CN106110398A - There is the preparation method of surface micro-structure degradable shape memory high molecule intravascular stent - Google Patents
There is the preparation method of surface micro-structure degradable shape memory high molecule intravascular stent Download PDFInfo
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- CN106110398A CN106110398A CN201610529586.XA CN201610529586A CN106110398A CN 106110398 A CN106110398 A CN 106110398A CN 201610529586 A CN201610529586 A CN 201610529586A CN 106110398 A CN106110398 A CN 106110398A
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/14—Macromolecular materials
- A61L27/18—Macromolecular materials obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
- A61L27/507—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials for artificial blood vessels
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
- A61L27/58—Materials at least partially resorbable by the body
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2400/00—Materials characterised by their function or physical properties
- A61L2400/16—Materials with shape-memory or superelastic properties
Abstract
The invention discloses a kind of preparation method with surface micro-structure degradable shape memory high molecule intravascular stent, select degradable shape memory high molecule material as the base material of intravascular stent；Utilize optical etching technology to prepare surface and there is the silicon chip template of micrographics；Then the shape memory macromeric materials of molten condition is cast in template, under certain environmental stimuli, pre-polymerization is monomer crosslinked, and then the surface obtaining having shape memory effect has the polymer sheet of micrographics, finally micro-for this polymer patterned substrates is prepared as tubulose by rolled fashion, it is thus achieved that target product has the shape memory high molecule intravascular stent inducing bionical micrographics surface.Present invention employs degradable shape memory high molecule material and controlled the growth behavior of cell, and then bionical formation blood vessel structure by the material of patterning, promote the generation of new vessels.
Description
Technical field
The present invention relates to biomaterial and functional polymer, particularly by surface micro-structure regulating cell growth function and shape
The intravascular tissue engineering support that the shape memory function of shape memory polymer combines.
Background technology
The degradable shape-memory materials such as polycaprolactone (PCL), polyurethane (PU), polylactic acid (PLA) are because it has
Preferably shape-memory properties, processing characteristics, biocompatibility and degradable character, it has more answering at biomedical sector
With, such as tissue engineering bracket and controlled release drug carrier materials etc..At present, the research of crosslinking shape-memory polymer belongs to application
One of study hotspot of Polymer Synthesizing manufacture field, compared with the line polymer of same molecular amount, the solution of its body sticks
Spend relatively low, and there is preferable dynamic mechanical, higher activity and relatively low melting viscosity, thus have preferably
Processing characteristics.Shape-memory polymer, as the intellectual material that a class is novel, although increasingly closed in bio-medical
Note, but its applied research in organizational project is the most few.But the performance of its dynamically changeable be more suitable in analogue body dynamic
State environment, is but important performances not possessing of other used in tissue engineering materials.
The surface topology of biomaterial can to the propagation of cell, adhere to, sprawl, be orientated, migrate, gene expression, egg
A series of biological behaviours such as white synthesis produce impact.Cell behavior is studied, because having certain bionical feature with micrographics
And cause and pay close attention to widely.A lot, so to the report of cell regulate and control effect about the static micrographics substrate of research at present
And organism is practically in the dynamic environment being continually changing, the cell in body is similarly in the DYNAMIC COMPLEX that is continually changing
In microenvironment, therefore from the point of view of bionics angle, the experimental result that cell regulate and control effect is obtained by the static micrographics substrate of research
Organism inner cell behavior cannot be reflected exactly.
Intravascular stent is the tubular-type support for keeping vascular patency, major part by rustless steel, marmem with
And other alloy makes.Put them in the diseased region of blood vessel, utilize the method for self expandable or balloon expandable to launch.By
Higher in the hardness of metal rack, processability and handling poor, thus limit its application.And can go out the most after the implants
The existing defect such as platelet aggregation, angiemphraxis, patient can only Long-term Oral or injection anticoagulant.
Intravascular tissue engineering support refer to preparation can the conduit of bionical autologous vein structure, have substantial amounts of research at present
Concentrate on the design of intravascular tissue engineering support.Good intravascular tissue engineering support can carry a certain amount of vascular cell, tool
There is the structure of native blood vessels, and the function of normal blood vessels can be exercised.
At normal Ink vessel transfusing, the smooth muscle cell circularizing arrangement plays the effect maintaining blood vessel mechanical strength, along
The endotheliocyte of blood flow direction arrangement has critically important effect in terms of bearing blood stream pressure.Controlled by the material of patterning
The growth behavior of cell processed, and then form blood vessel structure, this is a new think of of intravascular tissue engineering support Design in the recent period
Road.
Summary of the invention
In view of the deficiencies in the prior art, it is an object of the invention to provide the degradable shape memory of a kind of surface micro-patterning
The preparation method of macromolecule intravascular stent, is allowed to for being effectively facilitated new vascular generation, exercises the function of normal blood vessels.
It is an object of the invention to by following means realization: it is high that one has surface micro-structure degradable shape memory
The preparation method of molecule intravascular stent, selects degradable shape memory high molecule material as the base material of intravascular stent；
Utilize optical etching technology to prepare surface and there is the silicon chip template of micrographics；Then by the shape memory macromonomer of molten condition
Material is cast in template, and under certain environmental stimuli, pre-polymerization is monomer crosslinked, and then obtains the table with shape memory effect
Mask has the polymer sheet of micrographics, finally by rolled fashion, micro-for this polymer patterned substrates is prepared as tubulose, it is thus achieved that mesh
Mark product has the shape memory high molecule intravascular stent inducing bionical micrographics surface, and target product passes through in using environment
The growth behavior of the control of material cell of patterning, and then form blood vessel structure
Further, described degradable shape memory high molecule be polycaprolactone, polyurethane, polylactic acid and they
Derivant.
Further, the preparation of described micrographics template can use photoengraving, Soft lithograph, hot-die impressing, self assembly.
Further, described micrographics is the dot matrix such as triangular hill, triangular depression, circular protrusions and circular pit
Type, straight groove, arcuate furrow, craspedodrome groove and the compound pattern of arcuate furrow.
During use, making this support deform under being not less than human body temperature (such as 45 DEG C), 0 DEG C of cryofixation, by micro-
After wound implants, under the conditions of uniform temperature (40 DEG C) can be applied under body temperature environment or in vitro, surface compression is made to deform
Support gradually return back to the form initially with bionical micro structure.In this Recovery Process, this support can effectively capture
Endothelium, smooth muscle and endothelial progenitor cells etc., and gradually form new vascular tissue, exercise the function of normal blood vessels.
The present invention imitates the structure of normal blood vessels, have employed degradable shape memory high molecule material, devise table
Face micro structure degradable shape memory high molecule intravascular stent, is controlled the growth behavior of cell, enters by the material of patterning
And bionical formation blood vessel structure, promote the generation of new vessels.The introducing of shape-memory properties, it is possible to achieve the Wicresoft of operation plants
Enter, and in shape memory Recovery Process, also function to the effect of certain dynamically regulation, closer to the physiological environment of human body.
Detailed description of the invention
In addition to special instruction, listed related chemistry reagent is medical grade in this document.
The preparation of the degradable shape memory high molecule intravascular stent of surface of the present invention micro-patterning is divided into following steps:
The first step: prepared by degradable shape memory high molecule
4 arm Polyethylene Glycol (4arm PEG) and caprolactone (ε-Cl) are mixed, by a certain percentage at appropriate catalyst
Under the effect of SnCl2, react 6 hours under 140 DEG C of vacuum environments, then dissolve with dichloromethane, concentrated by rotary evaporation, then use nothing
Water ether sedimentation separates out and carries out vacuum drying and obtains white powder 4arm PEG-PCL.Again with dichloromethane as solvent, will
4armPEG-PCL and acryloyl chloride, triethylamine are by the ratio hybrid reaction 6 hours of 1:1:1, and rotation is evaporated off partial solvent, addition
Ice ethanol makes product Precipitation, obtains 4arm PEG-PCL-AC macromonomer, is dried under vacuum to constant weight.
Second step: there is the preparation of micro structure intravascular stent
First with optical etching technology, it is compound with what radial straight groove formed that prepared surface has donut groove
The silicon chip template of figure.Under the conditions of lucifuge, with dichloromethane as solvent, by 4arm PEG-PCL macromonomer with appropriate
Light trigger TPO mixes, and treats that solvent volatilize, put into the baking oven of 65 DEG C heat make sample to molten condition, and by molten condition
Polymer be cast in the silicon chip template with micrographics of the surface and sprawl uniformly.Give ultra-vioket radiation again 1 hour, make high score
Sub-material is full cross-linked.Surface is peeled off from silicon chip template surface with the c-4armPEG-PCL of micrographics, its cutting is grown up
Square sheet, is heated to high temperature 45 DEG C, and is wound on tubular die, be curled into tubulose.After finally fixing at 0 DEG C, thus
To the intravascular stent with micro structure.
It is discussed further can be expressed as examples below.
Embodiment 1
The preparation of the intravascular stent that the present invention has the shape memory function of bionical micro structure is divided into following steps:
The first step: the preparation of shape memory high molecule
Weigh appropriate 4arm PEG, ε-Cl, SnCl2 mixing respectively and add in single neck bottle, wherein 4arm PEG, ε-Cl's
Mass ratio is 1:2, room temperature evacuation 5h under conditions of magnetic agitation, then reacts 6h at 140 DEG C；Treat that it is cooled to room
Temperature, adds appropriate dichloromethane and dissolves, and pours substantial amounts of ice ethanol stirring Precipitation into, and then sucking filtration removes anhydrous second
Alcohol also carries out being dried under vacuum to constant weight and obtains 4arm PEG-PCL.Appropriate dichloromethane is added in single neck bottle, 4arm PEG-
PCL is sequentially added in the ratio of 1:1:1 with acryloyl chloride, triethylamine, and mix and blend reacts 6 hours, and rotation is evaporated off partial solvent,
Add ice ethanol and make product Precipitation, obtain 4arm PEG-PCL-AC macromonomer, be dried under vacuum to constant weight.
Second step: there is the preparation of micro structure intravascular stent
Obtaining width and ring-shaped groove that spacing is 10 μm by optical etching technology design, width is 15 μm, and the degree of depth is 5
The donut groove of μm, and the silicon chip of the compound pattern of radial straight groove and donut groove composition is as mould
Plate.Appropriate 4armPEG-PCL-AC macromonomer and light trigger TPO are placed in the 25ml beaker with aluminium foil encapsulating, add
Enter dichloromethane stirring and dissolving, mixed solution is poured in culture dish.After solvent volatilization completely, culture dish is put into 65 DEG C
In baking oven, heating makes sample be in molten condition, and the polymer of molten condition is cast in the surface silicon chip template with micrographics
On, and make it sprawl uniformly with Glass rod stirring.Polymer is placed in uviol lamp (100W, 400 μ W/ that wavelength is 360nm again
Cm2), under, irradiate and within 1 hour, make it carry out cross-linking the shape memory high molecule material obtaining surface with micrographics.Finally by surface
C-4arm PEG-PCL with micrographics peels off from silicon chip template surface, is cut into rectangular sheet, and is wound on one
On the tubular die of a diameter of 2mm, thus obtain the tubular bracket of 8mm × 2mm × 0.2mm (length × diameter × thickness) (in tube chamber
Wall is the picture surface after compression), thus obtain the intravascular stent with micro structure.
Embodiment 2
This example is substantially the same manner as Example 1, except that: when the first step prepares shape-memory polymer, according to matter
Amount weighs 4arm PEG and ε-Cl than for 1:2 and reacts.
Embodiment 3
This example is substantially the same manner as Example 1, except that: when the first step prepares shape-memory polymer, select poly-
Urethane is as shape-memory material.
Embodiment 4
This example is substantially the same manner as Example 1, except that: when the first step prepares shape-memory polymer, select poly-
Lactic acid is as shape-memory material.
Embodiment 5
This example is substantially the same manner as Example 1, except that: the figure that the silicon chip template surface of optical etching technology has is
Diameter and be highly the dot matrix of 5 μm circular protrusions.
Embodiment 6
This example is substantially the same manner as Example 1, except that: the figure that the silicon chip template surface of optical etching technology has is
The length of side is the dot matrix of the triangular hill of 3.5 μm.
The obtained target product of the inventive method is used to be capable of the propagation of hemocyte and functionalization spontaneously selectivity
Stick to the diverse location on target product substrate surface, form the micrographics substrate surface with bionical meaning, there is promotion
The performance that neovascularity generates thereon.
Claims (5)
1. there is a preparation method for surface micro-structure degradable shape memory high molecule intravascular stent, select degradable shape
Shape memory macromolecular material is as the base material of intravascular stent；Utilize optical etching technology to prepare surface and there is the silicon chip of micrographics
Template；Then the shape memory macromeric materials of molten condition is cast in template, pre-under certain environmental stimuli
Poly-monomer crosslinked, and then the surface obtaining having shape memory effect has the polymer sheet of micrographics, finally by this polymer
Micro-patterned substrates is prepared as tubulose by rolled fashion, it is thus achieved that target product has the shape memory inducing bionical micrographics surface
Macromolecule intravascular stent, target product passes through the growth behavior of the control of material cell of patterning, and then shape in using environment
Become blood vessel structure.
The most according to claim 1, there is the preparation side of surface micro-structure degradable shape memory high molecule intravascular stent
Method, it is characterised in that described degradable shape memory high molecule be polycaprolactone, polyurethane, polylactic acid and they
Derivant.
The most according to claim 1, there is the preparation side of surface micro-structure degradable shape memory high molecule intravascular stent
Method, it is characterised in that the preparation of described micrographics template can use photoengraving, Soft lithograph, hot-die impressing, self assembly.
The most according to claim 1, there is the preparation side of surface micro-structure degradable shape memory high molecule intravascular stent
Method, it is characterised in that described micrographics be the dot matrix types such as triangular hill, triangular depression, circular protrusions and circular pit,
Straight groove, arcuate furrow, craspedodrome groove and the compound pattern of arcuate furrow.
The most according to claim 1, there is the preparation side of surface micro-structure degradable shape memory high molecule intravascular stent
Method, it is characterised in that use following concrete steps:
1): prepared by degradable shape memory high molecule
4 arm Polyethylene Glycol and caprolactone are mixed by a certain percentage, under the effect of catalyst SnCl2, under 140 DEG C of vacuum environments
React 6 hours, then dissolve with dichloromethane, concentrated by rotary evaporation, then with absolute ether Precipitation and be vacuum dried
Obtain white powder 4arm PEG-PCL；Again with dichloromethane as solvent, 4arm PEG-PCL is pressed with acryloyl chloride, triethylamine
The ratio hybrid reaction of 1:1:1 6 hours, rotation is evaporated off partial solvent, adds ice ethanol and makes product Precipitation, obtains 4arm
PEG-PCL-AC macromonomer, is dried under vacuum to constant weight；Stand-by；
2): the preparation of micro structure intravascular stent
First with optical etching technology, prepared surface has the compound pattern of donut groove and radial straight groove composition
Silicon chip template；Under the conditions of lucifuge, with dichloromethane as solvent, by 1) gained 4arm PEG-PCL macromonomer is with appropriate
Light trigger TPO mixing, treat that solvent volatilize, put into the baking oven of 65 DEG C heat make sample to molten condition, and by molten
The polymer of state is cast in the silicon chip template with micrographics of the surface and sprawls uniformly, then gives ultra-vioket radiation 1 hour, high score
Sub-material is full cross-linked to be prepared surface with the c-4arm PEG-PCL of micrographics；Then by macromolecular material from silicon chip template
Sur-face peeling, is cut into rectangular sheet, is heated to high temperature 45 DEG C, and is wound on tubular die, is curled into tubulose；Finally
After fixing at 0 DEG C, thus obtain the intravascular stent with micro structure.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106913914A (en) * | 2017-04-04 | 2017-07-04 | 西南交通大学 | A kind of preparation method for visualizing shape memory high molecule intravascular stent |
| CN107236261A (en) * | 2017-05-24 | 2017-10-10 | 淮阴工学院 | Can be according to the preparation method of the shape-memory polymer film of the spontaneous regulation translucency of indoor temperature height |
| CN109096710A (en) * | 2018-06-26 | 2018-12-28 | 深圳先进技术研究院 | A kind of shape memory microstructure film and its preparation method and application |
| CN109692341A (en) * | 2017-10-24 | 2019-04-30 | 吕路可 | The guide-lighting biological fiber component with organizational integration |
| CN109971028A (en) * | 2019-03-18 | 2019-07-05 | 温州优巴信息技术有限公司 | A kind of shape-memory polymer base enclosure glycan nonwoven cloth material and preparation method thereof with micro- pattern |
| WO2020006882A1 (en) * | 2018-07-04 | 2020-01-09 | 凯斯蒂南京医疗器械有限公司 | Degradable spiral coated stent with controllable gradient, preparation method therefor and use thereof |
| CN111590914A (en) * | 2020-05-29 | 2020-08-28 | 临沂大学 | 4D deformed reticulated hollowed degradable intravascular stent with concave-convex structures on inner and outer surfaces and preparation and use methods thereof |
| CN111839810A (en) * | 2020-07-27 | 2020-10-30 | 北京理工大学 | Manufacturing method of intravascular stent |
| CN112625292A (en) * | 2020-12-17 | 2021-04-09 | 青岛博远高分子材料研究院有限公司 | Preparation method of degradable shape memory polymer medical splint |
| CN112812345A (en) * | 2021-02-10 | 2021-05-18 | 浙江大学 | Medical programmable anatomical form piece and preparation method thereof |
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| WO2020006882A1 (en) * | 2018-07-04 | 2020-01-09 | 凯斯蒂南京医疗器械有限公司 | Degradable spiral coated stent with controllable gradient, preparation method therefor and use thereof |
| CN109971028A (en) * | 2019-03-18 | 2019-07-05 | 温州优巴信息技术有限公司 | A kind of shape-memory polymer base enclosure glycan nonwoven cloth material and preparation method thereof with micro- pattern |
| CN111590914A (en) * | 2020-05-29 | 2020-08-28 | 临沂大学 | 4D deformed reticulated hollowed degradable intravascular stent with concave-convex structures on inner and outer surfaces and preparation and use methods thereof |
| CN111839810A (en) * | 2020-07-27 | 2020-10-30 | 北京理工大学 | Manufacturing method of intravascular stent |
| CN111839810B (en) * | 2020-07-27 | 2021-07-06 | 北京理工大学 | Manufacturing method of intravascular stent |
| CN112625292A (en) * | 2020-12-17 | 2021-04-09 | 青岛博远高分子材料研究院有限公司 | Preparation method of degradable shape memory polymer medical splint |
| CN112812345A (en) * | 2021-02-10 | 2021-05-18 | 浙江大学 | Medical programmable anatomical form piece and preparation method thereof |
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| CN106110398B (en) | 2019-04-16 |
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