CN109880152A - It is orientated the preparation method of connected porous bio-medical bracket and its bracket of preparation and the bracket is preparing the purposes in medical product - Google Patents
It is orientated the preparation method of connected porous bio-medical bracket and its bracket of preparation and the bracket is preparing the purposes in medical product Download PDFInfo
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- CN109880152A CN109880152A CN201910187906.1A CN201910187906A CN109880152A CN 109880152 A CN109880152 A CN 109880152A CN 201910187906 A CN201910187906 A CN 201910187906A CN 109880152 A CN109880152 A CN 109880152A
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Abstract
The present invention discloses the preparation method that a kind of polycaprolactone is orientated connected porous bio-medical bracket, the following steps are included: polycaprolactone and polyethylene oxide melt blending are obtained co-continuous blend by (1), which is obtained into the co-continuous substrate of polycaprolactone/polyethylene oxide；(2) the co-continuous substrate water extraction of polycaprolactone/polyethylene oxide obtained in step (1) is obtained into polycaprolactone porous scaffold to remove water-soluble polyethylene oxide phase；(3) polycaprolactone porous scaffold solid phase obtained in step (2) is stretched, pore morphology is made to be orientated deformation along draw direction generation, obtained polycaprolactone and be orientated connected porous bio-medical bracket.The polycaprolactone that it is prepared is orientated connected porous bio-medical bracket and apparent high connection, anisotropic porous structure is presented.Connected porous bio-medical bracket and the bracket, which are orientated, invention additionally discloses polycaprolactone is preparing the purposes in medical product.
Description
Technical field
The invention belongs to organizational project bio-medical field of stents, specifically, the present invention relates to be orientated connected porous life
The preparation method of object Medical rack and its bracket of preparation and the bracket are preparing the purposes in medical product.
Background technique
With aging of population aggravation and motion mode diversification, tissue damage become already endanger human health and
One of most common disease of normal life is mainly treated using the means of organizational project now.Tissue Engineering Study is existing
Regeneration for one of important component in bio-medical engineering technology, using suitable biological support, for organ and tissue
With reparation, recombination and significant (Czernuszka J T, the et al.European cells&materials of regeneration
2003,5(5),29；O'Brien F J,et al.Materials Today 2011,14(3),88).At present it is believed that reason
The bracket thought, which needs to grow for cell, provides suitable environment, not only acts as basic supporting role, and be nutriment
It draws the discharge with metabolic waste and channel is provided, meanwhile, bracket degradability is assigned, makes it in the mistake for promoting cambium to be formed
Degradation is gradually absorbed by organisms in journey.Polymerize Biodegradable three-dimensional porous rack by high-specific surface area, good pore morphology, easily
The advantage of processing, it is considered to be ideal bracket can dramatically promote adherency, proliferation and the differentiation of cell.It has can
Absorbability avoid second operation to patient bring pain (Lv W, et al.Biomaterials 2011,32 (29),
6900；Bastmeyer M,et al.Small 2012,8(3),336).
The method that existing production prepares porous polymer scaffold specifically includes that fibre cementing method (Fiber Bonding), molten
Agent casting/particle leaching technique (Solvent Casting/Particulate Leaching), freeze-drying (Freeze
Drying Method), gas foaming method (Gas Foaming Method), Thermal inactive technology (Thermally
Induced Phase Separation Technique), electrostatic spinning technique (Electrospinning Technique) with
And (Ma PX, the et al.Materials Today such as rapid shaping technique (Rapid Prototyping Technique)
2004,7(5),30；Clyne AM,et al.Journal of Heat Transfer 2011,133(3),034001).So
And be mostly isotropism pore structure using bracket made from above-mentioned processing method, although damaged tissues can be carried out regeneration and
It repairs, but generally requires long period (Liu CS, et al.Chem.Rev.2017,117,4376).Most of tissues of human body
(such as bone, tendon, nerve, blood vessel) is all anisotropic structure.In face of the regeneration and reparation of these tissues, building has orientation
The bracket of structure can inducing cell oriented growth ultimately form anisotropic cambium, to obtain faster and better group
Regeneration effect is knitted to be of great significance (K.Y.Suh, et al.Adv.Drug Deliv.Rev.2013,65,536；
E.S.Thian,et al.Sci.Adv.2018,4,4537)。
Currently, ice template method has been used for the porous support that preparation has 3 D tropism arrangement micro-tubular structure.The bracket is logical
Crossing orientation temperature gradient fields makes ice crystal oriented growth, is made after freeze-drying removal solvent phase.But this method preparation is porous
Between the micro- tubulus of bracket only by micropore connect, connectivity is poor and pore structure is imperfect, cause mechanical property it is poor (<
1MPa), while in preparation process introducing organic solvent also will affect biocompatibility (the Yang DZ, et of bracket itself
al.Materials Letters 2018,233,78).Therefore, it is current for how preparing the 3 D tropism porous support of high connection
Tissue engineering bracket field urgent problem to be solved.
Summary of the invention
The purpose of the present invention is to provide the preparation method that a kind of polycaprolactone is orientated connected porous bio-medical bracket,
The polycaprolactone of preparation is orientated connected porous bio-medical bracket and apparent high connection, anisotropic porous structure is presented, should
Polycaprolactone be orientated connected porous bio-medical bracket can be used in preparing medical product anisotropy tissue (such as bone, tendon,
Nerve, blood vessel etc.) regeneration and reparation.
The technical solution of the present invention for achieving the above object is as follows:
A kind of polycaprolactone is orientated the preparation method of connected porous bio-medical bracket, comprising the following steps:
(1) the co-continuous substrate preparation of polycaprolactone/polyethylene oxide: polycaprolactone and polyethylene oxide melt blending are obtained
To co-continuous blend, which is obtained into the co-continuous substrate of polycaprolactone/polyethylene oxide；
(2) prepared by polycaprolactone porous scaffold: polycaprolactone/polyethylene oxide obtained in the step (1) is connected altogether
Continuous substrate water extraction obtains polycaprolactone porous scaffold to remove water-soluble polyethylene oxide phase；
(3) polycaprolactone orientation intercommunicating pore bracket preparation: polycaprolactone porous scaffold obtained in the step (2) is solid
It mutually stretches, pore morphology is made to be orientated deformation along draw direction generation, obtain the polycaprolactone and be orientated connected porous bio-medical branch
Frame.
In the step (1), using mixer melting mixing polycaprolactone and polyethylene oxide, make the blend shape of the two
At co-cable transmission.
In the step (1), in the co-continuous blend polycaprolactone and the mass ratio of polyethylene oxide be 4:6~
6:4。
In the step (1), before melt blending, it is dry that vacuum is carried out to the polycaprolactone and the polyethylene oxide
It is dry.
In the step (1), compression moulding temperature is 70~150 DEG C.
In the step (2), the water is deionized water or distilled water.
In the step (3), the temperature that solid phase stretches is 30~60 DEG C, and the strain that solid phase stretches is 75%~400%.
It is a further object to provide a kind of polycaprolactones to be orientated connected porous bio-medical bracket, uses
It states preparation method to be made, apparent anisotropy porous structure is presented.
It is also another object of the present invention to provide the polycaprolactones prepared by above-mentioned preparation method to be orientated connected porous biology
Medical rack can be used for the regeneration and reparation of anisotropy tissue preparing the purposes in medical product, the medical product.
The beneficial effects of the present invention are:
Polycaprolactone proposed by the invention is orientated the technology of preparation method of connected porous bio-medical bracket, relative to existing
The technical method for thering is anisotropy porous support to prepare, as ice template method realizes hole knot under the premise of guaranteeing high connected ratio
Structure it is height-oriented.
(1) present invention is combined by co-cable transmission building, water (deionized water, distilled water etc.) extraction and solid phase stretching
Polycaprolactone made from mode is orientated connected porous bio-medical bracket, which is orientated connected porous bio-medical bracket
Apparent anisotropy porous structure is presented, can be used for anisotropy tissue (such as bone, tendon, nerve, blood vessel) regeneration and
It repairs；
(2) polycaprolactone produced by the present invention, which is orientated connected porous bio-medical bracket, has good connectivity, favorably
In the uniform inoculation and distribution of cell；
(3) organic solvent is not used in preparation method of the invention, does not influence the biocompatibility of bracket itself, meanwhile, work
Skill is simple, environmentally protective, is easy to industrial production.
Preparation process of the present invention is simple, has a good application prospect.
Detailed description of the invention
Fig. 1 is the scanning electron microscope diagram of comparative example 2.
Fig. 2-5, which is corresponding in turn to, to be quenched the scanning electron microscope diagram of section for embodiment 14-17 along draw direction.
Fig. 6 is the aperture size statistical result schematic diagram of embodiment 14-17 and comparative example 2.
Fig. 7 is the connected ratio test result schematic diagram of embodiment 14-17 and comparative example 2.
Fig. 8 is mechanical property (compression) test result schematic diagram of embodiment 14-17 and comparative example 2.
Specific embodiment
Examples given below is to specific descriptions of the invention, it is necessary to which indicated herein is that following embodiment is served only for
The present invention is further illustrated, should not be understood as limiting the scope of the invention.
Embodiment 1-33
Polycaprolactone is prepared as follows is orientated connected porous bio-medical bracket:
(1) the co-continuous substrate preparation of polycaprolactone/polyethylene oxide: weighing polycaprolactone and polyethylene oxide raw material, will
After the two vacuum drying, melting mixing is carried out using mixer and obtains co-continuous blend, by co-continuous blend compression moulding
Obtain the co-continuous substrate of polycaprolactone/polyethylene oxide；The mass ratio of polycaprolactone and polyethylene oxide in co-continuous blend
Example and compression moulding temperature are shown in Table 1；
(2) prepared by polycaprolactone porous scaffold: by the co-continuous base of polycaprolactone/polyethylene oxide obtained in step (1)
Material water (deionized water, distilled water etc.) is extracted to remove water-soluble polyethylene oxide phase, obtains polycaprolactone porous scaffold；
(3) polycaprolactone orientation intercommunicating pore bracket preparation: polycaprolactone porous scaffold solid phase obtained in step (2) is drawn
It stretches, pore morphology is made to be orientated deformation along draw direction generation, obtain polycaprolactone and be orientated connected porous bio-medical bracket；Wherein,
Solid phase draft temperature, solid phase elongation strain are shown in Table 1.
Comparative example 1-3
Isotropic polycaprolactone porous scaffold is prepared as follows:
(1) the co-continuous substrate preparation of polycaprolactone/polyethylene oxide: weighing polycaprolactone and polyethylene oxide raw material, will
After the two vacuum drying, melting mixing is carried out using mixer and obtains co-continuous blend, by co-continuous blend compression moulding
Obtain the co-continuous substrate of polycaprolactone/polyethylene oxide；The mass ratio of polycaprolactone and polyethylene oxide in co-continuous blend
Example and compression moulding temperature are shown in Table 1；
(2) prepared by polycaprolactone porous scaffold: by the co-continuous base of polycaprolactone/polyethylene oxide obtained in step (1)
Material is extracted with water (deionized water, distilled water etc.) and removes water-soluble polyethylene oxide phase, and obtain isotropism pore structure gathers oneself
Lactone porous support.
The formula and preparation process condition of table 1 Examples 1 to 33 and comparative example 1~3
Average pore size, draw ratio, connected ratio and the mechanical property of table 2 Examples 1 to 33 and comparative example 1~3
The present invention also describes a kind of connected porous bio-medical bracket of polycaprolactone orientation, uses above-mentioned preparation method system
, apparent anisotropy porous structure is presented.
The present invention describes the connected porous bio-medical bracket of the polycaprolactone prepared by above-mentioned preparation method orientation again and is making
Purposes in standby medical product, the medical product are used for the regeneration and reparation of anisotropy tissue.
From table 1,2 data:
(1) when compression moulding temperature, one timing of solid phase elongation strain, with the quality of polycaprolactone in co-continuous blend
The increase of percentage, the aperture size which is orientated connected porous bio-medical bracket are gradually reduced, mechanical property by
Cumulative plus (such as embodiment 1,10,22；Embodiment 4,14,26；Embodiment 7,18,30 etc.)；
(2) when the mass percent of polycaprolactone in co-continuous blend, one timing of solid phase elongation strain, with being pressed into
The promotion of type temperature, the aperture size which is orientated connected porous bio-medical bracket are gradually increased, mechanical property by
Gradually reduce (such as embodiment 1,4,7；Embodiment 10,14,18；Embodiment 22,26,30 etc.)；
(3) when the mass percent of polycaprolactone, one timing of compression moulding temperature in co-continuous blend, as solid phase is drawn
The increase of stretching strain, the aperture size which is orientated connected porous bio-medical bracket are gradually increased, mechanical property by
Cumulative plus (such as comparative example 1, embodiment 1,2,3；Comparative example 2, embodiment 14,15,16,17；Comparative example 3, embodiment 30,31,
32,33 etc.).
Embodiment 14-17 and comparative example 2 are further illustrated in conjunction with attached drawing hereinafter.As for except embodiment 14-17 and comparison
The relevant informations such as average pore size, draw ratio, connected ratio and the mechanical property of other embodiments and comparative example except example 2,
It has been expressed in table 2, it is corresponding identical as information expressed by Fig. 1-8, for simplicity, omits remove embodiment 14-17 herein
With the relevant drawings of other embodiments and comparative example except comparative example 2.
It is orientated the pore morphology of connected porous bio-medical bracket for characterization polycaprolactone, utilizes Flied emission scanning electron microscopy
Mirror (FE-SEM) observes embodiment 14-17 and comparative example 2 along the section of quenching of draw direction.Comparative example 2 shown in FIG. 1 is
Conventional polycaprolactone porous scaffold has isotropism pore structure, and aperture is more uniform, and is interconnected between hole.Shown in Fig. 2-5
Embodiment 14-17 be that the polycaprolactone of different stretch prepared by preparation method of the present invention strain is orientated connected porous bio-medical
Bracket, the high connectivity which is orientated connected porous bio-medical bracket still retains, and pore morphology is along draw direction
Different degrees of deformation occurs, shows apparent anisotropy porous structure.
Using the aperture size of image analysis software Statistics Implementation example 14-17 and comparative example 2, result is as shown in Figure 6.It is right
It is isotropic polycaprolactone porous scaffold shown in ratio 2, average pore size is about 12 μm, and shown in embodiment 14-17
Polycaprolactone prepared by preparation method of the present invention is orientated connected porous bio-medical bracket, aperture along long axis and short-axis direction with
The increase of elongation strain and increase, major diameter maximum up to 107 μm, minor axis maximum up to 22 μm, polycaprolactone orientation it is connected porous
The aperture of bio-medical bracket is all larger than polycaprolactone isotropism porous support；And as draw ratio increases, it is orientated the length in hole
For diameter than also constantly increasing, orientation form is more obvious.
To evaluate the connectivity that polycaprolactone prepared by preparation method of the present invention is orientated connected porous bio-medical bracket, benefit
The connected ratio of embodiment 14-17 and comparative example 2 are calculated with formula 1 hereinafter, result is as shown in fig. 7, all brackets are equal
Connected ratio close to 100%.
Formula 1:
In formula 1, mInitial p EOIndicate the quality of polyethylene oxide under original state, mFinal PEOIt indicates to remain after extracting by water
Polyethylene oxide quality.
To evaluate the mechanical property that polycaprolactone prepared by preparation method of the present invention is orientated connected porous bio-medical bracket,
By electronic universal cupping machine to embodiment 14-17 perpendicular to mechanics (compression) performance of draw direction and comparative example 2 into
Row test, result are as shown in Figure 8.Polycaprolactone shown in embodiment 14-17 is orientated the pressure of connected porous bio-medical bracket
Contracting intensity reaches as high as 17MPa, and compression modulus reaches as high as 19MPa, and polycaprolactone isotropism shown in comparative example 2 is porous
The compressive strength of bracket is only 10MPa, and compression modulus is only 12MPa, and comparison is it is found that the polycaprolactone is orientated connected porous biology
The compression performance of Medical rack is better than polycaprolactone isotropism porous support.
The present invention passes through melt blending using water soluble pore formers polyethylene oxide and the mutual exclusive principle of polycaprolactone
Obtain polycaprolactone/polyethylene oxide co-continuous blend；Water-soluble polycyclic oxygen second is extracted with water (deionized water, distilled water etc.)
After alkane phase, the polycaprolactone porous scaffold that is interconnected；Further by solid phase stretching induction intercommunicating pore along stretching side
It obtains polycaprolactone to occurring be orientated to deform and is orientated connected porous bio-medical bracket, form apparent anisotropic structure.?
On the basis of keeping porous support high connectivity, realize that three-dimensional polycaprolactone is orientated the preparation of connected porous bio-medical bracket；
Any organic solvent is not used in whole preparation process, and technique is easy to grasp, environmentally protective, convenient for large-scale production；Meanwhile it making
The polycaprolactone obtained is orientated connected porous bio-medical bracket and can apply to promote cell migration and accelerate anisotropy tissue
The regeneration and reparation of (such as bone, tendon, nerve, blood vessel) damage.
It should be noted that each particular technique feature described in above-mentioned specific embodiment, in reconcilable feelings
Under condition, it can be combined by any suitable mode.In order to avoid unnecessary repetition, the present invention is to various possible groups
Conjunction mode is not described.
Above with reference to embodiment to the present invention have been described in detail, be it is illustrative rather than restrictive, do not taking off
It is within the scope of the present invention from the change and modification under present general inventive concept.
Claims (9)
1. the preparation method that a kind of polycaprolactone is orientated connected porous bio-medical bracket, which comprises the following steps:
(1) the co-continuous substrate preparation of polycaprolactone/polyethylene oxide: polycaprolactone and polyethylene oxide melt blending are total to
The co-continuous blend compression moulding is obtained the co-continuous substrate of polycaprolactone/polyethylene oxide by continuous blend；
(2) prepared by polycaprolactone porous scaffold: by the co-continuous base of polycaprolactone/polyethylene oxide obtained in the step (1)
Material water is extracted to remove water-soluble polyethylene oxide phase, obtains polycaprolactone porous scaffold；
(3) polycaprolactone orientation intercommunicating pore bracket preparation: polycaprolactone porous scaffold solid phase obtained in the step (2) is drawn
It stretches, pore morphology is made to be orientated deformation along draw direction generation, obtain the polycaprolactone and be orientated connected porous bio-medical bracket.
2. preparation method according to claim 1, which is characterized in that in the step (1), using mixer melting mixing
Polycaprolactone and polyethylene oxide make the blend of the two form co-cable transmission.
3. preparation method according to claim 1, which is characterized in that in the step (1), in the co-continuous blend
Polycaprolactone and the mass ratio of polyethylene oxide are 4:6~6:4.
4. preparation method according to claim 1, which is characterized in that right before melt blending in the step (1)
The polycaprolactone and the polyethylene oxide are dried in vacuo.
5. preparation method according to claim 1, which is characterized in that in the step (1), compression moulding temperature be 70~
150℃。
6. preparation method according to claim 1, which is characterized in that in the step (2), the water be deionized water or
Distilled water.
7. preparation method according to claim 1, which is characterized in that in the step (3), the temperature that solid phase stretches is 30
~60 DEG C, the strain that solid phase stretches is 75%~400%.
8. a kind of connected porous biology doctor of polycaprolactone orientation of preparation method preparation according to claim 1-7
Use bracket.
9. being orientated connected porous bio-medical by polycaprolactone prepared by preparation method according to claim 1-7
Bracket is preparing the purposes in medical product, regeneration and reparation of the medical product for anisotropy tissue.
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| CN110917410A (en) * | 2019-11-14 | 2020-03-27 | 浙江大学 | Cardiovascular stent coating based on double-layer heterogeneous structure and preparation method thereof |
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Cited By (2)
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