CN102871772A - Porous degradable blood vessel and preparation method thereof - Google Patents
Porous degradable blood vessel and preparation method thereof Download PDFInfo
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- CN102871772A CN102871772A CN2011101952681A CN201110195268A CN102871772A CN 102871772 A CN102871772 A CN 102871772A CN 2011101952681 A CN2011101952681 A CN 2011101952681A CN 201110195268 A CN201110195268 A CN 201110195268A CN 102871772 A CN102871772 A CN 102871772A
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Abstract
The invention aims to provide a porous degradable blood vessel prepared by a wet method spinning process and a preparation method thereof. The blood vessel is prepared from hollow fiber, has rough and porous surface, contributes to adhesion and growth of vascular cells, and has an effect of regenerating vascular tissues. The preparation method is simple, economic and suitable for industrialized production. The blood vessel has the inner diameter of 0.01 mm to 1 cm, the outer diameter of 0.02 mm to 2 m and the thickness of 0.01 mm to 5 mm. The preparation method comprises the following steps: dissolving a PLC raw material and additives into an organic solvent to prepare a uniform and transparent spinning solution at a certain temperature; standing and defoaming the spinning solution for half an hour, injecting the spinning solution into spinning equipment, injecting core liquid and performing wet method spinning; continuously immersing the hollow fiber into washing liquid for 0.5 minute to 48 hours to remove the residual core liquid and additives; repeatedly washing with deionized water, soaking for 0.5 minute to 48 hours, performing vacuum drying, and intercepting to prepare a vascular stent.
Description
Technical background
Cardiovascular disease serious harm human body is healthy.Its main Therapeutic Method is vascular bypass surgery, needs the blood vessel graft of various diameters as patching material.Therefore, reconstructing blood vessel has very consequence in Clinical Surgery.Succeed in developing first the polyvinyl artificial blood vessel from nineteen fifty-two Voorhees, this method has played certain effect really, but this artificial blood vessel can hinder the formation of normal blood vessels structure.Other non-degraded such as PTFE and Dacron etc. have also hindered vascular cell and have formed collagen and elastin laminin, and these synthetic materials will become physical barrier in the prolonged application process of blood vessel.
The people such as L ' Heureux has made up in 1998 and has used unsupported engineering blood vessel in addition.Smooth muscle cell and fibroblast are put into the culture systems that contains ascorbic acid cultivate respectively, form thin smooth muscle cell tissue and fibroblast tissue after a period of time.They are wrapped in respectively on the same axle, and forming inner face is that layer of smooth muscle cells, outside are the multiple tubes of fibroblast layer.Again at layer of smooth muscle cells inner surface plantation endotheliocyte, so just formed structurally and the blood vessel graft with three-decker from body blood vessel basic simlarity.Because being cultured cell oneself, its extracellular matrix generates, so have good mechanical strength; And owing to there not being the participation of synthetic material, it can lower the generation of infection and immunity of organism rejection, is conducive to improve long-term patency rate.But, after the clinical trial, find that it also exists apparent in view shortcoming.It easily causes thrombosis, and obtains this replacement vessels and also need time of growing.So, bottleneck has also been appearred in its research, unsupported whole-cell biological blood vessel does not still have can extensive use
The research of engineering blood vessel has obtained larger progress in recent years.It is to use seed cell and relevant extracellular matrix (extracellularmatrix, ECM) be raw material, adopt tissue engineering technique, with cell seeding on three-dimensional intravascular stent, make it to stick, break up, grow, and secretion ECM, make up have that histocompatibility is good, non-immunogenicity, have growth potential, durability is long, plasticity is strong, and be difficult for calcification, infection and thrombotic vital replacement vessels, for the cardiovascular surgery blood vessel graft is opened up a new source.In the process of transplanting, the engineering blood vessel endothelialization is successful key, this vascular endothelial cell that depends on plantation is at the sticking of engineering blood vessel surface, growth and differentiation capability, should make it form the monolayer fused cell in blood vessel surface by high-density planting, cultivation, after guaranteeing that again blood vessel implants, can tolerate washing away of blood flow, membrane integrity in as far as possible keeping will guarantee that also Cultured endothelial cell has the normal differentiation function.Secondly, making up the bionical ambient stress of similar arteriopalmus, also is the key of cultivating functionalized organization's engineering blood vessel.Because different stress stimulation environment has visibly different impact to aspects such as the growth migration of the stem cell of engineering blood vessel, nutrient permeation in the intravascular stent and blood vessel are moulding, the optimum stress stimulation that engineering blood vessel forms is the rhythmic pulsation environment of normal tremulous pulse.
In general, desirable vascular stent material of tissue engineering should have following characteristics: avirulence, and namely material itself or its catabolite all can not produce inflammation and toxic reaction; Good biocompatibility; Biodegradability and degraded controllability; Do not cause the immunity of organism rejection; Plasticity and certain mechanical strength; Good surface activity namely has the 3 D stereo loose structure, is conducive to cell adhesion, growth, propagation.In a word, solid (tubulose) with specific three dimensional support must be provided when tissue engineering vessel, host material as the vascular cell plantation, make inoculating cell energy location, attaching, localization growing multiplication, material can make cell arranged evenly in order in rack space simultaneously, differentiation has specific function and synthetic suitable extracellular matrix (ECM), moreover engineering blood vessel when transplanting in the body timbering material also should have mechanics support function, anti-blood stream pressure etc. concurrently.Materials can be divided into biomaterial and synthetic material according to source and character.
Polycaprolactone (PCL) is a kind of more satisfactory tissue engineering bracket material, polycaprolactone (PCL) be a kind of biodegradable aliphatic polyester, have good biocompatibility.It is a kind of ideal stent material, and is nontoxic to body, absorbs gradually after the implantation, finally is degraded to CO
2And H
2O and good mechanical performance (Tadic et al.Comparison of different methods for the preparation of porous bone substitution materialsand structural investigations by synchrotron (micro)-computer tomography.Materialwissenschaft und Werkstofftechnik.2004,35).Have good medicine trafficability characteristic, good biocompatibility and mechanical property, these character make it in medicine control release field certain application potential be arranged, as can be used as material implanted and drug release material.Obtained at present the approval of U.S. FDA.Fix at orthopaedics, also there is major contribution in the field such as tissue renovation material and controlled drug delivery system.The present invention utilizes wet spinning to prepare the PCL hollow-fibre membrane and is used as engineering blood vessel.
Summary of the invention
The object of the invention is to propose a kind of doughnut with the wet spinning technology preparation, the intravascular stent of inventing has rough surface, many skies, is beneficial to adhesion and the growth of vascular cell, has the effect of regeneration vessel tissue.Preparation method is simple, economical, is fit to suitability for industrialized production.
Described vessel diameter is 0.01mm～1cm, and outer warp is 0.02mm～2m, thickness 0.01mm～5mm.
The method of a kind of degradable artificial blood vessel of preparation of the present invention comprises the steps:
With PCL raw material and additive, jointly be dissolved in the organic solvent, at a certain temperature, become the spinning solution of homogeneous transparent with magnetic stirrer.The parts by weight of PCL raw material and additive are 5～40; Organic solvent is 95～60; The weight rate of PCL and additive is 1/9～9/1;
Described PCL raw material degradable polyester weight average molecular weight is 1～3,000,000, and molecular weight distributing index 2～5, impurity weight content are below 1%;
Described additive be Organic substance polyvinylpyrrolidone (PVP), polyethylene glycol oxide (PEO), polyacrylamide, polyvinyl alcohol (PVA) etc. or inorganic material such as calcium carbonate, sodium chloride, ammonium bicarbonate etc. one or more.
Described organic solvent is one or more mixed solvents in oxolane, chloroform, dichloromethane, dichloroethanes, trichloroethane, methyl formate, hexafluoroisopropanol, trifluoroethanol, ethanol, DMF, the trifluoroacetic acid;
Described uniform temperature is 10～100 ℃.
Polymer spinning solution elder generation standing and defoaming is re-introduced in the spinning still half an hour, is connected on the propeller as shown in Figure 1; Spinneret is installed again, is injected core liquid, open and promote the moving as shown in Figure 1 pushed at high pressure device of core liquid stream, treat that the core liquid stream moves when stablizing, and restarts propeller.Carry out wet spinning;
Described core liquid is a kind of in ethanol, methanol, acetone, the water;
Described pushed at high pressure device can be a kind of in nitrogen, carbon dioxide, the helium;
Described propeller is a kind of in electric plating propulsion, the rotary screw.
Carry out wet spinning, receive doughnut with coagulating bath, fiber is drawn by conductive filament roller and godet, around to up-coiler.When fiber is uniform and stable, regulate up-coiler to desirable rotating speed;
Described coagulating bath can in water, ethanol, methanol, the acetone more than one.
Fiber is taken off, in cleaning mixture, continue submergence 0.5min～48h, to remove remaining core liquid and additive.Repeatedly clean with deionized water again, soaked again 0.5min～48h hour, vacuum drying, intercepting makes intravascular stent;
Described cleaning mixture be in water, ethanol, acetone, methanol, the ethyl acetate more than one.
This doughnut can be used for the fields such as intravascular stent, diafiltration material, cardiac stent, cerebrovascular, nerve trachea.
The invention benefit
1. biodegradable doughnut, not only have nonhazardous, nonirritant, chemical stability good, degrade, do not cause inflammation, without anaphylaxis, good biocompatibility, not carcinogenic, content of beary metal is low, pH value is little, do not cause the performances such as haemolysis and blood coagulation.And have required Physical and mechanical properties and processing characteristics, and can stand to disinfect.And implanting does not need again to take out, and reduces patient painful;
2. by the blood vessel of wet spinning technology preparation, have that operational approach is simple, Financial cost is lower, can suitability for industrialized production;
3. described prepared doughnut base artificial blood vessel has good biocompatibility and tissue regeneration ability; The degradation rate that is complementary with the tissue regeneration of human body corrupted; Energy is the organizational structure of simulated blood vessel better, rough surface, and macropore is beneficial to cell adhesion, creeps, breaks up and propagation; Reach intensity and the clinical operability of required repair tissue or organ.Larger hole can guarantee that neutrophilic leukocyte in the human body by repairing the hole of support, engulfs the antibacterial that easily causes infection, the healing at the position that is conducive to be wound and be difficult for causing the infection at position of being wound.
Description of drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of the blood vessel prepared of the embodiment of the invention 1.
Fig. 2 is the spinning technique flow chart of the embodiment of the invention 1 preparation blood vessel.
The specific embodiment
Below in conjunction with drawings and Examples the present invention is described in detail.
Fig. 1 is the photo that the present invention prepares degradable multiporous blood vessel.
Below by embodiment the present invention is carried out concrete description; it is to be noted; following examples just are used for the present invention is further specified; can not be interpreted as limiting the scope of the invention, the person skilled in the art in this field can make some nonessential improvement and adjustment to the present invention according to the invention described above content.
The preparation of spinning liquid:
With PCL raw material and PEO, jointly be dissolved in the oxolane, under 10 ℃, become the spinning solution of homogeneous transparent with magnetic stirrer.The total umber of the weight of PCL and PEO is 10; The oxolane umber is 90; The weight rate of PCL and PEO is 4: 1;
The doughnut preparation:
Spinning solution elder generation standing and defoaming is re-introduced in the spinning still half an hour, is connected on the electric plating propulsion as shown in Figure 1; Spinneret is installed again, is injected acetone, open and promote the high-pressure nitrogen bottle that acetone flows, treat that the core liquid stream moves when stablizing, and restarts propeller.Carry out wet spinning.
Carry out wet spinning, water and acetone weight proportion are 50/50 coagulating bath reception doughnut, and fiber is drawn by conductive filament roller and godet, around to up-coiler.When fiber is uniform and stable, regulate up-coiler to desirable rotating speed.
The blood vessel preparation:
Fiber is taken off from up-coiler, in alcoholic solution, continue submergence 48h, to remove remaining acetone and additive PEO.Repeatedly clean with deionized water again, soaked again 48h hour, vacuum drying, intercepting makes blood vessel.
The preparation of spinning liquid:
With PCL raw material and PVP, jointly be dissolved in the chloroform, under 50 ℃, become the spinning solution of homogeneous transparent with magnetic stirrer.The total umber of the weight of PCL and PVP is 40; The chloroform umber is 60; The weight rate of PCL and PVP is 1: 4;
The doughnut preparation:
Spinning solution elder generation standing and defoaming is re-introduced in the spinning still half an hour, is connected on the worm propeller as shown in Figure 1; Spinneret is installed again, is injected acetone, open and promote the high-pressure carbon dioxide bottle that ethanol flows, treat that the core liquid stream moves when stablizing, and restarts propeller.Carry out wet spinning.
Carry out wet spinning, water and acetone weight proportion are 100/0 coagulating bath reception doughnut, and fiber is drawn by conductive filament roller and godet, around to up-coiler.When fiber is uniform and stable, regulate up-coiler to desirable rotating speed.
The blood vessel preparation:
Fiber is taken off from up-coiler, in aqueous solution, continue submergence 48h, to remove remaining additive PVP.Vacuum drying, intercepting makes blood vessel.
Embodiment 3
The preparation of spinning liquid:
With PCL raw material and PVA, jointly be dissolved in the methyl formate, under 100 ℃, become the spinning solution of homogeneous transparent with magnetic stirrer.The total umber of the weight of PCL and PVA is 20; The methyl formate umber is 80; The weight rate of PCL and PVA is 9: 1;
The doughnut preparation:
Spinning solution elder generation standing and defoaming is re-introduced in the spinning still half an hour, is connected on the electric plating propulsion as shown in Figure 1; Spinneret is installed again, is injected acetone, open and promote the high-pressure carbon dioxide bottle that acetone flows, treat that the core liquid stream moves when stablizing, and restarts propeller.Carry out wet spinning.
Carry out wet spinning, receive doughnut with the acetone coagulating bath, fiber is drawn by conductive filament roller and godet, around to up-coiler.When fiber is uniform and stable, regulate up-coiler to desirable rotating speed.
The blood vessel preparation:
Fiber is taken off from up-coiler, is 80/20 solution for continuous submergence 48h in acetone and water proportioning, to remove remaining acetone and additive PVA.Repeatedly clean with deionized water again, soaked again 48h hour, vacuum drying, intercepting makes blood vessel.
Embodiment 4
The preparation of spinning liquid:
With PCL raw material and inorganic matter calcium carbonate, jointly be dissolved in the ethyl acetate, under 100 ℃, become the spinning solution of homogeneous transparent with magnetic stirrer.The total umber of the weight of PCL and inorganic matter calcium carbonate is 15; The ethyl acetate umber is 85; The weight rate of PCL and inorganic matter calcium carbonate is 7: 3;
The doughnut preparation:
Spinning solution elder generation standing and defoaming is re-introduced in the spinning still half an hour, is connected on the electric plating propulsion as shown in Figure 1; Spinneret is installed again, is injected acetone, open and promote the high-pressure carbon dioxide bottle that acetone flows, treat that the core liquid stream moves when stablizing, and restarts propeller.Carry out wet spinning.
Carry out wet spinning, receive doughnut with the acetone coagulating bath, fiber is drawn by conductive filament roller and godet, around to up-coiler.When fiber is uniform and stable, regulate up-coiler to desirable rotating speed.
The blood vessel preparation:
Fiber is taken off from up-coiler, is 20/80 solution for continuous submergence 48h in acetone and water proportioning, to remove remaining acetone and additive calcium carbonate.Repeatedly clean with deionized water again, soaked again 48h hour, vacuum drying, intercepting makes blood vessel.
Embodiment 5
With the doughnut in above-described embodiment 1～4, the centre penetrates softer fine rule or soft tinsel subsides to prevent fiber, then be wrapped on the spinning reel, stretching under 0～40 ℃ of temperature (can once step stretching, also can be divided into multi-step tension), with the intensity of enhancing doughnut, thus bearing capacity and the mechanical strength of raising blood vessel.
Claims (10)
1. one kind with a kind of porous, degradable blood vessel of wet spinning technology preparation and preparation method thereof, it is characterized in that blood vessel made by doughnut, and vessel diameter is 0.01mm～1cm, and outer warp is 0.02mm～2m, thickness 0.01mm～5mm.
2. such as claim 1 porous, degradable blood vessel, it is characterized in that described doughnut base material is the own Inner ester of biodegradable poly, molecular weight is 10,000 to 3,000,000, and molecular weight distributing index 2～5, impurity weight content are below 1%.
3. the preparation method of a porous, degradable tissue blood vessel is characterized in that adopting following steps:
With PCL raw material and additive, jointly be dissolved in the organic solvent, at a certain temperature, become the spinning solution of homogeneous transparent with magnetic stirrer.The parts by weight of PCL raw material and additive are 5～40; Organic solvent is 95～60; The weight rate of PCL and additive is 1/9～9/1;
The own Inner ester of described PCL raw material degradable poly such as claim 2;
Described additive such as claim 4;
Described organic solvent such as claim 5;
Polymer spinning solution elder generation standing and defoaming is re-introduced in the spinning still half an hour, is connected on the propeller as shown in Figure 1; Spinneret is installed again, is injected core liquid, open and promote the moving as shown in Figure 1 pushed at high pressure device of core liquid stream, treat that the core liquid stream moves when stablizing, restart propeller, carry out wet spinning;
Described core liquid such as claim 6;
Described core liquid such as claim 7;
Described propeller such as claim 8;
Carry out wet spinning, receive doughnut with coagulating bath, fiber is drawn by conductive filament roller and godet, around to up-coiler.When fiber is uniform and stable, regulate up-coiler to desirable rotating speed;
Described coagulating bath such as claim 9;
Fiber is taken off, in cleaning mixture, continue submergence 0.5min～48h, to remove remaining core liquid and additive.Repeatedly clean with deionized water again, soaked again 0.5min～48h hour, vacuum drying, intercepting makes intravascular stent;
Described cleaning mixture such as claim 10.
4. method according to claim 3, it is characterized in that, additive be in polyvinylpyrrolidone (PVP), polyethylene glycol oxide (PEO), Polyethylene Glycol (PEG), polyacrylamide, polyvinyl alcohol (PVA) etc. or inorganic material such as calcium carbonate, sodium chloride, the ammonium bicarbonate one or more.
5. method according to claim 3, it is characterized in that, described organic solvent is one or more mixed solvents in oxolane, chloroform, dichloromethane, dichloroethanes, trichloroethane, methyl formate, hexafluoroisopropanol, trifluoroethanol, ethanol, DMF, the trifluoroacetic acid.
6. method according to claim 3 is characterized in that, described uniform temperature is 10～100 ℃.
7. method according to claim 3 is characterized in that, described core liquid is a kind of in ethanol, methanol, acetone, the water.
8. method according to claim 3 is characterized in that, described thrust unit can be a kind of in nitrogen, carbon dioxide, helium high pressure propeller, the rotary screw thrust unit.
9. method according to claim 3 is characterized in that, described coagulating bath can in water, ethanol, methanol, the acetone more than one.；
10. method according to claim 3 is characterized in that, described cleaning mixture be in water, ethanol, acetone, methanol, the ethyl acetate more than one.
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| CN106109054A (en) * | 2016-08-19 | 2016-11-16 | 上海交通大学医学院附属上海儿童医学中心 | Large aperture parallel polycaprolactone electrospinning cotton is utilized to build autologous tissue's engineered blood vessels |
| CN106491240A (en) * | 2015-09-07 | 2017-03-15 | 先健科技(深圳)有限公司 | absorbable stopper |
| CN107296979A (en) * | 2017-07-02 | 2017-10-27 | 东华大学 | A kind of organizational project nanofiber intravascular stent and preparation method thereof |
| CN109260521A (en) * | 2018-10-16 | 2019-01-25 | 广州润虹医药科技股份有限公司 | A kind of degradable artificial bone and preparation method thereof |
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| CN103961750A (en) * | 2014-04-22 | 2014-08-06 | 中国人民武装警察部队后勤学院 | Small-caliber in-situ tissue engineering blood vessel and construction method thereof |
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| CN107296979A (en) * | 2017-07-02 | 2017-10-27 | 东华大学 | A kind of organizational project nanofiber intravascular stent and preparation method thereof |
| CN109260521A (en) * | 2018-10-16 | 2019-01-25 | 广州润虹医药科技股份有限公司 | A kind of degradable artificial bone and preparation method thereof |
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Application publication date: 20130116 |