CN102433684A - Superfine composite fiber film, preparation method and use thereof - Google Patents
Superfine composite fiber film, preparation method and use thereof Download PDFInfo
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- CN102433684A CN102433684A CN2011103472689A CN201110347268A CN102433684A CN 102433684 A CN102433684 A CN 102433684A CN 2011103472689 A CN2011103472689 A CN 2011103472689A CN 201110347268 A CN201110347268 A CN 201110347268A CN 102433684 A CN102433684 A CN 102433684A
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Abstract
The invention relates to a biodegradable and bioabsorbable superfine composite fiber film, which consists of poly lactic-co-glycolic acid of the weight ratio ranging from 75wt% to 100wt% and poly latic acid-b-polyethylene glycol of the weight ratio ranging from 0wt% to 25wt%. The preparation method includes the following steps of mixing the poly lactic-co-glycolic acid and the poly latic acid-b-polyethylene glycol into N, N-dimethylformamide or acetone or mixture of the N-dimethylformamide and the acetone so as to obtain uniform polymer solution, then stirring the uniform polymer solution at room temperature to obtain uniform mixed liquid, and finally injecting the uniform mixed liquid into an electrostatic spinning device to conduct electrostatic spinning, and accordingly the poly lactic-co-glycolic acid and the poly lactic acid-b-polyethylene glycol superfine composite fiber film is obtained. The superfine composite fiber film has excellent biocompatibility and adjustable biodegradation, has the advantages of light and soft texture and fine permeability simultaneously, and can be used as excellent internal adhesion-proof materials.
Description
Technical field
But the present invention relates to a kind of biodegradable superfine composite fiber film, Its Preparation Method And Use that reaches the post-operation adhesion preventing of bio-absorbable, relate in particular to superfine composite fiber film, the Its Preparation Method And Use of a kind of poly (glycolide-lactide) (PLGA) and polylactide-b-polyethylene glycol (PELA) preparation.
Background technology
Post-operation adhesion is the science difficult problem that surgical field has rate occurred frequently and recurrence rate.The caused complication of post-operation adhesion brings great misery not only for patient's daily life, and makes having a big risk of second operation increase greatly.Therefore, how to prevent post-operation adhesion, the misery that reduces patient becomes the problem of medical domain research.For a long time, medical circle is being done a large amount of work aspect the research that prevents postoperative intestinal adhesion, and effect surely belongs to the physical isolation method the most significantly.At present commercially available anti product mainly occurs with the form of gel, solid film and nonwoven fabric etc.
Adherence preventing material roughly is divided into the material of non-absorbent material and absorption.
Non-absorbent material comprises silicon chip, GoreTex sheet, comprises the anti-organ adhesion membrane of the aquagel membrane of mixed polymer, and said mixed polymer comprises the water-soluble polymer of polyvinyl alcohol and appointment.Although through sheet is attached on the damage location, thereby these sheets can make there is not adhesion by physical separation damage locations, and they can not be absorbed in vivo, have therefore produced artificial material and have been detained the problem in the body.In addition, not absorbing sheet of pasting like this or film itself can cause dysfunction through adhering to organ.In this situation, even also can not remove the sheet that adheres to like this on the organ through performing the operation once more.Therefore, but attempted developing the absorption base bottom material that high safety in vivo absorbs.
CN 101056662B discloses a kind of adherence preventing material, and it comprises water-absorbent crosslinked poly-gamma-glutamic acid as active ingredient, wherein water-absorbent crosslinked poly-gamma-glutamic acid being cross-linked to form through poly-gamma-glutamic acid and another poly-gamma-glutamic acid.
CN 100525778C discloses a kind of novel post-operation adhesion preventing material and preparation method, and its component and content are as follows by weight percentage: shitosan 10-90, polyanion or polyethylene glycol 90-10; Novel post-operation adhesion preventing preparation methods is 1) shitosan is dissolved in the acid solution of 0.1%-5%, be made into the chitosan solution that concentration is 0.5%-6%; Wherein: acid is hydrochloric acid, citric acid, acetic acid or tartaric acid; 2) solution concentration with polyanion and distilled water is made into 1%-15%; Or the solution concentration of polyethylene glycol and distilled water is made into 1%-30%.With above-mentioned 1) and 2) two solution mix, and promptly obtain the solution-type adherence preventing material.Adherence preventing material Anti Triplex can be film material, gel or solution.
CN 1876926A discloses a kind of preparation of nano-scale fiber bondedfibre fabric, reaches the application as the post-operation adhesion preventing film.This bondedfibre fabric adopts the method preparation of electrostatic spinning and gets.At first prepare spinning solution, aliphatic polyester is dissolved in solvent, stirring makes the aliphatic polyester spinning solution.The spinning solution solvent for use is a carrene, chloroform, acetone, tetrachloroethanes, one or both compound system such as dimethylacetylamide.Secondly on electrostatic spinning machine, make the aliphatic polyester superfine fibre through spinning solution dress notes, electrostatic spinning and two steps of collection superfine fibre, realize that electricity is spun into the bondedfibre fabric of nano-scale fiber, is used for post-operation adhesion preventing after sterilization is handled.
Clinical effectiveness shows; Though these products can play certain preventing adhesiving effect; But also have a lot of problems to need to be resolved hurrily, as material organize matching, degradability and operability etc., these all need further research and improve the purpose that improves preventing adhesiving effect to reach.
Summary of the invention
To the deficiency of prior art, but one of the object of the invention is to provide a kind of biodegradable superfine fibre composite membrane that reaches bio-absorbable and good biocompatibility.
Superfine composite fiber film of the present invention is made up of the poly (glycolide-lactide) of 75wt%～100wt% and the polylactide of 0wt%～25wt%-b-polyethylene glycol.
As optimal technical scheme, superfine composite fiber film of the present invention is made up of the poly (glycolide-lactide) of 85wt%～95wt% and the polylactide of 5wt%～15wt%-b-polyethylene glycol.
Poly (glycolide-lactide) is prepared by glycolide and lactide monomer ring opening copolymer, and is nontoxic, is prone to processing, has favorable biological degradability and biocompatibility, but owing to its hydrophobicity causes cellular affinity bad.Polylactide-b-polyethylene glycol is an amphipathic nature block polymer, has excellent biological compatibility and hydrophily, but its biological degradability is bad.Two kinds of materials all are safe in utilization through the FDA authentication, the material of excellent performance.The present invention in conjunction with both chiefs, uses rational mass distribution to obtain the suitable superfine composite fiber film of easily biological-degradable again of adhesiveness according to the characteristic of the two.
As optimal technical scheme, the weight average molecular weight of described poly (glycolide-lactide) is 40,000～200,000; Preferably, the mol ratio of lactide and glycolide is 95: 5～40: 60 in the poly (glycolide-lactide).
As optimal technical scheme, the weight average molecular weight of described polylactide-b-polyethylene glycol is 2000～80,000; Preferably, the mol ratio of polylactide and polyethylene glycol is 9: 1～2: 8 in polylactide-b-polyethylene glycol.
As optimal technical scheme, the fibre diameter of described fiber rete is 500nm～5000nm, preferred 1000nm～3000nm; The thickness of described fiber rete is 100 μ m～180 μ m, preferred 120 μ m～180 μ m.
The superfine composite fiber film that obtains can further carry out vacuumize under room temperature (as 25 ℃).As desirable adherence preventing material, superfine composite fiber film provided by the present invention has excellent biological compatibility, suitable tissue adherence, fully wound coverage surface and have RT in enough bodies; Can degraded and absorbed and do not need second operation that it is taken out; Can effectively prevent the normal healing that adhesion forms does not influence wound again; Also have certain mechanical strength and be convenient to implementation and operation etc.In addition, this film has the light weight softness through the electrostatic spinning technique preparation, and advantages such as high porosity especially have suitable thickness, can be used as the post-operation adhesion preventing material.
One of the object of the invention also is to provide a kind of preparation method of superfine composite fiber film.
The preparation method of superfine composite fiber film provided by the present invention comprises the steps: 1) poly (glycolide-lactide) and polylactide-b-polyethylene glycol mixing are dissolved in N, in dinethylformamide or acetone or its mixture, obtain homogeneous polymer solution; 2) the homogeneous polymer solution with the step 1) gained at room temperature stirs, and obtains the mixed liquor of homogeneous; 3) with step 2) mixed liquor of the homogeneous of gained injects electrostatic spinning apparatus and carries out electrostatic spinning, obtains the superfine composite fiber film of poly (glycolide-lactide) and polylactide-b-polyethylene glycol.
In recent years, along with the maturation of electrostatic spinning technique, the static spinning membrane of selecting for use biocompatibility macromolecule to prepare is adapted at Application as Medical Material owing to have characteristics such as super large specific area and super large porosity.The structure of the class cytoskeleton matrix on the static spinning membrane microcosmic not only has cell compatibility, and the structure of these porous has good gas permeability, is beneficial to the exchange and the transmission of endotrophic material.Adopt static spinning membrane can reach the effect of playing physical barrier as adherence preventing material, the circulation environment of nutriment and metabolite between can also guaranteeing to organize, thus when playing preventing adhesiving effect, also help normally carrying out of wound healing.
Yet, because the appearance of three-dimensional pore space structure, make to face a lot of problems in the research process of static spinning membrane as adherence preventing material.We find through the zoopery outcome research: if material is too thin, cell can penetrate film and grow, and can't play antiblocking effect; And material is too thick, causes rejection owing to the increase of implantation amount makes histocompatbility reduce, thereby to causing burden in the body.Therefore, when static spinning membrane is used as adherence preventing material, how to confirm that optimum thickness becomes a key breakthrough point of this technical field.The thickness of fiber rete of the present invention is selected both can play antiblocking effect during use between 100 μ m～180 μ m, can not cause burden to health again.The condition of electrostatic spinning can adopt prior art among the present invention, and voltage is that 15～30kV, liquid inventory are that 10～100L/min, receiving range are 5cm～25cm.
In the step 1) in the mixture of poly (glycolide-lactide) and polylactide-b-polyethylene glycol poly (glycolide-lactide) account for 75wt%～100wt% and polylactide-b-polyethylene glycol accounts for 0wt%～25wt%.
As preferably, the weight average molecular weight of poly (glycolide-lactide) is 40,000～200,000 in the step 1), and the mol ratio of lactide and glycolide is 95: 5～40: 60 in the preferred poly (glycolide-lactide).
As preferably, the weight average molecular weight of polylactide in the step 1)-b-polyethylene glycol is 2000～80,000, and the mol ratio of polylactide and polyethylene glycol is 9: 1～2: 8 in preferred polylactide-b-polyethylene glycol.
As preferably, N in the step 1), the volume ratio of dinethylformamide and acetone is 1: 9～9: 1.
As preferably, in the step 1) in the polymer solution the total mass and size percentage concentration of polymer be 25%～70%, the preferred mass concentration expressed in percentage by volume is 30%～60%, further the preferred mass concentration expressed in percentage by volume is 30%～50%.
One of the object of the invention also is to provide a kind of superfine composite fiber film to be used for resection in the body; Have good material compatibility and structural compatibility; Can fix certainly, promote wound healing and play good physical barrier effect, thereby play good preventing adhesiving effect.
Description of drawings
The surperficial SEM figure of the superfine fibre composite film material that PLGA and PELA prepare among Fig. 1 embodiment 1.
The section SEM figure of the superfine fibre composite film material that PLGA and PELA prepare among Fig. 2 embodiment 1.
The specific embodiment
For ease of understanding the present invention, it is following that the present invention enumerates embodiment.Those skilled in the art should understand, and said embodiment only is used for helping to understand the present invention, should not be regarded as concrete restriction of the present invention.
Embodiment one
(1) preparation of solution: (molecular weight is 80,000 with PLGA; Wherein the mol ratio of lactide and glycolide is 95: 5) (molecular weight is 10,000 with PELA; Wherein the mol ratio of polylactide and polyethylene glycol is 2: 8) be dissolved in N; In the mixed solvent of N dimethyl formamide (DMF) and acetone (volume ratio is 5: 5), obtain total polymer mass and size concentration and be 50% PLGA and the mixed solution of PELA.In the solution, the mass ratio of PLGA and PELA is 95: 5.
(2) electrostatic spinning: the PLGA solution that obtains in the step (1) is placed in the feed injector of electrospinning device.The distance of regulating between spinning head and the roller is 12cm, and the environment temperature of spinning is 25 ℃, and the air velocity in the environment is controlled at 0.5～0.8m
3/ hr opens high voltage source and feed injector pump, and regulation voltage is to 20kV, and the delivery rate of solution is 20 μ l/min, carries out spinning, and spinning time 100min obtains electrostatic spinning superfine fibre composite membrane on swing roller.
(3) with the tunica fibrosa of collecting in the step (2) repeatedly with behind the deionized water rinsing, vacuumize after 24 hours in 20 ℃ of vacuum drying chambers obtains superfine fibre composite film material biodegradable and that absorb.The superfine fibre composite film material is a nonwoven fabric construct, and the superfine fibre diameter is between 1～3 μ m, and is as shown in Figure 1; Have three-dimensional loose loose structure, as shown in Figure 2.The fibrage thickness is 100～180 μ m.
Embodiment two
(1) preparation of solution: (molecular weight is 200,000 with PLGA; Wherein the mol ratio of lactide and glycolide is 3: 1) (molecular weight is 10,000 with PELA; Wherein the mol ratio of polylactide and polyethylene glycol is 50: 50) be dissolved in N; In the mixed solvent of N dimethyl formamide (DMF) and acetone (volume ratio is 9: 1), obtain total polymer mass and size concentration and be 35% PLGA and the mixed solution of PELA.In the solution, the mass ratio of PLGA and PELA is 80: 20.
(2) electrostatic spinning: the PLGA solution that obtains in the step (1) is placed in the feed injector of electrospinning device.The distance of regulating between spinning head and the roller is 12cm, and the environment temperature of spinning is 25 ℃, and the air velocity in the environment is controlled at 0.5～0.8m
3/ hr opens high voltage source and feed injector pump, and regulation voltage is to 20kV, and the delivery rate of solution is 20 μ l/min, carries out spinning, and spinning time 150min obtains electrostatic spinning superfine fibre composite membrane on swing roller.
(3) with the tunica fibrosa of collecting in the step (2) repeatedly with behind the deionized water rinsing, vacuumize after 24 hours in 20 ℃ of vacuum drying chambers obtains superfine fibre composite film material biodegradable and that absorb.The superfine fibre composite film material is a nonwoven fabric construct, and the superfine fibre diameter is between 1～3 μ m; Has three-dimensional loose network-like structure.The fibrage thickness is 100～150 μ m.
Embodiment three
(1) preparation of solution: (molecular weight is 40,000 with PLGA; Wherein the mol ratio of lactide and glycolide is 3: 1) (molecular weight is 80,000 with PELA; Wherein the mol ratio of polylactide and polyethylene glycol is 9: 1) be dissolved in N; In the mixed solvent of N dimethyl formamide (DMF) and acetone (volume ratio is 1: 9), obtaining total polymer mass and size concentration is the PLGA of 45wt% and the mixed solution of PELA.In the solution, the mass ratio of PLGA and PELA is 75: 25.
(2) electrostatic spinning: the PLGA solution that obtains in the step (1) is placed in the feed injector of electrospinning device.The distance of regulating between spinning head and the roller is 12cm, and the environment temperature of spinning is 25 ℃, and the air velocity in the environment is controlled at 0.5～0.8m
3/ hr opens high voltage source and feed injector pump, and regulation voltage is to 20kV, and the delivery rate of solution is 20 μ l/min, carries out spinning, and spinning time 120min obtains electrostatic spinning superfine fibre composite membrane on swing roller.
(3) with the tunica fibrosa of collecting in the step (2) repeatedly with behind the deionized water rinsing, vacuumize after 24 hours in 20 ℃ of vacuum drying chambers obtains superfine fibre composite film material biodegradable and that absorb.The superfine fibre composite film material is a nonwoven fabric construct, and the superfine fibre diameter is between 1～5 μ m; Has three-dimensional loose loose structure.The fibrage thickness is 100～150 μ m.
Applicant's statement; The present invention explains detailed process equipment of the present invention and technological process through the foregoing description; But the present invention is not limited to above-mentioned detailed process equipment and technological process, does not mean that promptly the present invention must rely on above-mentioned detailed process equipment and technological process could be implemented.The person of ordinary skill in the field should understand, and to any improvement of the present invention, to the interpolation of the equivalence replacement of each raw material of product of the present invention and auxiliary element, the selection of concrete mode etc., all drops within protection scope of the present invention and the open scope.
Claims (9)
1. a superfine composite fiber film is characterized in that, is made up of the poly (glycolide-lactide) of 75wt%～100wt% and the polylactide of 0wt%～25wt%-b-polyethylene glycol.
2. superfine composite fiber film according to claim 1 is characterized in that, is made up of the poly (glycolide-lactide) of 85wt%～95wt% and the polylactide of 5wt%～15wt%-b-polyethylene glycol.
3. superfine composite fiber film according to claim 1 and 2 is characterized in that, the weight average molecular weight of described poly (glycolide-lactide) is 40,000～200,000;
Preferably, the mol ratio of lactide and glycolide is 95: 5～40: 60 in the poly (glycolide-lactide).
4. superfine composite fiber film according to claim 1 and 2 is characterized in that, the weight average molecular weight of described polylactide-b-polyethylene glycol is 2000～80,000;
Preferably, the mol ratio of polylactide and polyethylene glycol is 9: 1～2: 8 in polylactide-b-polyethylene glycol.
5. according to each described superfine composite fiber film of claim 1～4, it is characterized in that the fibre diameter of described fiber rete is 500nm～5000nm, preferred 1000nm～3000nm.
6. according to each described superfine composite fiber film of claim 1～5, it is characterized in that the thickness of described fiber rete is 100 μ m～180 μ m, preferred 100 μ m～150 μ m.
7. according to the preparation method of each described superfine composite fiber film of claim 1～6; Comprise the steps: 1) poly (glycolide-lactide) and polylactide-b-polyethylene glycol mixing are dissolved in N; In dinethylformamide or acetone or its mixture, obtain homogeneous polymer solution; 2) the homogeneous polymer solution with the step 1) gained at room temperature stirs, and obtains the mixed liquor of homogeneous; 3) with step 2) mixed liquor of the homogeneous of gained injects electrostatic spinning apparatus and carries out electrostatic spinning, obtains the superfine composite fiber film of poly (glycolide-lactide) and polylactide-b-polyethylene glycol.
8. method according to claim 7 is characterized in that, in the step 1) in the mixture of poly (glycolide-lactide) and polylactide-b-polyethylene glycol poly (glycolide-lactide) account for 75wt%～100wt% and polylactide-b-polyethylene glycol accounts for 0wt%～25wt%;
Preferably, the weight average molecular weight of poly (glycolide-lactide) is 40,000～200,000 in the step 1), and the mol ratio of lactide and glycolide is 95: 5～40: 60 in the preferred poly (glycolide-lactide);
Preferably, the weight average molecular weight of polylactide in the step 1)-b-polyethylene glycol is 2000～80,000, and the mol ratio of polylactide and polyethylene glycol is 9: 1～2: 8 in preferred polylactide-b-polyethylene glycol;
Preferably, N in the step 1), the volume ratio of dinethylformamide and acetone is 1: 9～9: 1;
Preferably, in the step 1) in the polymer solution the total mass and size percentage concentration of polymer be 30%～70%, the preferred mass concentration expressed in percentage by volume is 35%～60%, further the preferred mass concentration expressed in percentage by volume is 35%～50%.
9. according to the purposes of each described superfine composite fiber film of claim 1～6, it is characterized in that described superfine composite fiber film is used for resection in the body.
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| CN103768662A (en) * | 2014-02-26 | 2014-05-07 | 中国科学院长春应用化学研究所 | Preparation method of biodegradable medical surgical anti-adhesion membrane |
| CN107747165A (en) * | 2017-10-16 | 2018-03-02 | 苏州大学 | A kind of super hydrophilic polyester nano tunica fibrosa and preparation method thereof |
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| CN107747165B (en) * | 2017-10-16 | 2019-06-25 | 苏州大学 | A kind of super hydrophilic polyester nano tunica fibrosa and preparation method thereof |
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