CN100496618C - Antibacterial type blended electro spinning nanometer fiber membrane preparing method - Google Patents
Antibacterial type blended electro spinning nanometer fiber membrane preparing method Download PDFInfo
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Abstract
The invention discloses a blending electric spun nanometer fiber film biological compress and preparing method in medicinal biological compress technical domain, which is characterized by the following: choosing chitose or polyvinyl alcohol or water-soluble antibacterial drugs as main raw material; adopting electrostatic spinning method; producing nanometer fiber film. This product possesses the advantages of higher strength, good air perviousness and good biological compatibility.
Description
Technical field:
The present invention relates to a kind of preparation method, belong to medical bio dressing technical field with blended electro spinning nanometer fiber membrane of anti-microbial property.
Background technology:
Chitosan (Chitosan, CS) be a kind of abundant natural alkaline polysaccharide, be only second to cellulosic second largest living resources at nature, have excellent biological compatibility, biodegradability, human body affinity and antibiotic, hemostasis and promote excellent properties such as wound healing, can absorb voluntarily after the use, not cause allergy, can also accelerating wound healing, large-area burns there is protective effect, can promotes skin regeneration; With the medical adhesive-bonded fabric of its production, can use in burn wound and skin donor site, not only play the effect of covering, protection wound surface, and antigenicity is low.Therefore, the chitosan biological dressing more and more is being subject to people's attention in recent years, and uses in the bio-medical field as artificial skin, operation suture thread.
Traditional dressing, as gauze, regular meeting because of blood coagulation attached on the wound; again because of fiber coarse can't with tissue compatible, can't be organized absorption, cause the wound cambium impaired when changing dressings easily; prolonged wound healing time, also brought misery simultaneously to the patient.
Adopt casting films as dressing, shortcoming is that breathability is poor, easily irritates a wound, and prolongs healing time.The patent disclosure of publication number CN1395968 a kind of biological fluid dressing chitosan membrane and preparation method thereof, it has nontoxic, non-stimulated, the advantage of healing acceleration, but still there is the shortcoming of breathability difference in it; The patent disclosure of publication number CN1679972A a kind of burn dressing of chitin gel with gradient structure and preparation method thereof, advantage with water absorption and very good mechanical properties, but also be to adopt casting films as dressing and do not have to suppress or the germ killing drugs composition, do not possess initiatively antibacterial ability, easily cause the wound superinfection; The patent disclosure of publication number CN2676917Y the manufacture method of chitosan medicine film, have advantage easy to use, widely applicable, but adopt casting films as dressing, shortcoming is that breathability is poor, easily irritates a wound, and is difficult for healing.
The dressing of hydrogel class causes dressing in wound separation because of colloidal expansion behind a large amount of absorption exudates.On the degree that adapts to wound, it is lower than film dressing.The patent disclosure of publication number CN1640913 a kind of method for preparing crosslinked chitin-glycan-quaterisation collagen hydrolysate, the biological dressing that this method makes has the advantage of antibiotic property, good permeability, but its intensity is low; The patent disclosure of publication number CN1579559A a kind of polyvinyl alcohol hydrogel dressing that contains medicine, chitosan and preparation method thereof, the dressing of this method preparation has antibacterial ability initiatively, the characteristics of water content height, good permeability, but mechanical strength is lower, this method employing Co gamma-radiation or high-power electron beam x radiation x are crosslinked in addition, have the cost height, dangerous big, the shortcoming of destructible chitosan, polyvinyl alcohol and drug molecular structure.
The dressing of nonwoven dry goods, as the patent disclosure of publication number CN1493364A a kind of manufacture method of chitosan biological dressing, method is earlier chitosan to be made silk, respin and be made into gauze, the dressing of this method preparation has the good advantage of permeability, but it can not solve the too poor problem of the mechanical performance of chitosan own; The patent disclosure of publication number CN1115254A a kind of chitosan, collagen and calcium alginate composite biological non-woven cloth dressing, method is that non-woven fabrics successively is immersed in respectively in chitosan-collagen solution and the calcium alginate solution, the dressing of this method preparation has biocompatibility, infiltrative characteristics, but its working substance is only attached to nonwoven surface, drug releasing rate is fast, do not have slow-release function, the antibiotic time is short, causes the superinfection of wound easily.
The dressing of wet spinning class, as the patent disclosure of publication number CN1470679 a kind of chitin nonwoven fabric and production method thereof, has and preserve moisture that air permeable effect is good, the advantage of good biocompatibility, but its mechanical property is relatively poor.The patent disclosure of publication number CN1687499 blended fiber of sodium alginate/water soluble chitin and its production and use, the patent disclosure of publication number CN1699647 chitosan and hydroxypropyl cellulose blended fiber and preparation method and application, the dressing of these two kinds of wet spinning class dressing preparations all has water absorbing properties preferably, but can because of blood coagulation attached on the wound, again because of fiber coarse can't with tissue compatible, can't be organized absorption, cause the wound cambium impaired when changing dressings easily, prolonged wound healing time, also brought misery to the patient.
Summary of the invention:
The objective of the invention is at above-mentioned deficiency, a kind of preparation method of antibacterial type blended electro spinning nanometer fiber membrane is provided, with chitosan/polyvinyl alcohol/water solublity antibacterials is primary raw material, adopt method of electrostatic spinning to prepare nano fibrous membrane, it is higher to make the biological dressing that obtains have intensity, and good permeability, good biocompatibility, medicine have slow-releasing, the easier advantages such as absorption that are organized.
A kind of antibacterial type blended electro spinning nanometer fiber membrane of the present invention, with the chitosan through the polyvinyl alcohol reinforcement is base material, the nanometer fiber membrane biological dressing that contains the water solublity antibacterials in the fiber, it is characterized in that: the quality percentage composition of each component is: chitosan 50-81%, polyvinyl alcohol 6-15%, water solublity antibacterials 12-40%, fibre diameter is 50-350nm.
The preparation method of a kind of antibacterial type blended electro spinning nanometer fiber membrane biological dressing of the present invention adopts the method for electrostatic spinning preparation, and concrete steps are:
The preparation of A chitosan solution: at room temperature will glue all molecular weight M relatively
ηFor the chitosan of 12-80 ten thousand is dissolved in the acetic acid solution that concentration expressed in percentage by volume is 80-92%, stir, be mixed with the acetic acid solution that mass percentage concentration is the 3-10% chitosan;
The preparation of B poly-vinyl alcohol solution: with degree of polymerization 2500-3500, the polyvinyl alcohol of alcoholysis degree 88-98% is dissolved in the deionized water, is made into the solution that mass percentage concentration is 8%-10%;
Two kinds of solution that C obtains steps A and step B mix with the mass ratio of 5-9:1, obtain the chitosan/polyvinyl alcohol composite solution;
The preparation of D chitosan/polyvinyl alcohol/water solublity antibacterials blend solution: the water solublity antibacterials are joined in the composite solution that step C obtains, and it is 1-5% that the amount of adding makes the quality percentage composition of water solublity antibacterials in the solution, is stirred to dissolving fully;
The preparation of E chitosan/polyvinyl alcohol/water solublity antibacterials electrospun fiber membrane: chitosan/polyvinyl alcohol/water solublity antibacterials blend solution that step D is obtained joins in the electrostatic spinning apparatus.At electrostatic pressure is 10-35kv, and syringe pump flow velocity 0.05-1ml/h, spinning nozzle diameter are 0.3-1.0mm, accepts screen apart from electrostatic spinning film forming under the condition of 6-18cm apart from metal.
Said water solublity antibacterials can be aminoglycosides, as: gentamycin, amikacin, tobramycin, spectinomycin etc.; Tetracyclines, as: tetracycline, doxycycline, minocycline; Sulfonamides, as: sulphacetamide, Co.SMZ (bactrim) etc.; Quinolones, as: ofloxacin, levofloxacin, lomefloxacin, fleroxacin etc.
Its blended nanofibre diameter of the biological dressing that the present invention makes is 50-350nm, fibrous membrane has higher specific surface area and porosity, because medicine does not exist only in fiber surface and is present in fibrous inside yet, when drug-loading fibre contacts with human body wound tissue and is organized when absorbing, medicine can slowly release, and can continue antibioticly, prevents the superinfection of wound, promote wound healing, reduce dressing change frequency.The present invention can be widely used in the hemostasis and the wrapper material of wounds such as the hemostasis of operation process and operative incision, burn, scald.
The antibacterial type blended electro spinning nanometer fiber membrane biological dressing that the present invention obtained can be organized absorption gradually owing to being base material with the chitosan, quickens wound healing, and can reduce cicatrix.Therefore biological dressing of the present invention has intensity height, good permeability, biodegradability, good biocompatibility, human body affinity and antibiotic, hemostasis and promotes the advantage of wound healing.
The tensile strength of table 1 electrospun fiber membrane
| Embodiment | Tensile strength (σ b/MPa) |
| Embodiment 1 | 4.6989 |
| Embodiment 2 | 4.0526 |
| Embodiment 3 | 3.0249 |
| Embodiment 4 | 2.9449 |
| Embodiment 5 | 2.6148 |
| Embodiment 6 | 4.1170 |
| Embodiment 7 | 3.7983 |
| Embodiment 8 | 2.9491 |
| Embodiment 9 | 2.7027 |
| Embodiment 10 | 2.4000 |
| Embodiment 11 | 3.9457 |
| Embodiment 12 | 3.2281 |
| Embodiment 13 | 2.8702 |
| Embodiment 14 | 2.3183 |
| Embodiment 15 | 2.1417 |
The data of table 1 are to adopt American I NSTRON-1185 type universal testing machine, and according to the result that the product of 3354-82 couples of embodiment 1-15 of standard GB is tested, rate of extension is 10mm/min, the long 20.0mm of batten, wide 4.0mm.
Description of drawings:
Fig. 1 is the stereoscan photograph of the preceding blend superfine fibre film of blend non-woven fabrics drug release of embodiment 9, and amplification is 20,000 times.
As can be seen from the figure, the surface of blended fiber is all comparatively smooth and do not have tangible medicine crystal and separate out, and illustrates that minocycline has the good compatibility in blended fiber.Adopt image analysis software to get 30 fibers respectively in the drawings, the meansigma methods of measuring its diameter is 200nm.
Fig. 2 is the stereoscan photograph of the blend superfine fibre film behind the blend non-woven fabrics drug release of embodiment 9, and amplification is 5,000 times.
As can be seen from the figure after the release experiment, fiber is because the swelling chap, but still has more hole between the fiber, can keep breathability preferably, and this has great importance in the application aspect wound dressing, the hemostatic material.
Fig. 3 is the release in vitro curve of blend non-woven fabrics in the buffer of pH=7.40 of embodiment 17
Phosphate buffer with pH=7.40 is a simulated body fluid, and it has been carried out the vitro drug release experiment.Curve from Fig. 3 as can be seen, the cumulative release amount of pro-3h is about 50%, in addition 50% needs 7h just can discharge again, tangible slow release effect is arranged.
The specific embodiment:
Embodiment 1:
The preparation of A chitosan solution: at room temperature will gluing all molecular weight M η relatively and be 120,000 chitosan, to be dissolved in concentration expressed in percentage by volume be in 90% the acetic acid solution, be made into mass percentage concentration and be 7% solution, stirred 8 hours, and obtained translucent brown chitosan acetic acid solution;
The preparation of B poly-vinyl alcohol solution: with the degree of polymerization 3500, the polyvinyl alcohol of alcoholysis degree 88% is dissolved in the deionized water, is made into mass percentage concentration and is 10% solution;
C mixes with poly-vinyl alcohol solution above-mentioned chitosan solution by mass ratio 5/1, obtain the chitosan/polyvinyl alcohol complex solution;
The preparation of D chitosan/polyvinyl alcohol/ofloxacin blend solution: with the ofloxacin grind into powder, add that to account for the solution quality percentage concentration be 1% ofloxacin in the above-mentioned chitosan/polyvinyl alcohol complex solution respectively, be stirred to dissolving fully;
The preparation of E chitosan/polyvinyl alcohol/ofloxacin electrospun fiber membrane: chitosan/polyvinyl alcohol/ofloxacin blend solution that step D is obtained joins in the electrostatic spinning apparatus.At electrostatic pressure is 25kv, and syringe pump flow velocity 0.4ml/h, spinning nozzle diameter are 0.57mm, accepts screen apart from electrostatic spinning film forming under the condition of 10cm apart from metal, and obtaining the drug-loading fibre diameter is the fibrous membrane of 100-300nm.
Embodiment 2:
The preparation of A chitosan solution: with embodiment 1;
The preparation of B poly-vinyl alcohol solution: with embodiment 1;
C is with embodiment 1;
The preparation of D chitosan/polyvinyl alcohol/ofloxacin blend solution: the preparation of chitosan/polyvinyl alcohol/ofloxacin blend solution: with the ofloxacin grind into powder, add that to account for the solution quality percentage concentration be 2% ofloxacin in the above-mentioned chitosan/polyvinyl alcohol complex solution respectively, be stirred to dissolving fully;
The preparation of E chitosan/polyvinyl alcohol/ofloxacin electrospun fiber membrane: with embodiment 1.
Embodiment 3:
The preparation of A chitosan solution: with embodiment 1;
The preparation of B poly-vinyl alcohol solution: with embodiment 1;
C is with embodiment 1;
The preparation of D chitosan/polyvinyl alcohol/ofloxacin blend solution: the preparation of chitosan/polyvinyl alcohol/ofloxacin blend solution: with the ofloxacin grind into powder, add that to account for the solution quality percentage concentration be 3% ofloxacin in the above-mentioned chitosan/polyvinyl alcohol complex solution respectively, be stirred to dissolving fully;
The preparation of E chitosan/polyvinyl alcohol/ofloxacin electrospun fiber membrane: with embodiment 1;
Embodiment 4:
The preparation of A chitosan solution: with embodiment 1;
The preparation of B poly-vinyl alcohol solution: with embodiment 1;
C is with embodiment 1;
The preparation of D chitosan/polyvinyl alcohol/ofloxacin blend solution: the preparation of chitosan/polyvinyl alcohol/ofloxacin blend solution: with the ofloxacin grind into powder, add that to account for the solution quality percentage concentration be 4% ofloxacin in the above-mentioned chitosan/polyvinyl alcohol complex solution respectively, be stirred to dissolving fully;
The preparation of E chitosan/polyvinyl alcohol/ofloxacin electrospun fiber membrane: with embodiment 1.
Embodiment 5:
The preparation of A chitosan solution: with embodiment 1;
The preparation of B poly-vinyl alcohol solution: with embodiment 1;
C is with embodiment 1;
The preparation of D chitosan/polyvinyl alcohol/ofloxacin blend solution: the preparation of chitosan/polyvinyl alcohol/ofloxacin blend solution: with the ofloxacin grind into powder, add that to account for the solution quality percentage concentration be 5% ofloxacin in the above-mentioned chitosan/polyvinyl alcohol complex solution respectively, be stirred to dissolving fully;
The preparation of E chitosan/polyvinyl alcohol/ofloxacin electrospun fiber membrane: with embodiment 1.
Embodiment 6:
The preparation of A chitosan solution: with embodiment 1;
The preparation of B poly-vinyl alcohol solution: with embodiment 1;
C mixes with poly-vinyl alcohol solution above-mentioned chitosan solution by mass ratio 7/1, obtain the chitosan/polyvinyl alcohol complex solution;
The preparation of D chitosan/polyvinyl alcohol/ofloxacin blend solution: the preparation of chitosan/polyvinyl alcohol/ofloxacin blend solution: with the ofloxacin grind into powder, add that to account for the solution quality percentage concentration be 1% ofloxacin in the above-mentioned chitosan/polyvinyl alcohol complex solution respectively, be stirred to dissolving fully;
The preparation of E chitosan/polyvinyl alcohol/ofloxacin electrospun fiber membrane: with embodiment 1.
Embodiment 7:
The preparation of A chitosan solution: with embodiment 1;
The preparation of B poly-vinyl alcohol solution: with embodiment 1;
C mixes with poly-vinyl alcohol solution above-mentioned chitosan solution by mass ratio 7/1, obtain the chitosan/polyvinyl alcohol complex solution;
The preparation of D chitosan/polyvinyl alcohol/ofloxacin blend solution: the preparation of chitosan/polyvinyl alcohol/ofloxacin blend solution: with the ofloxacin grind into powder, add that to account for the solution quality percentage concentration be 2% ofloxacin in the above-mentioned chitosan/polyvinyl alcohol complex solution respectively, be stirred to dissolving fully;
The preparation of E chitosan/polyvinyl alcohol/ofloxacin electrospun fiber membrane: with embodiment 1.
Embodiment 8:
The preparation of A chitosan solution: with embodiment 1;
The preparation of B poly-vinyl alcohol solution: with embodiment 1;
C mixes with poly-vinyl alcohol solution above-mentioned chitosan solution by mass ratio 7/1, obtain the chitosan/polyvinyl alcohol complex solution;
The preparation of D chitosan/polyvinyl alcohol/ofloxacin blend solution: the preparation of chitosan/polyvinyl alcohol/ofloxacin blend solution: with the ofloxacin grind into powder, add that to account for the solution quality percentage concentration be 3% ofloxacin in the above-mentioned chitosan/polyvinyl alcohol complex solution respectively, be stirred to dissolving fully;
The preparation of E chitosan/polyvinyl alcohol/ofloxacin electrospun fiber membrane: with embodiment 1.
Embodiment 9:
The preparation of A chitosan solution: with embodiment 1;
The preparation of B poly-vinyl alcohol solution: with embodiment 1;
C mixes with poly-vinyl alcohol solution chitosan solution by mass ratio 7/1, obtain the chitosan/polyvinyl alcohol complex solution;
The preparation of D chitosan/polyvinyl alcohol/ofloxacin blend solution: the preparation of chitosan/polyvinyl alcohol/ofloxacin blend solution: with the ofloxacin grind into powder, add that to account for the solution quality percentage concentration be 4% ofloxacin in the above-mentioned chitosan/polyvinyl alcohol complex solution respectively, be stirred to dissolving fully;
The preparation of E chitosan/polyvinyl alcohol/ofloxacin electrospun fiber membrane: with embodiment 1.
Embodiment 10:
The preparation of A chitosan solution: with embodiment 1;
The preparation of B poly-vinyl alcohol solution: with embodiment 1;
C mixes with poly-vinyl alcohol solution above-mentioned chitosan solution by mass ratio 7/1, obtain the chitosan/polyvinyl alcohol complex solution;
The preparation of D chitosan/polyvinyl alcohol/ofloxacin blend solution: the preparation of chitosan/polyvinyl alcohol/ofloxacin blend solution: with the ofloxacin grind into powder, add that to account for the solution quality percentage concentration be 5% ofloxacin in the above-mentioned chitosan/polyvinyl alcohol complex solution respectively, be stirred to dissolving fully;
The preparation of E chitosan/polyvinyl alcohol/ofloxacin electrospun fiber membrane: with embodiment 1.
Embodiment 11:
The preparation of A chitosan solution: with embodiment 1;
The preparation of B poly-vinyl alcohol solution: with embodiment 1;
C mixes with poly-vinyl alcohol solution above-mentioned chitosan solution by mass ratio 9/1, obtain the chitosan/polyvinyl alcohol complex solution;
The preparation of D chitosan/polyvinyl alcohol/ofloxacin blend solution: the preparation of chitosan/polyvinyl alcohol/ofloxacin blend solution: with the ofloxacin grind into powder, add that to account for the solution quality percentage concentration be 1% ofloxacin in the above-mentioned chitosan/polyvinyl alcohol complex solution respectively, be stirred to dissolving fully;
The preparation of E chitosan/polyvinyl alcohol/ofloxacin electrospun fiber membrane: with embodiment 1.
Embodiment 12:
The preparation of A chitosan solution: with embodiment 1;
The preparation of B poly-vinyl alcohol solution: with embodiment 1;
C mixes with poly-vinyl alcohol solution above-mentioned chitosan solution by mass ratio 9/1, obtain the chitosan/polyvinyl alcohol complex solution;
The preparation of D chitosan/polyvinyl alcohol/ofloxacin blend solution: the preparation of chitosan/polyvinyl alcohol/ofloxacin blend solution: with the ofloxacin grind into powder, add that to account for the solution quality percentage concentration be 2% ofloxacin in the above-mentioned chitosan/polyvinyl alcohol complex solution respectively, be stirred to dissolving fully;
The preparation of E chitosan/polyvinyl alcohol/ofloxacin electrospun fiber membrane: with embodiment 1.
Embodiment 13:
The preparation of A chitosan solution: with embodiment 1;
The preparation of B poly-vinyl alcohol solution: with embodiment 1;
C mixes with poly-vinyl alcohol solution above-mentioned chitosan solution by mass ratio 9/1, obtain the chitosan/polyvinyl alcohol complex solution;
The preparation of D chitosan/polyvinyl alcohol/ofloxacin blend solution: the preparation of chitosan/polyvinyl alcohol/ofloxacin blend solution: with the ofloxacin grind into powder, add that to account for the solution quality percentage concentration be 3% ofloxacin in the above-mentioned chitosan/polyvinyl alcohol complex solution respectively, be stirred to dissolving fully;
The preparation of E chitosan/polyvinyl alcohol/ofloxacin electrospun fiber membrane: with embodiment 1.
Embodiment 14:
The preparation of A chitosan solution: with embodiment 1;
The preparation of B poly-vinyl alcohol solution: with embodiment 1;
C mixes with poly-vinyl alcohol solution above-mentioned chitosan solution by mass ratio 9/1, obtain the chitosan/polyvinyl alcohol complex solution;
The preparation of D chitosan/polyvinyl alcohol/ofloxacin blend solution: the preparation of chitosan/polyvinyl alcohol/ofloxacin blend solution: with the ofloxacin grind into powder, add that to account for the solution quality percentage concentration be 4% ofloxacin in the above-mentioned chitosan/polyvinyl alcohol complex solution respectively, be stirred to dissolving fully;
The preparation of E chitosan/polyvinyl alcohol/ofloxacin electrospun fiber membrane: with embodiment 1.
Embodiment 15:
The preparation of A chitosan solution: with embodiment 1;
The preparation of B poly-vinyl alcohol solution: with embodiment 1;
C mixes with poly-vinyl alcohol solution above-mentioned chitosan solution by mass ratio 9/1, obtain the chitosan/polyvinyl alcohol complex solution;
The preparation of D chitosan/polyvinyl alcohol/ofloxacin blend solution: the preparation of chitosan/polyvinyl alcohol/ofloxacin blend solution: with the ofloxacin grind into powder, add that to account for the solution quality percentage concentration be 5% ofloxacin in the above-mentioned chitosan/polyvinyl alcohol complex solution respectively, be stirred to dissolving fully;
The preparation of E chitosan/polyvinyl alcohol/ofloxacin electrospun fiber membrane: with embodiment 1.
Embodiment 16:
The preparation of A chitosan solution: with embodiment 1;
The preparation of B poly-vinyl alcohol solution: with embodiment 1;
C mixes with poly-vinyl alcohol solution above-mentioned chitosan solution by mass ratio 7/1, obtain the chitosan/polyvinyl alcohol complex solution;
The preparation of D chitosan/polyvinyl alcohol/levofloxacin blend solution: with the levofloxacin grind into powder, add that to account for the solution quality percentage concentration be 4% levofloxacin in the chitosan/polyvinyl alcohol complex solution, be stirred to dissolving fully;
The preparation of E chitosan/polyvinyl alcohol/levofloxacin electrospun fiber membrane: chitosan/polyvinyl alcohol/levofloxacin blend solution that step D is obtained joins in the electrostatic spinning apparatus.At electrostatic pressure is 35kv, and syringe pump flow velocity 1.0ml/h, spinning nozzle diameter are 1.0mm, accepts screen apart from electrostatic spinning film forming under the condition of 16cm apart from metal, and obtaining the drug-loading fibre diameter is the fibrous membrane of 50-250nm.
Embodiment 17:
The preparation of A chitosan solution: at room temperature will gluing all molecular weight M η relatively and be 400,000 chitosan, to be dissolved in concentration expressed in percentage by volume be in 85% the acetic acid solution, be made into mass percentage concentration and be 8% solution, stirred 9 hours, and obtained translucent brown chitosan acetic acid solution;
The preparation of B poly-vinyl alcohol solution: with the degree of polymerization 1700, the polyvinyl alcohol of alcoholysis degree 98% is dissolved in the deionized water, is made into mass percentage concentration and is 8% solution;
C mixes with poly-vinyl alcohol solution above-mentioned chitosan solution by mass ratio 9/1, obtain the chitosan/polyvinyl alcohol complex solution;
The preparation of D chitosan/polyvinyl alcohol/ofloxacin blend solution: with the ofloxacin grind into powder, add that to account for the solution quality percentage concentration be 1% ofloxacin in the chitosan/polyvinyl alcohol complex solution, be stirred to dissolving fully;
The preparation of E chitosan/polyvinyl alcohol/ofloxacin electrospun fiber membrane: chitosan/polyvinyl alcohol/ofloxacin blend solution that step D is obtained joins in the electrostatic spinning apparatus.At electrostatic pressure is 25kv, and syringe pump flow velocity 0.6ml/h, spinning nozzle diameter are 0.57mm, accepts screen apart from electrostatic spinning film forming under the condition of 10cm apart from metal, and obtaining the drug-loading fibre diameter is the fibrous membrane of 50-350nm.
Embodiment 18:
The preparation of A chitosan solution: at room temperature will gluing all molecular weight M η relatively and be 650,000 chitosans, to be dissolved in concentration expressed in percentage by volume be in 85% the acetic acid solution, be made into mass percentage concentration and be 6% solution, stirred 10 hours, and obtained translucent brown chitosan acetic acid solution;
The preparation of B poly-vinyl alcohol solution: with the degree of polymerization 2500, the polyvinyl alcohol of alcoholysis degree 98% is dissolved in the deionized water, is made into mass percentage concentration and is 9% solution;
C mixes with poly-vinyl alcohol solution chitosan solution by mass ratio 6/1, obtain the chitosan/polyvinyl alcohol complex solution;
The preparation of D chitosan/polyvinyl alcohol/bactrim blend solution: with the bactrim grind into powder, add that to account for the solution quality percentage concentration be 5% bactrim in the chitosan/polyvinyl alcohol complex solution, be stirred to dissolving fully;
The preparation of E chitosan/polyvinyl alcohol/bactrim electrospun fiber membrane: chitosan/polyvinyl alcohol/bactrim blend solution that step D is obtained adds in the electrostatic spinning apparatus.At electrostatic pressure is 15kv, and syringe pump flow velocity 0.75ml/h, spinning nozzle diameter are 0.77mm, accepts screen apart from electrostatic spinning film forming under the condition of 8cm apart from metal, and obtaining the drug-loading fibre diameter is the fibrous membrane of 80-200nm.
Embodiment 19:
The preparation of A chitosan solution: at room temperature will gluing all molecular weight M η relatively and be 1,000,000 chitosan, to be dissolved in concentration expressed in percentage by volume be in 80% the acetic acid solution, be made into mass percentage concentration and be 3% solution, stirred 12 hours, and obtained translucent brown chitosan acetic acid solution;
The preparation of B poly-vinyl alcohol solution: with embodiment 18;
C mixes with poly-vinyl alcohol solution chitosan solution by mass ratio 5/1, obtain the chitosan/polyvinyl alcohol complex solution;
The preparation of D chitosan/polyvinyl alcohol/sulphacetamide blend solution: with the sulfadiazine grind into powder, add that to account for the solution quality percentage concentration be 2% sulphacetamide in the chitosan/polyvinyl alcohol complex solution, be stirred to dissolving fully;
The preparation of E chitosan/polyvinyl alcohol/sulphacetamide electrospun fiber membrane: chitosan/polyvinyl alcohol/sulphacetamide blend solution that step D is obtained adds in the electrostatic spinning apparatus.At electrostatic pressure is 10kv, and syringe pump flow velocity 0.05ml/h, spinning nozzle diameter are 0.30mm, accepts screen apart from electrostatic spinning film forming under the condition of 6cm apart from metal, and obtaining the drug-loading fibre diameter is the fibrous membrane of 100-350nm.
Embodiment 20:
The preparation of A chitosan solution: at room temperature will glue all molecular weight M relatively
ηBe 800,000 chitosan to be dissolved in concentration expressed in percentage by volume be in 80% the acetic acid solution, be made into mass percentage concentration and be 4% solution, stirred 10 hours, obtain translucent brown chitosan acetic acid solution;
The preparation of B poly-vinyl alcohol solution: with embodiment 17;
C mixes with poly-vinyl alcohol solution chitosan solution by mass ratio 8/1, obtain the chitosan/polyvinyl alcohol complex solution;
The preparation of D chitosan/polyvinyl alcohol/minocycline blend solution: with the minocycline grind into powder, add that to account for the solution quality percentage concentration be 3% minocycline in the chitosan/polyvinyl alcohol complex solution, be stirred to dissolving fully;
The preparation of E chitosan/polyvinyl alcohol/minocycline electrospun fiber membrane: chitosan/polyvinyl alcohol/minocycline blend solution that step D is obtained adds in the electrostatic spinning apparatus.At electrostatic pressure is 20kv, and syringe pump flow velocity 0.6ml/h, spinning nozzle diameter are 0.57mm, accepts screen apart from electrostatic spinning film forming under the condition of 10cm apart from metal, and obtaining the drug-loading fibre diameter is the fibrous membrane of 50-320nm.
Embodiment 21:
The preparation of A chitosan solution: with embodiment 20;
The preparation of B poly-vinyl alcohol solution: with embodiment 18;
C mixes with poly-vinyl alcohol solution chitosan solution by mass ratio 7/1, obtain the chitosan/polyvinyl alcohol complex solution;
The preparation of D chitosan/polyvinyl alcohol/amikacin blend solution:, add that to account for the solution quality percentage concentration be that 1% amikacin is stirred to dissolving fully in the chitosan/polyvinyl alcohol complex solution with the amikacin grind into powder;
The preparation of E chitosan/polyvinyl alcohol/amikacin electrospun fiber membrane: chitosan/polyvinyl alcohol/amikacin blend solution that step D is obtained adds in the electrostatic spinning apparatus.At electrostatic pressure is 26.5kv, and syringe pump flow velocity 0.8ml/h, spinning nozzle diameter are 0.77mm, accepts screen apart from electrostatic spinning film forming under the condition of 10cm apart from metal, and obtaining the drug-loading fibre diameter is the fibrous membrane of 50-250nm.
Claims (1)
1. the preparation method of an antibacterial type blended electro spinning nanometer fiber membrane adopts the method for electrostatic spinning preparation, and concrete steps are:
The preparation of A chitosan solution: at room temperature will glue all molecular weight M relatively
ηFor the chitosan of 12-80 ten thousand is dissolved in the acetic acid solution that concentration expressed in percentage by volume is 80-92%, stir, be mixed with the acetic acid solution that mass percentage concentration is the 3-10% chitosan;
The preparation of B poly-vinyl alcohol solution: with degree of polymerization 2500-3500, the polyvinyl alcohol of alcoholysis degree 88-98% is dissolved in the deionized water, is made into the solution that mass percentage concentration is 8-10%;
Two kinds of solution that C obtains steps A and step B mix with the mass ratio of 5-9:1, obtain the chitosan/polyvinyl alcohol composite solution;
The preparation of D chitosan/polyvinyl alcohol/water solublity antibacterials blend solution: the water solublity antibacterials are joined in the composite solution that step C obtains, it is 1-5% that the amount that adds makes the quality percentage composition of water solublity antibacterials in the solution, is stirred to dissolving fully;
The preparation of E chitosan/polyvinyl alcohol/water solublity antibacterials electrospun fiber membrane: chitosan/polyvinyl alcohol/water solublity antibacterials blend solution that step D is obtained joins in the electrostatic spinning apparatus, at electrostatic pressure is 10-35kv, syringe pump flow velocity 0.05-1ml/h, the spinning nozzle diameter is 0.3-1.0mm, accepts screen apart from electrostatic spinning film forming under the condition of 6-18cm apart from metal.
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| CN101538775B (en) * | 2009-04-10 | 2011-02-09 | 东华大学 | Method for electrostatic interweaving and modifying of nylon cellulose acetate compound nanofibre membrane |
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