CN109568339A - A kind of ceria composite nano materials, preparation method and its usage - Google Patents
A kind of ceria composite nano materials, preparation method and its usage Download PDFInfo
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- CN109568339A CN109568339A CN201811481515.2A CN201811481515A CN109568339A CN 109568339 A CN109568339 A CN 109568339A CN 201811481515 A CN201811481515 A CN 201811481515A CN 109568339 A CN109568339 A CN 109568339A
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- nano materials
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- ruthenium dye
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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
- A61K33/24—Heavy metals; Compounds thereof
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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
- A61K47/54—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 organic compound
- A61K47/545—Heterocyclic compounds
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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
Abstract
The present invention provides a kind of ceria composite nano materials comprising nano ceric oxide and carboxylic acids bipyridyl ruthenium dye, ruthenium dye pass through carboxylic-bond to nano ceric oxide surface.The present invention also provides the preparation method of the composite nano materials and purposes.Composite nano materials provided by the invention are coated with carboxylic acids bipyridyl ruthenium dye by bonding pattern in ceria surface, the two binding force is more preferable, the structure of composite material is more stable, the pattern of nano ceric oxide will not be changed, have excellent SOD and intend enzymatic activity, can be used as a kind of very with the SOD analogies of application potential；Preparation method provided by the invention has many advantages, such as that easy to operate, reaction condition is mild, low in cost, repeatable strong.
Description
Technical field
The present invention relates to nano material and its preparation fields, and in particular to a kind of ceria composite nano materials, its system
Preparation Method and purposes.
Background technique
It has now been found that a variety of nano materials have catalytic activity, can be used as nano artificial enzyme, many metal oxides
Nano material is developed to simulate the activity of a variety of native enzymes, can be used as potential natural enzyme mimics, to play catalysis
Activity, to be had potential application in biomedicine field.
The intracorporal free radical of people is divided into oxygen radical and non-oxygen radical, and wherein oxygen radical accounts for the exhausted big portion of free radical
Point.Free radical has duality in the intracorporal bioactivity of machine, and the generation and removing of machine interior free yl should be balance, machine
Body can just keep fit.If free radical generates the decline of excessive or body Scavenging ability, just have in vivo it is extra from
By base, these free radicals generate irreversible damage to tissue, make histocyte that destructive altered chemical structure occur, directly
Lead to the generation of many diseases and aging.The study found that oxygen radical and more than 70 kinds of diseases have it is direct or potential
System.In vivo in the existing enzyme system for removing free radical, superoxide dismutase (SOD) be it is most important, it is main
It is present in the cells of organs such as the heart, liver, the brain of people, innocuous substance can be converted by peroxide.However, SOD system is eliminated certainly
It can be weakened because of the increase at the age of people by the ability of base, until reaching minimum point when old.From external supplement free radical scavenger or
Radical reaction inhibitor, so that it may radical reaction be made to slow down or be suppressed.
Existing lot of documents reports nano ceric oxide (CeO2) there are a variety of catalytic activity similar to nature enzyme, this
A little enzymes include SOD and catalase (CAT) etc..It is compared with natural enzyme, nano ceric oxide is low with synthesis cost, catalysis is lived
The adjustable, high catalytic efficiency of property and the advantages that have good stability.However, research it has also been found that, only titanium dioxide of the partial size less than 5 nanometers
There is cerium excellent SOD to intend enzymatic activity, and the catalytic capability of nano ceric oxide of the partial size greater than 5 nanometers is easy inactivation.
Summary of the invention
To overcome existing nano ceric oxide existing drawbacks described above, an object of the present invention in terms of quasi- enzymatic activity to be
A kind of ceria composite nano materials are provided, the activity of nano ceric oxide can be significantly improved.
It is a further object of the present invention to provide the preparation methods of the ceria composite nano materials.
A further object of the invention is to provide the purposes of the ceria composite nano materials.
Ceria composite nano materials provided by the invention include nano ceric oxide and carboxylic acids bipyridyl ruthenium dye
Material, wherein the carboxylic acids bipyridyl ruthenium dye passes through carboxylic-bond to the nano ceric oxide surface.
In composite nano materials provided by the invention, carboxyl contained by carboxylic acids bipyridyl ruthenium dye and nano ceric oxide
The Ce ion on surface is bonded together to form by coordination, and in conjunction with stronger, resulting structures are more stable, and ruthenium dye is not easy from nanometer two
It falls off on cerium oxide, moreover, being different from physical absorption, composite material of the invention only needs a small amount of ruthenium dye to be remarkably improved to receive
The quasi- enzymatic activity of rice ceria, is based on these features, and composite material of the invention is more suitable for field of biomedicine, big absolutely
Stable structure and higher activity can be kept under most physiological conditions.It is of the invention compound to receive in addition, as shown in Figure 1B
Rice material will not change the pattern of ceria, it helps improve the activity of nano ceric oxide.
In composite nano materials provided by the invention, the dosage of the nano ceric oxide and carboxylic acids bipyridyl ruthenium dye
It is easy to control, as the ratio of ruthenium dye increases, the enzymatic activity of composite nano materials can be accordingly improved, therefore can be according to work
Property needs, application field, cost etc. are conveniently adjusted in a certain range.Preferably, the nano ceric oxide and carboxylic acid
The weight ratio of class bipyridyl ruthenium dye can be 1000 ﹕ 9~40.
In composite nano materials provided by the invention, the average grain diameter of the nano ceric oxide can be for greater than 5nm, can
Not by the limitation of ceria particle size, resulting composite material not only quasi- enzymatic activity with higher, but also not easy in inactivation.
Preferably, the average grain diameter of the nano ceric oxide can be 5~10nm.
In composite nano materials provided by the invention, the carboxylic acids bipyridyl ruthenium dye can join for common containing carboxyl
The dye sensitizing agent of pyridine ruthenium complex compound, for example, N718 ruthenium dye, N3MZ ruthenium dye etc.；It is preferred that can be N718 ruthenium dye.
The preparation methods of the ceria composite nano materials provided by the invention the following steps are included:
S1: precipitating reagent and cerous nitrate are mixed, cerous cerium hydroxide solution is made；And
S2: the carboxylic acids bipyridyl ruthenium dye is added into cerous cerium hydroxide solution made from step S1 at 60~90 DEG C
Material, is thus made the ceria composite nano materials.
In preparation method provided by the invention, the step S1 can further comprise: by hexamethylenetetramine (HMT) conduct
Precipitating reagent and cerous nitrate (Ce (NO3)3·6H2O it) is configured to aqueous solution respectively, is mixed at 60~90 DEG C and obtains hydroxide
Sub- cerium solution.
Further, cerous nitrate solution is added in HMT solution, it, can be by HMT solution before cerous nitrate solution addition
It is previously heated to 60~90 DEG C.
Further, with being vigorously stirred during precipitant solution is mixed with cerous nitrate solution, speed of agitator can
Think 400rpm or more.
In preparation method provided by the invention, the molar ratio of the hexamethylenetetramine and cerous nitrate can be 10~40 ﹕
3。
In preparation method provided by the invention, the step S2 can further comprise following procedure: made from step S1
After cerous cerium hydroxide solution is formed, the carboxylic acids bipyridyl ruthenium dye is soon added thereto at 70~80 DEG C and is protected from light and stirs
It mixes 2~5 hours, is then stored at room temperature and obtains within 4~8 hours the ceria composite nano materials.
When ruthenium dye being added into cerous cerium hydroxide solution, the formation of ceria can be interfered and influence its shape
Looks, at the same also be easy influence composite material combination effect, then influence resulting materials quasi- enzymatic activity, therefore ruthenium dye plus
It is most important to enter opportunity.In step S1, when obtaining the clear solution of light violet magenta after precipitating reagent and cerous nitrate mixing, as
Cerous cerium hydroxide solution is formd, the composite nano materials that ruthenium dye may make are added immediately at this time and live with optimal catalysis
Property, and it is able to maintain preferable ceria pattern, opportunity is added too early or too late, the activity of resulting composite nano materials all can
It is substantially reduced.
In preparation method provided by the invention, the step S2 can also further comprise: obtained ceria is compound
Nano material is separated and is washed.
Further, isolated mode can be common separation method, such as be centrifugated, the revolving speed of centrifuge separation can
Think that 9000~11000rpm, centrifugation time can be 25~30 minutes.
Purposes the present invention also provides the ceria composite nano materials as superoxide dismutase mimics.
Ceria composite nano materials provided by the invention are coated with carboxylic acid by bonding pattern in ceria surface
Class bipyridyl ruthenium dye, the two binding force is more preferable, and the structure of composite material is more stable, will not change the shape of nano ceric oxide
Looks, so as to so that nano ceric oxide keeps itself characteristic, and ruthenium dye can transmit electronics, excite in green laser
Under, the ability that nano ceric oxide catalysis superoxide anion decomposes can be promoted, equally even if ceria of the partial size greater than 5nm
Can have good catalytic activity.Ceria composite nano materials provided by the invention have the quasi- enzyme activity of excellent SOD as a result,
Property, and do not limited by ceria particle size, activity can also be kept even if under 80 DEG C of higher temperature, can be used as one kind
Very with the SOD analogies of application potential.Preparation method provided by the invention have easy to operate, reaction condition it is mild, at
The advantages that this is cheap, repeatable strong.
Detailed description of the invention
Figure 1A is the transmission electron microscope picture of nano ceric oxide.
Figure 1B is N719 ruthenium dye-ceria composite nano materials transmission electron microscope picture made from embodiment.
Fig. 2 is N719 ruthenium dye-ceria composite nano materials FTIR made from N719 ruthenium dye and embodiment
Spectrogram.
Fig. 3 is to measure N719 ruthenium dye-ceria composite nano materials using xanthine oxidase-cromoci method
The result chart of superoxide anion vigor is removed in catalysis, wherein abscissa is the time, and ordinate is each reaction system in 550nm
Absorbance under wavelength.
Specific embodiment
Below by embodiment, the present invention is described in detail, so that the features and advantages of the present invention become apparent from.But it answers
This points out that for embodiment for understanding design of the invention, the scope of the present invention is not limited only to reality listed herein
Apply example.
Experimental method used in following embodiments is conventional method unless otherwise specified.Institute in following embodiments
Material, reagent etc., are commercially available unless otherwise specified.
Embodiment
1. the preparation of cerous cerium hydroxide solution
By hexamethylenetetramine (HMT) and Ce (NO3)3·6H2O forms 160mL concentration after being respectively dissolved in water as 0.5M's
Ce (the NO that HMT solution and 160mL concentration are 0.0375M3)3Solution, then by Ce (NO3)3Solution is added to 75 DEG C of HMT
In solution.The clear solution of light violet magenta is obtained after being vigorously stirred several minutes at 75 DEG C to get cerous cerium hydroxide solution is arrived.
The preparation of 2.N719 ruthenium dye-ceria composite nano materials
When the formation of the clear solution of aforementioned light violet magenta, 35mg N719 ruthenium dye is soon added to it at 75 DEG C
In and be protected from light stirring, obtain kermesinus suspension, after stirring being further continued at 75 DEG C 3 hours, be cooled to room temperature in air, stand 5
The composite nano materials of kermesinus are obtained after a hour.Supernatant is abandoned, is centrifugated at 10000rpm, and with secondary water washing three
It is secondary.The composite material of synthesis is collected, completely cuts off air, is protected from light storage.
As shown in Figure 1A, 1B, Figure 1A is the transmission electron microscope picture of nano ceric oxide, in contrast, Figure 1B shows N719 ruthenium
Coating dye has not been changed the pattern of ceria on the surface of nano ceric oxide, the average grain diameter of nano ceric oxide
About 8nm.
As shown in Fig. 2, 1710cm in FTIR spectrogram-1Locate carbonylic stretching vibration peak to disappear, show ruthenium dye by carboxyl and
Coordination between the Ce ion on nano ceric oxide surface is bonded together, and bonding does not change nano ceric oxide particle
Ingredient or pattern.
Test case 1
It measures the catalysis of N719 ruthenium dye-ceria composite nano materials made from embodiment and removes superoxide anion
Vigor, experiment condition and each reagent pipetting volume amount are shown in Table 1.
1 xanthine oxidase of table-cromoci method measurement SOD vigor sample introduction
The amount and sequence indicated according to table 1 sequentially add classes of agents.It is 10ng/mL composite nano materials in measurement concentration
Catalytic activity before, using wavelength be 532nm, power be 150mW laser it is irradiated 30 minutes.To after reaction,
It shakes up reaction system, at Yu Bochang 550nm, in 1cm optical path slit cuvette, after distilled water zeroing, measures absorbance.Reaction is altogether
Measurement 5 minutes, it is primary every measurement in 20 seconds.
Compound concentration is respectively the CuZn-SOD enzyme standard items of 0,1,2,5,10,15 and 20U/mL, using same method
It measures its catalysis and removes the ability of superoxide anion, and draw standard curve, SOD vigor and measurement institute are obtained by digital simulation
Obtain the relationship between straight slope.
As shown in figure 3, the curve that the absorbance of each sample and CuZn-SOD enzyme standard items at 550nm changes over time.
From the figure 3, it may be seen that the catalytic activity that concentration is 10ng/mL composite nano materials (Nanoceria@N719) is about 15U/mL, and
The nano ceric oxide (Nanoceria) of 10ng/mL, catalytic activity and blank group are suitable.This explanation, passes through N719 ruthenium dye
Ceria is coated, so that the ceria that partial size is about 8 nanometers has excellent SOD and intends enzymatic activity.
Test case 2
N719 ruthenium dye-ceria composite nano materials are prepared according to the method for embodiment.Wherein, N719 ruthenium dye
Addition opportunity is respectively as follows:
1) Best Times window, i.e. precipitating reagent obtain the clear solution of light violet magenta after mixing with cerous nitrate when；2) best
5min before time window；And 3) 15min after Best Times window.
It the use of wavelength is 532nm, power is the laser illumination 1h of 0.1W, according to the method detection of test case 1, is fitted
SOD vigor out, the results are shown in Table 2, illustrates that chance generates weight to the activity of composite nano materials when the addition of N719 ruthenium dye
It influences.
Table 2
Unless limited otherwise, term used herein is the normally understood meaning of those skilled in the art.
Embodiment described in the invention is merely for exemplary purpose, the protection scope being not intended to limit the invention,
Those skilled in the art can be made within the scope of the invention various other replacements, changes and improvements, thus, the present invention is not limited to
Above embodiment, and be only defined by the claims.
Claims (10)
1. a kind of ceria composite nano materials, which is characterized in that it includes nano ceric oxide and carboxylic acids bipyridyl
Ruthenium dye, the carboxylic acids bipyridyl ruthenium dye pass through carboxylic-bond to the nano ceric oxide surface.
2. composite nano materials according to claim 1, which is characterized in that the nano ceric oxide and the carboxylic acids
The weight ratio of bipyridyl ruthenium dye is 1000 ﹕ 9~40.
3. composite nano materials according to claim 1 or 2, which is characterized in that the average grain of the nano ceric oxide
Diameter is greater than 5nm；Preferably 5~10nm.
4. composite nano materials according to claim 1 or 2, which is characterized in that the carboxylic acids bipyridyl ruthenium dye is
N719 ruthenium dye.
5. the preparation method of the described in any item ceria composite nano materials of claim 1-4, which is characterized in that including with
Lower step:
S1: precipitating reagent and cerous nitrate are mixed, cerous cerium hydroxide solution is made；And
S2: being added the carboxylic acids bipyridyl ruthenium dye at 60~90 DEG C into cerous cerium hydroxide solution made from step S1,
Thus the ceria composite nano materials are made.
6. preparation method according to claim 5, which is characterized in that the step S1 includes: to make hexamethylenetetramine
It is configured to aqueous solution respectively for precipitating reagent and cerous nitrate, is mixed at 60~90 DEG C and cerous cerium hydroxide solution is made.
7. preparation method according to claim 6, which is characterized in that the molar ratio of the hexamethylenetetramine and cerous nitrate
For 10~40 ﹕ 3.
8. preparation method according to claim 5, which is characterized in that the step S2 includes: the hydrogen made from the step S1
After the sub- cerium solution of oxidation is formed, the carboxylic acids bipyridyl ruthenium dye is soon added thereto at 70~80 DEG C and is protected from light stirring
It 2~5 hours, is then stored at room temperature and obtains within 4~8 hours the ceria composite nano materials.
9. preparation method according to claim 8, which is characterized in that the step S2 further includes the dioxy that will be obtained
Change cerium composite nano materials to separate and wash.
10. use of any one of the claim 1-4 ceria composite nano materials as superoxide dismutase mimics
On the way.
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| CN113694935A (en) * | 2021-06-24 | 2021-11-26 | 南开大学 | Method for improving activity of nano-material peroxidase |
| CN113916948A (en) * | 2021-09-18 | 2022-01-11 | 哈尔滨商业大学 | Based on nanometer CeO2Electrochemical sensor for detecting xanthine and preparation method and application thereof |
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Cited By (4)
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| CN113694935A (en) * | 2021-06-24 | 2021-11-26 | 南开大学 | Method for improving activity of nano-material peroxidase |
| CN113694935B (en) * | 2021-06-24 | 2023-11-03 | 南开大学 | Method for improving activity of nano-material peroxidase |
| CN113916948A (en) * | 2021-09-18 | 2022-01-11 | 哈尔滨商业大学 | Based on nanometer CeO2Electrochemical sensor for detecting xanthine and preparation method and application thereof |
| CN113916948B (en) * | 2021-09-18 | 2024-03-01 | 哈尔滨商业大学 | Based on nanometer CeO 2 Electrochemical sensor for detecting xanthine as well as preparation method and application thereof |
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