CN113876998A - Antibacterial bone cement and preparation method thereof - Google Patents
Antibacterial bone cement and preparation method thereof Download PDFInfo
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- CN113876998A CN113876998A CN202111171622.7A CN202111171622A CN113876998A CN 113876998 A CN113876998 A CN 113876998A CN 202111171622 A CN202111171622 A CN 202111171622A CN 113876998 A CN113876998 A CN 113876998A
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- 239000002639 bone cement Substances 0.000 title claims abstract description 72
- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title abstract description 13
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 claims abstract description 115
- 239000000843 powder Substances 0.000 claims abstract description 73
- 239000002131 composite material Substances 0.000 claims abstract description 46
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 45
- 239000004332 silver Substances 0.000 claims abstract description 45
- 229910000367 silver sulfate Inorganic materials 0.000 claims abstract description 36
- 239000007788 liquid Substances 0.000 claims abstract description 28
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N Hydroquinone Chemical compound OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000004342 Benzoyl peroxide Substances 0.000 claims abstract description 13
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims abstract description 13
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims abstract description 13
- 235000019400 benzoyl peroxide Nutrition 0.000 claims abstract description 13
- GYVGXEWAOAAJEU-UHFFFAOYSA-N n,n,4-trimethylaniline Chemical compound CN(C)C1=CC=C(C)C=C1 GYVGXEWAOAAJEU-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 10
- 229920000058 polyacrylate Polymers 0.000 claims abstract description 9
- 229910052709 silver Inorganic materials 0.000 claims abstract description 9
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 60
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 30
- 238000002156 mixing Methods 0.000 claims description 27
- 238000001035 drying Methods 0.000 claims description 12
- 238000005245 sintering Methods 0.000 claims description 8
- 238000000498 ball milling Methods 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 2
- 229920003229 poly(methyl methacrylate) Polymers 0.000 abstract description 9
- 239000004926 polymethyl methacrylate Substances 0.000 abstract description 9
- 239000000463 material Substances 0.000 abstract description 3
- 239000003242 anti bacterial agent Substances 0.000 abstract description 2
- 230000010478 bone regeneration Effects 0.000 abstract description 2
- 238000012360 testing method Methods 0.000 description 6
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 4
- 230000006835 compression Effects 0.000 description 3
- 238000007906 compression Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 108020000946 Bacterial DNA Proteins 0.000 description 2
- 241000588724 Escherichia coli Species 0.000 description 2
- 230000004071 biological effect Effects 0.000 description 2
- 229910000389 calcium phosphate Inorganic materials 0.000 description 2
- 239000001506 calcium phosphate Substances 0.000 description 2
- 235000011010 calcium phosphates Nutrition 0.000 description 2
- 230000004663 cell proliferation Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000003013 cytotoxicity Effects 0.000 description 2
- 231100000135 cytotoxicity Toxicity 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 description 2
- 239000004925 Acrylic resin Substances 0.000 description 1
- 229920000178 Acrylic resin Polymers 0.000 description 1
- 241000894006 Bacteria Species 0.000 description 1
- 230000004543 DNA replication Effects 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 239000004599 antimicrobial Substances 0.000 description 1
- 230000001580 bacterial effect Effects 0.000 description 1
- 230000003385 bacteriostatic effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000005313 bioactive glass Substances 0.000 description 1
- 210000000988 bone and bone Anatomy 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 210000002421 cell wall Anatomy 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000004925 denaturation Methods 0.000 description 1
- 230000036425 denaturation Effects 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910052588 hydroxylapatite Inorganic materials 0.000 description 1
- 238000000338 in vitro Methods 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- XYJRXVWERLGGKC-UHFFFAOYSA-D pentacalcium;hydroxide;triphosphate Chemical compound [OH-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O XYJRXVWERLGGKC-UHFFFAOYSA-D 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- -1 silver ions Chemical class 0.000 description 1
- GGCZERPQGJTIQP-UHFFFAOYSA-N sodium;9,10-dioxoanthracene-2-sulfonic acid Chemical compound [Na+].C1=CC=C2C(=O)C3=CC(S(=O)(=O)O)=CC=C3C(=O)C2=C1 GGCZERPQGJTIQP-UHFFFAOYSA-N 0.000 description 1
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/02—Inorganic materials
- A61L27/04—Metals or alloys
- A61L27/047—Other specific metals or alloys not covered by A61L27/042 - A61L27/045 or A61L27/06
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/02—Inorganic materials
- A61L27/025—Other specific inorganic materials not covered by A61L27/04 - A61L27/12
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/14—Macromolecular materials
- A61L27/16—Macromolecular materials obtained by reactions only involving carbon-to-carbon unsaturated bonds
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
- A61L27/54—Biologically active materials, e.g. therapeutic substances
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/10—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing inorganic materials
- A61L2300/102—Metals or metal compounds, e.g. salts such as bicarbonates, carbonates, oxides, zeolites, silicates
- A61L2300/104—Silver, e.g. silver sulfadiazine
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/40—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a specific therapeutic activity or mode of action
- A61L2300/404—Biocides, antimicrobial agents, antiseptic agents
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2430/00—Materials or treatment for tissue regeneration
- A61L2430/02—Materials or treatment for tissue regeneration for reconstruction of bones; weight-bearing implants
Abstract
The invention relates to the technical field of biomedical materials, in particular to antibacterial bone cement and a preparation method thereof. The antibacterial bone cement is prepared from powder and liquid according to the addition ratio of (1-3) g: 1mL, and the powder mainly comprises the following raw materials in percentage by mass: 55-89% of polyacrylate, 10-40% of silver and barium sulfate composite powder and 1-5% of benzoyl peroxide; the liquid mainly comprises the following raw materials in percentage by mass: 0.5 to 5 percent of N, N-dimethyl-p-toluidine, 0.05 to 2 percent of hydroquinone and 93 to 99.45 percent of methyl methacrylate. According to the invention, silver and barium sulfate are compounded and then added into PMMA, and the silver element is uniformly dispersed, so that the antibacterial agent has the characteristics of good antibacterial property and high strength, and also has good biocompatibility and bone regeneration.
Description
Technical Field
The invention relates to the technical field of biomedical materials, in particular to antibacterial bone cement and a preparation method thereof.
Background
The most widely used bone cement in clinical practice is acrylic resin bone cement (PMMA). The epoxy resin has the advantages of high mechanical strength, high curing speed and the like, but has the following significant defects: the elastic modulus is 4-40 times of that of the spongy bone of the vertebral body, and excessively high elastic modulus leads to excessive increase of the hardness of the formed vertebral body and stress concentration, so that the adjacent vertebral body is compressed and fractured again; lack biological activity, can not be degraded and absorbed, exist in the vertebral body in the form of foreign bodies for a long time, and the like. In order to overcome the defects of PMMA, substitute materials including calcium phosphate bone cement, calcium sulfate bone cement and composite bone cement of the calcium phosphate bone cement and the calcium sulfate bone cement are researched, but the mechanical strength and the degradation speed are not ideal.
Silver has been extensively studied as one of the most common antimicrobial agents, such as silver hydroxyapatite coatings [ DiNunzio S, Vitale Brovarone C, Spriano S, et al. silver containing bioactive glasses p prepared by molybdenum salton-exchange. J Eur ceramic Soc,2004,24: 2935-: 2383-. It has been shown that silver ions can penetrate the cell wall of bacteria and can cause structural denaturation of bacterial DNA, hindering bacterial DNA replication and thereby causing bacterial death. However, no report has been found on the research of directly using silver salt to reduce silver to enhance antibacterial property of bone cement during the preparation process of bone cement.
Disclosure of Invention
The invention aims to provide antibacterial bone cement and a preparation method thereof, which overcome the defects of the prior art, compound silver and barium sulfate, and add the compound silver and barium sulfate into PMMA, so that silver is uniformly dispersed, and the antibacterial bone cement has the characteristics of good antibacterial property and high strength, and also has good biocompatibility and bone regeneration.
The technical scheme adopted by the invention for solving the technical problems is as follows:
an antibacterial bone cement is prepared from powder and liquid according to the addition ratio of (1-3) g: 1mL, wherein: the powder mainly comprises the following raw materials in percentage by mass: 55-89% of polyacrylate, 10-40% of silver and barium sulfate composite powder and 1-5% of benzoyl peroxide; the liquid mainly comprises the following raw materials in percentage by mass: 0.5 to 5 percent of N, N-dimethyl-p-toluidine, 0.05 to 2 percent of hydroquinone and 93 to 99.45 percent of methyl methacrylate.
Preferably, in the silver and barium sulfate composite powder, silver accounts for 0.3-5% of the total mass of the silver and barium sulfate composite powder.
Preferably, the particle size of the silver and barium sulfate composite powder is 0.5-45 μm.
A preparation method of antibacterial bone cement comprises the following steps:
s1, preparing a silver nitrate solution with the mass percentage of 1-20%;
s2, adding the barium sulfate powder into a silver nitrate solution, and mixing for 10-60min, wherein the mass ratio of barium sulfate to silver nitrate solution is 2-4: 1;
s3, drying the mixture in an oven for 5 to 24 hours after mixing, and performing ball milling after drying to obtain 0.5 to 45 mu m silver nitrate and barium sulfate composite powder;
s4, transferring the silver nitrate and barium sulfate composite powder into a sintering furnace to be sintered for 2-8h, then gradually cooling to room temperature, and grinding to obtain 0.5-45 mu m silver and barium sulfate composite powder.
S5, uniformly mixing the prepared silver and barium sulfate composite powder with polyacrylate and benzoyl peroxide according to a specified mass percentage to obtain bone cement powder; uniformly mixing N, N-dimethyl-p-toluidine, hydroquinone and methyl methacrylate according to the specified mass percentage to obtain bone cement liquid;
s6, mixing the powder with the liquid (1-3) g: and adding the bone cement liquid into the bone cement powder according to the proportion of 1mL, uniformly stirring, and curing to obtain the antibacterial bone cement.
Preferably, the temperature of the oven in the step S3 is 60-120 ℃.
Preferably, the temperature of the sintering furnace in the step S4 is maintained at 450-700 ℃.
The invention has the beneficial effects that: compared with the prior art, the invention has the advantages thatThe bone cement and the preparation method thereof have the following advantages: the invention uses Ag/BaSO4As a developer and an antibacterial agent, the problem of uniform mixing of silver powder in PMMA is solved, certain antibacterial property is given to bone cement, and the biological activity, antibacterial property and strength of the bone cement are enhanced.
Drawings
FIG. 1 is a graph showing the inhibition cycle of the antibacterial bone cement prepared in example 1 against the gram-negative bacterium Escherichia coli.
Detailed Description
Example 1
The antibacterial bone cement mainly comprises the following raw materials in percentage by mass: the powder comprises 55% of polyacrylate, 40% of silver and barium sulfate composite powder and 5% of benzoyl peroxide; the liquid comprises 0.5 percent of N, N-dimethyl-p-toluidine, 0.05 percent of hydroquinone and 99.45 percent of methyl methacrylate; in the silver and barium sulfate composite powder, the mass percentage of Ag in the silver and barium sulfate composite powder is 0.5%.
The preparation method of the antibacterial bone cement comprises the following steps:
s1, preparing a silver nitrate solution with the mass percentage of 1.57%;
s2, adding the barium sulfate powder into a silver nitrate solution, and mixing for 60min, wherein the mass ratio of barium sulfate to the silver nitrate solution is 2: 1;
s3, drying in an oven at 120 ℃ for 5 hours, and ball-milling to obtain silver nitrate/barium sulfate composite powder of 0.5-45 mu m after drying;
s4, transferring the silver nitrate/barium sulfate composite powder into a sintering furnace, keeping the temperature for 8 hours at 450 ℃, gradually cooling to room temperature, and grinding to obtain the silver/barium sulfate composite powder with the particle size of 0.5-45 mu m.
S5, uniformly mixing the prepared silver/barium sulfate composite powder with PMMA and benzoyl peroxide according to the proportion to obtain bone cement powder; uniformly mixing N, N-dimethyl-p-toluidine, hydroquinone and methyl methacrylate according to the specified mass percentage to obtain bone cement liquid;
s6, mixing powder and liquid 3 g: and adding the bone cement liquid into the bone cement powder according to the proportion of 1mL, uniformly stirring, and curing to obtain the antibacterial bone cement.
The bone cement is made into a disc shape of phi 12mm multiplied by 2mm, and an antibacterial experiment is carried out on the disc shape, as shown in figure 1, a bacteriostatic ring is clear and distinguishable, which shows that the antibacterial bone cement has good antibacterial property on escherichia coli.
Example 2
The antibacterial bone cement mainly comprises the following raw materials in percentage by mass: the powder comprises 89% of polyacrylate, 10% of silver and barium sulfate composite powder and 1% of benzoyl peroxide; the liquid comprises 5 percent of N, N-dimethyl-p-toluidine, 2 percent of hydroquinone and 93 percent of methyl methacrylate; in the silver and barium sulfate composite powder, the mass percentage of Ag in the silver and barium sulfate composite powder is 5%.
The preparation method of the antibacterial bone cement in the embodiment comprises the following steps:
s1, preparing a silver nitrate solution with the mass percentage of 20%;
s2, adding the barium sulfate powder into a silver nitrate solution, and mixing for 30min, wherein the mass ratio of barium sulfate to the silver nitrate solution is 2.54: 1;
s3, drying for 24 hours in an oven at 60 ℃, and performing ball milling after drying to obtain silver nitrate/barium sulfate composite powder of 0.5-45 mu m;
s4, transferring the silver nitrate/barium sulfate composite powder into a sintering furnace, keeping the temperature for 2 hours at 700 ℃, gradually cooling to room temperature, and grinding to obtain 0.5-45 mu m silver and barium sulfate composite powder.
S5, uniformly mixing the prepared silver and barium sulfate composite powder with PMMA and benzoyl peroxide according to the proportion to obtain bone cement powder; uniformly mixing N, N-dimethyl-p-toluidine, hydroquinone and methyl methacrylate according to the specified mass percentage to obtain bone cement liquid;
s6, mixing powder and liquid 1 g: and adding the bone cement liquid into the bone cement powder according to the proportion of 1mL, uniformly stirring, and curing to obtain the antibacterial bone cement.
Example 3
The antibacterial bone cement mainly comprises the following raw materials in percentage by mass: the powder comprises 68% of polyacrylate, 30% of silver and barium sulfate composite powder and 2% of benzoyl peroxide; the liquid comprises 2 percent of N, N-dimethyl-p-toluidine, 0.1 percent of hydroquinone and 97.9 percent of methyl methacrylate. In the silver and barium sulfate composite powder, the mass percentage of Ag in the silver and barium sulfate composite powder is 1%.
The preparation method of the antibacterial bone cement comprises the following steps:
s1, preparing a silver nitrate solution with the mass percentage of 4.78%;
s2, adding the barium sulfate powder into a silver nitrate solution, and mixing for 30min, wherein the mass ratio of barium sulfate to the silver nitrate solution is 3: 1;
s3, drying in an oven at 100 ℃ for 24 hours, and ball-milling to obtain silver nitrate/barium sulfate composite powder of 0.5-45 mu m after drying;
s4, transferring the silver nitrate/barium sulfate composite powder into a sintering furnace, keeping the temperature for 4 hours at 600 ℃, gradually cooling to room temperature, and grinding to obtain 0.5-45 mu m silver and barium sulfate composite powder.
S5, uniformly mixing the prepared silver and barium sulfate composite powder with PMMA and benzoyl peroxide according to the proportion to obtain bone cement powder; uniformly mixing N, N-dimethyl-p-toluidine, hydroquinone and methyl methacrylate according to the specified mass percentage to obtain bone cement liquid;
s6, mixing powder and liquid 2 g: and adding the bone cement liquid into the bone cement powder according to the proportion of 1mL, uniformly stirring, and curing to obtain the antibacterial bone cement.
Example 4
The antibacterial bone cement mainly comprises the following raw materials in percentage by mass: the powder comprises 73 percent of polyacrylate, 25 percent of silver and barium sulfate composite powder and 2 percent of benzoyl peroxide; the liquid comprises 1.5 percent of N, N-dimethyl-p-toluidine, 1 percent of hydroquinone and 97.5 percent of methyl methacrylate. In the silver and barium sulfate composite powder, the mass percentage of Ag in the silver and barium sulfate composite powder is 0.3%.
The preparation method of the antibacterial bone cement comprises the following steps:
s1, preparing a silver nitrate solution with the mass percentage of 1%;
s2, adding the barium sulfate powder into a silver nitrate solution, and mixing for 10-60min, wherein the mass ratio of barium sulfate to the silver nitrate solution is 2: 1;
s3, drying in an oven at 120 ℃ for 5h, and ball-milling to obtain silver nitrate/barium sulfate composite powder of 0.5-45 mu m after drying;
s4, transferring the silver nitrate/barium sulfate composite powder into a sintering furnace, keeping the temperature for 2 hours at 700 ℃, gradually cooling to room temperature, and grinding to obtain 0.5-45 mu m silver and barium sulfate composite powder.
S5, uniformly mixing the prepared silver and barium sulfate composite powder with PMMA and benzoyl peroxide according to the proportion to obtain bone cement powder; uniformly mixing N, N-dimethyl-p-toluidine, hydroquinone and methyl methacrylate according to the specified mass percentage to obtain bone cement liquid;
s6, mixing powder and liquid 2 g: and adding the bone cement liquid into the bone cement powder according to the proportion of 1mL, uniformly stirring, and curing to obtain the antibacterial bone cement.
Test example 1
The antibacterial bone cement prepared in examples 1 to 4 was filled in a sample preparation mold, and after curing, samples having a diameter of 6.0mm and a length of 12mm were obtained, and the samples were subjected to a compressive strength test on a universal mechanical testing machine, and an average compression modulus was measured, and the test results are shown in table 1:
TABLE 1
| Test items | Example 1 | Example 2 | Example 3 | Example 4 |
| Average compressive Strength (MPa) | 83.52 | 103.15 | 94.28 | 95.87 |
| Average modulus of compression (MPa) | 2453.15 | 2600.30 | 3025.48 | 2607.36 |
As can be seen from Table 1, the bone cements prepared in examples 1 to 4 of the present invention have excellent compression resistance.
The bone cements resulting from examples 1-4 were tested for cytotoxicity using the MTT method, and the results are shown in table 2:
TABLE 2
| Test items | Example 1 | Example 2 | Example 3 | Example 4 |
| Relative cell proliferation Rate (%) | 96 | 88 | 84 | 95 |
| Rank of | Class I | Class I | Class I | Class I |
As can be seen from Table 2, the relative cell proliferation rates of the bone cements prepared in examples 1 to 4 of the present invention are all class I, and meet the requirements for in vitro cytotoxicity.
The above embodiments are only specific examples of the present invention, and the protection scope of the present invention includes but is not limited to the product forms and styles of the above embodiments, and any suitable changes or modifications made by those skilled in the art according to the claims of the present invention shall fall within the protection scope of the present invention.
Claims (6)
1. An antibacterial bone cement, which is characterized in that: mainly comprises powder and liquid according to the addition ratio (1-3) g: 1mL, wherein: the powder mainly comprises the following raw materials in percentage by mass: 55-89% of polyacrylate, 10-40% of silver and barium sulfate composite powder and 1-5% of benzoyl peroxide; the liquid mainly comprises the following raw materials in percentage by mass: 0.5 to 5 percent of N, N-dimethyl-p-toluidine, 0.05 to 2 percent of hydroquinone and 93 to 99.45 percent of methyl methacrylate.
2. An antibacterial bone cement according to claim 1, characterized in that: in the silver and barium sulfate composite powder, the silver accounts for 0.3-5% of the total mass of the silver and barium sulfate composite powder.
3. An antibacterial bone cement according to claim 1, characterized in that: the grain diameter of the silver and barium sulfate composite powder is 0.5-45 mu m.
4. The method for preparing antibacterial bone cement according to claim 1, characterized in that: the method comprises the following steps:
s1, preparing a silver nitrate solution with the mass percentage of 1-20%;
s2, adding the barium sulfate powder into a silver nitrate solution, and mixing for 10-60min, wherein the mass ratio of barium sulfate to silver nitrate solution is 2-4: 1;
s3, drying the mixture in an oven for 5 to 24 hours after mixing, and performing ball milling after drying to obtain 0.5 to 45 mu m silver nitrate and barium sulfate composite powder;
s4, transferring the silver nitrate and barium sulfate composite powder into a sintering furnace to be sintered for 2-8h, then gradually cooling to room temperature, and grinding to obtain 0.5-45 mu m silver and barium sulfate composite powder.
S5, uniformly mixing the prepared silver and barium sulfate composite powder with polyacrylate and benzoyl peroxide according to a specified mass percentage to obtain bone cement powder; uniformly mixing N, N-dimethyl-p-toluidine, hydroquinone and methyl methacrylate according to the specified mass percentage to obtain bone cement liquid;
s6, mixing the powder with the liquid (1-3) g: and adding the bone cement liquid into the bone cement powder according to the proportion of 1mL, uniformly stirring, and curing to obtain the antibacterial bone cement.
5. The method for preparing antibacterial bone cement according to claim 4, wherein: the temperature of the oven in the step S3 is 60-120 ℃.
6. The method for preparing antibacterial bone cement according to claim 4, wherein: the temperature of the sintering furnace in the step S4 is maintained at 450-700 ℃.
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| US4526909A (en) * | 1984-01-09 | 1985-07-02 | Regents Of The University Of California | Polymethylmethacrylate delivery system for bone morphogenetic protein |
| CN102380126A (en) * | 2011-10-28 | 2012-03-21 | 中国医学科学院北京协和医院 | Novel nano silver bone cement |
| CN102863166A (en) * | 2012-09-26 | 2013-01-09 | 中国科学院宁波材料技术与工程研究所 | Synthesis method of bone cement containing surface-modification nano barium sulfate |
| WO2014185600A1 (en) * | 2013-05-15 | 2014-11-20 | 한국세라믹기술원 | Bone cement composition and preparation method therefor |
| CN106075587A (en) * | 2016-06-07 | 2016-11-09 | 山东明德生物医学工程有限公司 | Polynary codope bone cement and preparation method |
| CN107982576A (en) * | 2017-11-27 | 2018-05-04 | 山东明德生物医学工程有限公司 | A kind of bone cement and preparation method |
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| US4526909A (en) * | 1984-01-09 | 1985-07-02 | Regents Of The University Of California | Polymethylmethacrylate delivery system for bone morphogenetic protein |
| CN102380126A (en) * | 2011-10-28 | 2012-03-21 | 中国医学科学院北京协和医院 | Novel nano silver bone cement |
| CN102863166A (en) * | 2012-09-26 | 2013-01-09 | 中国科学院宁波材料技术与工程研究所 | Synthesis method of bone cement containing surface-modification nano barium sulfate |
| WO2014185600A1 (en) * | 2013-05-15 | 2014-11-20 | 한국세라믹기술원 | Bone cement composition and preparation method therefor |
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