrahigh superoxide dismutase activity.
Catalase detection Kit (Catalase Assay Kit) detected Catalase activity. Is a simple and easy reagent kit for detecting the catalase activity in a sample through chromogenic reaction. In the case of relatively abundant hydrogen peroxide, catalase can catalyze hydrogen peroxide to produce water and oxygen. The chromogenic substrate may be oxidized by the catalysis of residual hydroperoxidase to produce a red product with a maximum absorption wavelength of 520 nm. And (3) preparing a standard curve by using the hydrogen peroxide standard substance, so that how much hydrogen peroxide is catalyzed by catalase in the sample in unit volume of unit time and converted into water and oxygen can be calculated, and the enzyme activity of the catalase in the sample can be calculated. The final concentration of the sample used was 4ug mL-1。
A240Detection of H2O2Indirectly detecting the catalase activity. In the presence of 10mM H2O2，25ug mL-1Pt @ CDs in a 25mM PBS reaction system at pH 7.4, diluted appropriately by the same factor, and subjected to dynamic assay A240Absorption of (2).
It is shown in FIG. 4 that CDs do not have catalase activity, Pt NPs have lower catalase activity, and Pt @ CDs have significantly higher catalase activity. Indicating that Pt @ CDs have ultrahigh catalase activity.
In the presence of 0.25mM MB, 5mM H2O2，5mM Fe2+25ug/ml Pt @ CDs in 25mM PBS reaction at pH 7.4, diluted appropriately by the same factor, and assayed for A675Absorption of (2).
FIG. 5 shows that CDs do not have hydroxyl radical scavenging properties, whereas Pt @ CDs have significantly higher hydroxyl radical scavenging properties. Indicating that Pt @ CDs have ultrahigh activity of scavenging hydroxyl radicals.
A total oxidation resistance detection kit (ABTS method) is a kit which adopts ABTS as a color developing agent and detects the total oxidation resistance of various antioxidant solutions. Dynamic detection of A by adding Pt @ CDs solutions of different concentrations734Absorption of (2).
The overall antioxidant capacity of Pt @ CDs is shown in FIG. 6 to be significantly better than that of CDs.
Example 2
Preparation of CDs: adding activated carbon to mixed acid (H) using a convenient oxidative reflux process2SO4/HNO31:1), boiling the mixture until the activated carbon is completely oxidized to obtain a brown yellow liquid, then cooling the brown yellow liquid at room temperature, and collecting to obtain a CDs solution, wherein the concentration of the mixture is 14ug mL-1(ii) a Since the brown yellow liquid obtained above is in a strong acid environment, for further purification NaHCO is used3Carrying out neutralization; filtering the obtained neutralized CDs solution through 0.22 μm BIOSHARPP membrane filter, transferring into a dialysis bag with molecular cut-off of 3500Dalton, and dialyzing for 6 d; filtering the CDs solution after dialysis with 0.22 μm BIOSHARPP membrane again to remove a small amount of insoluble substances, ultrafiltering the obtained filtrate with ultrafiltration tube with molecular cut-off of 100kDa, and separating to obtain CDs solution with molecular cut-off of less than 100 kDa.
Preparation of Pt @ CDs: 0.5mg mL of each of the solutions was added in a volume ratio of 4:1-1CDs solution and 10mM H2PtCl6The solution was placed in a 20mL scintillation vialMagnetically stirring for 30min to obtain a mixed solution; to enable more efficient reduction of the Pt atoms, the pH was adjusted to 12 with NaOH solution. According to the addition of H2PtCl6The content of the solution is 10mg mL-1NaBH dropwise added according to the volume ratio of 2:154The solution was magnetically stirred for 3h, then left to stand at room temperature for 24h, and the pH was adjusted to neutral with HCl solution. The resulting solution was first filtered through a 0.22 μm BIOSHARPP membrane filter and transferred to a dialysis bag with a molecular cut-off of 3500Dalton for dialysis for 3 d. The solution after dialysis was again filtered through a 0.22 μm BIOSHARPP membrane to remove a small amount of insoluble matter, the obtained filtrate was ultrafiltered through an ultrafiltration tube having a molecular cut-off of 100kDa, and after separation, a Pt @ CDs solution having a molecular cut-off of less than 100kDa was obtained.
Example 3
Preparation of CDs: adding activated carbon to mixed acid (H) using a convenient oxidative reflux process2SO4/HNO3Obtaining a mixed solution in the ratio of 1:1), boiling the mixed solution until activated carbon is completely oxidized to obtain a brown yellow liquid, then cooling the liquid at room temperature, and collecting the obtained CDs solution, wherein the concentration of the mixed solution is 17ug mL-1(ii) a Since the brown yellow liquid obtained above is in a strong acid environment, for further purification NaHCO is used3Carrying out neutralization; filtering the obtained neutralized CDs solution through a 0.22 μm BIOSHARPP membrane filter, transferring into a dialysis bag with molecular cut-off of 3500Dalton, and dialyzing for 7 d; filtering the CDs solution after dialysis with 0.22 μm BIOSHARPP membrane again to remove a small amount of insoluble substances, ultrafiltering the obtained filtrate with ultrafiltration tube with molecular cut-off of 100kDa, and separating to obtain CDs solution with molecular cut-off of less than 100 kDa.
Preparation of Pt @ CDs: 0.5mg mL of each of the solutions was added in a volume ratio of 4:1-1CDs solution and 10mM H2PtCl6Placing the solution in a 20mL scintillation bottle, and magnetically stirring for 30min to obtain a mixed solution; to enable more efficient reduction of the Pt atoms, the pH was adjusted to 12 with NaOH solution. According to the addition of H2PtCl6The content of the solution is 10mg mL-1NaBH dropwise added according to the volume ratio of 2:154Magnetically stirring the solution for 3h, standing at room temperature for 24h, and adjusting with HCl solutionThe pH was adjusted to neutral. The resulting solution was first filtered through a 0.22 μm BIOSHARPP membrane filter and transferred to a dialysis bag with a molecular cut-off of 3500Dalton for dialysis for 3 d. The solution after dialysis was again filtered through a 0.22 μm BIOSHARPP membrane to remove a small amount of insoluble matter, the obtained filtrate was ultrafiltered through an ultrafiltration tube having a molecular cut-off of 100kDa, and after separation, a Pt @ CDs solution having a molecular cut-off of less than 100kDa was obtained.
Claims (9)
1. A preparation method of Pt @ CDs composite nano-materials is characterized by comprising the following steps:
step 1, the concentration is 0.5mg mL-1And 10mM H2PtCl6Uniformly mixing the solution according to the volume ratio of 4:1 to obtain a mixed solution;
step 2, preparing the obtained mixed solution into an alkaline solution;
step 3, adding NaBH with the concentration of 10mg mL-1 into the alkaline solution4And (3) stirring the solution uniformly, standing and removing impurities in sequence to obtain the Pt @ CDs solution.
2. The method for preparing Pt @ CDs composite nanomaterial according to claim 1, wherein in step 1, the CDs solution is prepared by:
adding activated carbon into mixed acid, and preparing by oxidation reflux method to obtain 10-17ug mL-1The mixed solution of (1); and purifying the obtained mixed solution to obtain a CDs solution.
3. The method as recited in claim 2, wherein the mixed acid comprises H2SO4Solution and HNO3Solution of, wherein H2SO4Solution and HNO3The solutions were mixed in a volume ratio of 1: 1.
4. The preparation method of the Pt @ CDs composite nanomaterial according to claim 2, wherein the specific method for purifying the obtained mixed solution is as follows:
adding NaHCO into the mixed solution3Carrying out neutralization;
and sequentially filtering, dialyzing, filtering and ultrafiltering the neutralized mixed solution to obtain a CDs solution with the molecular interception amount of less than 100 kDa.
5. The method for preparing Pt @ CDs composite nanomaterial according to claim 1, wherein in step 1, the molecular cut-off of the CDs solution is less than 100 kDa.
6. The method for preparing Pt @ CDs composite nanomaterial according to claim 1, wherein in step 3, NaBH4Solution and H2PtCl6The volume ratio of the solution was 2: 15.
7. The method of claim 1, wherein in step 3, the Pt @ CDs solution has a molecular cut-off of less than 100 kDa.
8. The method for preparing Pt @ CDs composite nanomaterial according to claim 1, wherein in the step 3, the process conditions for removing impurities are as follows:
and adjusting the pH value of the solution after standing to be neutral, and then sequentially filtering, dialyzing, filtering and ultrafiltering to obtain a Pt @ CDs solution with the molecular interception amount of less than 100 kDa.
9. A Pt @ CDs composite nanomaterial, wherein the Pt @ CDs composite nanomaterial is prepared based on the method for preparing the Pt @ CDs composite nanomaterial described in any one of claims 1 to 8.
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