CN108744051A - A kind of composite fibre and its preparation method and application for artificial anterior cruciate ligament - Google Patents
A kind of composite fibre and its preparation method and application for artificial anterior cruciate ligament Download PDFInfo
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- CN108744051A CN108744051A CN201810507241.3A CN201810507241A CN108744051A CN 108744051 A CN108744051 A CN 108744051A CN 201810507241 A CN201810507241 A CN 201810507241A CN 108744051 A CN108744051 A CN 108744051A
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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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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/14—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyester as constituent
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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
- A61L2430/00—Materials or treatment for tissue regeneration
- A61L2430/10—Materials or treatment for tissue regeneration for reconstruction of tendons or ligaments
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Abstract
The invention belongs to technical field of biological material, disclose a kind of composite fibre and its preparation method and application for artificial anterior cruciate ligament.The present invention carries out the own ester of polyhydroxybutyrate with polyglycolic acid compound, the composite fibre obtained combines the advantages of the two, the performances such as the good biocompatibility of the existing own ester of polyhydroxybutyrate, and the performances such as the excellent physical mechanical performance for thering is polyglycolic acid to assign and cellular affinity.In addition, based on collaboration enhancing mechanism, composite fibre has performance more superior than one-component.When composite fibre for the characteristics of when preparing artificial anterior cruciate ligament, NEW TYPE OF COMPOSITE ligament shows strong wearability, good organization's compatibility and cellular affinity, strong mechanical performance, the basic demand needed for artificial anterior cruciate ligament can be met.
Description
Technical field
The invention belongs to technical field of biological material, more particularly to a kind of composite fibre and its system for artificial anterior cruciate ligament
Preparation Method and application.
Background technology
In the ligamentous injury of knee joint of daily life and sports, cross ligament damage be most common type it
One.In addition, it is difficult to self-healing after its damage, and expectant treatment is substantially invalid, and functional rehabilitation is imperfect.In this regard, therapy one
As be Healing in Anterior Cruciate Ligament Reconstruction, usually for its selection graft there are three types of：Self tendon, tendon allograft and artificial tough
Band.The possibility for for self tendon, being widely used, but thering is graft to occur for complication such as area's defect and postoperative pains
Property；For tendon allograft, can avoid sacrificing self tendon tissue, but there are limited source, transmission, immunological rejections
The problems such as risk (Cooper J A, Lu H H, Ko F K, Laurencin C T.Fiber-based tissue
engineered scaffold for ligament replacement：design considerations and in
Vitro evaluation [J] .Biomaterials, 2005,26 (13)：1523-1532.).
Artificial ligament without disadvantages mentioned above, and possess operation simplify, wound it is small, in art can get some strength, post-operative recovery
The advantages that very fast, thus it is more favored by people and in-depth study, has wide and good application prospect.When
Before, it is used in ligament reconstructive graft there are many artificial ligament, including Meadox ligaments, Gore-Tex ligaments, Leeds-
(the Bernardino S.ACL prosthesis such as Keio ligaments, ABC ligaments, Kennedy LAD ligaments and Trevira ligaments：
any promise for the future？[J] .Knee Surg.Sport.Tr.A., 2010,18 (6)：797-804.).
In different artificial ligaments, LARS ligaments have the features such as can fighting repetition distortion, bending and hyper-traction, are mesh
The more popular and ripe artificial anterior cruciate ligament in the preceding whole world.It is can express out in clinical application using LARS artificial ligaments higher
Satisfaction, such as patient's postoperative ankle function improve, postoperative curative effect preferably (Machotka Z, Scarborough I,
Duncan W, Kumar S, Perraton L.Anterior cruciate ligament repair with LARS
(ligament advanced reinforcement system)：a systematic review[J].Sports
Med.Arthrosc.Rehabil.Ther.Technol., 2010,2：29.).In order to further increase the comprehensive of LARS ligaments
Can, (the Shanghai development [D] of Li Hong novel surface modificationization polyethylene terephthalate (PET) artificial ligament Li Hong：It is multiple
Denier university, 2012.) LARS ligaments are surface modified using substances such as hydroxyapatite and bio-vitrics, to enhance it
Clinical efficacy.But the LARS ligaments being made of hydrophobicity pet fiber still have itself inherently
Defect, such as the intensity of ligament is insufficient, wear resistance is low, cellular affinity is poor (Bernardino S.ACL
prosthesis：Any promise for the future [J] .Knee Surg.Sport.Tr.A., 2010,18 (6)：
797-804.).Therefore, prepare and develop the Utopian artificial anterior cruciate ligament with superior physical properties and biocompatibility
Become the research hotspot in the field.
Invention content
In order to overcome the shortcomings and deficiencies of the prior art described above, the primary purpose of the present invention is that providing a kind of for artificial
The composite fibre of anterior cruciate ligament.
Another object of the present invention is to provide the preparation method of the above-mentioned composite fibre for artificial anterior cruciate ligament.
Still a further object of the present invention is to provide the application of the above-mentioned composite fibre for artificial anterior cruciate ligament.
The purpose of the present invention is realized by following proposal：
A kind of preparation method of composite fibre for artificial anterior cruciate ligament, mainly includes the following steps that：
(1) the own ester of polyhydroxybutyrate and polyglycolic acid are taken, is separately dried, it is spare；
(2) the own ester of polyhydroxybutyrate and polyglycolic acid after will be dry in step (1) be added in solvent, in stirring condition
Under be heated to reflux and make fully to dissolve, be then removed by filtration insoluble impurity, then deaeration, obtain mixed solution, for use；
(3) use dry spinning technology, by the mixed solution in step (2) from spinneret capillary extrusion solution thread
The solvent in solution thread is set quickly to volatilize by the effect of hot-air in path into spinning shaft, solution thread is gradual
Concentration and solidification occurs while sloughing solvent, to form the own ester of polyhydroxybutyrate/polyglycolic acid as-spun fibre；
(4) it comes out, is washed out by the as-spun fibre of step (3) by draw-off godet and by winch spool by auxiliary traction, do
It is dry, obtain the own ester of polyhydroxybutyrate/polyglycolic acid composite fibre.
The numeral molecular weight of the own ester of polyhydroxybutyrate described in step (1) is preferably 1.9 × 105~2.6 × 105；It is described
The molecular weight of polyglycolic acid be preferably 55000~72000.
Drying described in step (1) refers both at 50~70 DEG C vacuum drying 12~for 24 hours；
The mass ratio of the own ester of polyhydroxybutyrate and polyglycolic acid after drying described in step (2) is 1: 1~6；
Solvent described in step (2) is deionized water, absolute ethyl alcohol, dimethylformamide, dimethylacetylamide, diformazan
One kind in base sulfoxide, hexafluoroisopropanol, trifluoroethanol, dichloromethane, chloroform, ether, petroleum ether.
It refers to the heating under the mixing speed of 500~850r/min to be heated to reflux under stirring condition described in step (2)
To 80~95 DEG C of 3~8h of reflux；
Being filtered into described in step (2) is filtered under diminished pressure；
Deaeration mode described in step (2) is deaeration under vacuum state, and temperature is 70~85 DEG C, and the time is 1~3h.
The total concentration of solutes of obtained mixed solution is 2~8wt.% in step (2).
Hot-air described in step (3) is the mixed gas of air and vapor, and the velocity ratio of the two is 1: 10~20.
The as-spun fibre of the step of described in step (4) (3) residence time in path is 15~45s.
Washing described in step (4) is to be washed successively with absolute ethyl alcohol and deionized water, and washing times are 3~5 times.
Drying described in step (4) is natural air drying under normal temperature and pressure.
A kind of composite fibre for artificial anterior cruciate ligament being prepared by the above method.
The above-mentioned application for the composite fibre of artificial anterior cruciate ligament in preparing artificial anterior cruciate ligament.
The application for the composite fibre of artificial anterior cruciate ligament in preparing artificial anterior cruciate ligament specifically by
Following steps are realized：It is 1 beam by a certain amount of composite fibre using twisting weaving method, 3 beams are twisted 1 strand, and 3 strands are twisted cord,
The ropy of a diameter of 4~6mm is twisted after cord doubling, it is 20~30cm to be truncated to length, tightens both ends with steel wire, utilizes seam
Bundle mode with silk thread again fix both ends, successively use absolute ethyl alcohol and deionized water supersound washing, ultrasonic power be 200~
400W, wash time be 10~20min, washing times be 2~3 times, natural air drying under normal temperature and pressure, obtain polyhydroxybutyrate oneself
The compound ligament of ester/polyglycolic acid.
The present invention mechanism be：
The own ester of polyhydroxybutyrate and polyglycolic acid are carried out to compound, the advantages of both the composite fibre obtained combines,
The performances such as the good biocompatibility of the existing own ester of polyhydroxybutyrate, but have polyglycolic acid assign excellent physical mechanical performance with
The performances such as cellular affinity.
In addition, based on collaboration enhancing mechanism, composite fibre has performance more superior than one-component.When composite fibre is used
Come when preparing artificial anterior cruciate ligament, NEW TYPE OF COMPOSITE ligament show strong wearability, good organization's compatibility and cellular affinity,
The characteristics of strong mechanical performance, can meet the basic demand needed for artificial anterior cruciate ligament.
The present invention compared with the existing technology, has the following advantages and advantageous effect：
(1) the obtained own ester of the polyhydroxybutyrate/polyglycolic acid composite fibre of the present invention is as a kind of new fiber materials,
Preparation method is simple.Enhance mechanism based on collaboration, the advantages of composite fibre has organically combined each component has histocompatbility
Good, excellent in mechanical performance, the advantages that cellular affinity is strong, wearability is high, the requirement of artificial anterior cruciate ligament is substantially met, it can quilt
Using in the related art.
(2) researchs such as the preparation method of composite fibre through the invention and performance evaluation can be preceding intersection artificial from now on
Further explore of ligament material provides the theoretical foundation with experiment and reference with application.
Specific implementation mode
With reference to embodiment, the present invention is described in further detail, and embodiments of the present invention are not limited thereto.
Agents useful for same can routinely be bought unless otherwise specified from market in embodiment.
Embodiment 1
(1) weigh polyhydroxybutyrate own ester (be purchased from Dongguan City Su Zhan plastic cement Co., Ltd, number-average molecular weight is 1.9 ×
105) and polyglycolic acid (being purchased from Bo Li biomaterials Co., Ltd of Shenzhen, number-average molecular weight 55000), vacuum is dry at 50 DEG C
Dry 12h, it is spare.
(2) the own ester of polyhydroxybutyrate and polyglycolic acid after will be dry in step (1) be in mass ratio 1: 1 be added to from
In sub- water, under the mixing speed of 500r/min, 80 DEG C of reflux 3h is heated to, make fully to dissolve, then decompression filters, vacuum shape
The lower 70 DEG C of deaeration 1h of state obtain the mixed solution that total concentration of solutes is 2wt.%, for use.
(3) use dry spinning technology, by the mixed solution in step (2) from spinneret capillary extrusion solution thread
Into spinning shaft, by hot-air in path, (velocity ratio of the mixed gas of air and vapor, the two is 1: 10) work
With, so that the solvent in solution thread is quickly volatilized, concentration and solidification occur while gradually sloughing solvent for solution thread, to
Form the own ester of polyhydroxybutyrate/polyglycolic acid as-spun fibre.
(4) as-spun fibre of step (3) is come out by auxiliary traction by the draw-off godet and winch spool by, as-spun fibre is in river in Zhejiang Province
The residence time is 15s in road, is washed 3 times with absolute ethyl alcohol and deionized water successively, natural air drying under normal temperature and pressure obtains poly- hydroxyl
Base n-hexyl butyrate/polyglycolic acid composite fibre.
Embodiment 2
(1) weigh polyhydroxybutyrate own ester (be purchased from Dongguan City Su Zhan plastic cement Co., Ltd, number-average molecular weight is 2.0 ×
105) and polyglycolic acid (being purchased from Bo Li biomaterials Co., Ltd of Shenzhen, number-average molecular weight 58000), vacuum is dry at 50 DEG C
Dry 18h, it is spare.
(2) the own ester of polyhydroxybutyrate after being dried in step (1) and polyglycolic acid are added to for 1: 2 in mass ratio anhydrous
In ethyl alcohol, under the mixing speed of 550r/min, 85 DEG C of reflux 4h is heated to, make fully to dissolve, then decompression filters, vacuum shape
The lower 75 DEG C of deaeration 1h of state obtain the mixed solution that total concentration of solutes is 3wt.%, for use.
(3) use dry spinning technology, by the mixed solution in step (2) from spinneret capillary extrusion solution thread
Into spinning shaft, by hot-air in path, (velocity ratio of the mixed gas of air and vapor, the two is 1: 10) work
With, so that the solvent in solution thread is quickly volatilized, concentration and solidification occur while gradually sloughing solvent for solution thread, to
Form the own ester of polyhydroxybutyrate/polyglycolic acid as-spun fibre.
(4) as-spun fibre of step (3) is come out by auxiliary traction by the draw-off godet and winch spool by, as-spun fibre is in river in Zhejiang Province
The residence time is 20s in road, is washed 3 times with absolute ethyl alcohol and deionized water successively, natural air drying under normal temperature and pressure obtains poly- hydroxyl
Base n-hexyl butyrate/polyglycolic acid composite fibre.
Embodiment 3
(1) weigh polyhydroxybutyrate own ester (be purchased from Dongguan City Su Zhan plastic cement Co., Ltd, number-average molecular weight is 2.1 ×
105) and polyglycolic acid (being purchased from Bo Li biomaterials Co., Ltd of Shenzhen, number-average molecular weight 61000), vacuum is dry at 50 DEG C
It is dry for 24 hours, it is spare.
(2) the own ester of polyhydroxybutyrate after being dried in step (1) and polyglycolic acid are added to diformazan for 1: 3 in mass ratio
In yl acetamide, under the mixing speed of 600r/min, 85 DEG C of reflux 6h is heated to, make fully to dissolve, then decompression filters, very
The lower 75 DEG C of deaeration 1.5h of dummy status obtain the mixed solution that total concentration of solutes is 4wt.%, for use.
(3) use dry spinning technology, by the mixed solution in step (2) from spinneret capillary extrusion solution thread
Into spinning shaft, by hot-air in path, (velocity ratio of the mixed gas of air and vapor, the two is 1: 15) work
With, so that the solvent in solution thread is quickly volatilized, concentration and solidification occur while gradually sloughing solvent for solution thread, to
Form the own ester of polyhydroxybutyrate/polyglycolic acid as-spun fibre.
(4) as-spun fibre of step (3) is come out by auxiliary traction by the draw-off godet and winch spool by, as-spun fibre is in river in Zhejiang Province
The residence time is 25s in road, is washed 4 times with absolute ethyl alcohol and deionized water successively, natural air drying under normal temperature and pressure obtains poly- hydroxyl
Base n-hexyl butyrate/polyglycolic acid composite fibre.
Embodiment 4
(1) weigh polyhydroxybutyrate own ester (be purchased from Dongguan City Su Zhan plastic cement Co., Ltd, number-average molecular weight is 2.2 ×
105) and polyglycolic acid (being purchased from Bo Li biomaterials Co., Ltd of Shenzhen, number-average molecular weight 65000), vacuum is dry at 60 DEG C
It is dry for 24 hours, it is spare.
(2) the own ester of polyhydroxybutyrate after being dried in step (1) and polyglycolic acid are added to diformazan for 1: 4 in mass ratio
In base sulfoxide, under the mixing speed of 650r/min, 90 DEG C of reflux 7h is heated to, make fully to dissolve, then decompression filters, vacuum
The lower 80 DEG C of deaeration 2h of state obtain the mixed solution that total concentration of solutes is 5wt.%, for use.
(3) use dry spinning technology, by the mixed solution in step (2) from spinneret capillary extrusion solution thread
Into spinning shaft, by hot-air in path, (velocity ratio of the mixed gas of air and vapor, the two is 1: 15) work
With, so that the solvent in solution thread is quickly volatilized, concentration and solidification occur while gradually sloughing solvent for solution thread, to
Form the own ester of polyhydroxybutyrate/polyglycolic acid as-spun fibre.
(4) as-spun fibre of step (3) is come out by auxiliary traction by the draw-off godet and winch spool by, as-spun fibre is in river in Zhejiang Province
The residence time is 30s in road, is washed 4 times with absolute ethyl alcohol and deionized water successively, natural air drying under normal temperature and pressure obtains poly- hydroxyl
Base n-hexyl butyrate/polyglycolic acid composite fibre.
Embodiment 5
(1) weigh polyhydroxybutyrate own ester (be purchased from Dongguan City Su Zhan plastic cement Co., Ltd, number-average molecular weight is 2.4 ×
105) and polyglycolic acid (being purchased from Bo Li biomaterials Co., Ltd of Shenzhen, number-average molecular weight 69000), vacuum is dry at 70 DEG C
Dry 12h, it is spare.
(2) the own ester of polyhydroxybutyrate after being dried in step (1) and polyglycolic acid are added to trichlorine for 1: 5 in mass ratio
In methane, under the mixing speed of 750r/min, 90 DEG C of reflux 8h is heated to, make fully to dissolve, then decompression filters, vacuum shape
The lower 80 DEG C of deaeration 2.5h of state obtain the mixed solution that total concentration of solutes is 6wt.%, for use.
(3) use dry spinning technology, by the mixed solution in step (2) from spinneret capillary extrusion solution thread
Into spinning shaft, by hot-air in path, (velocity ratio of the mixed gas of air and vapor, the two is 1: 20) work
With, so that the solvent in solution thread is quickly volatilized, concentration and solidification occur while gradually sloughing solvent for solution thread, to
Form the own ester of polyhydroxybutyrate/polyglycolic acid as-spun fibre.
(4) as-spun fibre of step (3) is come out by auxiliary traction by the draw-off godet and winch spool by, as-spun fibre is in river in Zhejiang Province
The residence time is 35s in road, is washed 5 times with absolute ethyl alcohol and deionized water successively, natural air drying under normal temperature and pressure obtains poly- hydroxyl
Base n-hexyl butyrate/polyglycolic acid composite fibre.
Embodiment 6
(1) weigh polyhydroxybutyrate own ester (be purchased from Dongguan City Su Zhan plastic cement Co., Ltd, number-average molecular weight is 2.6 ×
105) and polyglycolic acid (being purchased from Bo Li biomaterials Co., Ltd of Shenzhen, number-average molecular weight 72000), vacuum is dry at 70 DEG C
It is dry for 24 hours, it is spare.
(2) the own ester of polyhydroxybutyrate after being dried in step (1) and polyglycolic acid are added to oil for 1: 6 in mass ratio
In ether, under the mixing speed of 850r/min, 95 DEG C of reflux 8h is heated to, make fully to dissolve, then decompression filters, vacuum state
Lower 85 DEG C of deaeration 3h obtain the mixed solution that total concentration of solutes is 8wt.%, for use.
(3) use dry spinning technology, by the mixed solution in step (2) from spinneret capillary extrusion solution thread
Into spinning shaft, by hot-air in path, (velocity ratio of the mixed gas of air and vapor, the two is 1: 20) work
With, so that the solvent in solution thread is quickly volatilized, concentration and solidification occur while gradually sloughing solvent for solution thread, to
Form the own ester of polyhydroxybutyrate/polyglycolic acid as-spun fibre.
(4) as-spun fibre of step (3) is come out by auxiliary traction by the draw-off godet and winch spool by, as-spun fibre is in river in Zhejiang Province
The residence time is 45s in road, is washed 5 times with absolute ethyl alcohol and deionized water successively, natural air drying under normal temperature and pressure obtains poly- hydroxyl
Base n-hexyl butyrate/polyglycolic acid composite fibre.
Embodiment 7
Artificial preceding intersection is applied to the own ester of polyhydroxybutyrate/polyglycolic acid composite fibre that Examples 1 to 6 is prepared
In ligament, detailed process and steps are as follows：
It is 1 beam by 50 composite fibres using twisting weaving method, 3 beams are twisted 1 strand, and 3 strands are twisted cord, cord pair
The ropy of a diameter of 5mm is twisted after folding, it is 25cm to be truncated to length, tightens both ends with steel wire, silk thread is used in the way of tying
Again fix both ends, successively use absolute ethyl alcohol and deionized water supersound washing, ultrasonic power 300W, wash time 15min,
Washing times are 3 times, and natural air drying under normal temperature and pressure obtains the own compound ligament of ester/polyglycolic acid of polyhydroxybutyrate.
The comparative example of Examples 1 to 6 is set simultaneously, the own ester of polyhydroxybutyrate in (1) the step of embodiment 1 is all replaced
It is changed to polyglycolic acid, remaining is constant, and obtained artificial anterior cruciate ligament is denoted as comparative sample 1A；By (1) the step of embodiment 1
In polyglycolic acid all replace with the own ester of polyhydroxybutyrate, remaining is constant, and obtained artificial anterior cruciate ligament is denoted as pair
Than sample 1B；The own ester of polyhydroxybutyrate in (1) the step of embodiment 2 is all replaced with into polyglycolic acid, remaining is constant, obtains
To artificial anterior cruciate ligament be denoted as comparative sample 2A；Polyglycolic acid in (1) the step of embodiment 2 is all replaced with into poly- hydroxyl
N-hexyl butyrate, remaining is constant, and obtained artificial anterior cruciate ligament is denoted as comparative sample 2B；It will be in (1) the step of embodiment 3
The own ester of polyhydroxybutyrate all replaces with polyglycolic acid, remaining is constant, and obtained artificial anterior cruciate ligament is denoted as comparative sample
3A；Polyglycolic acid in (1) the step of embodiment 3 is all replaced with into the own ester of polyhydroxybutyrate, remaining is constant, obtains
Artificial anterior cruciate ligament is denoted as comparative sample 3B；The own ester of polyhydroxybutyrate in (1) the step of embodiment 4 is all replaced with into poly- second
Alkyd, remaining is constant, and obtained artificial anterior cruciate ligament is denoted as comparative sample 4A；By the poly- second in (1) the step of embodiment 4
Alkyd all replaces with the own ester of polyhydroxybutyrate, remaining is constant, and obtained artificial anterior cruciate ligament is denoted as comparative sample 4B；It will
The own ester of polyhydroxybutyrate in the step of embodiment 5 (1) all replaces with polyglycolic acid, remaining is constant, and what is obtained is artificial
Anterior cruciate ligament is denoted as comparative sample 5A；By the polyglycolic acid in (1) the step of embodiment 5 all replace with polyhydroxybutyrate oneself
Ester, remaining is constant, and obtained artificial anterior cruciate ligament is denoted as comparative sample 5B；By the poly- hydroxyl in (1) the step of embodiment 6
N-hexyl butyrate all replaces with polyglycolic acid, remaining is constant, and obtained artificial anterior cruciate ligament is denoted as comparative sample 6A；It will be real
Polyglycolic acid in the step of applying example 6 (1) all replaces with the own ester of polyhydroxybutyrate, remaining is constant, obtain it is artificial before
Ligamentaum cruciatum is denoted as comparative sample 6B.
Investigate gained the compound ligament of the own ester/polyglycolic acid of polyhydroxybutyrate and corresponding comparative example obtain it is artificial before
Mechanical property, wearability, cellular affinity and the histocompatbility of ligament product, specific test process and steps are as follows：
(1) mechanical property
Mechanics Performance Testing is carried out using omnipotent test machine (LLOYD LR100K, China).After both ends fixture is fixed, with
The speed of 10mm/min is stretched.Experiment repeat 5 times, result is expressed as (average value ± standard deviation), as table 1~
Shown in 6.
The compound ligament of gained and its mechanical experimental results of comparative sample in 1 embodiment 1 of table
| Sample | Maximum load (N) | Tensile strength (MPa) | Elasticity modulus (GPa) |
| Embodiment 1 | 690.33±11.09 | 36.23±2.12 | 0.36±0.04 |
| Comparative sample 1A | 600.01±12.01 | 30.89±1.73 | 0.22±0.03 |
| Comparative sample 1B | 420.51±10.03 | 24.11±1.89 | 0.11±0.03 |
The compound ligament of gained and its mechanical experimental results of comparative sample in 2 embodiment 2 of table
The compound ligament of gained and its mechanical experimental results of comparative sample in 3 embodiment 3 of table
| Sample | Maximum load (N) | Tensile strength (MPa) | Elasticity modulus (GPa) |
| Embodiment 3 | 710.89±12.84 | 39.44±2.45 | 0.38±0.03 |
| Comparative sample 3A | 612.76±11.39 | 33.05±1.79 | 0.26±0.03 |
| Comparative sample 3B | 448.03±15.04 | 29.31±2.05 | 0.16±0.04 |
The compound ligament of gained and its mechanical experimental results of comparative sample in 4 embodiment 4 of table
| Sample | Maximum load (N) | Tensile strength (MPa) | Elasticity modulus (GPa) |
| Embodiment 4 | 739.58±16.21 | 44.62±2.17 | 0.44±0.04 |
| Comparative sample 4A | 654.84±15.09 | 35.11±2.13 | 0.32±0.02 |
| Comparative sample 4B | 473.12±13.69 | 29.35±1.97 | 0.19±0.02 |
The compound ligament of gained and its mechanical experimental results of comparative sample in 5 embodiment 5 of table
| Sample | Maximum load (N) | Tensile strength (MPa) | Elasticity modulus (GPa) |
| Embodiment 5 | 778.41±13.27 | 50.38±2.51 | 0.51±0.05 |
| Comparative sample 5A | 697.31±11.78 | 39.89±1.19 | 0.37±0.03 |
| Comparative sample 5B | 514.34±11.52 | 31.25±2.01 | 0.23±0.03 |
The compound ligament of gained and its mechanical experimental results of comparative sample in 6 embodiment 6 of table
| Sample | Maximum load (N) | Tensile strength (MPa) | Elasticity modulus (GPa) |
| Embodiment 6 | 751.32±16.55 | 47.26±2.19 | 0.47±0.02 |
| Comparative sample 6A | 668.91±13.02 | 38.97±2.21 | 0.32±0.04 |
| Comparative sample 6B | 500.16±18.09 | 31.62±2.54 | 0.23±0.02 |
As can be seen that the mechanical property of the obtained own compound ligament of ester/polyglycolic acid of polyhydroxybutyrate from table 1~6
Than one-component than get well, and the mechanical property of the two has been organically combined, with high mechanics mechanical strength.
(2) wearability
Wearability experiment carries out on the omnipotent frictional testing machine of MMW-1A types.Sample is mounted in fixture and is fixed on rotation axis
Circumferential slippage is made in lower section centered on GCr15 is on mill by main shaft.Wherein, moving radius 12mm, gliding cable structure are
100r/min, sliding time 5min, sliding distance 150m, counterweight weight are 10N, lever moment 0.35MPa.
The quality of sample is weighed before experiment with electronic analytical balance；Sample is first washed 3 times simultaneously with deionized water after experiment
Drying, then the quality with electronic analytical balance weighing sample.The wear rate of sample is calculated with weight-loss method, and sample is weighed with this
Wearability.Experiment repeats 3 times, and result takes the average value of experimental data, as shown in table 7~12.
The wearability test result of the compound ligament of gained and its comparative sample in 7 embodiment 1 of table
| Sample | Wear rate (mm3/m) |
| Embodiment 1 | 0.32×10-3 |
| Comparative sample 1A | 0.41×10-3 |
| Comparative sample 1B | 0.66×10-3 |
The wearability test result of the compound ligament of gained and its comparative sample in 8 embodiment 2 of table
| Sample | Wear rate (mm3/m) |
| Embodiment 2 | 0.28×10-3 |
| Comparative sample 2A | 0.39×10-3 |
| Comparative sample 2B | 0.68×10-3 |
The wearability test result of the compound ligament of gained and its comparative sample in 9 embodiment 3 of table
| Sample | Wear rate (mm3/m) |
| Embodiment 3 | 0.31×10-3 |
| Comparative sample 3A | 0.44×10-3 |
| Comparative sample 3B | 0.69×10-3 |
The wearability test result of the compound ligament of gained and its comparative sample in 10 embodiment 4 of table
| Sample | Wear rate (mm3/m) |
| Embodiment 4 | 0.25×10-3 |
| Comparative sample 4A | 0.37×10-3 |
| Comparative sample 4B | 0.64×10-3 |
The wearability test result of the compound ligament of gained and its comparative sample in 11 embodiment 5 of table
| Sample | Wear rate (mm3/m) |
| Embodiment 5 | 0.21×10-3 |
| Comparative sample 5A | 0.33×10-3 |
| Comparative sample 5B | 0.59×10-3 |
The wearability test result of the compound ligament of gained and its comparative sample in 12 embodiment 6 of table
| Sample | Wear rate (mm3/m) |
| Embodiment 6 | 0.23×10-3 |
| Comparative sample 6A | 0.34×10-3 |
| Comparative sample 6B | 0.61×10-3 |
As can be seen that the obtained own compound ligament of ester/polyglycolic acid of polyhydroxybutyrate organically combines from table 7~12
The performance of two components, wear resistance is good, can meet the needs of artificial anterior cruciate ligament.
(3) cellular affinity
According to ISO 10993-5：The requirement and suggestion of 1999 and GB/T 16886.5-2003, using polyhydroxybutyrate oneself
The method of the compound ligament leaching liquor MTT colorimetric methods of ester/polyglycolic acid, the cellular affinity of test compound ligament.Wherein, cell toxicant
Property classification rating scale it is as shown in table 13, classification numerical value it is smaller, indicate that the cytotoxicity of material is lower, then the cell of material is affine
Property is better, and cellular affinity result is as shown in table 14~19.
13 cytotoxicity of table is classified rating scale
(4) histocompatbility
According to ISO 10993-6：The requirement and suggestion of 1994 and GB/T 16886.6-1997, it is short-term using subcutaneous tissue
(9 weeks) method of implantation, the histocompatbility of test compound ligament.The result of histocompatbility is as shown in table 14~19.
The compound ligament of gained and its cellular affinity of comparative sample and the result of histocompatbility in 14 embodiment 1 of table
The compound ligament of gained and its cellular affinity of comparative sample and the result of histocompatbility in 15 embodiment 2 of table
The compound ligament of gained and its cellular affinity of comparative sample and the result of histocompatbility in 16 embodiment 3 of table
The compound ligament of gained and its cellular affinity of comparative sample and the result of histocompatbility in 17 embodiment 4 of table
The compound ligament of gained and its cellular affinity of comparative sample and the result of histocompatbility in 18 embodiment 5 of table
The compound ligament of gained and its cellular affinity of comparative sample and the result of histocompatbility in 19 embodiment 6 of table
It is found that the own compound ligament of ester/polyglycolic acid of obtained polyhydroxybutyrate has organically combined two from table 14~19
The biological property of a component, cytotoxicity are 0 grade, i.e. its no cytotoxicity, cellular affinity is good.And its histocompatbility
It is excellent, body tissue organ is had no significant effect.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, it is other it is any without departing from the spirit and principles of the present invention made by changes, modifications, substitutions, combinations, simplifications,
Equivalent substitute mode is should be, is included within the scope of the present invention.
Claims (10)
1. a kind of preparation method of composite fibre for artificial anterior cruciate ligament, it is characterised in that mainly include the following steps that：
(1) the own ester of polyhydroxybutyrate and polyglycolic acid are taken, is separately dried, it is spare；
(2) the own ester of polyhydroxybutyrate after being dried in step (1) and polyglycolic acid are added in solvent, are added under agitation
Heat reflux makes fully to dissolve, and is then removed by filtration insoluble impurity, then deaeration, obtains mixed solution, for use；
(3) dry spinning technology is used, extrusion solution thread enters from spinneret capillary by the mixed solution in step (2)
Spinning shaft makes the solvent in solution thread quickly volatilize by the effect of hot-air in path, and solution thread is gradually being sloughed
Concentration and solidification occur while solvent, to form the own ester of polyhydroxybutyrate/polyglycolic acid as-spun fibre；
(4) it comes out, is washed out by the as-spun fibre of step (3) by draw-off godet and by winch spool by auxiliary traction, it is dry, it obtains
To the own ester of polyhydroxybutyrate/polyglycolic acid composite fibre.
2. the preparation method of the composite fibre according to claim 1 for artificial anterior cruciate ligament, it is characterised in that：
The numeral molecular weight of the own ester of polyhydroxybutyrate described in step (1) is 1.9 × 105~2.6 × 105；The polyethanol
The molecular weight of acid is 55000~72000；
Drying described in step (1) refers both at 50~70 DEG C vacuum drying 12~for 24 hours.
3. the preparation method of the composite fibre according to claim 1 for artificial anterior cruciate ligament, it is characterised in that：
The mass ratio of the own ester of polyhydroxybutyrate and polyglycolic acid after drying described in step (2) is 1: 1~6；
The total concentration of solutes of obtained mixed solution is 2~8wt.% in step (2).
4. the preparation method of the composite fibre according to claim 1 for artificial anterior cruciate ligament, it is characterised in that：
Solvent described in step (2) is deionized water, absolute ethyl alcohol, dimethylformamide, dimethylacetylamide, dimethyl Asia
One kind in sulfone, hexafluoroisopropanol, trifluoroethanol, dichloromethane, chloroform, ether, petroleum ether.
5. the preparation method of the composite fibre according to claim 1 for artificial anterior cruciate ligament, it is characterised in that：
Be heated to reflux under stirring condition described in step (2) refers to being heated to 80 under the mixing speed of 500~850r/min
~95 DEG C of 3~8h of reflux；
Being filtered into described in step (2) is filtered under diminished pressure；
Deaeration mode described in step (2) is deaeration under vacuum state, and temperature is 70~85 DEG C, and the time is 1~3h.
6. the preparation method of the composite fibre according to claim 1 for artificial anterior cruciate ligament, it is characterised in that：
Hot-air described in step (3) is the mixed gas of air and vapor, and the velocity ratio of the two is 1: 10~20.
7. the preparation method of the composite fibre according to claim 1 for artificial anterior cruciate ligament, it is characterised in that：
The as-spun fibre of the step of described in step (4) (3) residence time in path is 15~45s；
Washing described in step (4) is to be washed successively with absolute ethyl alcohol and deionized water, and washing times are 3~5 times；
Drying described in step (4) is natural air drying under normal temperature and pressure.
8. a kind of being used for the compound of artificial anterior cruciate ligament according to what claim 1~7 any one of them method was prepared
Fiber.
9. the composite fibre according to claim 8 for artificial anterior cruciate ligament is in preparing artificial anterior cruciate ligament
Using.
10. the composite fibre according to claim 9 for artificial anterior cruciate ligament is in preparing artificial anterior cruciate ligament
Application, it is characterised in that mainly realized by following steps：
It is 1 beam by a certain amount of composite fibre using twisting weaving method, 3 beams are twisted 1 strand, and 3 strands are twisted cord, cord doubling
It is twisted the ropy of a diameter of 4~6mm afterwards, it is 20~30cm to be truncated to length, tightens both ends with steel wire, is used in the way of tying
Silk thread fixes both ends again, uses absolute ethyl alcohol and deionized water supersound washing successively, ultrasonic power is 200~400W, when washing
Between be 10~20min, washing times be 2~3 times, natural air drying under normal temperature and pressure obtains the own ester/polyglycolic acid of polyhydroxybutyrate
Compound ligament.
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| CN115154666A (en) * | 2022-07-18 | 2022-10-11 | 上海市养志康复医院（上海市阳光康复中心） | Degradable artificial ligament capable of being used for repairing nerve loop and preparation method thereof |
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