CN117815453A - Preparation method of sisal fiber reinforced chitosan-based antibacterial porous material with high osteogenesis activity - Google Patents
Preparation method of sisal fiber reinforced chitosan-based antibacterial porous material with high osteogenesis activity Download PDFInfo
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- 229920001661 Chitosan Polymers 0.000 title claims abstract description 60
- 239000011148 porous material Substances 0.000 title claims abstract description 44
- 239000000835 fiber Substances 0.000 title claims abstract description 29
- 244000198134 Agave sisalana Species 0.000 title claims abstract description 28
- 230000000844 anti-bacterial effect Effects 0.000 title abstract description 38
- 230000000694 effects Effects 0.000 title abstract description 14
- 230000011164 ossification Effects 0.000 title abstract description 10
- 238000002360 preparation method Methods 0.000 title abstract description 9
- 229910052586 apatite Inorganic materials 0.000 claims abstract description 41
- VSIIXMUUUJUKCM-UHFFFAOYSA-D pentacalcium;fluoride;triphosphate Chemical compound [F-].[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 VSIIXMUUUJUKCM-UHFFFAOYSA-D 0.000 claims abstract description 26
- IMQLKJBTEOYOSI-GPIVLXJGSA-N Inositol-hexakisphosphate Chemical compound OP(O)(=O)O[C@H]1[C@H](OP(O)(O)=O)[C@@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@@H]1OP(O)(O)=O IMQLKJBTEOYOSI-GPIVLXJGSA-N 0.000 claims abstract description 22
- IMQLKJBTEOYOSI-UHFFFAOYSA-N Phytic acid Natural products OP(O)(=O)OC1C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C1OP(O)(O)=O IMQLKJBTEOYOSI-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000000467 phytic acid Substances 0.000 claims abstract description 22
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- OGSPWJRAVKPPFI-UHFFFAOYSA-N Alendronic Acid Chemical compound NCCCC(O)(P(O)(O)=O)P(O)(O)=O OGSPWJRAVKPPFI-UHFFFAOYSA-N 0.000 claims abstract description 15
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- 239000000243 solution Substances 0.000 claims description 27
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- DHEQXMRUPNDRPG-UHFFFAOYSA-N strontium nitrate Chemical compound [Sr+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O DHEQXMRUPNDRPG-UHFFFAOYSA-N 0.000 claims description 8
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- 230000002188 osteogenic effect Effects 0.000 abstract description 9
- 229910052712 strontium Inorganic materials 0.000 abstract description 7
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 abstract description 7
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- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 6
- 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 6
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- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
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- 208000001132 Osteoporosis Diseases 0.000 description 1
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- Materials For Medical Uses (AREA)
Abstract
The invention discloses a sisal fiber reinforced chitosan-based antibacterial porous material with high osteogenic activity and a preparation method thereof. The porous material has strong ion crosslinking effect due to the sisal fiber of polyanion and the chitosan acid solution of cation, so that the mechanical property of the porous material is greatly improved; the added hybridized nano apatite is doped with strontium and contains a small amount of alendronate, so that the osteogenesis activity is better; in addition, phytic acid is also introduced into the hybridized nano-apatite to chelate the hybridized nano-apatite, and sodium houttuyfonate is also loaded in the porous material, so that the slow and fast dual-release antibacterial effect can be coordinated. The novel porous material has rich sources of raw materials, the preparation method is simple and easy to implement, the mechanical property, degradation property, osteogenesis activity and antibacterial property of the novel porous material can be regulated and controlled by changing the content of each component of the porous material, and the novel porous material is expected to obtain the bone tissue engineering scaffold material with excellent performance.
Description
Technical Field
The invention relates to a sisal fiber reinforced chitosan-based antibacterial porous material with high osteogenic activity and a preparation method thereof, belonging to the field of biomedical materials.
Background
The porous material is used as a carrier of cells and signal molecules, can provide a special microstructure and microenvironment for bone tissue growth, plays a vital role in new bone growth, and is a key problem in bone tissue engineering research. The clinical bone tissue engineering scaffold material must meet the following conditions: has a porous structure with high mechanical strength, good bone conductivity, good bone inducibility and proper degradation rate, and has good antibacterial property. Based on the bionic principle, the preparation of porous materials by compounding the inorganic component nano hydroxyapatite (n-HA) of natural bone and Chitosan (CS) polymer with good biocompatibility is considered as the first choice research object of the bone tissue engineering scaffold. However, in clinical application, the chitosan matrix HAs poor mechanical properties and n-HA nano particles are easy to agglomerate, so that the high-strength n-HA/CS composite material is difficult to obtain, particularly, the interpenetrating highly porous structure required by the tissue engineering scaffold is more difficult to maintain the stress of bone tissue regeneration due to the mechanical properties; in addition, the synthesized n-HA structural component generally does not contain trace components such as carbonate, fluorine, silicon, magnesium, sodium and the like in the biological apatite, so that the osteogenesis activity is poorer than that of the biological apatite, and the vascularized bone formation is difficult to meet; meanwhile, the traditional n-HA/CS composite scaffold HAs insufficient antibacterial property, is difficult to prevent the repeatability and the tardiness of bacterial infection in orthopaedics operation areas, and is easy to directly cause bone tissue repair failure. Therefore, the problems of insufficient mechanical property, osteogenesis activity, antibacterial property and the like of the traditional n-HA/CS composite scaffold are the problems to be solved in the bone tissue engineering scaffold material.
To improve the mechanical properties of n-HA/CS, metal ion, aldehyde or crown ether type cross-linking agents are generally used to cross-link chitosan, but the remaining toxic cross-linking agents are harmful to human body. The chitosan is subjected to ionic crosslinking by adopting the polyanion polymer, so that the mechanical property of the chitosan can be effectively improved, and particularly, the mechanical property of the CS-based composite material can be improved by using some carboxylated modified natural fibers for chitosan crosslinking. Sisal fibers have the characteristics of high mechanical strength, abrasion resistance, corrosion resistance, green and renewable properties and the like, and have been widely applied to polymer reinforced materials. Therefore, if sisal fiber is carboxylated into polyanion high polymer for ionic crosslinking with chitosan, the mechanical properties of the n-HA/CS porous composite material are expected to be improved.
In order to improve the osteogenic activity of the sisal fiber reinforced n-HA/CS material, researchers based on the component bionic principle carry out doping on various microelements such as carbonate, silicon, strontium and the like in the biological apatite on the n-HA, so that the biological performance of the n-HA can be improved, and the doping of the strontium is more advantageous. In addition, alendronate sodium is an anti-osteoporosis drug with strong anti-bone resorption capability, and two terminal groups of biphosphate in the structure of the alendronate sodium have special affinity with n-HA, and are usually fixed on the surface of n-HA through chemical bonding so as to exert a lasting effect of promoting the osteogenesis activity. Literature [ACS Appl. Mater. & Inter. 2018, 10: 25547-25560]Demonstration of alendronate and Fe 3 O 4 Can self-assemble on the surface of nano apatite, and has remarkable promotion effect on osteoblasts. Therefore, if the alendronate and the trace element strontium are introduced together to prepare the hybridized nano-apatite, the sisal fiber reinforced n-HA/CS material is expected to be endowed with higher osteogenic activity.
In order to improve the antibacterial property of the sisal fiber reinforced n-HA/CS material, the phytic acid is a natural nontoxic small molecule with unique biological activity widely existing in plant seeds, fruits and vegetables, the phytic acid determines the super-strong chelating property due to the unique structure (the cyclic molecule contains six phosphate groups and 12 free hydrogen), and meanwhile, the research discovers that the phytic acid HAs the functions of oxidation resistance, anticancer, antibacterial and the like, and the antibacterial functions of the phytic acidThe antimicrobial film properties can be used not only in dentistry, but also to provide new strategies for other fields where antimicrobial resistance is required. Literature [Inter J Appl Ceram Tech, 2022, 19: 1498-1510]The strong chelating property of phytic acid is reported to be applicable to the preparation of hydroxyapatite, and simultaneously, higher antibacterial property is also ensured. Therefore, if phytic acid, alendronate and strontium are introduced together, the hybrid nano-apatite with high osteogenic activity and lasting antibacterial property is expected to be prepared.
In order to further improve the antibacterial property of the sisal fiber reinforced hybrid nano-apatite/CS porous material, an effective method is adopted to directly load antibacterial drugs on the porous material so as to enable the porous material to exert antibacterial effect through rapid release in the initial stage. The houttuynin sodium which is the main active component of houttuynin has stable chemical structure, has a certain antibacterial effect on escherichia coli, staphylococcus aureus, pseudomonas aeruginosa, candida albicans and the like besides the antibacterial effect in vivo, wherein the effects on staphylococcus aureus and candida albicans are most obvious. With the further development of medicine, researchers also find that sodium houttuyfonate has a certain effect in the aspect of treating osteoporosis, so that if herba houttuyniae is loaded in the sisal fiber reinforced hybrid nano apatite/CS porous material, the sodium houttuyfonate can play a dual antibacterial effect of rapid and lasting release together with the chelated phytic acid in the hybrid nano apatite structure so as to better meet the antibacterial property of the bone tissue engineering scaffold.
Disclosure of Invention
In view of the above, the present invention aims to provide a chitosan-based antibacterial porous material with high osteogenic activity reinforced by sisal fibers and a preparation method thereof. The porous material prepared by the invention has better mechanical property, osteogenesis activity, antibacterial activity and biocompatibility, is a novel degradable porous material, and can meet the basic requirements of the bone tissue engineering scaffold material.
The invention adopts the following technical scheme: sisal fibers refer to carboxylated modified hemp fibers; chitosan is
The degree of deacetylation is more than 90%, and the viscosity average molecular weight is about 40 ten thousand; phytic acid is a 70% aqueous solution purchased in the market; the hybridized nano-apatite refers to hybridized nano-apatite prepared by co-introducing strontium-doped, alendronate and phytic acid; houttuynin refers to sodium houttuyfonate powder purchased from market.
The surface carboxylated sisal fiber is characterized in that the sisal fiber (average length is 0.5-1 mm) is firstly treated with 8% NaOH solution and H 2 O 2 Pretreating and stirring for 2 hours at room temperature, washing with water to neutrality, drying, adding into citric acid solution with concentration of 10% (m/v), wherein the citric acid content is 4 times of the mass of sisal fibers, simultaneously adding potassium dihydrogen phosphate with the mass of 30% of sisal fibers, stirring for 1 hour at room temperature, heating to 120 ℃ for reaction for 3 hours, washing with water to neutrality, and drying to obtain the sisal fibers with carboxylated surfaces.
The hybridized nano apatite is characterized in that strontium nitrate and calcium nitrate are dissolved in aqueous solution, wherein the content of the strontium nitrate is that the mole ratio of Sr/(Sr+Ca) is 2-10%, phytic acid is added for reaction for 1 hour, and solution A is set, wherein the content of phosphate radical in the phytic acid accounts for 10-40% of the mole ratio of total phosphate radical; adding 5-10wt% of alendronate into sodium phosphate solution, reacting for 1 hr to obtain solution B, slowly dripping solution B into solution A, maintaining Ca/P molar ratio at 1.67, regulating pH to above 10 with 1 mol/L sodium hydroxide, heating at 70deg.C for 5 hr under stirring, aging for 48 hr, washing with deionized water to neutrality, drying, and grinding into powder.
The invention provides a fibrilia-reinforced chitosan-based antibacterial composite porous material with high osteogenesis activity, which is realized by the following technical scheme and is characterized by adopting the following process steps:
adding water into a certain amount of fibrilia, performing ultrasonic dispersion, slowly dripping ultrasonic dispersion hybridized nano apatite slurry, adding a certain amount of chitosan powder and houttuynin sodium powder, mechanically stirring at a high speed for 4 hours, and adding glacial acetic acid with the concentration of 2% to obtain compound gel; freezing at-20deg.C for 12 hr, and freeze drying; the dried porous material was soaked in 10% NaOH solution for 30 minutes, then washed with deionized water to neutrality, and dried under vacuum at 40 ℃ to constant weight.
Compared with the existing porous material, the porous material has the advantages that:
(1) The natural fibrilia and chitosan used in the invention are natural degradable polymers with good biocompatibility, and the raw materials have wide sources and low price; and the natural fibrilia is negatively charged after carboxylation modification, and can generate ionic crosslinking with positively charged chitosan solution, so that the mechanical property of the composite porous material is improved, and the support stress for cell adhesion proliferation is favorably provided; the added hybridized nano-apatite is doped with strontium, alendronate and phytic acid, wherein the microelements strontium and alendronate can endow the nano-hydroxyapatite with better bone conductivity and can be continuously and slowly released; more importantly, the introduced phytic acid has antibacterial property, and can play a role of slow and quick release double-bed antibacterial effect in cooperation with sodium houttuyfonate loaded in the porous material; in addition, due to the introduction of the alendronate and the phytic acid molecules, the hybrid nano-apatite structure has a certain steric hindrance effect, but the nano-hydroxyapatite particles have better dispersibility, so that the hybrid nano-apatite structure has good interface compatibility with a sisal fiber-chitosan matrix, and the mechanical property of the hybrid nano-apatite structure is better. In conclusion, the natural sisal fibers and the hybridized nano apatite selected by the invention are beneficial to improving the mechanical property, the osteogenic activity and the antibacterial property of the n-HA/CS composite porous material.
(2) The sisal fiber reinforced chitosan-based antibacterial composite porous material with high osteogenic activity provided by the invention has the advantages of simple and feasible preparation process, low production cost, environment friendliness and suitability for mass production; and the mechanical property, degradation property, bone conductivity and antibacterial property of the porous composite material can be regulated and controlled by regulating the content of each component so as to obtain the bone tissue engineering scaffold material meeting various performance requirements.
Drawings
Fig. 1 is an SEM photograph of a sisal fiber reinforced chitosan-based antibacterial composite porous material with high osteogenic activity. (a) internal microstructure of the porous material under the low power mirror, (b) internal microstructure of the porous material under the high power mirror, (c) surface microstructure of the porous material under the low power mirror (d) surface microstructure of the porous material under the high power mirror.
Description of the embodiments
Example 1: dispersing 1.0 g carboxylated modified fibrilia in 100 ml deionized water, adding 3.0 g chitosan, simultaneously dispersing 5.5 g hybridized nano-apatite containing 5 wt% of alenphosphate, 2% of Sr molar content and 10% of phytic acid molar content in 100 ml deionized water, dripping the dispersed solution into the mixed solution of fibrilia and chitosan, adding 0.2 g sodium houttuyfonate, continuing ultrasonic magnetic stirring for 4 h, and adding 4 ml glacial acetic acid to obtain the ternary composite gel of fibrilia/chitosan and hybridized nano-apatite. Freezing 24. 24 h in a refrigerator at-20deg.C, and lyophilizing to constant weight. Finally, the mixture is placed in 10 percent NaOH solution for soaking for 30 minutes, washed to be neutral and dried. The obtained product was cut into a block of 10 mm ×10 mm ×10 mm, and the obtained product was measured to have a compressive strength of about 0.5 MPa, a porosity of 78% and an average pore diameter of 300 μm; the in vitro simulated body fluid is soaked in 8 w, a large amount of bone-like apatite is deposited on the surface, and the compressive strength can still be maintained at about 0.3 MPa; the antibacterial rate is 90%.
Example 2: dispersing 1.5. 1.5 g carboxylated modified fibrilia in 100 ml deionized water, adding 2.0 g chitosan, simultaneously dispersing 1.0 g containing 10wt% of alendronate, 10% of Sr molar content and 30% of phytic acid molar content in 150 ml deionized water, dripping the dispersed 1.0 g into the mixed solution of fibrilia and chitosan, adding 0.4. 0.4 g sodium houttuyfonate, continuing ultrasonic magnetic stirring for 4 h, and adding 5 ml glacial acetic acid to obtain the ternary composite gel of fibrilia/chitosan and hybridized nano apatite. Freezing 24. 24 h in a refrigerator at-20deg.C, and lyophilizing to constant weight. Finally, the mixture is placed in 10 percent NaOH solution for soaking for 30 minutes, washed to be neutral and dried. The obtained product was cut into a block of 10 mm ×10 mm ×10 mm, and the obtained product was measured to have a compressive strength of about 0.6 MPa, a porosity of 74% and an average pore diameter of 260 μm; the in vitro simulated body fluid is soaked in 8 w, a large amount of bone-like apatite is deposited on the surface, and the compressive strength can still be maintained at about 0.4 MPa; the antibacterial rate is 93%.
Example 3: dispersing 2.0 g carboxylated modified fibrilia in 200 ml deionized water, adding 2.0 g chitosan, simultaneously dispersing 1.0 g containing 5 wt% of alenphosphate, 10% of Sr molar content and 40% of phytic acid molar content in 150 ml deionized water, dripping the dispersed solution into the mixed solution of fibrilia and chitosan, adding 0.6 g sodium houttuyfonate, continuing ultrasonic magnetic stirring for 4 h, and adding 7 ml glacial acetic acid to obtain the ternary composite gel of fibrilia, chitosan and hybridized nano apatite. Freezing 24. 24 h in a refrigerator at-20deg.C, and lyophilizing to constant weight. Finally, the mixture is placed in 10 percent NaOH solution for soaking for 30 minutes, washed to be neutral and dried. The obtained product was cut into a block of 10 mm ×10 mm ×10 mm, and the obtained product was measured to have a compressive strength of about 0.8 MPa, a porosity of 75% and an average pore diameter of 250 μm; the in vitro simulated body fluid is soaked in 8 w, a large amount of bone-like apatite is deposited on the surface, and the compressive strength can still be maintained at about 0.4 MPa; the antibacterial rate is 95%.
Example 4: dispersing 1.0 g carboxylated modified fibrilia in 100 ml deionized water, adding 2.0 g chitosan, simultaneously dispersing 5.0 g hybridized nano-apatite containing 5 wt% of alenphosphate, 10% of Sr molar content and 40% of phytic acid molar content in 150 ml deionized water, dripping the dispersed solution into the mixed solution of fibrilia and chitosan, adding 0.4 g sodium houttuyfonate, continuing ultrasonic magnetic stirring for 4 h, and adding 5 ml glacial acetic acid to obtain the ternary composite gel of fibrilia/chitosan and hybridized nano-apatite. Freezing 24. 24 h in a refrigerator at-20deg.C, and lyophilizing to constant weight. Finally, the mixture is placed in 10 percent NaOH solution for soaking for 30 minutes, washed to be neutral and dried. The obtained product was cut into a block of 10 mm ×10 mm ×10 mm, and the obtained product was measured to have a compressive strength of about 0.7 MPa, a porosity of 76% and an average pore diameter of 320 μm; the in vitro simulated body fluid is soaked in 8 w, a large amount of bone-like apatite is deposited on the surface, and the compressive strength can still be maintained at about 0.4 MPa; the antibacterial rate was 94%.
Comparative example 1: weighing 2.0 g chitosan, adding 100 ml deionized water, adding 2 ml glacial acetic acid, stirring until the solution is dissolved, dripping 1.0 g nano hydroxyapatite into 100 ml water, and continuing ultrasonic magnetic stirring for 2 h to obtain the nano hydroxyapatite/chitosan binary composite gel. Freezing 24. 24 h in a refrigerator at-20deg.C, and lyophilizing to constant weight. Then soaking in 10% NaOH solution for 30 min, washing to neutrality, and drying. The obtained product was cut into a block of 10 mm ×10 mm ×10 mm, and the obtained product was found to have a compressive strength of about 0.3 MPa, a porosity of 75% and an average pore diameter of 160 um; soaking 4 w in vitro simulated body fluid, wherein the porous material is degraded into powder; the antibacterial rate is 60%.
Comparative example 2: dispersing 1.0 g unmodified fibrilia in 100 ml deionized water, adding 2.0 g chitosan, simultaneously dispersing 5 wt% of alendronate, 10% of Sr mol content and 40% of phytic acid mol content of hybridized nano apatite in 150 ml deionized water by ultrasonic dispersion, then dripping the dispersed nano apatite into the mixed solution of fibrilia and chitosan, adding 0.4 g sodium houttuyfonate, continuing ultrasonic magnetic stirring for 4 h, and adding 5 ml glacial acetic acid to obtain the ternary composite gel of fibrilia, chitosan and hybridized nano apatite. Freezing 24. 24 h in a refrigerator at-20deg.C, and lyophilizing to constant weight. Finally, the mixture is placed in 10 percent NaOH solution for soaking for 30 minutes, washed to be neutral and dried. The obtained product was cut into a block of 10 mm ×10 mm ×10 mm, and the obtained product was measured to have a compressive strength of about 0.5 MPa, a porosity of 75% and an average pore diameter of 280 μm; the in vitro simulated body fluid is soaked in 8 w, a large amount of bone-like apatite is deposited on the surface, and the compressive strength can still be maintained at about 0.2 MPa; the antibacterial rate is 93%.
Comparative example 3: dispersing 1.0 g carboxylated modified fibrilia in 100 ml deionized water, adding 2.0 g chitosan, simultaneously dispersing 1.0 g nano hydroxyapatite in 150 ml deionized water by ultrasonic, dripping the dispersed 1.0 nano hydroxyapatite in the mixed solution of the fibrilia and the chitosan, adding 0.4 g sodium houttuyfonate, continuing ultrasonic magnetic stirring for 4 h, and adding 5 ml glacial acetic acid to obtain the ternary composite gel of the fibrilia, the chitosan and the hybridized nano apatite. Freezing 24. 24 h in a refrigerator at-20deg.C, and lyophilizing to constant weight. Finally, the mixture is placed in 10 percent NaOH solution for soaking for 30 minutes, washed to be neutral and dried. The obtained product was cut into a block of 10 mm ×10 mm ×10 mm, and the obtained product was measured to have a compressive strength of about 0.5 MPa, a porosity of 77% and an average pore diameter of 320 μm; the in vitro simulated body fluid is soaked in 8 w, a small amount of bone-like apatite is deposited on the surface, and the compressive strength can still be maintained at about 0.3 MPa; the antibacterial rate was 94%.
Comparative example 4: dispersing 1.0 g carboxylated modified fibrilia in 100 ml deionized water, adding 2.0 g chitosan, simultaneously dispersing 5 wt% of alendronate, 10% of Sr mol content and 40% of phytic acid mol content of hybridized nano-apatite in 150 ml deionized water, then dripping the dispersed nano-apatite into the mixed solution of fibrilia and chitosan, continuing ultrasonic magnetic stirring for 4 h, and adding 5 ml glacial acetic acid to obtain the ternary composite gel of fibrilia, chitosan and hybridized nano-apatite. Freezing 24. 24 h in a refrigerator at-20deg.C, and lyophilizing to constant weight. Finally, the mixture is placed in 10 percent NaOH solution for soaking for 30 minutes, washed to be neutral and dried. The obtained product was cut into a block of 10 mm ×10 mm ×10 mm, and the obtained product was measured to have a compressive strength of about 0.4 MPa, a porosity of 76% and an average pore diameter of 300 μm; the in vitro simulated body fluid is soaked in 8 w, a large amount of bone-like apatite is deposited on the surface, and the compressive strength can still be maintained at about 0.2 MPa; the antibacterial rate is 65%.
Compressive strength test conditions: the cut 10 mm ×10× 10 mm ×10 mm block material was tested for compression set to 40% by a universal material tester (sanctum 4503, shenzhen SANS corporation, china). The test temperature was 20 ℃ + -2℃and the loading rate was 1 mm/min. Five replicates were tested for each group and the results averaged.
Determination of porosity: adding proper amount of absolute ethanol into vector cylinder, and weighing cut 10 mm ×10 mm ×10 mm block materials as dry weight m 1 Placing into absolute ethanol, and recording initial volumes of ethanol and sample as V 1 . Soaking at room temperature for 1 week, taking out the material, and weighing the wet weight of the material to be m 2 The residual ethanol volume is V 2 . The porosity is:
three replicates were measured for each sample and averaged.
Determination of antibacterial properties: coli (E.coli, DH5 a)In a Lysogenic Broth (LB) in an incubator for 3 hours, at which time a 5 mL bacterial suspension (10 5 CFU/mL) and a quarter-piece sterile disc were incubated in a shaking incubator for 24 hours at 37 ℃. Finally, the retention of bacteria in suspension is counted. The sterilization rate was calculated using the following formula.
Claims (1)
1. The sisal fiber/chitosan/hybridized nano apatite composite porous material is characterized by being prepared by the following method: adding water into a certain amount of sisal fiber, performing ultrasonic dispersion, slowly dripping ultrasonic dispersion hybridized nano apatite slurry, adding a certain amount of chitosan powder and houttuynin sodium powder, mechanically stirring at a high speed for 4 hours, adding glacial acetic acid with the concentration of 2% to obtain composite gel, freeze-drying, soaking in 10% NaOH solution for 30 minutes, washing with deionized water to be neutral, and vacuum-drying at 40 ℃ to constant weight; the sisal fiber is carboxylated modified sisal fiber, the diameter is about 1mm, the diameter is 0.1-0.2 mm, the mass ratio of the sisal fiber to the chitosan is 1/3-1/1, the mass ratio of the hybrid nano-apatite to the composite porous material is 10% -25%, and the cordate houttuynia content is 4% -12%; the hybridized nano apatite is prepared by the following method: dissolving strontium nitrate and calcium nitrate in an aqueous solution, wherein the content of strontium nitrate is that the mole ratio of Sr/(Sr+Ca) is 2-10%, adding phytic acid to react for 1 hour, and setting the solution A, wherein the mole ratio of phosphate radical in the phytic acid to total phosphate radical is 10-40%; adding 5-10wt% of alendronate into sodium phosphate solution, reacting for 1 hr to obtain solution B, slowly dripping solution B into solution A, maintaining Ca/P molar ratio at 1.67, regulating pH to above 10 with 1 mol/L sodium hydroxide, heating at 70deg.C for 5 hr under stirring, aging for 48 hr, washing with deionized water to neutrality, drying, and grinding into powder.
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