CN102210324B - Selective bactericide with composite nanoparticles as well as preparation and application thereof - Google Patents
Selective bactericide with composite nanoparticles as well as preparation and application thereof Download PDFInfo
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- CN102210324B CN102210324B CN 201010146745 CN201010146745A CN102210324B CN 102210324 B CN102210324 B CN 102210324B CN 201010146745 CN201010146745 CN 201010146745 CN 201010146745 A CN201010146745 A CN 201010146745A CN 102210324 B CN102210324 B CN 102210324B
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Abstract
The invention relates to an antimicrobial bactericide and in particular relates to a selective bactericide with composite nanoparticles as well as a preparation and an application thereof. The bactericide comprises the following components by weight percent: 65-80% of nano-silver, 15-30% of nano-titanium dioxide, 5-10% of silicon dioxide and 0.01-1% of antibiotics. The selective bactericide is prepared through the following steps: using glucose to reduce a silver ammonia solution so as to prepare the nano-silver in a nuclear structure, then covering a silicon dioxide layer, further preparing titanium dioxide in a shell structure on the surface of the silicon dioxide layer, and finally modifying the antibiotics on the surface of the titanium dioxide through a chemical cross-linking agent. The selective bactericide has a bactericidal action against Gram-positive or Gram-negative bacteria and antibiotics-sensitive bacteria with selectivity when being applied in an ultraviolet or dark place. The obtained functional antimicrobial not only has the sterilization action, but also has a certain sterilization action under dark conditions; and in addition, the antimicrobial bactericide has a selective sterilization effect.
Description
Technical field
The present invention relates to antibiotic bactericide, specifically a kind of selectivity bactericide of composite nanometer particle and preparation and application.
Background technology
Titanium dioxide itself is nontoxic, has been widely used in food, medicine, the various fields such as cosmetics.Photocatalysis similar photosynthetic light-catalyzed reaction of meeting generation under the irradiation of light (oxidation-reduction reaction, produce oxidability extremely strong free hydroxy and active oxygen, but these product kill bacteria and decomposing organic pollutants.And organic pollutant is resolved into to free of contamination water (H
2o) and carbonic acid gas (CO
2), simultaneously it has the functions such as sterilization, deodorizing, antifouling, hydrophilic, antiultraviolet.Photocatalysis also can be done reaction under faint light, if under ultraviolet irradiation, and light-catalysed active can the reinforcement.After the optically catalytic TiO 2 phenomenon is found, utilizes the optically catalytic TiO 2 degradation water, purify air and patent that sterilization is antibiotic occurs in succession.Chinese patent ZL02119304.5 discloses a kind of porous titanium dioxide thin-film preparation with antibiotic and sterilizing activity, and for seawater and the sterilization of running water medium, but the method sterilization only realizes under the effect of ultraviolet light.Chinese patent ZL02114732.9 discloses a kind of sterilization pesticide, by inorganic material, formed, there is photocatalytic activity and stronger sterilizing function, its preparation method be by modifying titanium dioxide suspension or modified titanium dioxide sol high degree of dispersion on the nanometer titanium dioxide silicon substrate, synthetic uniform titanium-silicon composite particles, form and have the cancellated suspension of Ti-O-Si.But this bactericide does not have special bactericidal property.
In recent years, vancomycin combining nano particle is strengthened its antibacterial characteristics and has also been obtained application.Such as thereby the next specific microorganism that kills the vancomycin sensitivity of its antibiotic sterilization ability is strengthened on the surface of vancomycin being modified to golden nanometer particle.Referring to document 1, Nano Letters, in 2003,3,12611263, thereby vancomycin is modified the surface of golden nanometer particle and is strengthened its antibiotic sterilization ability and carry out the specific microorganism that kills the vancomycin sensitivity.Document 2, Small, in 2008,5:51-56, vancomycin is modified tri-iron tetroxide and golden composite nanometer particle surface, by tri-iron tetroxide enrichment and the antibiotic selectivity sterilization of functionalization strengthen sterilizing and antibacterial effect.
But vancomycin, titanium dioxide be there is no to report with the bactericide that the Nano Silver composite nanometer particle is combined.
Summary of the invention
The object of the invention is to provide a kind of selectivity bactericide and preparation and application of composite nanometer particle.
For achieving the above object, the technical solution used in the present invention is:
A kind of selectivity bactericide of composite nanometer particle: nano titanium oxide, 5～10% silica and the antibiotic of 0.01-1% of counting by weight Nano Silver, the 15-30% of 65-80%.
2. by the selectivity bactericide of composite nanometer particle claimed in claim 1, it is characterized in that:
Described Nano Silver particle diameter 70～90nm, nano titanium oxide particle diameter 10～30nm, the diameter of the whole nucleocapsid structure of selectivity bactericide of composite nanometer particle is 80～150nm.
Described antibiotic is the antibiotic to Gram-positive or the selective effect of Gram-negative bacteria.Described antibiotic is vancomycin or polymixin.
The preparation method of the selectivity bactericide of composite nanometer particle:
1) Nano silver grain: under the condition stirred, ammonia spirit is joined in the acid silver that concentration is 1-10mM, until reactant liquor becomes the silver ammino solution of clarification, then add the glucose of the 10-50ml that concentration is 10-300mM, obtain the Nano silver grain that particle diameter is 70～90nm;
2) the Nano Silver compound particle that titanium dioxide covers: above-mentioned Nano silver grain is joined in silester Nano silver grain fully is hydrolyzed, then acidifying in hydrochloric acid, the last mixed liquor that adds again isopropyl titanium and isopropyl alcohol, reaction 8-16 hour, obtain the Nano Silver compound particle that titanium dioxide covers;
3) the Nano Silver compound particle that the selectivity bactericide of composite nanometer particle: by step 2) gained titanium dioxide covers joins in dopamine solution, reaction 1-5 hour, then be connected with antibiotic by two cross-linking reagents, obtain the selectivity bactericide of composite nanometer particle.
Described step 1) after adding glucose in, add again 10-50ml, the sodium cetanesulfonate that concentration is 0.01-0.5M, and then make the pH of reaction system be transferred to 11.5 with sodium hydroxide, question response 3-10h, obtain Nano silver grain.Described step 2) Nano silver grain joins in silester when making the Nano silver grain hydrolysis and need add ammoniacal liquor and water, and Nano silver grain fully is hydrolyzed.Described step 3) in, two cross-linking reagents are suberic acid two (N-hydroxy ester); Antibiotic is the antibiotic to Gram-positive or the selective effect of Gram-negative bacteria.Described antibiotic is vancomycin or polymixin.
The application of the selectivity bactericide of composite nanometer particle: at ultraviolet or dark place, the bacterium for the antibiotic sensitive of Gram-positive or the selective effect of Gram-negative bacteria has bactericidal action to described selectivity bactericide.
The present invention has advantages of: the surface that the present invention modifies titanium dioxide and Nano Silver by the nucleocapsid structure of vancomycin functionalization obtains the sterilizing microbial inoculum of composite nanometer particle.The antibacterial agent of the functionalization of gained not only has bactericidal action under uviol lamp, has certain bactericidal action simultaneously under dark condition.Can also there is optionally sterilization in addition.
The accompanying drawing explanation
The XRD figure (wherein abscissa is 2 θ) that Fig. 1 is the prepared composite nanometer particle of the embodiment of the present invention.
Fig. 2 is that (wherein abscissa is wavelength Wavelength (nm) to the prepared functionalization bactericide ultraviolet-visible spectrum of the invention process; Curve a is vancomycin, the composite nanometer particle that curve b is titanium dioxide and Nano Silver, the titanium dioxide that curve c is the vancomycin functionalization and the composite nanometer particle of Nano Silver.)。
Embodiment
Below by embodiment, the present invention will be further described.
Embodiment 1
Get the 0.51g silver nitrate and be dissolved in 50ml water, then under the condition stirred, slowly add the ammoniacal liquor of 1.0M, start solution system flavescence look, then become the clarification silver ammino solution.Then under the condition stirred, add the glucose (0.1M) of 20ml, 10ml sodium cetanesulfonate (0.2M), finally be transferred to 11.5 to the pH of reaction system with sodium hydroxide again, reaction 5h, and reaction temperature is 25
-c, and the Nano silver grain that to obtain particle diameter be 70～90nm (referring to document J.Phys.Chem.C2008,112,5825-5834).The 0.1g Nano silver grain of getting preparation is dispersed in ethanolic solution, then adds 2.25ml ammoniacal liquor, 2.25ml water and 0.5 silester, reaction 4h.Obtain the Nano silver grain that silica covers.Then the Nano silver grain acidifying in the 0.5ml HCl silica of preparation covered, then add the mixed liquor of 0.5ml isopropyl titanium and 4.5ml isopropyl alcohol, react 8h.Can obtain the Nano Silver compound particle that titanium dioxide covers.Subsequently, the Nano Silver compound particle of getting the covering of 0.1g titanium dioxide joins in 50ml dopamine (20m M) solution, reaction 1h.The two cross-linking reagent DSS that are 1mg/ml by 10ml concentration again, load to its surface to vancomycin, obtains the selectivity bactericide of composite nanometer particle, and the diameter of the whole nucleocapsid structure of its bactericide is 80～150nm.
The test light degradation effect:
Get the above-mentioned selectivity bactericide for preparing the gained composite nanometer particle and the common nano particle that there is no a functionalization, the nano silver particles TiO of coated by titanium dioxide
2each 10mg of@Ag, join respectively 50ml, in the methylene blue solution system that concentration is 10mg/L, irradiate 60min apart from fluorescent tube 30cm under the 50W uviol lamp, then get solution and measure its light transmittance with uv-vis spectra, result is showed the nano particle that there is no functionalization, the nano silver particles light transmittance of coated by titanium dioxide is reduced to 0.051 about one hour, the methylene blue solution light transmittance of nano silver particles the present embodiment bactericide effect of the coated by titanium dioxide that same vancomycin is modified is reduced to 0.063. and wherein usings the light transmittance of the methylene blue that do not add the photocatalytic nanometer particle and do not have the nano particle of functionalization to have similar photocatalysis effect as the selectivity bactericide of 1. visible the present embodiment gained composite nanometer particles is common, the selectivity bactericide degradation efficiency of its gained composite nanometer particle of the present invention can reach more than 95%.
Embodiment 2
Difference from Example 1:
Get the 0.51g silver nitrate and be dissolved in 50ml water, then under the condition stirred, slowly add the ammoniacal liquor of 1.0M, start solution system flavescence look, then become the clarification silver ammino solution.Then under the condition stirred, the glucose (0.1M) that adds 20ml, 10ml sodium cetanesulfonate (0.2M), finally be transferred to 11.5 to the ph of reaction system with sodium hydroxide again, reaction 5h, obtain by hydrothermal synthesis method the Nano silver grain that particle diameter is 70～90nm.The 0.1g Nano silver grain of getting preparation is dispersed in ethanolic solution, then adds 2.25ml ammoniacal liquor, 2.25ml water and 0.5 silester, reaction 4h.Obtain the Nano silver grain that silica covers.Then the Nano silver grain acidifying in the 0.5ml HCl silica of preparation covered, then add the mixed liquor of 0.5ml isopropyl titanium and 4.5ml isopropyl alcohol, react 8h.Can obtain the Nano Silver compound particle that titanium dioxide covers.Subsequently, the Nano Silver compound particle of getting the covering of 0.1g titanium dioxide joins in 50ml dopamine (20m M) solution, reaction 1h.The two cross-linking reagent DSS that are 1mg/ml by 10ml concentration again, load to its surface to polymixin, obtains the selectivity bactericide of composite nanometer particle, and the diameter of the whole nucleocapsid structure of its bactericide is 80～150nm.
Embodiment 3
The sterilizing ability of gained bactericide in test implementation example 1.At 50ml sulfate reducing bacteria bacterium liquid 1.7 * 10
7in cfu/mL, add 25mg embodiment 1 gained bactericide, irradiate 60min apart from fluorescent tube 30cm under the 50W uviol lamp, then get 5ml bacterium liquid, by Maximum probable number method (MPN) (Abd-El-Malek and Y., Rizk, S.G., 1958.Nature 182 (4634), 538-538) microbe colony is counted, cultivated 15d in constant incubator, after both can having obtained irradiating 1h under uviol lamp, in bacterium liquid, bacterial content only has the bacterium colony of tens left and right, and the efficiency of its sterilization can reach 99%.
Embodiment 4
The sterilizing ability of gained bactericide in test implementation example 1.At 50ml sulfate reducing bacteria bacterium liquid (1.7 * 10
7cfu/mL) in, add 25mg embodiment 1 gained bactericide, stir 60min at the dark place, then get 5ml bacterium liquid, by Maximum probable number method, microbe colony is counted, cultivate 15d in constant incubator,, in bacterium liquid, bacterial content only has 10
4～10
5cfu/mL.Visible gained bactericide of the present invention also can have certain inhibitory action to microorganism at dark condition.
Embodiment 5
The sterilizing ability of gained bactericide in test implementation example 1.At 50ml sulfate reducing bacteria bacterium liquid (1.7 * 10
7cfu/mL) and 50ml Vibrio anguillarum (1.1 * 10
7cfu/mL) in, add respectively 25mg embodiment 1 gained bactericide, irradiate 60min apart from fluorescent tube 30cm under the 50W uviol lamp, then get 5ml bacterium liquid, cultivate 15d in constant incubator,, almost there is no microorganism in bacterium liquid for sulfate reducing bacteria, and only have 10 for the Vibrio anguillarum bacterial content
4～10
5cfu/mL.Visible gained microbial inoculum of the present invention has optionally bactericidal action.
Claims (8)
1. the selectivity bactericide of a composite nanometer particle is characterized in that: nano titanium oxide, 5～10% silica and the antibiotic of 0.01-1% of counting by weight Nano Silver, the 15-30% of 65-80%;
Described Nano Silver particle diameter 70～90nm, nano titanium oxide particle diameter 10～30nm, the diameter of the whole nucleocapsid structure of selectivity bactericide of composite nanometer particle is 80～150nm;
The preparation method of the selectivity bactericide of described composite nanometer particle is:
1) Nano silver grain: under the condition stirred, ammonia spirit is joined in the acid silver that concentration is 1-10mM, until reactant liquor becomes the silver ammino solution of clarification, then add the glucose of the 10-50ml that concentration is 10-300mM, obtain the Nano silver grain that particle diameter is 70～90nm;
2) the Nano Silver compound particle that titanium dioxide covers: above-mentioned Nano silver grain is joined in silester Nano silver grain fully is hydrolyzed, then acidifying in hydrochloric acid, the last mixed liquor that adds again isopropyl titanium and isopropyl alcohol, reaction 8-16 hour, obtain the Nano Silver compound particle that titanium dioxide covers;
3) the Nano Silver compound particle that the selectivity bactericide of composite nanometer particle: by step 2) gained titanium dioxide covers joins in dopamine solution, reaction 1-5 hour, then be connected with antibiotic by two cross-linking reagents, obtain the selectivity bactericide of composite nanometer particle;
Described step 1) after adding glucose in, add again 10-50ml, the sodium cetanesulfonate that concentration is 0.01-0.5M, and then make the pH of reaction system be transferred to 11.5 with sodium hydroxide, question response 3-10h, obtain Nano silver grain.
2. by the selectivity bactericide of composite nanometer particle claimed in claim 1, it is characterized in that: described antibiotic is the antibiotic to Gram-positive or the selective effect of Gram-negative bacteria.
3. by the selectivity bactericide of composite nanometer particle claimed in claim 2, it is characterized in that: described antibiotic is vancomycin or polymixin.
4. the preparation method by the selectivity bactericide of composite nanometer particle claimed in claim 1 is characterized in that:
1) Nano silver grain: under the condition stirred, ammonia spirit is joined in the acid silver that concentration is 1-10mM, until reactant liquor becomes the silver ammino solution of clarification, then add the glucose of the 10-50ml that concentration is 10-300mM, obtain the Nano silver grain that particle diameter is 70～90nm;
2) the Nano Silver compound particle that titanium dioxide covers: above-mentioned Nano silver grain is joined in silester Nano silver grain fully is hydrolyzed, then acidifying in hydrochloric acid, the last mixed liquor that adds again isopropyl titanium and isopropyl alcohol, reaction 8-16 hour, obtain the Nano Silver compound particle that titanium dioxide covers;
3) the Nano Silver compound particle that the selectivity bactericide of composite nanometer particle: by step 2) gained titanium dioxide covers joins in dopamine solution, reaction 1-5 hour, then be connected with antibiotic by two cross-linking reagents, obtain the selectivity bactericide of composite nanometer particle;
Described step 1) after adding glucose in, add again 10-50ml, the sodium cetanesulfonate that concentration is 0.01-0.5M, and then make the pH of reaction system be transferred to 11.5 with sodium hydroxide, question response 3-10h, obtain Nano silver grain;
Described Nano Silver particle diameter 70～90nm, nano titanium oxide particle diameter 10～30nm, the diameter of the whole nucleocapsid structure of selectivity bactericide of composite nanometer particle is 80～150nm.
5. press the preparation method of the selectivity bactericide of composite nanometer particle claimed in claim 4, it is characterized in that: described step 2) Nano silver grain joins in silester when making the Nano silver grain hydrolysis and need add ammoniacal liquor and water, and Nano silver grain fully is hydrolyzed.
6. press the preparation method of the selectivity bactericide of composite nanometer particle claimed in claim 4, it is characterized in that: described step 3), two cross-linking reagents are suberic acid two (N-hydroxy ester); Antibiotic is the antibiotic to Gram-positive or the selective effect of Gram-negative bacteria.
7. press the preparation method of the selectivity bactericide of composite nanometer particle claimed in claim 6, it is characterized in that: described antibiotic is vancomycin or polymixin.
8. the application by the non-therapeutic purposes of selectivity bactericide of composite nanometer particle claimed in claim 1 is characterized in that: described selectivity bactericide has the bactericidal action to the bacterium of Gram-positive or the selective antibiotic sensitive of Gram-negative bacteria in ultraviolet or dark place.
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| CN102719824A (en) * | 2012-06-12 | 2012-10-10 | 天津大学 | Dopamine-nanosilver composite coating and preparation method thereof |
| CN102845471B (en) * | 2012-07-27 | 2014-04-30 | 烟台大学 | Silver-based composite particle, preparation method of the silver-based composite particle and antibacterial agent containing the silver-based composite particle |
| CN103042227B (en) * | 2012-12-18 | 2014-12-31 | 广东省微生物研究所 | Nano-silver sol antibacterial agent and preparation method thereof |
| CN103894191B (en) * | 2014-04-15 | 2015-11-04 | 安徽大学 | A kind of layering Ag@TiO 2the preparation method of Core-shell Structure Nanoparticles |
| CN106729611A (en) * | 2015-11-23 | 2017-05-31 | 上海来益生物药物研究开发中心有限责任公司 | A kind of bacteria inhibiting composition |
| CN106818866A (en) * | 2016-12-13 | 2017-06-13 | 新昌县奥而特农业科技有限公司 | The bactericide of composite nanometer particle and its preparation and application |
| CN106818901A (en) * | 2016-12-13 | 2017-06-13 | 新昌县奥而特农业科技有限公司 | The medicament-fertilizer mixture of preventing and treating crops virus infection |
| CN106879630A (en) * | 2017-01-23 | 2017-06-23 | 嵊州市派特普科技开发有限公司 | Composite nanometer particle bactericide and its preparation and application |
| CN108187742A (en) * | 2018-01-03 | 2018-06-22 | 南京医科大学 | Nano composition, its synthetic method and purposes |
| CN112690287A (en) * | 2020-12-01 | 2021-04-23 | 张晓龙 | Novel inorganic nano photocatalyst bactericide spray and preparation method thereof |
| CN114831137B (en) * | 2022-05-24 | 2023-06-16 | 湖南普泰尔环境股份有限公司 | Deodorant with antibacterial effect |
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