CN111334934B - Chitosan crosslinked antibacterial nanofiber membrane and preparation method thereof - Google Patents
Chitosan crosslinked antibacterial nanofiber membrane and preparation method thereof Download PDFInfo
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H3/00—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
- D04H3/005—Synthetic yarns or filaments
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0015—Electro-spinning characterised by the initial state of the material
- D01D5/003—Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
- D01D5/0092—Electro-spinning characterised by the electro-spinning apparatus characterised by the electrical field, e.g. combined with a magnetic fields, using biased or alternating fields
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
- D01F1/103—Agents inhibiting growth of microorganisms
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H3/00—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
- D04H3/02—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of forming fleeces or layers, e.g. reorientation of yarns or filaments
- D04H3/03—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of forming fleeces or layers, e.g. reorientation of yarns or filaments at random
- D04H3/033—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of forming fleeces or layers, e.g. reorientation of yarns or filaments at random reorientation immediately after yarn or filament formation
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Abstract
The invention belongs to the technical field of textile material processing, and discloses a chitosan cross-linked antibacterial nanofiber membrane and a preparation method thereof. The preparation method comprises the steps of preparing terpinen-4-ol liposome; preparing an antibacterial protective cross-linking agent by using oleuropein acid and bitter apricot kernels; dissolving chitosan and polyoxyethylene in 90% acetic acid solution, stirring, adding terpinene-4-alcohol liposome and antibacterial protective cross-linking agent, and electrostatic spinning to obtain chitosan cross-linked nano-fiber membrane. The nanofiber membrane prepared by the preparation method disclosed by the invention is good in mechanical property and good in antibacterial effect.
Description
Technical Field
The invention relates to the technical field of textile material processing, in particular to a chitosan cross-linked antibacterial nanofiber membrane and a preparation method thereof.
Background
Electrostatic spinning is a novel spinning technology capable of preparing nano or micron fibers, is suitable for most polymers, and has the advantages of economy, flexibility, convenience, high efficiency and the like. The nanofiber prepared by electrostatic spinning is widely applied in the fields of filtration, biological tissue engineering, biological drug loading, wound dressing, composite reinforcement, sensors, protective clothing, electricity, optics and the like. Because an unstable whip state exists in the spinning process, the received fibers are disordered and have relatively poor mechanical properties, and the industrial production of electrostatic spinning and the popularization and application of products thereof are limited.
Although the nanofiber membrane has many excellent properties, the mechanical properties of the electrospun nanofiber membrane are generally poor due to the high porosity of the nanofiber membrane, so that the application of the nanofiber membrane in many fields is greatly limited. Common methods for improving the mechanical properties of the nano-material include: adding rigid inorganic nano particles, chemical crosslinking, thermal annealing treatment and the like.
Disclosure of Invention
In view of the above, the present invention aims to provide a chitosan crosslinked antibacterial nanofiber membrane and a preparation method thereof, wherein the nanofiber membrane has good mechanical properties and an antibacterial effect.
In order to solve the technical problems, the invention provides a preparation method of a chitosan cross-linked antibacterial nanofiber membrane, which comprises the following steps:
s1, adding soybean lecithin, cholesterol and terpinene-4-ol into chloroform, fully stirring to completely dissolve the soybean lecithin, cholesterol and terpinene-4-ol, performing rotary evaporation at room temperature to remove chloroform, injecting the solution into water which is 5-7 times the volume of the solution and contains 3-5 g/L of surfactant, homogenizing at the speed of 10000-12000 r/min, dialyzing and concentrating the solution by using 10-20 g/L of polyvinyl alcohol 6000 solution to 1/5-1/7 volumes, and preparing the terpinene-4-ol liposome;
s2, crushing the antioxidant and the bitter apricot seeds, adding the crushed antioxidant and the crushed bitter apricot seeds into PBS buffer solution together with oleuropein, homogenizing for 5-8 min at the speed of 10000-12000 r/min under ice bath, stirring and reacting for 8-10 h at the temperature of 20-28 ℃, filtering, ultrafiltering, and spray-drying to obtain the antibacterial protective cross-linking agent;
s3, mixing chitosan with the relative molecular weight of 20-50 kDa and the degree of deacetylation of 80-100% and the relative molecular weight of 105～107The polyoxyethylene is dissolved in 90% v/v acetic acid solution, fully stirred, added with terpinene-4-alcohol liposome and antibacterial protective cross-linking agent, and is subjected to electrostatic spinning to form the chitosan cross-linked nanofiber membrane.
Preferably, in step S1, the ratio of soybean lecithin, cholesterol, terpinen-4-ol and chloroform is: (0.5-0.7) g, (0.1-0.3) g, (0.3-0.5) ml and 20 ml.
Preferably, in step S1, the injection rate is 4 to 6 ml/min.
Preferably, in step S1, the surfactant is one of DMSS (disodium cocomonoethanolamide sulfosuccinate), MAP (monolauryl phosphate), and CDEA (cocodiethanolamide).
Preferably, in the step S2, the ratio of the antioxidant to the bitter apricot seeds to the oleuropein to the PBS buffer solution is (0.1-0.2) g, (4-5) g, (2-4) g, (50-75) ml.
Preferably, in step S2, the antioxidant is one of BHA (butyl hydroxyanisole), BHT (dibutyl hydroxytoluene), and TBHQ (tert-butyl hydroquinone).
Preferably, in the step S2, the inlet temperature of the spray drying is 160-200 ℃, the outlet temperature is 40-80 ℃, and the feeding rate is 10-20 ml/min.
Preferably, in step S3, the ratio of the chitosan, the polyethylene oxide, the acetic acid solution, the terpinen-4-ol liposome and the antibacterial protective cross-linking agent is 1g (0.1-0.2) g to 50ml (0.2-0.5) ml (0.2-0.4) g.
Preferably, in step S3, the electrospinning conditions are: the spinning voltage is 12-18 kV, the flow rate is 0.5-1 ml/h, and the receiving distance is 12-20 cm.
The invention also provides the chitosan cross-linked antibacterial nanofiber membrane prepared by the preparation method.
Compared with the prior art, the invention has the following beneficial effects:
1) the invention removes the glycosyl of oleuropein acid by using beta-glucanase in bitter almond to form active aglycone, the aglycone (a chemical structural formula shown in a formula (1)) is secoiridoid, and the aglycone has three sites which can be grafted with amino, one more site than genipin and two phenolic hydroxyl groups, which shows that the aglycone also has a certain antibacterial effect. The chitosan can be well crosslinked through the chitosan nano-fiber membrane, so that the mechanical property of the chitosan nano-fiber membrane is obviously enhanced.
2) The aglycone is treated by the antioxidant, so that the activity of phenolic hydroxyl can be effectively protected, and the stability of terpinene-4-alcohol in the terpinene-4-alcohol liposome is facilitated.
3) The preparation method is a green manufacturing technology and is environment-friendly.
Drawings
FIG. 1 is a scanning electron microscope image of the chitosan crosslinked antibacterial nanofiber membrane prepared in example 1.
Fig. 2 is a graph comparing bacteriostatic time curves of nanofiber membranes prepared according to the example of the present invention and the comparative example method.
Detailed Description
For a further understanding of the invention, reference will now be made to the preferred embodiments of the present invention by way of example, and it is to be understood that the description is intended to further illustrate features and advantages of the present invention and is not intended to limit the scope of the claims which follow.
Example 1
A chitosan cross-linked antibacterial nanofiber membrane and a preparation method thereof comprise the following steps:
1. adding 0.6g of soybean lecithin, 0.2g of cholesterol and 0.4ml of terpinen-4-ol into 20ml of chloroform, fully stirring to completely dissolve the soybean lecithin, removing the chloroform by rotary evaporation at room temperature, injecting the soybean lecithin, the cholesterol and the terpinen-4-ol into 6 times volume of water containing 4g/L of MAP by using an injector at the speed of 5ml/min, homogenizing at the speed of 11000r/min, dialyzing and concentrating by using 15g/L of polyvinyl alcohol 6000 solution to 1/6 volumes, and preparing the terpinen-4-ol liposome;
2. crushing 0.15g BHT and 4.5g bitter almond, adding the crushed materials and 3g oleuropein acid into 60ml PBS buffer solution, homogenizing for 7min at the speed of 11000r/min under ice bath, stirring and reacting for 9h at 24 ℃, filtering and ultrafiltering, and spray-drying at the inlet temperature of 180 ℃, the outlet temperature of 60 ℃ and the feeding rate of 15ml/min to obtain the antibacterial protection cross-linking agent;
3. 1g of chitosan with the relative molecular weight of 40kDa and the degree of deacetylation of 90 percent and 0.15g of chitosan with the relative molecular weight of 106Dissolving polyoxyethylene in 50ml of 90% acetic acid solution, stirring thoroughly, adding 0.4ml of terpinen-4-ol liposome and 0.3g of antibacterial protective cross-linking agent, and electrospinning at a voltage of 15kV, a flow rate of 0.7ml/h and a receiving distance of 15cmThe scanning electron microscope image of the silk-formed chitosan crosslinked nanofiber membrane A is shown in figure 1.
Example 2
A chitosan cross-linked antibacterial nanofiber membrane and a preparation method thereof comprise the following steps:
1. adding 0.5g of soybean lecithin, 0.1g of cholesterol and 0.3ml of terpinen-4-ol into 20ml of chloroform, fully stirring to completely dissolve the soybean lecithin, removing the chloroform by rotary evaporation at room temperature, then injecting the soybean lecithin, the cholesterol and the terpinen-4-ol into 5 times volume of water containing 3g/L of DMSS by using a syringe at the speed of 4ml/min, homogenizing at the speed of 10000r/min, dialyzing and concentrating by using 10g/L of polyvinyl alcohol 6000 solution to 1/5 volumes, and preparing the terpinen-4-ol liposome;
2. crushing 0.1g of BHA and 4g of bitter almond, adding the crushed materials and 2g of oleuropein acid into 50ml of PBS buffer solution, homogenizing for 5min at 10000r/min under ice bath, stirring and reacting for 8h at 20 ℃, filtering, ultrafiltering, and spray-drying at an inlet temperature of 160 ℃, an outlet temperature of 40 ℃ and a feeding rate of 10ml/min to obtain the antibacterial protective cross-linking agent;
3. 1g of chitosan with the relative molecular weight of 20kDa and the degree of deacetylation of 80 percent and 0.1g of chitosan with the relative molecular weight of 105The polyethylene oxide is dissolved in 50ml of 90 percent acetic acid solution, fully stirred, added with 0.2ml of terpinen-4-ol liposome and 0.2g of antibacterial protection cross-linking agent, and is subjected to electrostatic spinning under the conditions of 12kV voltage, 0.5ml/h flow rate and 12cm receiving distance to form the chitosan cross-linked nanofiber membrane B.
Example 3
A chitosan cross-linked antibacterial nanofiber membrane and a preparation method thereof comprise the following steps:
1. adding 0.7g of soybean lecithin, 0.3g of cholesterol and 0.5ml of terpinen-4-ol into 20ml of chloroform, fully stirring to completely dissolve the soybean lecithin, removing the chloroform by rotary evaporation at room temperature, then injecting the soybean lecithin, the cholesterol and the terpinen-4-ol into 7 times volume of water containing 5g/L of CDEA by using a syringe at the speed of 6ml/min, homogenizing at the speed of 12000r/min, dialyzing and concentrating by using 20g/L of polyvinyl alcohol 6000 solution to 1/7 volumes to prepare the terpinen-4-ol liposome;
2. crushing 0.2g of TBHQ and 5g of bitter almond, adding the crushed materials and 4g of oleuropein acid into 75ml of PBS buffer solution, homogenizing for 8min at 12000r/min under ice bath, stirring and reacting for 10h at 28 ℃, filtering, ultrafiltering, and spray-drying at an inlet temperature of 200 ℃, an outlet temperature of 80 ℃ and a feeding rate of 20ml/min to obtain the antibacterial protection cross-linking agent;
3. 1g of chitosan with a relative molecular weight of 50kDa and a degree of deacetylation of 100 percent and 0.2g of chitosan with a relative molecular weight of 107The polyethylene oxide is dissolved in 50ml of 90 percent acetic acid solution, fully stirred, added with 0.5ml of terpinen-4-ol liposome and 0.4g of antibacterial protection cross-linking agent, and is subjected to electrostatic spinning under the conditions of 18kV voltage, 1ml/h flow rate and 20cm receiving distance to form the chitosan cross-linked nanofiber membrane C.
COMPARATIVE EXAMPLE 1 (Low antioxidant)
A chitosan crosslinking nanofiber membrane and a preparation method thereof comprise the following steps:
1. adding 0.6g of soybean lecithin, 0.2g of cholesterol and 0.4ml of terpinen-4-ol into 20ml of chloroform, fully stirring to completely dissolve the soybean lecithin, removing the chloroform by rotary evaporation at room temperature, then injecting the soybean lecithin, the cholesterol and the terpinen-4-ol into 6 times volume of water containing 4g/L of MAP by using an injector at the speed of 5ml/min, homogenizing at the speed of 11000r/min, dialyzing and concentrating by using 15g/L of polyvinyl alcohol 6000 solution to 1/6 volumes, and preparing the terpinen-4-ol liposome;
2. crushing 4.5g of bitter almond, adding the crushed bitter almond and 3g of oleuropein acid into 60ml of PBS buffer solution, homogenizing for 7min at the speed of 11000r/min under ice bath, stirring and reacting for 9h at 24 ℃, filtering, ultrafiltering, and spray-drying at the inlet temperature of 180 ℃, the outlet temperature of 60 ℃ and the feeding rate of 15ml/min to obtain the antibacterial protection cross-linking agent;
3. 1g of chitosan with the relative molecular weight of 40kDa and the degree of deacetylation of 90 percent and 0.15g of chitosan with the relative molecular weight of 106The polyethylene oxide is dissolved in 50ml of 90 percent acetic acid solution, fully stirred, added with 0.4ml of terpinene-4-ol liposome and 0.3g of antibacterial protection cross-linking agent, and is subjected to electrostatic spinning under the conditions that the voltage is 15kV, the flow rate is 0.7ml/h and the receiving distance is 15cm to form the chitosan cross-linked nanofiber membrane D.
COMPARATIVE EXAMPLE 2 (Shaohao almond)
A chitosan crosslinking nanofiber membrane and a preparation method thereof comprise the following steps:
1. adding 0.6g of soybean lecithin, 0.2g of cholesterol and 0.4ml of terpinen-4-ol into 20ml of chloroform, fully stirring to completely dissolve the soybean lecithin, removing the chloroform by rotary evaporation at room temperature, then injecting the soybean lecithin, the cholesterol and the terpinen-4-ol into 6 times volume of water containing 4g/L of MAP by using an injector at the speed of 5ml/min, homogenizing at the speed of 11000r/min, dialyzing and concentrating by using 15g/L of polyvinyl alcohol 6000 solution to 1/6 volumes, and preparing the terpinen-4-ol liposome;
2. adding 0.15g BHT and 3g oleuropein into 60ml PBS buffer solution, homogenizing for 7min at 11000r/min under ice bath, stirring and reacting for 9h at 24 ℃, filtering and ultrafiltering, and spray drying at 180 ℃ inlet temperature, 60 ℃ outlet temperature and 15ml/min feeding rate to obtain the antibacterial protective cross-linking agent;
3. 1g of chitosan with the relative molecular weight of 40kDa and the degree of deacetylation of 90 percent and 0.15g of chitosan with the relative molecular weight of 106The polyethylene oxide is dissolved in 50ml of 90 percent acetic acid solution, fully stirred, added with 0.4ml of terpinene-4-ol liposome and 0.3g of antibacterial protection cross-linking agent, and is subjected to electrostatic spinning under the conditions that the voltage is 15kV, the flow rate is 0.7ml/h and the receiving distance is 15cm to form the chitosan cross-linked nanofiber membrane E.
Comparative example 3 (Eluropein acid)
A chitosan crosslinking nanofiber membrane and a preparation method thereof comprise the following steps:
1. adding 0.6g of soybean lecithin, 0.2g of cholesterol and 0.4ml of terpinen-4-ol into 20ml of chloroform, fully stirring to completely dissolve the soybean lecithin, removing the chloroform by rotary evaporation at room temperature, then injecting the soybean lecithin, the cholesterol and the terpinen-4-ol into 6 times volume of water containing 4g/L of MAP by using an injector at the speed of 5ml/min, homogenizing at the speed of 11000r/min, dialyzing and concentrating by using 15g/L of polyvinyl alcohol 6000 solution to 1/6 volumes, and preparing the terpinen-4-ol liposome;
2. crushing 0.15g BHT and 4.5g bitter almond, adding the crushed materials into 60ml PBS buffer solution, homogenizing for 7min at the speed of 11000r/min under ice bath, stirring and reacting for 9h at 24 ℃, filtering and ultrafiltering, and spray drying at the inlet temperature of 180 ℃, the outlet temperature of 60 ℃ and the feeding rate of 15ml/min to prepare the antibacterial protection cross-linking agent;
3. 1g of the relative moleculeChitosan in an amount of 40kDa and a degree of deacetylation of 90% was mixed with 0.15g of a relative molecular mass of 106The polyethylene oxide is dissolved in 50ml of 90 percent acetic acid solution, fully stirred, added with 0.4ml of terpinene-4-ol liposome and 0.3g of antibacterial protection cross-linking agent, and is subjected to electrostatic spinning to form the chitosan cross-linked nanofiber membrane F under the conditions that the voltage is 15kV, the flow rate is 0.7ml/h and the receiving distance is 15 cm.
Mechanical Property test
The nanofiber membranes of examples 1-3 and comparative examples 1-3 were subjected to uniaxial tensile test using a multifunctional tensile tester of KES-G1 model manufactured by Kato-Tech corporation of Japan, and the test pieces were 6cm X0.5 cm in size, 4cm in holding distance, and 0.05cm/s in tensile rate. The results of the nanofiber mechanical property test are shown in table 1.
TABLE 1 nanofiber mechanical Properties test results
| Sample (I) | Maximum tensile stress (MPa) | Maximum tensile strain (%) | Young's modulus (MPa) |
| Example 1 | 17.6±0.2 | 80.8±1.6 | 0.22±0.01 |
| Example 2 | 16.5±0.5 | 67.7±2.2 | 0.24±0.00 |
| Example 3 | 16.3±0.3 | 73.4±2.6 | 0.22±0.00 |
| Comparative example 1 | 12.0±0.5 | 50.1±4.2 | 0.24±0.01 |
| Comparative example 2 | 12.4±0.4 | 45.8±2.6 | 0.27±0.02 |
| Comparative example 3 | 11.6±0.1 | 47.9±2.6 | 0.24±0.01 |
According to the table 1, the maximum tensile stress of the nanofiber membrane prepared in the embodiment of the invention is improved by 4-6 MPa compared with that of the comparative example, and the maximum tensile strain is also improved by 30-70%. While the young's modulus of the nanofiber membranes of the examples and comparative examples were not significantly different.
Test of antibacterial Property
1g of the nanofiber membranes prepared in examples 1 to 3 and comparative examples 1 to 3 were put in a dialysis bag and placed in 200ml of PBS buffer solution, and release was performed by magnetic stirring. After a period of time, the material was removed and tested for its bacteriostatic effect against staphylococcus aureus and enterobacter coli using AATCC100-2004 standard, with the test results shown in fig. 2. In fig. 2, a is the bacteriostatic time curve of example 1, B is the bacteriostatic time curve of example 2, C is the bacteriostatic time curve of example 3, D is the bacteriostatic time curve of comparative example 1, E is the bacteriostatic time curve of comparative example 2, and F is the bacteriostatic time curve of comparative example 3.
According to fig. 2, it can be found that the nanofiber membranes prepared in examples 1 to 3 can still maintain a better bacteriostatic effect on staphylococcus aureus and escherichia coli after being released for 21 days, while the nanofiber membranes prepared in comparative examples 1 to 3 can reduce the bacteriostatic rate on staphylococcus aureus and escherichia coli to below 40% after being released for 3 days, the detectable bacteriostatic effect on staphylococcus aureus disappears after being released for 6 days, and the detectable bacteriostatic effect on escherichia coli disappears after being released for 9 days. The result shows that the nanofiber membrane prepared by the invention has more excellent slow-release antibacterial performance.
The present invention provides a chitosan cross-linked antibacterial nanofiber membrane and a method and a thinking for implementing the method, and a method for implementing the method, and the method and the way for implementing the technical scheme are many, and the above description is only a preferred embodiment of the present invention, it should be noted that, for those skilled in the art, a plurality of improvements and decorations can be made without departing from the principle of the present invention, and these improvements and decorations should also be regarded as the protection scope of the present invention. All the components not specified in the present embodiment can be realized by the prior art.
Claims (7)
1. A preparation method of a chitosan cross-linked antibacterial nanofiber membrane is characterized by comprising the following steps:
s1, adding soybean lecithin, cholesterol and terpinene-4-ol into chloroform, fully stirring to completely dissolve the soybean lecithin, cholesterol and terpinene-4-ol, removing the chloroform by rotary evaporation at room temperature, injecting the mixture into water which is 5-7 times the volume of the mixture and contains 3-5 g/L of surfactant, homogenizing at the speed of 10000-12000 r/min, dialyzing and concentrating the mixture by using 10-20 g/L of polyvinyl alcohol 6000 solution to 1/5-1/7 volumes, and preparing the terpinene-4-ol liposome;
s2, crushing the antioxidant and the bitter apricot seeds, adding the crushed antioxidant and the crushed bitter apricot seeds into PBS buffer solution together with oleuropein, homogenizing for 5-8 min at the speed of 10000-12000 r/min under ice bath, stirring and reacting for 8-10 h at the temperature of 20-28 ℃, filtering, ultrafiltering, and spray-drying to obtain the antibacterial protective cross-linking agent; the proportion of the antioxidant, the bitter apricot seeds, the oleuropein acid and the PBS buffer solution is (0.1-0.2), (4-5), (2-4), (50-75) ml; the antioxidant is one of BHA, BHT and TBHQ;
s3, mixing chitosan with the relative molecular weight of 20-50 kDa and the degree of deacetylation of 80-100% and the relative molecular weight of 105～107Dissolving polyoxyethylene in 90% v/v acetic acid solution, fully stirring, adding the terpinene-4-ol liposome and the antibacterial protective cross-linking agent, and performing electrostatic spinning to obtain a chitosan cross-linked nanofiber membrane; the proportion of the chitosan, the polyoxyethylene, the acetic acid solution, the terpinene-4-alcohol liposome and the antibacterial protection cross-linking agent is 1g (0.1-0.2) g, 50ml (0.2-0.5) ml (0.2-0.4) g.
2. The method of claim 1, wherein in step S1, the ratio of the soybean lecithin, the cholesterol, the terpinen-4-ol, and the chloroform is: (0.5-0.7) g, (0.1-0.3) g, (0.3-0.5) ml and 20 ml.
3. The method of claim 1, wherein the injection rate is 4-6 ml/min in step S1.
4. The method of claim 1, wherein in step S1, the surfactant is one of DMSS, MAP and CDEA.
5. The method for preparing a chitosan crosslinked antibacterial nanofiber membrane as claimed in claim 1, wherein in step S2, the spray drying inlet temperature is 160-200 ℃, the outlet temperature is 40-80 ℃, and the feeding rate is 10-20 ml/min.
6. The method of claim 1, wherein in step S3, the electrospinning conditions are as follows: the spinning voltage is 12-18 kV, the flow rate is 0.5-1 ml/h, and the receiving distance is 12-20 cm.
7. The chitosan cross-linked antibacterial nanofiber membrane prepared by the preparation method according to any one of claims 1-6.
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