CN113527769B - Synthesis method of eucommia polysaccharide nano silver, synthesized eucommia polysaccharide nano silver and application thereof - Google Patents
Synthesis method of eucommia polysaccharide nano silver, synthesized eucommia polysaccharide nano silver and application thereof Download PDFInfo
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- A61Q17/005—Antimicrobial preparations
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- A61K2800/413—Nanosized, i.e. having sizes below 100 nm
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Abstract
The invention discloses a method for synthesizing eucommia polysaccharide nano-silver, which relates to the technical field of nano-silver and comprises the following steps: (1) mixing 5-10g/L eucommia polysaccharide solution with 0.5-1g/L silver nitrate solution according to a volume ratio of 1-5:2-5, shading, collecting precipitate, cleaning and drying to obtain eucommia polysaccharide nano-silver compound; (2) mixing the eucommia polysaccharide nano-silver compound, the mesoporous silica, the beta-cyclodextrin and the deionized water according to the mass ratio of 1-2:0.2-0.5:10-30:970-1000, stirring, centrifuging, and drying the precipitate to obtain the eucommia polysaccharide nano-silver. The invention also provides the eucommia polysaccharide nano silver synthesized by the method and application thereof. The invention has the beneficial effects that: the problems of high cost, easy agglomeration and the like of the synthesized nano silver are overcome, and on the other hand, the synthesized nano silver has polysaccharide coated load and strong stability.
Description
Technical Field
The invention relates to the technical field of nano silver, in particular to a method for synthesizing eucommia polysaccharide nano silver, the synthesized eucommia polysaccharide nano silver and application thereof.
Background
In modern life, due to the pollution of haze and corrosive substances in the air, the irradiation of sunlight by strong ultraviolet rays, the lack of attention to personal cleanness and sanitation and the like, facial skin loses moisture, luster and elasticity, becomes rough, deposits pigments, even causes bacterial infection to generate acne, and seriously affects the facial appearance and aesthetic feeling. The existing product for treating acne is mainly prepared from hormone, antibiotic, tretinoin, tartaric acid and the like, has high irritation and is easy to generate drug resistance, and can cause harm to human health after long-term use.
As a rare noble metal, silver has long been recognized as having antibacterial and bactericidal effects and is widely used in tableware, currency, jewelry, photography, dental material production, and anti-infectious treatment. In recent years, with the rapid development of nanotechnology, the nano-silver substance (nanosilver) becomes one of the nano-materials with great development potential due to its unique physicochemical and biological properties. Compared with the conventional Silver products, the Silver nanoparticles (Ag-NPs) not only have low biological toxicity, but also have the advantages of broad-spectrum antibacterial performance and high-efficiency antibacterial activity, more importantly, the Silver nanoparticles are not easy to cause the microorganisms to generate drug resistance and the like, become a new generation of excellent antibacterial agent, and are widely applied to various medical materials, such as wound dressings, medical surgical instruments, tissues implanted into human bodies and the like, and the production of antibacterial fibers, antibacterial coatings and the like. However, the conventional nano silver synthesis mainly adopts a physical and chemical method, including arc discharge, an energy ball milling method, a chemical reduction method, an electrochemical method, a radiation-assisted chemical method and the like. The methods either need special instruments and equipment and have high energy consumption, or involve the addition of toxic chemical reducing agents, stabilizing agents and dispersing agents, so that the application range of the nano silver in the biomedical field is limited. More importantly, when the particle size of the nano silver prepared by the traditional method is small or the concentration of the nano silver is high, the nano silver is easy to agglomerate, the accuracy of the subsequent toxicological experiment operation is influenced, a stabilizer must be added, the safety risk is increased, and the exertion of the antibacterial performance of the nano silver is limited.
The biological method for synthesizing the nano silver has the advantages of mild reaction conditions, low cost and environmental friendliness, and the synthesized nano silver has stronger stability than the nano silver synthesized by the conventional method, so the method becomes a research hotspot for synthesizing the nano silver at present. The plant extract is adopted to synthesize the nano-silver, so that the method is green and environment-friendly, the effects of the plant extract and the nano-silver can be organically combined, the nano-silver with various beneficial functions can be synthesized, and the application potential is huge. Polysaccharides (polysaccharides) are a fourth important class of biomacromolecules except nucleic acids, proteins and lipids, and have high yield and strong activity, and the application of the polysaccharides in the aspects of biomedicine, food production, cosmetics and the like is expanding in recent years. Eucommia ulmoides (Eucommia ulmoides) belongs to Eucommiaceae deciduous trees of Eucommiaceae of Hamamelidae of Magnoliaceae, and is a famous and precious medicinal plant in China. The eucommia polysaccharide extracted from eucommia bark and leaves has the functions of resisting bacteria, benefiting gallbladder, stopping bleeding, increasing leukocyte, resisting virus, etc.
Patent publication No. CN103949658A discloses a method for green synthesis of nano-silver by using water extract of eucommia, but the method synthesizes nano-silver by simply mixing the water extract of eucommia with silver nitrate, and because no load is added, the synthesized nano-silver still has the problems of poor stability and easy agglomeration. No report of a method for preparing nano-silver by utilizing eucommia ulmoides polysaccharide is found in the prior art.
Disclosure of Invention
The invention aims to solve the technical problems that in the prior art, the nano silver synthesized by adopting the eucommia ulmoides water extract still has the problems of poor stability and easy agglomeration, and provides a synthesis method of eucommia ulmoides polysaccharide nano silver, the synthesized eucommia ulmoides polysaccharide nano silver and application thereof.
The invention solves the technical problems through the following technical means:
a method for synthesizing eucommia polysaccharide nano-silver comprises the following steps:
(1) mixing 5-10g/L eucommia polysaccharide solution with 0.5-1g/L silver nitrate solution according to a volume ratio of 1-5:2-5, shading, collecting precipitate, cleaning and drying to obtain eucommia polysaccharide nano-silver compound;
(2) mixing the eucommia polysaccharide nano-silver compound, the mesoporous silica, the beta-cyclodextrin and the deionized water according to the mass ratio of 1-2:0.2-0.5:10-30:970-1000, stirring, centrifuging, and drying the precipitate to obtain the eucommia polysaccharide nano-silver.
Has the advantages that: the method utilizes the eucommia polysaccharide to synthesize the nano silver, on one hand, the problems that the cost for synthesizing the nano silver is high, the nano silver is easy to agglomerate, and residual chemicals in the synthesizing process can cause pollution and potential safety hazards in the prior art are solved, on the other hand, the synthesized nano silver has polysaccharide wrapping load and strong stability, and more importantly, the synthesized eucommia polysaccharide nano silver has stronger biological activity and has the antibacterial, anti-inflammatory and hemostatic effects of the nano silver and the eucommia polysaccharide.
Meanwhile, the eucommia polysaccharide nano silver is loaded by adopting the combined action of the mesoporous silica and the beta-cyclodextrin, so that the eucommia polysaccharide nano silver can form a stable nano sol system in an aqueous solution, the stability is strong, the biological safety is further enhanced, and the preparation of the nano silver is also greatly improved.
After the eucommia polysaccharide nano silver without the added load is placed for one week, a large amount of agglomerates can be generated; after the beta-cyclodextrin is loaded, the agglomeration phenomenon is relieved, and the particle size of the particles is reduced; after the silicon dioxide and the beta-cyclodextrin are jointly loaded, the stability is obviously enhanced, the particle size is small, and no obvious agglomeration phenomenon exists.
Preferably, shaking mixing is adopted in the step (1) for 8-14 h.
Preferably, the precipitate is collected by centrifugation at 10000-.
Preferably, the collected precipitate is dissolved with deionized water, and then centrifuged at 10000-.
Preferably, the step (2) is stirred at room temperature for 2-4h, and centrifuged at 10000-.
The invention also provides the eucommia polysaccharide nano silver synthesized by the method.
Has the advantages that: the nano silver synthesized by the invention has polysaccharide coating load and strong stability, and more importantly, the synthesized eucommia polysaccharide nano silver has stronger biological activity and has the antibacterial, anti-inflammatory and hemostatic effects of the nano silver and the eucommia polysaccharide.
Meanwhile, the synthesized eucommia polysaccharide nano silver forms a stable nano sol system in the water solution, so that the stability is strong, and the biological safety is further enhanced.
The invention also provides a preparation method of the eucommia polysaccharide nano-silver antibacterial and anti-inflammatory lotion, which comprises the following steps:
(1) preparation of the first mixture: mixing hexadecanol, lanolin, squalane, triethanolamine and deionized water according to the mass ratio of 1-2:2-3:1-2:2-5:980-1000, stirring, and then preserving heat at 75-80 ℃ to obtain a first mixture;
(2) preparation of the second mixture: mixing and stirring glycerol and deionized water according to the mass ratio of 5-10:90-95 to obtain a second mixture;
(3) preparation of the basic component: mixing the first mixture and the second mixture according to the volume ratio of 1:1, stirring and uniformly mixing, and then keeping the temperature at 70-80 ℃;
(4) and (3) cooling the basic component in the step (3) to 35-45 ℃, adding the prepared eucommia polysaccharide nano silver into the basic component according to the mass ratio of 1-5%, and stirring to obtain the eucommia polysaccharide nano silver antibacterial and anti-inflammatory lotion.
Has the advantages that: the eucommia polysaccharide nano silver is loaded by the combined action of the mesoporous silicon dioxide and the beta-cyclodextrin, so that the eucommia polysaccharide nano silver can form a stable nano sol system in an aqueous solution, the dispersity, the uniformity and the stability of the toning lotion are further improved, and the quality guarantee period and the effect of a product are prolonged.
Meanwhile, the nano-silver toning lotion has the antibacterial, anti-inflammatory and hemostatic effects of nano-silver and eucommia polysaccharide, the nano-silver toning lotion and the eucommia polysaccharide have synergistic effects, and compared with the traditional toning lotion, the nano-silver toning lotion prepared by the nano-silver toning lotion has stronger antibacterial and anti-inflammatory effects and better skin repairing effect.
Preferably, the stirring in step (1) is carried out at 75-80 ℃ for 4-8 h.
Preferably, the stirring in step (2) is carried out at 75-80 ℃ for 1-2 h.
Preferably, the temperature in the step (3) is kept at 70-80 ℃ for 30-60 min.
The invention also provides the eucommia polysaccharide nano-silver antibacterial and anti-inflammatory toning lotion prepared by the method.
Has the advantages that: the toning lotion disclosed by the invention has good dispersibility, uniformity and stability, and the shelf life and the efficacy of the product are prolonged.
Meanwhile, the nano-silver toning lotion has the antibacterial, anti-inflammatory and hemostatic effects of the nano-silver and the eucommia polysaccharide, the nano-silver toning lotion and the eucommia polysaccharide have a synergistic effect, and compared with the traditional toning lotion, the nano-silver toning lotion prepared from the nano-silver toning lotion has stronger antibacterial and anti-inflammatory effects and better skin repairing effect.
The invention has the advantages that: the method utilizes the eucommia polysaccharide to synthesize the nano silver, on one hand, the problems that the cost for synthesizing the nano silver is high, the nano silver is easy to agglomerate, and residual chemicals in the synthesizing process can cause pollution and potential safety hazards in the prior art are solved, on the other hand, the synthesized nano silver has polysaccharide wrapping load and strong stability, and more importantly, the synthesized eucommia polysaccharide nano silver has stronger biological activity and has the antibacterial, anti-inflammatory and hemostatic effects of the nano silver and the eucommia polysaccharide.
Meanwhile, the eucommia polysaccharide nano silver is loaded by adopting the combined action of the mesoporous silica and the beta-cyclodextrin, so that the eucommia polysaccharide nano silver can form a stable nano sol system in an aqueous solution, the stability is strong, the biological safety is further enhanced, and the preparation of the nano silver is also greatly improved.
After the eucommia polysaccharide nano silver without the added load is placed for one week, a large amount of agglomerates can be generated; after the beta-cyclodextrin is loaded, the agglomeration phenomenon is relieved, and the particle size of the particles is reduced; after the silicon dioxide and the beta-cyclodextrin are jointly loaded, the stability is obviously enhanced, the particle size is small, and no obvious agglomeration phenomenon exists.
The eucommia polysaccharide nano silver is loaded by the combined action of the mesoporous silicon dioxide and the beta-cyclodextrin, so that the eucommia polysaccharide nano silver can form a stable nano sol system in an aqueous solution, the dispersity, the uniformity and the stability of the toning lotion are further improved, and the quality guarantee period and the effect of a product are prolonged.
Meanwhile, the nano-silver toning lotion has the antibacterial, anti-inflammatory and hemostatic effects of nano-silver and eucommia polysaccharide, the nano-silver toning lotion and the eucommia polysaccharide have synergistic effects, and compared with the traditional toning lotion, the nano-silver toning lotion prepared by the nano-silver toning lotion has stronger antibacterial and anti-inflammatory effects and better skin repairing effect.
Drawings
Fig. 1 is an electron microscope image of eucommia ulmoides polysaccharide nano silver in example 1 of the present invention.
FIG. 2 shows the result of EDX spectroscopy analysis of the eucommia ulmoides polysaccharide nanosilver in example 1 of the present invention.
FIG. 3 is a diagram showing the bacteriostatic effect of different plant extract polysaccharides on Staphylococcus aureus and Pseudomonas aeruginosa according to the present invention.
Fig. 4 is a graph showing the comparison result of the antioxidant properties of the eucommia ulmoides polysaccharide nano silver and other polysaccharide nano silver in example 1 of the present invention.
FIG. 5 is a comparison graph of eucommia ulmoides polysaccharide nano silver synthesized by eucommia ulmoides polysaccharide and silver nitrate with different mass concentration ratios.
FIG. 6 is a graph showing the effect of the addition of the load on the stability of the eucommia ulmoides polysaccharide nano silver in comparative example 4, comparative example 5 and example 1.
Fig. 7 is a graph showing the stability comparison results of the nano-silver antiseptic and anti-inflammatory lotions prepared by the first mixture and the second mixture of the present invention and different ratios of silica/beta-cyclodextrin.
FIG. 8 is a scanning electron microscope image of the bacteriostatic effect of the nano-silver antibacterial anti-inflammatory water on Escherichia coli in example 1 of the present invention.
FIG. 9 shows the inhibitory effect of biological nano-silver antibacterial and anti-inflammatory astringent with different concentrations on Staphylococcus epidermidis.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The test materials and reagents used in the following examples, etc., are commercially available unless otherwise specified.
The specific techniques or conditions not specified in the examples can be performed according to the techniques or conditions described in the literature in the field or according to the product specification.
Eucommia ulmoides polysaccharide from the following examples was purchased
Example 1
The method for synthesizing the eucommia polysaccharide nano silver specifically comprises the following steps:
1) preparing an eucommia polysaccharide nano silver compound:
dissolving eucommia ulmoides polysaccharide in deionized water to prepare 5g/L eucommia ulmoides polysaccharide solution. Silver nitrate was dissolved in deionized water to prepare a 0.5g/L silver nitrate solution. Respectively taking the eucommia polysaccharide solution and the silver nitrate solution, mixing according to the volume ratio of 1:2, shading, shaking and mixing for 8 hours, centrifuging at 10000rpm for 10 minutes, and collecting the precipitate. The precipitate was dissolved in deionized water, centrifuged at 10000rpm for 10 minutes, the precipitate was collected, and the washing process was repeated 3 times. And freeze-drying the obtained brown precipitate to obtain the eucommia polysaccharide nano silver compound.
2) Eucommia polysaccharide nano silver load
Mixing the eucommia polysaccharide nano-silver, the mesoporous silicon dioxide, the beta-cyclodextrin and the deionized water according to the mass ratio of 1:0.2:10:990, stirring for 2 hours at room temperature, centrifuging for 10 minutes at 10000rpm, and freeze-drying the obtained precipitate to obtain the beta-cyclodextrin and silicon dioxide functionalized eucommia polysaccharide nano-silver.
The method for preparing the antibacterial and anti-inflammatory toning lotion by adopting the eucommia polysaccharide nano-silver in the embodiment 1 specifically comprises the following steps:
1) preparation of the first mixture
Mixing hexadecanol, lanolin, squalane, triethanolamine and deionized water according to the mass ratio of 1:2:1:2:1000, stirring for 4 hours at 75 ℃, and preserving heat for 30 minutes at 75 ℃ to obtain a first mixture.
2) Preparation of the second mixture
Mixing and stirring glycerol and deionized water according to the mass ratio of 5:95, and stirring for 1 hour at 75 ℃ to obtain a second mixture.
3) Preparation of the base component
Mixing the first mixture and the second mixture according to the volume ratio of 1:1, stirring and uniformly mixing, and then keeping the temperature at 70 ℃ for 30 minutes;
4) and (3) when the basic component prepared in the step 3) is cooled to 35 ℃, adding the eucommia polysaccharide nano-silver prepared in the embodiment 1 into the basic component according to the mass ratio of 1%, and uniformly stirring to obtain the novel biological nano-silver antibacterial and anti-inflammatory lotion.
Example 2
The method for synthesizing the eucommia polysaccharide nano silver specifically comprises the following steps:
1) preparing an eucommia polysaccharide nano silver compound:
dissolving eucommia ulmoides polysaccharide in deionized water to prepare 8g/L eucommia ulmoides polysaccharide solution. Silver nitrate was dissolved in deionized water to prepare a 1g/L silver nitrate solution. Respectively taking the eucommia polysaccharide solution and the silver nitrate solution, mixing according to the volume ratio of 5:2, shading, shaking and mixing for 14 hours, centrifuging at 15000rpm for 20 minutes, and collecting precipitates. The precipitate was dissolved in deionized water, centrifuged at 15000rpm for 20 minutes, the precipitate was collected, and the washing process was repeated 3 times. And freeze-drying the obtained brown precipitate to obtain the eucommia polysaccharide nano silver compound.
2) Eucommia polysaccharide nano silver load
Mixing the eucommia polysaccharide nano silver, the mesoporous silicon dioxide, the beta-cyclodextrin and the deionized water according to the mass ratio of 2:0.3:20:980, stirring for 4 hours at room temperature, centrifuging for 20 minutes at 15000rpm, and freeze-drying the obtained precipitate to obtain the beta-cyclodextrin and silicon dioxide functionalized eucommia polysaccharide nano silver.
The method for preparing the antibacterial and anti-inflammatory toning lotion by adopting the eucommia polysaccharide nano-silver in the embodiment 2 specifically comprises the following steps:
1) preparation of the first mixture
Mixing hexadecanol, lanolin, squalane, triethanolamine and deionized water according to the mass ratio of 1:3:1.5:5:985, stirring for 8 hours at 80 ℃, and preserving heat for 30 minutes at 80 ℃ to obtain a first mixture.
2) Preparation of the second mixture
Mixing and stirring glycerol and deionized water according to the mass ratio of 8:92, and stirring for 1 hour at 80 ℃ to obtain a second mixture.
3) Preparation of the base component
Mixing the first mixture and the second mixture according to the volume ratio of 1:1, stirring and uniformly mixing, and then keeping the temperature at 80 ℃ for 45 minutes;
4) and (3) when the basic component prepared in the step 3) is cooled to 40 ℃, adding the eucommia polysaccharide nano-silver prepared in the embodiment 2 into the basic component according to the mass ratio of 3%, and uniformly stirring to obtain the novel biological nano-silver antibacterial and anti-inflammatory lotion.
Example 3
The method for synthesizing the eucommia polysaccharide nano silver specifically comprises the following steps:
1) preparing an eucommia polysaccharide nano silver compound:
dissolving eucommia ulmoides polysaccharide in deionized water to prepare 10g/L eucommia ulmoides polysaccharide solution. Silver nitrate was dissolved in deionized water to prepare a 1g/L silver nitrate solution. Respectively taking the eucommia polysaccharide solution and the silver nitrate solution, mixing according to the volume ratio of 5:5, shading, shaking and mixing for 14 hours, centrifuging at 15000rpm for 15 minutes, and collecting precipitates. The precipitate was dissolved in deionized water, centrifuged at 15000rpm for 15 minutes, the precipitate was collected, and the washing process was repeated 3 times. And freeze-drying the obtained brown precipitate to obtain the eucommia polysaccharide nano silver compound.
2) Eucommia polysaccharide nano silver load
Mixing the eucommia polysaccharide nano-silver, the mesoporous silicon dioxide, the beta-cyclodextrin and the deionized water according to the mass ratio of 2:0.5:30:970, stirring for 3 hours at room temperature, centrifuging for 15 minutes at 15000rpm, and freeze-drying the obtained precipitate to obtain the beta-cyclodextrin and silicon dioxide functionalized eucommia polysaccharide nano-silver.
The method for preparing the antibacterial and anti-inflammatory toning lotion by adopting the eucommia polysaccharide nano-silver in the embodiment 3 specifically comprises the following steps:
1) preparation of the first mixture
Mixing hexadecanol, lanolin, squalane, triethanolamine and deionized water according to the mass ratio of 2:3:2:5:990, stirring for 6 hours at 80 ℃, and preserving heat for 50 minutes at 80 ℃ to obtain a first mixture.
2) Preparation of the second mixture
Mixing and stirring glycerol and deionized water according to the mass ratio of 10:90, and stirring for 2 hours at 80 ℃ to obtain a second mixture.
3) Preparation of the base component
Mixing the first mixture and the second mixture according to the volume ratio of 1:1, stirring and uniformly mixing, and then keeping the temperature at 80 ℃ for 60 minutes;
4) and (3) when the basic component prepared in the step 3) is cooled to 45 ℃, adding the eucommia polysaccharide nano-silver prepared in the embodiment 3 into the basic component according to the mass ratio of 5%, and uniformly stirring to obtain the novel biological nano-silver antibacterial and anti-inflammatory lotion.
Comparative example 1
Synthesizing psoralea polysaccharide nano silver: the eucommia ulmoides polysaccharide in example 1 was replaced with the same amount of psoralen polysaccharide.
The preparation method of the toning lotion comprises the following steps: the eucommia ulmoides polysaccharide nano silver in the embodiment 1 is replaced by the same amount of psoralen polysaccharide nano silver.
Comparative example 2
And (3) synthesis of bletilla polysaccharide nano silver: the eucommia ulmoides polysaccharide in the example 1 is replaced by equal amount of bletilla striata polysaccharide.
The preparation method of the toning lotion comprises the following steps: the eucommia ulmoides polysaccharide nano silver in the embodiment 1 is replaced by the bletilla striata polysaccharide nano silver with the same quantity.
Comparative example 3
Synthesizing sweet wormwood polysaccharide nano silver: the eucommia ulmoides polysaccharide in example 1 was replaced with the same amount of artemisia apiacea polysaccharide.
The preparation method of the toning lotion comprises the following steps: the eucommia polysaccharide nano silver in the embodiment 1 is replaced by the same amount of sweet wormwood polysaccharide nano silver.
Comparative example 4
This comparative example differs from example 1 in that: mesoporous silicon dioxide and beta-cyclodextrin are not added in the synthesis process of the eucommia polysaccharide nano silver, and then the synthesized eucommia polysaccharide nano silver is adopted to prepare the toning lotion.
Comparative example 5
This comparative example differs from example 1 in that: mesoporous silica is not added in the synthesis process of the eucommia polysaccharide nano silver, and then the synthesized eucommia polysaccharide nano silver is adopted to prepare the toning lotion.
Experimental data and analysis:
eucommia polysaccharide nano silver
Fig. 1 is an electron microscope image of the eucommia ulmoides polysaccharide nano silver in example 1, wherein the nano silver particles obtained in examples 1 to 3 are measured by a nano laser particle size analyzer, and the particle size ranges are 20 to 50 nm.
And (3) characterizing the element content in the eucommia polysaccharide nano silver sample by using an energy spectrometer (EDS). As shown in fig. 2, the EDX spectrum showed characteristic peaks of Ag, indicating that the prepared nanoparticles were nano silver particles.
The inhibition effect of different plant extract polysaccharides was determined by oxford cup method, and the results are shown in fig. 3 and table 1. FIG. 3 shows the bacteriostatic effect of polysaccharides extracted from different plants on Staphylococcus aureus EMRSA16 and Pseudomonas aeruginosa ATCC9027, wherein fructus Psoraleae represents aqueous solution of Psoralea corylifolia polysaccharide, rhizoma Bletillae represents aqueous solution of bletilla polysaccharide, herba Artemisiae Annuae represents aqueous solution of Artemisia annua polysaccharide, Eucommiae cortex represents aqueous solution of Eucommiae cortex polysaccharide, and Kan represents kanamycin. As can be seen from fig. 3, the eucommia ulmoides polysaccharide and Kan have good bacteriostatic effects on staphylococcus aureus, and the artemisia apiacea polysaccharide and the eucommia ulmoides polysaccharide have good bacteriostatic effects on pseudomonas aeruginosa.
Table 1 shows the bacteriostatic activity of eucommia ulmoides polysaccharide nano silver on several common pathogenic bacteria
Wherein the concentration of the eucommia ulmoides polysaccharide solution in the table 1 is 0.05 g/mL; eucommia ulmoides nano silver is eucommia ulmoides polysaccharide nano silver in example 2, and is dissolved in deionized water, wherein the concentration of the eucommia ulmoides polysaccharide nano silver is 0.05 g/mL; the silver nitrate is silver nitrate water solution with the concentration of 0.05 g/mL; kanamycin concentration was 50. mu.g/mL.
As can be seen from Table 1, the antibacterial performance of the eucommia polysaccharide nano-silver on Escherichia coli, Pseudomonas aeruginosa, Salmonella typhi and Staphylococcus aureus is obviously superior to that of the eucommia polysaccharide solution and silver nitrate, the eucommia polysaccharide and the nano-silver have a synergistic effect, and the antibacterial effect is similar to that of kanamycin.
According to the national standard GB/T39100-2020, the antioxidant capacity of nano silver of different polysaccharides is evaluated by adopting a DPPH free radical scavenging capacity test. As shown in fig. 4, it can be seen that the capacity of eucommia ulmoides nano silver for scavenging DPPH free radicals is significantly higher than that of psoralea corylifolia nano silver in comparative example 1, bletilla striata nano silver in comparative example 2 and artemisia apiacea nano silver in comparative example 3, and the difference is smaller compared with vitamin C.
FIG. 5 shows the eucommia ulmoides polysaccharide nano silver synthesized by eucommia ulmoides polysaccharide water solution, eucommia ulmoides polysaccharide and silver nitrate according to different mass concentration ratios. 1 is eucommia polysaccharide water solution with the concentration of 1mg/mL, and 2-6 is nano silver synthesized by eucommia polysaccharide and silver nitrate with different mass concentration ratios (1: 1,5:1,10:1,20:1 and 1:5 respectively). The figure shows that the synthesis efficiency of the nano silver is high when the mass concentration ratio of the eucommia polysaccharide to the silver nitrate is 10:1-20:1, and when the concentration of the silver nitrate is too high, the solution forms black particles, so that the synthesis efficiency is influenced.
Fig. 6 is an electron microscope image of the eucommia ulmoides polysaccharide nano silver without the loading substance (comparative example 4), the eucommia ulmoides polysaccharide nano silver loaded by beta-cyclodextrin (comparative example 5) and the eucommia ulmoides polysaccharide nano silver in example 1, respectively, from left to right, and it can be seen that a large amount of agglomerates can be generated after the eucommia ulmoides polysaccharide nano silver without the loading substance is placed for one week; after the beta-cyclodextrin is loaded, the agglomeration phenomenon is relieved, and the particle size of the particles is reduced; after the silicon dioxide and the beta-cyclodextrin are jointly loaded, the stability is obviously enhanced, the particle size is small, and no obvious agglomeration phenomenon exists. The electron microscopic results of the eucommia ulmoides polysaccharide nano silver in the other examples are the same as those of example 1.
(II) biological nano-silver antibacterial and anti-inflammatory toning lotion
Fig. 7 is a stability comparison of the first mixture and the second mixture and the nano-silver antiseptic and anti-inflammatory lotion prepared by different ratios of silicon dioxide/beta-cyclodextrin, which shows from left to right: the volume ratios of the first mixture and the second mixture are respectively 2:1, 1:1, 1:2 and 1: 3; the mass ratio of silicon dioxide to beta-cyclodextrin is 1:10, 3:20, 1:20 and 1:30 respectively. As can be seen, the different ratios of the first and second mixtures and the silica/β -cyclodextrin have a greater effect on the stability of the lotions. When the volume ratio of the first mixture to the second mixture is 1:1 and the mass ratio of the silicon dioxide to the beta-cyclodextrin is 3:20, the stability of the produced lotion is highest, and when the volume ratio of the first mixture to the second mixture exceeds 1:2, the lotion is easily turbid, precipitates appear, and the stability is deteriorated.
FIG. 8 is a scanning electron microscope image of the bacteriostatic effect of the nano-silver antibacterial anti-inflammatory water on Escherichia coli in example 1, and it can be seen that after Escherichia coli is treated with the anti-inflammatory water, the thallus of Escherichia coli becomes rough, wrinkles and irregularities appear, and the Escherichia coli is seriously ruptured, compared with an untreated group. The results of the remaining examples were the same as those of example 1.
FIG. 9 shows the inhibitory effect of biological nano-silver antibacterial and anti-inflammatory astringent on Staphylococcus epidermidis CMCC (B)26069 at different concentrations. 1,2 and 3 are biological nano-silver toning lotion, wherein the mass concentration of the nano-silver is 1 percent, 2 percent and 3 percent respectively. Van is vancomycin and the concentration is 3 mug/mL. When the mass concentration of the nano-silver in the toning lotion is 3%, the bacteriostatic effect is similar to that of kanamycin.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (10)
1. A method for synthesizing eucommia polysaccharide nano-silver is characterized by comprising the following steps: the method comprises the following steps:
(1) mixing 5-10g/L eucommia polysaccharide solution with 0.5-1g/L silver nitrate solution according to a volume ratio of 1-5:2-5, shading, collecting precipitate, cleaning and drying to obtain eucommia polysaccharide nano-silver compound;
(2) mixing the eucommia polysaccharide nano-silver compound, the mesoporous silica, the beta-cyclodextrin and the deionized water according to the mass ratio of 1-2:0.2-0.5:10-30:970-1000, stirring, centrifuging, and drying the precipitate to obtain the eucommia polysaccharide nano-silver.
2. The method for synthesizing eucommia ulmoides polysaccharide nano silver according to claim 1, which is characterized in that: in the step (1), shaking mixing is adopted for 8-14 h.
3. The method for synthesizing eucommia ulmoides polysaccharide nano silver according to claim 1, which is characterized in that: the precipitate is collected by centrifugation at 10000-.
4. The method for synthesizing eucommia ulmoides polysaccharide nano silver according to claim 1, which is characterized in that: dissolving the collected precipitate with deionized water, centrifuging at 10000-15000rpm for 10-20min, collecting the precipitate, and repeating the washing process for 2-3 times.
5. The method for synthesizing eucommia ulmoides polysaccharide nano silver as claimed in claim 1, wherein the method comprises the following steps: stirring at room temperature for 2-4h in the step (2), and centrifuging at 10000-.
6. Eucommia polysaccharide nanosilver synthesized by the method of any one of claims 1-5.
7. A preparation method of eucommia polysaccharide nano-silver antibacterial and anti-inflammatory lotion is characterized by comprising the following steps: the method comprises the following steps:
(1) preparation of the first mixture: mixing hexadecanol, lanolin, squalane, triethanolamine and deionized water according to the mass ratio of 1-2:2-3:1-2:2-5:980-1000, stirring, and then preserving heat at 75-80 ℃ to obtain a first mixture;
(2) preparation of the second mixture: mixing and stirring glycerol and deionized water according to the mass ratio of 5-10:90-95 to obtain a second mixture;
(3) preparation of the basic component: mixing the first mixture and the second mixture according to the volume ratio of 1:1, stirring and uniformly mixing, and then keeping the temperature at 70-80 ℃;
(4) cooling the basic component in the step (3) to 35-45 ℃, adding the eucommia polysaccharide nano silver synthesized by the method of any one of claims 1-5 into the basic component according to the mass ratio of the eucommia polysaccharide nano silver to the basic component of 1-5%, and stirring to obtain the eucommia polysaccharide nano silver antibacterial and anti-inflammatory lotion.
8. The method for preparing the eucommia ulmoides polysaccharide nano-silver antibacterial and anti-inflammatory lotion according to claim 7, which is characterized by comprising the following steps: stirring for 4-8h at 75-80 ℃ in the step (1).
9. The method for preparing the eucommia ulmoides polysaccharide nano-silver antibacterial and anti-inflammatory lotion according to claim 7, which is characterized by comprising the following steps: stirring for 1-2h at 75-80 ℃ in the step (2).
10. An eucommia ulmoides polysaccharide nano silver antibacterial and anti-inflammatory lotion prepared by the method of any one of claims 7 to 9.
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