CN104548198B - A kind of preparation technology loading dipyridamole polyurethane anticoagulant material - Google Patents
A kind of preparation technology loading dipyridamole polyurethane anticoagulant material Download PDFInfo
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- CN104548198B CN104548198B CN201410855065.4A CN201410855065A CN104548198B CN 104548198 B CN104548198 B CN 104548198B CN 201410855065 A CN201410855065 A CN 201410855065A CN 104548198 B CN104548198 B CN 104548198B
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- dipyridamole
- fluid
- polyurethane
- blood vessel
- preparation technology
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Abstract
The invention discloses a kind of load dipyridamole polyurethane anticoagulant material and preparation technology thereof, material is core shell structure, and internal layer is dipyridamole load layer, and outer layer is PU body layer.The material of the present invention as artificial blood vessel transplanted time, can be with long-acting slow-release dipyridamole, the platelet gathering of sticking on artificial blood vessel surface is inhibited to activate, enhance the blood compatibility of this artificial blood vessel, it is prevented effectively from Acute thrombosis and neointimal hyperplasia, the transplanting succeed rate of artificial blood vessel can be effectively improved.
Description
Technical field
The present invention relates to a kind of interventional therapy material and preparation technology thereof, load dipyridamole polyurethane particularly to one
Anticoagulant material and preparation technology thereof.
Background technology
The heavy caliber artificial blood vessel's technology maturation used clinically at present, has good patency rate, but little for bore
In the region that the blood vessel of 6mm or blood flow rate are slow, such as coronary artery or inferior genicular artery, the mortality of synthetic vascular grafts is very
High.Trace it to its cause, mainly due to Acute thrombosis and neointimal hyperplasia.It is to make that platelet activates at artificial blood vessel's surface adhesion
Becoming the initiation factor of this reason, being very important so adding antiplatelet drug in artificial blood vessel.Polyurethane has
Good compliance, is commonly used for artificial blood vessel's material.For antiplatelet drug wherein to improve its blood phase further
Capacitive, current rare report.
Dipyridamole is a kind of little molecule antiplatelet drug, trade name persantin, and it can be by improving in platelet
Portion's cAMP concentration suppresses hematoblastic and sticks gathering, and can make vasodilation high concentration when.
Electrostatic spinning technique is to prepare superfine fibre by electrostatic force as pull strength.In electrostatic spinning process, poly-
Polymer solution or liquation are coupled with the high-pressure electrostatic of thousand of to several ten thousand volts, thus produce between the reception device of capillary tube and ground connection
One powerful electric field force.Electric field force puts on the surface of liquid and produces electric current, and the characteristic utilizing like charges to repel each other makes
Electric field force is in opposite direction with the surface tension of liquid.When the size of electric field force is equal to macromolecular solution or the surface tension of melt
Time, charged drop is just suspended on the end of capillary tube and is in poised state.Along with the increase of electric field force, capillary end is in half
Spherical drop will be drawn into coniform under the effect of electric field force, i.e. Taylor bores.When additional electrostatic pressure increases and exceedes
During a certain marginal value, electric field force suffered by polymer solution will overcome itself surface tension and viscous force and to form injection thin
Stream.Injection thread drafted thousands of times within a few tens of milliseconds, along unstable helical trajectory curvature movement.Along with waving of solvent
Sending out, jet solidify to form micron to nano grade superfine fibre, is arranged on collection device with disordered state, forms non-woven fabrics.
Coaxial electrostatic spinning is one of impressive progress of electrostatic spinning, its can conveniently prepare have core-shell knot
The micro nanometer fiber of structure.The principle of coaxial electrically spun is similar with common electrospinning, and Main Differences is that single capillary tube spinning nozzle is improved
Compound capillary shower nozzle for concentric shafts.The solution of core material and Shell Materials is attached separately in two propelling containers, and shell is molten
Liquid enters compound spinning appts inner chamber, the then ring-type sky between inside and outside capillary spinning nozzle under the driving of micro-injection pump
Flow out at gap；Core solution flows out from interior capillary shower nozzle.Because diameter less internal layer capillary shower nozzle is placed in is relatively large in diameter outer layer hair
In thin shower nozzle and keep coaxially, thus shell and core solution in coaxial device for spinning not in contact with, and at Coaxial nozzle end
Collecting at Kou and form compound drop, when connecting high voltage electric field, electric field force overcomes surface tension and the viscous force of itself, is formed
Core-shell structure jet because two kinds of solution are asked the shortest during coaxial electrostatic spinning when converging at spinning nozzle, add two kinds molten
The diffusion coefficient of liquid is relatively low, does not haves miscible before solidification, therefore can form core-shell structure fiber.But actually coaxial electrically spun
Technical parameter is complicated far beyond common electrostatic spinning, needs repeatedly to debug inside and outside fluid solution formula and regulation electrospinning parameter, ability
Obtain stable electro-spinning process and do not have product defective.
At present, utilized electrostatic spinning technique to prepare artificial blood vessel, but these artificial blood vessels are the most only
Only it is made up of polyurethane, is limited to the feature of self of electrostatic spinning process, in prior art, do not have technique well to make
Standby obtain having core-shell structure, be loaded with the artificial blood vessel of anti-platelet agents.
Summary of the invention
It is an object of the invention to provide a kind of load dipyridamole polyurethane anticoagulant material and preparation technology thereof.
The technical solution used in the present invention is:
A kind of load dipyridamole polyurethane anticoagulation tubular material, this material is core-shell structure, and internal layer is dipyridamole
Load layer, outer layer is PU body layer.
A kind of preparation technology loading dipyridamole polyurethane anticoagulation tubular material, comprises the steps:
1) configuration outer fluid: outer fluid is polyurethane solutions, and its solvent is oxolane and DMF
Mixed solution；
2) fluid in configuration: interior fluid is made up of dipyridamole, thickening agent and solvent, and solvent is chloroform；
3) in using, fluid, outer fluid carry out coaxial electrostatic spinning, are dried to obtain load dipyridamole polyurethane anticoagulation
Tubular material.
The quality proportioning of interior fluid is: dipyridamole 0.55～1.24%, thickening agent 20～40%, surplus are solvent three chloromethane
Alkane；Preferably, dipyridamole 0.55～1.08%, thickening agent 20～30%, surplus are solvent chloroform.
In outer fluid, the mass body volume concentrations of polyurethane is 10～15%(g/ml), oxolane and N, N-dimethyl formyl
The mixing ratio of amine is 3:7～7:3；Preferably, in outer fluid, the mass body volume concentrations of polyurethane is 10～13%, oxolane and
The mixing ratio of N,N-dimethylformamide is 3:7～5:5.
Thickening agent be pharmaceutically acceptable number-average molecular weight 10000～15000 high molecular polymer.Particularly,
Thickening agent is selected from Polyethylene Glycol, polyacrylate, polystyrene, polymethacrylates, polycaprolactone, polyvinylpyrrolidine
Ketone.
The flow velocity of interior fluid is 0.1～0.2 mL/h, and the flow velocity of outer fluid is 0.7～1.0mL/h, most preferably interior fluid
Flow velocity is 0.1 mL/h, and the flow velocity of outer fluid is 0.7mL/h.
The invention has the beneficial effects as follows:
The material of the present invention, for having the artificial blood vessel of core-shell structure, its core is anti-platelet agents dipyridamole, and shell is
Polyurethane material.This material as artificial blood vessel transplanted time, can be with long-acting slow-release dipyridamole, it is suppressed that platelet is manually
Blood vessel surface stick gathering activation, enhance the blood compatibility of this artificial blood vessel, be prevented effectively from Acute thrombosis and interior
Film hypertrophy, can be effectively improved the transplanting succeed rate of artificial blood vessel.
The artificial blood vessel that present invention process prepares, has obvious core-shell structure, and homogeneity is good, ties without pearl joint etc.
Structure, safe and reliable.
Present invention process is easily operated, by changing the mould of different diameters, can conveniently prepare different tube diameters
Artificial blood vessel, meet the needs of different occasions.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of the artificial blood vessel that embodiment 1 prepares；
Fig. 2 is the transmission electron microscope picture of the nanofiber that embodiment 1 prepares；
Fig. 3 is the transmission electron microscope picture of the nanofiber that comparative example 1 prepares；
Fig. 4 is the release profiles of the artificial blood vessel for preparing of embodiment 1 dipyridamole in vitro；
Fig. 5 is the artificial blood vessel's tablets in vitro for preparing of embodiment 1 platelet adhesion reaction experimental result after 30 days；
Fig. 6 is the artificial blood vessel's tablets in vitro for preparing of comparative example 1 platelet adhesion reaction experimental result after 30 days.
Detailed description of the invention
A kind of load dipyridamole polyurethane anticoagulation tubular material, this material is core-shell structure, and internal layer is dipyridamole
Load layer, outer layer is PU body layer.
A kind of preparation technology loading dipyridamole polyurethane anticoagulation tubular material, comprises the steps:
4) configuration outer fluid: outer fluid is polyurethane solutions, and its solvent is oxolane and DMF
Mixed solution；
5) fluid in configuration: interior fluid is made up of dipyridamole, thickening agent and solvent, and solvent is chloroform；
6) in using, fluid, outer fluid carry out coaxial electrostatic spinning, are dried to obtain load dipyridamole polyurethane anticoagulation
Tubular material.
The quality proportioning of interior fluid is: dipyridamole 0.55～1.24%, thickening agent 20～40%, surplus are solvent three chloromethane
Alkane；Preferably, dipyridamole 0.55～1.08%, thickening agent 20～30%, surplus are solvent chloroform.
In outer fluid, the mass body volume concentrations of polyurethane is 10～15%(g/ml), oxolane and N, N-dimethyl formyl
The mixing ratio of amine is 3:7～7:3；Preferably, in outer fluid, the mass body volume concentrations of polyurethane is 10～13%, oxolane and
The mixing ratio of N,N-dimethylformamide is 3:7～5:5.
Thickening agent be pharmaceutically acceptable number-average molecular weight 10000～15000 high molecular polymer.Particularly,
Thickening agent is selected from Polyethylene Glycol, polyacrylate, polystyrene, polymethacrylates, polycaprolactone, polyvinylpyrrolidine
Ketone.
The flow velocity of interior fluid is 0.1～0.2 mL/h, and the flow velocity of outer fluid is 0.7～1.0mL/h, most preferably interior fluid
Flow velocity is 0.1 mL/h, and the flow velocity of outer fluid is 0.7mL/h.
Below in conjunction with embodiment, further illustrate technical scheme.
Embodiment 1:
1) configuration outer fluid: 1.5g polyurethane is dissolved in oxolane and N, N-dimethyl methyl that 10ml volume ratio is 5:5
The mixed solution of amide, is stirred overnight；
2) fluid in configuration: 30mg dipyridamole and 1.1g polycaprolactone (molecular weight 8000～10000) are dissolved in 4.4g
Chloroform, shakes 10 minutes；
3) coaxial electrostatic spinning: inner fluid speed: 0.1ml/h, outer fluid flow velocity: 0.7ml/h；Outside coaxial spinning nozzle
Pipe diameter 1.54mm, diameter of inner pipe 0.51mm；Voltage: 15～20KV, ground wire is added to blood vessel mould, keep coaxial spinning nozzle and
The distance of blood vessel mould is at 20cm, and the rotating speed of blood vessel mould is 100 revs/min；Keep electrospinning the temperature inside the box 40 DEG C, humidity 30%
～40%.Electrospinning time 2～3 hours；
4) after electrospinning terminates, artificial blood vessel is taken off from mould, 80 DEG C of dried in vacuum overnight.
Embodiment 2:
1) configuration outer fluid: 1g polyurethane is dissolved in oxolane and N, N-dimethyl formyl that 10ml volume ratio is 7:3
The mixed solution of amine, is stirred overnight；
2) fluid in configuration: 60mg dipyridamole and 1.1g polyethylene glycol 6000 are dissolved in 4.4g chloroform, shakes 10
Minute；
3) coaxial electrostatic spinning: inner fluid speed: 0.1ml/h, outer fluid flow velocity: 0.7ml/h；Outside coaxial spinning nozzle
Pipe diameter 1.54mm, diameter of inner pipe 0.51mm；Voltage: 15～20KV, ground wire is added to blood vessel mould, keep coaxial spinning nozzle and
The distance of blood vessel mould is at 20cm, and the rotating speed of blood vessel mould is 100 revs/min；Keep electrospinning the temperature inside the box 40 DEG C, humidity 30%
～40%.Electrospinning time 2～3 hours；
4) after electrospinning terminates, artificial blood vessel is taken off from mould, 80 DEG C of dried in vacuum overnight.
Embodiment 3:
1) configuration outer fluid: 1.2g polyurethane is dissolved in oxolane and N, N-dimethyl methyl that 10ml volume ratio is 3:7
The mixed solution of amide, is stirred overnight；
2) fluid in configuration: 80mg dipyridamole and 2.0g polyethylene glycol 6000 are dissolved in 4.4g chloroform, shakes 10
Minute；
3) coaxial electrostatic spinning: inner fluid speed: 0.2ml/h, outer fluid flow velocity: 1.0ml/h；Outside coaxial spinning nozzle
Pipe diameter 1.54mm, diameter of inner pipe 0.51mm；Voltage: 15～20KV, ground wire is added to blood vessel mould, keep coaxial spinning nozzle and
The distance of blood vessel mould is at 20cm, and the rotating speed of blood vessel mould is 100 revs/min；Keep electrospinning the temperature inside the box 40 DEG C, humidity 30%
～40%.Electrospinning time 2～3 hours；
4) after electrospinning terminates, artificial blood vessel is taken off from mould, 80 DEG C of dried in vacuum overnight.
Embodiment 4:
1) configuration outer fluid: 1.6g polyurethane is dissolved in oxolane and N, N-dimethyl methyl that 10ml volume ratio is 4:6
The mixed solution of amide, is stirred overnight；
2) fluid in configuration: 70mg dipyridamole and 1.5g polyethylene glycol 6000 are dissolved in 4.4g chloroform, shakes 10
Minute；
3) coaxial electrostatic spinning: inner fluid speed: 0.15ml/h, outer fluid flow velocity: 0.85ml/h；Coaxial spinning nozzle
Outer tube diameter 1.54mm, diameter of inner pipe 0.51mm；Voltage: 15～20KV, ground wire is added to blood vessel mould, keeps coaxial spinning nozzle
With the distance of blood vessel mould at 20cm, the rotating speed of blood vessel mould is 100 revs/min；Keep electrospinning the temperature inside the box 40 DEG C, humidity
30%～40%.Electrospinning time 2～3 hours；
4) after electrospinning terminates, artificial blood vessel is taken off from mould, 80 DEG C of dried in vacuum overnight.
Comparative example 1:
1) configuration outer fluid: 1.5g polyurethane is dissolved in oxolane and N, N-dimethyl methyl that 10ml volume ratio is 5:5
The mixed solution of amide, is stirred overnight；
2) fluid in configuration: 30mg dipyridamole and 1.1g polycaprolactone (molecular weight 8000～10000) are dissolved in 4.4g
Chloroform, shakes 10 minutes；
3) coaxial electrostatic spinning: inner fluid speed: 0.3ml/h, outer fluid flow velocity: 0.7ml/h；Outside coaxial spinning nozzle
Pipe diameter 1.54mm, diameter of inner pipe 0.51mm；Voltage: 15～20KV, ground wire is added to blood vessel mould, keep coaxial spinning nozzle and
The distance of blood vessel mould is at 20cm, and the rotating speed of blood vessel mould is 100 revs/min；Keep electrospinning the temperature inside the box 40 DEG C, humidity 30%
～40%.Electrospinning time 2～3 hours；
4) after electrospinning terminates, artificial blood vessel is taken off from mould, 80 DEG C of dried in vacuum overnight.
Such as Fig. 3, it is impossible to form obvious coaxial configuration.
Performance detects:
Microstructure:
The scanning electron microscope (SEM) photograph of the artificial blood vessel that embodiment 1 prepares is as it is shown in figure 1, it can be seen that artificial blood
The microstructure of pipe is homogeneous, without the structure such as pearl, joint, has the microstructure of excellence.
The transmission electron microscope picture of the artificial blood vessel that embodiment 1 prepares is as in figure 2 it is shown, it can be seen that artificial blood
Pipe has obvious core-shell structure, and dipyridamole is evenly distributed in polyurethane outer.
The mensuration of external dipyridamole release profiles:
The artificial blood vessel that embodiment 1 method prepares is cut into the thin film of 5mm 5mm, immerses 3ml0.01M HCL water-soluble
Liquid.Set the burst size of time point ultraviolet spectrophotometer mensuration dipyridamole, and make preparation～time song
Line.Matched group is the nano fibrous membrane of comparative example 1.
The release profiles of external dipyridamole as shown in Figure 4, it can be seen that the artificial blood vessel of the present invention reduces
Burst drug release, drug release is more steady.
External platelet adhesion reaction is tested:
The artificial blood vessel that embodiment 1 method prepares is cut into the thin film of 5mm 5mm, enters pH=7.4 phosphate buffer
In, to take out setting time point, be then immersed in 300 μ L rich platelet suspensions, 37 DEG C of water-baths are taken out after hatching 2 hours, use pH=
After 7.4 phosphate buffers flush three times, 2% glutaraldehyde solution fixes 4 hours, subsequently with 30%, 50%, 70%, 85%, 95% and 100%
Gradient elution using ethanol, critical drying instrument is observed with the Low-vacuum mode of environmental scanning electronic microscope after drying.Matched group is contrast
The nano fibrous membrane of example 1.
Artificial blood vessel's tablets in vitro that embodiment 1 method prepares after 30 days platelet adhesion reaction experiment ESEM scheme such as Fig. 5
Shown in.It can be seen that there is no platelet adhesion at material surface.And in matched group, have larger amount of platelet adhesion
At material surface (Fig. 6).Visible, the product of embodiment can prevent platelet adhesion well, is difficult to blood coagulation occur.
Claims (4)
1. loading a preparation technology for dipyridamole polyurethane anticoagulation tubular material, this material is core-shell structure, and internal layer is
Dipyridamole load layer, outer layer is PU body layer, and preparation technology comprises the steps:
1) configuration outer fluid: outer fluid is polyurethane solutions, and its solvent is the mixing of oxolane and DMF
Solution, in outer fluid, the mass body volume concentrations of polyurethane is 10～15%, oxolane and the volume of DMF
Mixing ratio is (3:7)～(7:3)；
2) fluid in configuration: interior fluid is made up of dipyridamole, thickening agent and solvent, and solvent is chloroform；The matter of interior fluid
Amount proportioning is: dipyridamole 0.55～1.24%, thickening agent 20～40%, surplus are solvent chloroform；Thickening agent is pharmaceutically
Acceptable number-average molecular weight 10000～15000 high molecular polymer, selected from Polyethylene Glycol, polyacrylate, polyphenyl second
Alkene, polymethacrylates, polycaprolactone, polyvinylpyrrolidone；
3) in using, fluid, outer fluid carry out coaxial electrostatic spinning, are dried to obtain load dipyridamole polyurethane anticoagulation tubulose
Material, wherein, the flow velocity of interior fluid is (0.1～0.2) mL/h, and the flow velocity of outer fluid is (0.7～1.0) mL/h.
Preparation technology the most according to claim 1, it is characterised in that: the quality proportioning of interior fluid is: dipyridamole (0.55
～1.08) %, thickening agent (20～30) %, surplus be solvent chloroform.
Preparation technology the most according to claim 1, it is characterised in that: in outer fluid, the mass body volume concentrations of polyurethane is
10～13%, the volumetric mixture ratio of oxolane and DMF is (3:7)～(5:5).
4. according to the preparation technology described in claims 1 to 3 any one, it is characterised in that: the flow velocity of interior fluid is 0.1 mL/
H, the flow velocity of outer fluid is 0.7mL/h.
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| CN105294971A (en) * | 2015-11-24 | 2016-02-03 | 无锡中科光远生物材料有限公司 | Material for artificial blood vessels and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101396337A (en) * | 2008-10-24 | 2009-04-01 | 东华大学 | Paclitaxel loaded sustained release nano fiber and preparation method and use thereof |
| CN101509153A (en) * | 2009-03-23 | 2009-08-19 | 东华大学 | Method for producing shell-core structure medicament nano-fibre with coaxial electrostatic spinning technology |
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| US7691461B1 (en) * | 2002-04-01 | 2010-04-06 | Advanced Cardiovascular Systems, Inc. | Hybrid stent and method of making |
| CN102817105A (en) * | 2012-08-24 | 2012-12-12 | 上海交通大学 | Preparation method of core-shell structured synthetic polymer-natural polymer composite fiber |
| JP6594295B2 (en) * | 2013-04-18 | 2019-10-23 | ボード・オブ・リージエンツ，ザ・ユニバーシテイ・オブ・テキサス・システム | Antibacterial catheter |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101396337A (en) * | 2008-10-24 | 2009-04-01 | 东华大学 | Paclitaxel loaded sustained release nano fiber and preparation method and use thereof |
| CN101509153A (en) * | 2009-03-23 | 2009-08-19 | 东华大学 | Method for producing shell-core structure medicament nano-fibre with coaxial electrostatic spinning technology |
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