CN111362264A - Oxygen-containing nano-diamond for antibacterial treatment and preparation method thereof - Google Patents

Oxygen-containing nano-diamond for antibacterial treatment and preparation method thereof Download PDF

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CN111362264A
CN111362264A CN202010198511.4A CN202010198511A CN111362264A CN 111362264 A CN111362264 A CN 111362264A CN 202010198511 A CN202010198511 A CN 202010198511A CN 111362264 A CN111362264 A CN 111362264A
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oxygen
diamond
nano
containing nano
antibacterial
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方蛟
李红东
刘钧松
周延民
王启亮
成绍恒
高楠
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Jilin University
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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
    • C01B32/25—Diamond
    • C01B32/28—After-treatment, e.g. purification, irradiation, separation or recovery
    • 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
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P1/00—Drugs for disorders of the alimentary tract or the digestive system
    • A61P1/02—Stomatological preparations, e.g. drugs for caries, aphtae, periodontitis
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P31/00—Antiinfectives, i.e. antibiotics, antiseptics, chemotherapeutics
    • A61P31/04—Antibacterial agents
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures

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Abstract

The invention relates to an oxygen-containing nano diamond for antibacterial treatment and a preparation method thereof, belonging to the technical field of medical antibacterial materials. The diameter of the oxygen-containing nano diamond is 5-10 nm, surface groups are carboxyl, carbonyl and hydroxyl, the surface oxygen content is 15-20%, and the preparation method comprises the following steps: dispersing the nano-diamond in H2SO4And HNO3Heating the mixture, adding the obtained sample into a sodium hydroxide solution, cooling and dialyzing, dispersing the product in hydrochloric acid, heating, dialyzing again and the like. The invention has simple and convenient preparation process, easy operation, low cost and preparationThe oxygen-containing nano-diamond has good peroxidase-like activity and good destruction effect on bacterial plaque biological membranes formed by periodontal pathogens.

Description

Oxygen-containing nano-diamond for antibacterial treatment and preparation method thereof
Technical Field
The invention belongs to the technical field of medical antibacterial materials, and particularly relates to an oxygen-containing nano-diamond for antibacterial treatment and a preparation method and application thereof.
Background
Periodontitis affects about 10-15% of the adult population worldwide, is an oral infectious disease caused by periodontal pathogens, which exists as a plaque biofilm and causes destruction of the supporting tissues of the teeth. Plaque biofilms consist of clusters of bacteria surrounded by extracellular macromolecules of bacteria that adhere strongly to the surfaces of teeth and periodontal tissues. The biofilm responsible for periodontitis, under the action of toxic species (such as Porphyromonas gingivalis), produces numerous virulence factors that directly or indirectly lead to destruction of periodontal tissues by modulating host inflammatory responses.
Current approaches to periodontitis-biofilm are limited to conventional antibacterial agents, including hydrogen peroxide (H)2O2) Chlorhexidine, and the like. Although chlorhexidine is able to kill bacteria in suspension, it is not as effective against plaque biofilm, does not prevent periodontitis, and is not suitable for daily oral use due to its adverse effects, including tartar formation and staining of teeth. In addition, H2O2As a medical reagent, the medical composition is widely used for wound disinfection and sterilization in oral clinical treatment. But used in oral disinfection H2O2The effect of the concentration (1-3%) on the plaque biofilm was not significant. And high concentration of H2O2Harmful to healthy tissue and even delay wound healing. Therefore, an antibacterial material with excellent biocompatibility is found, is applied to destroy dental plaque biomembranes, and provides a new way for preventing periodontal bacterial infection in the oral cavity.
At present, methods for treating bacterial infectious diseases are mostly limited to conventional antibiotics and antibacterial agents, but these inorganic antibacterial agents often have certain problems, such as easy generation of drug resistance, high cost, complex manufacturing process, or difficulty in treating or removing bacterial biofilms. Inspired by a number of enzymatic reactions within biological systems, peroxidases are capable of catalyzing oxidation or peroxidation of peroxides. Based on this catalytic effect, peroxide mimetics can be used as OH sensitizers for antibacterial therapy. However, further clinical applications of nanoenzymes are largely limited by their biological properties, and must strictly meet the requirements of biological safety and functionality.
The nano diamond is an important carbon-based nano material, and has low production cost and excellent physical and chemical properties. The nano-diamond has various oxygen-containing functional groups on the surface after oxidation treatment, has low cytotoxicity and good biocompatibility, and is widely applied to the biomedical fields of medicine carrying, biological marking and the like. Furthermore, the oxidized nanodiamond has peroxidase-like activity and can catalyze H2O2The bacterial plaque is decomposed and converted into hydroxyl free radical (. OH), and the bacterial plaque biological membrane is damaged, thereby having the treatment effect on bacterial infectious diseases.
The present invention relates to a method for purifying nano diamond, which is a Chinese patent application with application number 201810633095.9, and the method is characterized by that the nano diamond is purified in the mixed liquor of sulfuric acid and phosphoric acid so as to attain the goal of removing metal impurity and removing graphite. However, the reaction time of the nano-diamond prepared by the method is short, the oxygen-containing groups on the surface of the purified nano-diamond are few, and the nano-diamond does not have the property of peroxidase mimic enzyme and cannot be applied as an antibacterial material.
The present invention also relates to Chinese patent application No. 201910287560.2, which is similar to the present invention, and is green oxidized nano diamond monodisperse colloid solution and its preparation, secondary dispersing process and antibacterial application. However, the nano-diamond prepared by the method is not purified, only has the capacity of simply inhibiting the growth of bacteria, does not have peroxidase-like activity, cannot damage the formed bacterial plaque biomembrane, and is not suitable for clinical medical application.
Disclosure of Invention
The technical problem to be solved by the invention is to overcome the defects in the background technology, and prepare the traditional nano diamond particles by a simple and environment-friendly novel oxidation method to obtain a novel peroxide mimic enzyme material with low cost and good cell compatibility.
The specific technical scheme of the invention is as follows:
an oxygen-containing nano-diamond for antibacterial treatment is characterized in that the diameter of the oxygen-containing nano-diamond is 5-10 nm, surface groups are carboxyl, carbonyl and hydroxyl, and the surface oxygen content is 15-20%.
A preparation method of oxygen-containing nano-diamond for antibacterial therapy comprises the following steps:
1) dispersing the nano diamond with the diameter of 5-10 nm in H2SO4And HNO3In the mixture of (1), H2SO4And HNO3The volume ratio of (A) is 3:1, heating is carried out at the temperature of 90-120 ℃, and the heating lasts for 24 hours;
2) after the reaction is finished, adding the obtained sample into a sodium hydroxide solution for cooling, and dialyzing;
3) dispersing the dialyzed product in hydrochloric acid, heating at 90-120 deg.c for 2 hr, dialyzing again, and freeze drying to obtain oxygen-containing nanometer diamond.
The concentration of the hydrochloric acid in the step 3) is preferably 0.1 mol/L.
And (3) performing dialysis, preferably using a dialysis bag with the molecular weight cutoff of 3500-5000 kDa.
Has the advantages that:
the oxygen-containing nano-diamond prepared by the method has good peroxidase-like activity and has good destruction effect on bacterial plaque biological membranes formed by periodontal pathogenic bacteria. The surface of the obtained oxygen-containing nano-diamond contains rich oxygen-containing functional groups, the oxygen content reaches 15-20%, the oxygen-containing nano-diamond can efficiently catalyze the oxidation and decomposition of low-concentration hydrogen peroxide into hydroxyl radicals, and the oxygen-containing nano-diamond has strong antibacterial performance, can kill periodontal pathogenic bacteria and destroy a generated bacterial plaque biomembrane. The antibacterial performance is higher than that of the antibacterial capability of the pure hydrogen peroxide.
The oxygen-containing nano-diamond with peroxidase-like activity can be applied to treatment of periodontal pathogen infection, and the preparation process of the oxygen-containing nano-diamond is simple and convenient, easy to operate and low in cost.
Description of the drawings:
fig. 1 is a transmission electron microscope image of the prepared oxygen-containing nanodiamond.
Fig. 2 is an X-ray photoelectron spectrum of the prepared oxygen-containing nanodiamond.
Fig. 3 is a graph showing peroxidase activity detection of the prepared oxygen-containing nanodiamonds.
FIG. 4 is a cytotoxicity diagram of oxygen-containing nanodiamond detected by a CCK-8 experiment.
Fig. 5 is a graph of the antibacterial rate of oxygen-containing nano-diamond in combination with hydrogen peroxide to combat periodontal pathogens.
FIG. 6 is a scanning electron microscope image of oxygen-containing nanodiamond and low-concentration hydrogen peroxide for resisting periodontal pathogens.
Fig. 7 is a bacterial live/dead staining pattern of oxygen-containing nanodiamond and low-concentration hydrogen peroxide anti-plaque biofilm.
Detailed Description
The present application is described in further detail below with reference to the accompanying drawings and examples, which are intended to facilitate the understanding of the present application and are not intended to limit the same in any way.
Example 1 preparation of oxygen-containing nanodiamond
Synthesizing the oxygen-containing nano-diamond containing specific oxygen groups by adopting a chemical water bath method. Dispersing nano diamond powder with the diameter of 5-10 nm in H2SO4With HNO3In the mixture of (1), H2SO4With HNO3The volume ratio is 3:1, heating to 90 ℃, and keeping the reaction for 24 hours. After the reaction is finished, adding a sodium hydroxide solution into the sample for neutralization and cooling. The above samples were put into a dialysis bag with a cut-off molecular weight of 3500kDa for dialysis. Then, the dialyzed product was dispersed in 0.1mol/mL HCl solution at 90 deg.CThe mixture was heated for 2 hours. Finally, dialysis was performed again and the product was freeze-dried to obtain nanodiamonds (O-NDs) having abundant specific oxygen-containing groups (see FIG. 1 for transmission electron microscopy images), the surface oxygen content of which is shown in FIG. 2.
Example 2: enzyme activity detection of oxygen-containing nanodiamond
The absorbance value (625nm) of the O-NDs/TMB system was measured by an ultraviolet spectrophotometer, and the O-NDs was added to an acetic acid buffer solution (pH 4.0) having a reaction volume of 25mM at 25 ℃ for the experiment; before recording the absorbance, 1mM TMMB was added to start the reaction; by measuring O-NDs at 652 nm/TMB/H within 200 seconds2O2Changes in absorbance values within the system, and the peroxidase activity of O-NDs was analyzed using steady state kinetics. The results are shown in FIG. 3, where O-NDs are in H2O2In the presence of the compound, the compound can catalyze TMB to generate blue reaction and shows good peroxidase-like activity.
Example 3: cytotoxicity experimental detection of oxygen-containing nanodiamond
Third-generation log-phase-grown gingival fibroblasts were digested with 1mL of 0.25% trypsin as per 6 × 103The seed/well concentration is inoculated into a 24-well plate and placed in CO2Constant temperature incubator (5% CO)295% air, saturation humidity, 37 ℃) for 24h, changing the culture medium and adding O-NDs with the concentrations of 0. mu.g/mL, 25. mu.g/mL, 50. mu.g/mL, 100. mu.g/mL, 300. mu.g/mL, 500. mu.g/mL and the cell-free group (blank group), respectively. After culturing for 24h in a constant temperature incubator, 10. mu.L of CCK-8 solution is added to each well under the condition of keeping out of the light, and the incubator is incubated for 1.5 h. mu.L of each well was transferred to a 96-well plate, and absorbance was measured at 450nm using a microplate reader. The experimental results show that no concentration-dependent cytotoxicity effect of O-NDs is found when the O-NDs and cells are cultured for 24 hours. O-NDs at concentrations of 25. mu.g/mL, 50. mu.g/mL, 100. mu.g/mL, 300. mu.g/mL and 500. mu.g/mL had no effect on the cell viability of human gingival fibroblasts (as shown in FIG. 4).
Example 4: antibacterial performance detection of oxygen-containing nanodiamond
Porphyromonas gingivalis (P.g) using the gram-negative periodontal pathogeningivalis) was added to the BHI broth, and the concentration of the bacterial liquid was adjusted to 106CFU/mL. Bacteria were treated with different concentrations of H2O2Co-culturing, detecting bacterial survival rate and evaluating O-NDs combined with H2O2Antibacterial effect and antibacterial concentration of the antibacterial system on periodontal pathogenic bacteria. FIG. 5, O-NDs and H2O2The combined application can effectively enhance the single use of H2O2The antibacterial ability of (1). While NDs without oxygen treatment do not promote H2O2The antibacterial property of (1). When only H is present2O2Or in ND, the bacteriostatic action is reduced sharply, and the survival rate of Porphyromonas gingivalis is higher than 25%; when O-NDs and H are present2O2In the presence of both, the survival rate of P.gingivalis was significantly reduced to 9.5%.
Get 106Adding CFU/mL bacterial solution into control group, O-NDs group and H2O2Group and O-NDs + H2O2Culturing in an incubator for 24 hours under anaerobic conditions, taking out, washing with PBS, fixing with 2.5% glutaraldehyde, dehydrating with 50%, 70%, 80%, 90% and 100% absolute ethyl alcohol, spraying gold, dripping on a silicon wafer, and observing the bacterial forms of each group by using a scanning electron microscope. FIG. 6 shows that the shape of the bacteria with only O-NDs added is similar to that of the control group, and the bacteria are all oval and have smooth edges; and H2O2The smoothness of the edges of the visible thalli of the bacteria is reduced, and the surfaces of the visible thalli are rough; O-NDs + H2O2The cell membranes of the group bacteria are obviously broken, and the cytoplasm of the bacteria is exuded, so that the bacteria are finally killed. Demonstration of O-NDs with H2O2The combined application can further enhance H2O2The antibacterial property of (1) and inhibiting infectious diseases caused by bacteria.
Example 5: biofilm disruption capability detection of oxygen-containing nanodiamonds
The following materials were added to the plaque biofilm formed by Porphyromonas gingivalis. Control group: only 1mL of medium was added; h2O2Experimental groups: 100mM H2O2(ii) a O-NDs Experimental group: 100. mu.g/mL O-NDs; h2O2+ O-NDs Experimental group: 100mM H was added2O2And 100. mu.g/mL O-NDs for 15 minutes. LIVE/DEAD bacteria activity detection kit was used to examine the viability of bacteria within plaque biofilms. 2.5 μ M SYTO 9 stain was mixed with 2.5 μ M PI stain and each sample was stained for 15 minutes. Intact bacteria were stained with SYTO 9 to give green fluorescence, while membrane-damaged bacteria were stained with propidium iodide to show red fluorescence. Images of the biofilm were taken and collected with a confocal laser fluorescence microscope. The experimental results are shown in FIG. 7, the Porphyromonas gingivalis biofilms of the control group and the O-NDs group are relatively complete, and only a very small amount of bacteria die; through 100mMH2O2A small amount of dead bacteria appear in the treated single-strain plaque biomembrane, and the treated single-strain plaque biomembrane presents yellow-green alternate colors, which shows that the single low-concentration H is pure2O2The capacity of destroying the bacterial plaque biological film is limited, only partial bacteria on the surface layer of the biological film are killed, but bacteria in the deep layer of the film are not influenced, and the concentration H is low2O2Insufficient to combat plaque biofilm; while low concentrations of H are added with O-NDs2O2(H2O2+ O-NDs experimental group) all showed a mass-dead orange color, demonstrating H2O2the/O-NDs antimicrobial system is more effective in disrupting the formed Porphyromonas gingivalis biofilm. (note: the drawings described in this example have all been converted to grayscale pictures since the drawings of the patent application do not support color).

Claims (4)

1. An oxygen-containing nano-diamond for antibacterial treatment is characterized in that the diameter of the oxygen-containing nano-diamond is 5-10 nm, surface groups are carboxyl, carbonyl and hydroxyl, and the surface oxygen content is 15-20%.
2. A method for preparing oxygen-containing nanodiamond for antibacterial treatment according to claim 1, comprising the steps of:
1) dispersing the nano diamond with the diameter of 5-10 nm in H2SO4And HNO3In the mixture of (1), H2SO4And HNO3Is heated at 90-120 ℃ in a volume ratio of 3:1, and is continuously heated24 hours;
2) after the reaction is finished, adding the obtained sample into a sodium hydroxide solution for cooling, and dialyzing;
3) dispersing the dialyzed product in hydrochloric acid, heating at 90-120 deg.c for 2 hr, dialyzing again, and freeze drying to obtain oxygen-containing nanometer diamond.
3. The method for preparing oxygen-containing nanodiamonds for antibacterial treatment according to claim 2, wherein the concentration of hydrochloric acid in step 3) is 0.1 mol/L.
4. The method for preparing oxygen-containing nanodiamonds for antimicrobial therapy according to claim 2, wherein the dialysis in the step 2) and the step 3) uses a dialysis bag having a cut-off molecular weight of 3500 to 5000 kDa.
CN202010198511.4A 2020-03-19 2020-03-19 Oxygen-containing nano-diamond for antibacterial treatment and preparation method thereof Pending CN111362264A (en)

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Application publication date: 20200703