CN106267323A - A kind of preparation method of degradable medicine carrying poly (lactic acid-glycolic acid) operation suture thread - Google Patents

A kind of preparation method of degradable medicine carrying poly (lactic acid-glycolic acid) operation suture thread Download PDF

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CN106267323A
CN106267323A CN201610743094.0A CN201610743094A CN106267323A CN 106267323 A CN106267323 A CN 106267323A CN 201610743094 A CN201610743094 A CN 201610743094A CN 106267323 A CN106267323 A CN 106267323A
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lactic acid
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侯英
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS 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
    • A61L17/00Materials for surgical sutures or for ligaturing blood vessels ; Materials for prostheses or catheters
    • A61L17/14Post-treatment to improve physical properties
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS 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
    • A61L17/00Materials for surgical sutures or for ligaturing blood vessels ; Materials for prostheses or catheters
    • A61L17/005Materials for surgical sutures or for ligaturing blood vessels ; Materials for prostheses or catheters containing a biologically active substance, e.g. a medicament or a biocide
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS 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
    • A61L17/00Materials for surgical sutures or for ligaturing blood vessels ; Materials for prostheses or catheters
    • A61L17/06At least partially resorbable materials
    • A61L17/10At least partially resorbable materials containing macromolecular materials
    • A61L17/12Homopolymers or copolymers of glycolic acid or lactic acid
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G63/00Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
    • C08G63/02Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
    • C08G63/06Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from hydroxycarboxylic acids
    • C08G63/08Lactones or lactides
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/10Other agents for modifying properties
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/88Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
    • D01F6/92Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyesters
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS 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
    • A61L2300/00Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
    • A61L2300/60Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a special physical form
    • A61L2300/62Encapsulated active agents, e.g. emulsified droplets
    • A61L2300/622Microcapsules

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Abstract

The present invention relates to the preparation method of a kind of degradable medicine carrying poly (lactic acid-glycolic acid) operation suture thread, the hollow silica sub-micron ball loading medicine is dispersed in the aqueous solution of degradable poly y, makes degradable medicine carrying poly (lactic acid-glycolic acid) operation suture thread operation suture thread by using spinning process to be embedded in degradable poly y fiber by the hollow silica sub-micron ball loading medicine;The preparation process of described degradable poly y includes: be 1) raw material by technical grade lactic acid aqueous solution and glycolic, carries out dehydration under vacuum refined, obtains y oligomer;2) by step 1) the y oligomer that obtains mixes with catalyst, adds in reaction vessel, under vacuum, and reacting by heating, obtain poly (lactic acid-glycolic acid) intermediate product;3) in step 2) in reaction vessel in add chain extender MDI, under vacuum, reacting by heating, obtain poly-lactic acid in high molecular weight glycolic.

Description

A kind of preparation method of degradable medicine carrying poly (lactic acid-glycolic acid) operation suture thread
Technical field
The present invention relates to biomedicine field, concrete, relate to a kind of degradable medicine carrying poly (lactic acid-glycolic acid) operation stitching The preparation method of line.
Background technology
The most domestic surgical sewing thread used clinically mainly divides nonabsorable stitching thread and absorbable suture Two kinds.Nonabsorable stitching thread has nylon wire, polypropylene line, formal wire etc..These materials, as surgical sewing thread, are opened Force intensity is high, and tissue reaction is low, but a disadvantage is that knotting difficulty, the most de-knot, it is impossible to degraded and absorbed, needs to take out stitches.Absorbable seam Zygonema has cashmere line, polyglycolide, chitin, collagen fiber etc..Advanced absorbable suture should have stronger tension force Intensity, good operating characteristics, material is homogeneous, stable, and no antigen, tissue reaction is low, is better than nonabsorable stitching thread.At present The absorbable suture of China is also faced with three big problems: (1) preparation technology is limited, and Mechanical Properties of Products is the most as one wishes.(2) more Advanced absorbable suture is the most expensive;(3) need to improve intensity and the solution of the polymer as absorbable suture Certainly implant untoward reaction and the complication etc. in human body later stage.Due to these reasons, absorbable suture China clinically should With also comparing limitation.
Summary of the invention
The technical problem to be solved is to provide a kind of degradable medicine carrying poly (lactic acid-glycolic acid) operation suture thread Preparation method.
The technical scheme is that a kind of degradable medicine carrying poly (lactic acid-glycolic acid) operation seam The preparation method of zygonema, is dispersed in the water-soluble of degradable poly y by the hollow silica sub-micron ball loading medicine In liquid, by using spinning process that the hollow silica sub-micron ball loading medicine is embedded in degradable poly y Fiber is made degradable medicine carrying poly (lactic acid-glycolic acid) operation suture thread operation suture thread;
The preparation process of described degradable poly y includes:
1) it is raw material by technical grade lactic acid aqueous solution and glycolic, carries out dehydration under vacuum refined, obtain lactic acid Glycolic acid oligomer;
2) by step 1) the y oligomer that obtains mixes with catalyst, adds in reaction vessel, at vacuum bar Under part, reacting by heating, obtain poly (lactic acid-glycolic acid) intermediate product;
3) in step 2) in reaction vessel in add chain extender MDI, under vacuum, reacting by heating, obtain high score Son amount poly (lactic acid-glycolic acid).
Further, step 1) in vacuum be 2-4kPa, dewatering time is 0.5-10 hour, dehydration temperaturre scope 45- 100 DEG C, described lactic acid is 1:1-3 with the mol ratio of glycolic.
Further, step 2) in vacuum be 0.5-2kPa, range of reaction temperature 150-180 DEG C, the response time is 2-5 Hour, with mechanical agitation during reaction.
Further, step 2) in catalyst be two or three in stannous chloride, stannous octoate, p-methyl benzenesulfonic acid Mixture, its gross mass is the 0.5%~1% of y oligomer quality.
Further, step 3) in vacuum be 1-3kPa, range of reaction temperature 130-160 DEG C, the response time is that 1-4 is little Time, with mechanical agitation during reaction.
Further, step 3) in the 0.5%-that quality is poly (lactic acid-glycolic acid) intermediate product quality expanding even agent MDI 1.3%.
Further, step 3) in the adding method of chain extender, be to be directly added into reaction system, after melting mixing, then occur Chain extending reaction.
Further, step 3) in the adding method of chain extender, be chain extender to be dissolved in solvent injection add, mixed process In, solvent is discharged by vacuum system.
Further, the described hollow silica sub-micron ball preparation method loading medicine is: by hollow silica Sub-micron ball is immersed in the aqueous solution of water soluble drug, stirs 1 day~4 days, be then 4 DEG C in temperature at temperature is 4 DEG C Lower centrifugal, clean gained solid product, lyophilization with deionized water, obtain being loaded with the hollow silica of water soluble drug Sub-micron ball;Or hollow silica sub-micron ball is immersed in the organic solvent of fat-soluble medicine, stir at temperature is 4 DEG C Mix 1 day~4 days, then centrifugal at temperature is 4 DEG C, clean gained solid product, lyophilization with deionized water, loaded The hollow silica sub-micron ball of fat-soluble medicine.
Further, described curative drug selected from neomycin, ribostamycin, micronomicin, A Si mycin, tetracycline, Oxytetracycline, chlortetracycline, doxycycline, chloromycetin, thiamphenicol, erythromycin, albomycin, erythromycin ethylsuccinate, azithromycin, acetyl Spiramycin, midecamycin, josamycin, lincomycin, clindamycin, vancomycin, bacitracin, polymyxin, phosphorus are mould Element, ciramycin, cycloserine, griseofulvin, mitomycin, bleomycin, ciclosporin, metronidazole, penicillin, penicillin sodium, One in benzylpenicillin potassium, ampicillin, amoxicillin, piperacillin, benzylpenicillin potassium or more than more than one;Or selected from upper State the one in the derivant of curative drug or more than more than one;Or selected from above-mentioned curative drug and above-mentioned therapeutic medicine A kind of in the derivant of thing or more than more than one mixture.
The invention has the beneficial effects as follows: obtain that a kind of molecular weight is high, hot strength is good, degradable and be mounted with medicine Poly (lactic acid-glycolic acid) operation suture thread.
Detailed description of the invention
Principle and feature to the present invention are described below, and example is served only for explaining the present invention, is not intended to limit Determine the scope of the present invention.
Embodiment 1
The preparation method of a kind of degradable medicine carrying poly (lactic acid-glycolic acid) operation suture thread, will load the hollow titanium dioxide of medicine Silicon sub-micron ball is dispersed in the aqueous solution of degradable poly y, by using spinning process will to load the hollow of medicine Silicon dioxide sub-micron sphere is embedded in degradable poly y fiber makes the operation of degradable medicine carrying poly (lactic acid-glycolic acid) Stitching thread operation suture thread;
The preparation process of described degradable poly y includes:
1) it is raw material by technical grade lactic acid aqueous solution and glycolic, carries out dehydration under vacuum refined, obtain lactic acid Glycolic acid oligomer;
2) by step 1) the y oligomer that obtains mixes with catalyst, adds in reaction vessel, at vacuum bar Under part, reacting by heating, obtain poly (lactic acid-glycolic acid) intermediate product;
3) in step 2) in reaction vessel in add chain extender MDI, under vacuum, reacting by heating, obtain high score Son amount poly (lactic acid-glycolic acid).
Step 1) in vacuum be 4kPa, dewatering time is 10 hours, dehydration temperaturre scope 100 DEG C, described lactic acid with The mol ratio of glycolic is 1:3.
Step 2) in vacuum be 2kPa, range of reaction temperature 180 DEG C, the response time is 5 hours, with machine during reaction Tool stirs.
Step 2) in catalyst be in stannous chloride, stannous octoate, p-methyl benzenesulfonic acid two or three mixture, Its gross mass is the 1% of y oligomer quality.
Step 3) in vacuum be 3kPa, range of reaction temperature 160 DEG C, the response time is 4 hours, with machine during reaction Tool stirs.
Step 3) in expand quality is poly (lactic acid-glycolic acid) intermediate product quality the 1.3% of even agent MDI.
Step 3) in the adding method of chain extender, be to be directly added into reaction system, after melting mixing, then occur chain extension anti- Should.
Further, the described hollow silica sub-micron ball preparation method loading medicine is: by hollow silica Sub-micron ball is immersed in the aqueous solution of water soluble drug, stirs 1 day~4 days, be then 4 DEG C in temperature at temperature is 4 DEG C Lower centrifugal, clean gained solid product, lyophilization with deionized water, obtain being loaded with the hollow silica of water soluble drug Sub-micron ball;Or hollow silica sub-micron ball is immersed in the organic solvent of fat-soluble medicine, stir at temperature is 4 DEG C Mix 1 day~4 days, then centrifugal at temperature is 4 DEG C, clean gained solid product, lyophilization with deionized water, loaded The hollow silica sub-micron ball of fat-soluble medicine.
Further, described curative drug selected from neomycin, ribostamycin, micronomicin, A Si mycin, tetracycline, Oxytetracycline, chlortetracycline, doxycycline, chloromycetin, thiamphenicol, erythromycin, albomycin, erythromycin ethylsuccinate, azithromycin, acetyl Spiramycin, midecamycin, josamycin, lincomycin, clindamycin, vancomycin, bacitracin, polymyxin, phosphorus are mould Element, ciramycin, cycloserine, griseofulvin, mitomycin, bleomycin, ciclosporin, metronidazole, penicillin, penicillin sodium, One in benzylpenicillin potassium, ampicillin, amoxicillin, piperacillin, benzylpenicillin potassium or more than more than one;Or selected from upper State the one in the derivant of curative drug or more than more than one;Or selected from above-mentioned curative drug and above-mentioned therapeutic medicine A kind of in the derivant of thing or more than more than one mixture.
Embodiment 2
The preparation method of a kind of degradable medicine carrying poly (lactic acid-glycolic acid) operation suture thread, will load the hollow titanium dioxide of medicine Silicon sub-micron ball is dispersed in the aqueous solution of degradable poly y, by using spinning process will to load the hollow of medicine Silicon dioxide sub-micron sphere is embedded in degradable poly y fiber makes the operation of degradable medicine carrying poly (lactic acid-glycolic acid) Stitching thread operation suture thread;
The preparation process of described degradable poly y includes:
1) it is raw material by technical grade lactic acid aqueous solution and glycolic, carries out dehydration under vacuum refined, obtain lactic acid Glycolic acid oligomer;
2) by step 1) the y oligomer that obtains mixes with catalyst, adds in reaction vessel, at vacuum bar Under part, reacting by heating, obtain poly (lactic acid-glycolic acid) intermediate product;
3) in step 2) in reaction vessel in add chain extender MDI, under vacuum, reacting by heating, obtain high score Son amount poly (lactic acid-glycolic acid).
Step 1) in vacuum be 2kPa, dewatering time is 0.5 hour, dehydration temperaturre scope 45 DEG C, described lactic acid with The mol ratio of glycolic is 1:1.
Step 2) in vacuum be 0.5kPa, range of reaction temperature 130 DEG C, the response time is 2 hours, adjoint during reaction Mechanical agitation.
Step 2) in catalyst be in stannous chloride, stannous octoate, p-methyl benzenesulfonic acid two or three mixture, Its gross mass is the 0.5% of y oligomer quality.
Step 3) in vacuum be 1kPa, range of reaction temperature 130 DEG C, the response time is 1 hour, with machine during reaction Tool stirs.
Step 3) in expand quality is poly (lactic acid-glycolic acid) intermediate product quality the 0.5% of even agent MDI.
Step 3) in the adding method of chain extender, be chain extender to be dissolved in solvent injection add, in mixed process, solvent Discharged by vacuum system.
Further, the described hollow silica sub-micron ball preparation method loading medicine is: by hollow silica Sub-micron ball is immersed in the aqueous solution of water soluble drug, stirs 1 day~4 days, be then 4 DEG C in temperature at temperature is 4 DEG C Lower centrifugal, clean gained solid product, lyophilization with deionized water, obtain being loaded with the hollow silica of water soluble drug Sub-micron ball;Or hollow silica sub-micron ball is immersed in the organic solvent of fat-soluble medicine, stir at temperature is 4 DEG C Mix 1 day~4 days, then centrifugal at temperature is 4 DEG C, clean gained solid product, lyophilization with deionized water, loaded The hollow silica sub-micron ball of fat-soluble medicine.
Further, described curative drug selected from neomycin, ribostamycin, micronomicin, A Si mycin, tetracycline, Oxytetracycline, chlortetracycline, doxycycline, chloromycetin, thiamphenicol, erythromycin, albomycin, erythromycin ethylsuccinate, azithromycin, acetyl Spiramycin, midecamycin, josamycin, lincomycin, clindamycin, vancomycin, bacitracin, polymyxin, phosphorus are mould Element, ciramycin, cycloserine, griseofulvin, mitomycin, bleomycin, ciclosporin, metronidazole, penicillin, penicillin sodium, One in benzylpenicillin potassium, ampicillin, amoxicillin, piperacillin, benzylpenicillin potassium or more than more than one;Or selected from upper State the one in the derivant of curative drug or more than more than one;Or selected from above-mentioned curative drug and above-mentioned therapeutic medicine A kind of in the derivant of thing or more than more than one mixture.
Embodiment 3
The preparation method of a kind of degradable medicine carrying poly (lactic acid-glycolic acid) operation suture thread, will load the hollow titanium dioxide of medicine Silicon sub-micron ball is dispersed in the aqueous solution of degradable poly y, by using spinning process will to load the hollow of medicine Silicon dioxide sub-micron sphere is embedded in degradable poly y fiber makes the operation of degradable medicine carrying poly (lactic acid-glycolic acid) Stitching thread operation suture thread;
The preparation process of described degradable poly y includes:
1) it is raw material by technical grade lactic acid aqueous solution and glycolic, carries out dehydration under vacuum refined, obtain lactic acid Glycolic acid oligomer;
2) by step 1) the y oligomer that obtains mixes with catalyst, adds in reaction vessel, at vacuum bar Under part, reacting by heating, obtain poly (lactic acid-glycolic acid) intermediate product;
3) in step 2) in reaction vessel in add chain extender MDI, under vacuum, reacting by heating, obtain high score Son amount poly (lactic acid-glycolic acid).
Step 1) in vacuum be 2.5kPa, dewatering time is 4 hours, dehydration temperaturre scope 80 DEG C, described lactic acid with The mol ratio of glycolic is 1:1.5.
Step 2) in vacuum be 2kPa, range of reaction temperature 150 DEG C, the response time is 4 hours, with machine during reaction Tool stirs.
Step 2) in catalyst be in stannous chloride, stannous octoate, p-methyl benzenesulfonic acid two or three mixture, Its gross mass is the 0.5% of y oligomer quality.
Step 3) in vacuum be 1.2kPa, range of reaction temperature 140 DEG C, the response time is 2 hours, adjoint during reaction Mechanical agitation.
Step 3) in expand quality is poly (lactic acid-glycolic acid) intermediate product quality the 0.8% of even agent MDI.
Step 3) in the adding method of chain extender, be chain extender to be dissolved in solvent injection add, in mixed process, solvent Discharged by vacuum system.
Further, the described hollow silica sub-micron ball preparation method loading medicine is: by hollow silica Sub-micron ball is immersed in the aqueous solution of water soluble drug, stirs 1 day~4 days, be then 4 DEG C in temperature at temperature is 4 DEG C Lower centrifugal, clean gained solid product, lyophilization with deionized water, obtain being loaded with the hollow silica of water soluble drug Sub-micron ball;Or hollow silica sub-micron ball is immersed in the organic solvent of fat-soluble medicine, stir at temperature is 4 DEG C Mix 1 day~4 days, then centrifugal at temperature is 4 DEG C, clean gained solid product, lyophilization with deionized water, loaded The hollow silica sub-micron ball of fat-soluble medicine.
Further, described curative drug selected from neomycin, ribostamycin, micronomicin, A Si mycin, tetracycline, Oxytetracycline, chlortetracycline, doxycycline, chloromycetin, thiamphenicol, erythromycin, albomycin, erythromycin ethylsuccinate, azithromycin, acetyl Spiramycin, midecamycin, josamycin, lincomycin, clindamycin, vancomycin, bacitracin, polymyxin, phosphorus are mould Element, ciramycin, cycloserine, griseofulvin, mitomycin, bleomycin, ciclosporin, metronidazole, penicillin, penicillin sodium, One in benzylpenicillin potassium, ampicillin, amoxicillin, piperacillin, benzylpenicillin potassium or more than more than one;Or selected from upper State the one in the derivant of curative drug or more than more than one;Or selected from above-mentioned curative drug and above-mentioned therapeutic medicine A kind of in the derivant of thing or more than more than one mixture.
Embodiment 4
The preparation method of a kind of degradable medicine carrying poly (lactic acid-glycolic acid) operation suture thread, will load the hollow titanium dioxide of medicine Silicon sub-micron ball is dispersed in the aqueous solution of degradable poly y, by using spinning process will to load the hollow of medicine Silicon dioxide sub-micron sphere is embedded in degradable poly y fiber makes the operation of degradable medicine carrying poly (lactic acid-glycolic acid) Stitching thread operation suture thread;
The preparation process of described degradable poly y includes:
1) it is raw material by technical grade lactic acid aqueous solution and glycolic, carries out dehydration under vacuum refined, obtain lactic acid Glycolic acid oligomer;
2) by step 1) the y oligomer that obtains mixes with catalyst, adds in reaction vessel, at vacuum bar Under part, reacting by heating, obtain poly (lactic acid-glycolic acid) intermediate product;
3) in step 2) in reaction vessel in add chain extender MDI, under vacuum, reacting by heating, obtain high score Son amount poly (lactic acid-glycolic acid).
Step 1) in vacuum be 2.2kPa, dewatering time is 6 hours, dehydration temperaturre scope 80 DEG C, described lactic acid with The mol ratio of glycolic is 1:2.
Step 2) in vacuum be 1.2kPa, range of reaction temperature 160 DEG C, the response time is 4 hours, adjoint during reaction Mechanical agitation.
Step 2) in catalyst be in stannous chloride, stannous octoate, p-methyl benzenesulfonic acid two or three mixture, Its gross mass is the 1% of y oligomer quality.
Step 3) in vacuum be 1.5kPa, range of reaction temperature 150 DEG C, the response time is 2 hours, adjoint during reaction Mechanical agitation.
Step 3) in expand quality is poly (lactic acid-glycolic acid) intermediate product quality the 0.7% of even agent MDI.
Step 3) in the adding method of chain extender, be to be directly added into reaction system, after melting mixing, then occur chain extension anti- Should.
Further, the described hollow silica sub-micron ball preparation method loading medicine is: by hollow silica Sub-micron ball is immersed in the aqueous solution of water soluble drug, stirs 1 day~4 days, be then 4 DEG C in temperature at temperature is 4 DEG C Lower centrifugal, clean gained solid product, lyophilization with deionized water, obtain being loaded with the hollow silica of water soluble drug Sub-micron ball;Or hollow silica sub-micron ball is immersed in the organic solvent of fat-soluble medicine, stir at temperature is 4 DEG C Mix 1 day~4 days, then centrifugal at temperature is 4 DEG C, clean gained solid product, lyophilization with deionized water, loaded The hollow silica sub-micron ball of fat-soluble medicine.
Further, described curative drug selected from neomycin, ribostamycin, micronomicin, A Si mycin, tetracycline, Oxytetracycline, chlortetracycline, doxycycline, chloromycetin, thiamphenicol, erythromycin, albomycin, erythromycin ethylsuccinate, azithromycin, acetyl Spiramycin, midecamycin, josamycin, lincomycin, clindamycin, vancomycin, bacitracin, polymyxin, phosphorus are mould Element, ciramycin, cycloserine, griseofulvin, mitomycin, bleomycin, ciclosporin, metronidazole, penicillin, penicillin sodium, One in benzylpenicillin potassium, ampicillin, amoxicillin, piperacillin, benzylpenicillin potassium or more than more than one;Or selected from upper State the one in the derivant of curative drug or more than more than one;Or selected from above-mentioned curative drug and above-mentioned therapeutic medicine A kind of in the derivant of thing or more than more than one mixture.
Comparative example 1
Commercially available poly (lactic acid-glycolic acid) operation suture thread.
Respectively the sample 1-4 obtained in embodiment 1-4 is carried out the test of molecular weight, hot strength and degradation property, its Data see table:
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all spirit in the present invention and Within principle, any modification, equivalent substitution and improvement etc. made, should be included within the scope of the present invention.

Claims (10)

1. the preparation method of a degradable medicine carrying poly (lactic acid-glycolic acid) operation suture thread, it is characterised in that medicine will be loaded Hollow silica sub-micron ball is dispersed in the aqueous solution of degradable poly y, by using spinning process to load The hollow silica sub-micron ball of medicine is embedded in degradable poly y fiber makes degradable medicine carrying polylactic acid Glycolic operation suture thread operation suture thread;
The preparation process of described degradable poly y includes:
1) it is raw material by technical grade lactic acid aqueous solution and glycolic, carries out dehydration under vacuum refined, obtain lactic acid ethanol Acid oligomer;
2) by step 1) the y oligomer that obtains mixes with catalyst, adds in reaction vessel, under vacuum, Reacting by heating, obtains poly (lactic acid-glycolic acid) intermediate product;
3) in step 2) in reaction vessel in add chain extender MDI, under vacuum, reacting by heating, obtain high molecular Poly (lactic acid-glycolic acid).
A kind of preparation method of degradable medicine carrying poly (lactic acid-glycolic acid) operation suture thread, its feature Be, step 1) in vacuum be 2-4kPa, dewatering time is 0.5-10 hour, and dehydration temperaturre scope 45-100 DEG C is described Lactic acid is 1:1-3 with the mol ratio of glycolic.
A kind of preparation method of degradable medicine carrying poly (lactic acid-glycolic acid) operation suture thread, its feature Be, step 2) in vacuum be 0.5-2kPa, range of reaction temperature 150-180 DEG C, the response time is 2-5 hour, reaction Time with mechanical agitation.
The preparation method of a kind of degradable medicine carrying poly (lactic acid-glycolic acid) operation suture thread the most according to claim 3, it is special Levy and be, step 2) in catalyst be in stannous chloride, stannous octoate, p-methyl benzenesulfonic acid two or three mixture, Its gross mass is the 0.5%~1% of y oligomer quality.
A kind of preparation method of degradable medicine carrying poly (lactic acid-glycolic acid) operation suture thread, its feature Be, step 3) in vacuum be 1-3kPa, range of reaction temperature 130-160 DEG C, the response time is 1-4 hour, during reaction With mechanical agitation.
A kind of preparation method of degradable medicine carrying poly (lactic acid-glycolic acid) operation suture thread, its feature Be, step 3) in the 0.5%-1.3% that quality is poly (lactic acid-glycolic acid) intermediate product quality expanding even agent MDI.
7. according to the preparation method of the arbitrary described a kind of degradable medicine carrying poly (lactic acid-glycolic acid) operation suture thread of claim 1-6, It is characterized in that, step 3) in the adding method of chain extender, be to be directly added into reaction system, after melting mixing, then chain extension occur Reaction.
8. according to the preparation method of the arbitrary described a kind of degradable medicine carrying poly (lactic acid-glycolic acid) operation suture thread of claim 1-6, It is characterized in that, step 3) in the adding method of chain extender, be chain extender to be dissolved in solvent injection add, in mixed process, Solvent is discharged by vacuum system.
9., according to the preparation method of degradable medicine carrying poly (lactic acid-glycolic acid) operation suture thread a kind of described in claim 7 or 8, it is special Levying and be, the described hollow silica sub-micron ball preparation method loading medicine is: by hollow silica sub-micron ball It is immersed in the aqueous solution of water soluble drug, stirs at temperature is 4 DEG C 1 day~4 days, then centrifugal at temperature is 4 DEG C, use Deionized water cleans gained solid product, lyophilization, obtains being loaded with the hollow silica sub-micron ball of water soluble drug; Or hollow silica sub-micron ball is immersed in the organic solvent of fat-soluble medicine, stir 1 day~4 at temperature is 4 DEG C My god, then centrifugal at temperature is 4 DEG C, clean gained solid product, lyophilization with deionized water, obtain being loaded with fat-soluble The hollow silica sub-micron ball of medicine.
10. according to the preparation method of degradable medicine carrying poly (lactic acid-glycolic acid) operation suture thread a kind of described in claim 7 or 8, its Be characterised by, described curative drug selected from neomycin, ribostamycin, micronomicin, A Si mycin, tetracycline, oxytetracycline, Chlortetracycline, doxycycline, chloromycetin, thiamphenicol, erythromycin, albomycin, erythromycin ethylsuccinate, azithromycin, acetyl spiral are mould Element, midecamycin, josamycin, lincomycin, clindamycin, vancomycin, bacitracin, polymyxin, fosfomycin, volume are mould Element, cycloserine, griseofulvin, mitomycin, bleomycin, ciclosporin, metronidazole, penicillin, penicillin sodium, penicillin One in potassium, ampicillin, amoxicillin, piperacillin, benzylpenicillin potassium or more than more than one;Or selected from above-mentioned treatment Property medicine derivant in one or more than more than one;Or spreading out selected from above-mentioned curative drug and above-mentioned curative drug A kind of in biology or more than more than one mixture.
CN201610743094.0A 2016-08-27 2016-08-27 A kind of preparation method of degradable medicine carrying poly (lactic acid-glycolic acid) operation suture thread Pending CN106267323A (en)

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CN1624019A (en) * 2004-10-25 2005-06-08 安徽中人科技有限责任公司 Method for preparing poly (L-lactic acid-glycollic acid)
CN101721739A (en) * 2008-10-10 2010-06-09 陈东 Polymer composite fiber surgical suture line capable of sustaining and controlling release of therapeutic medicaments and preparation method thereof
CN103254411A (en) * 2013-06-07 2013-08-21 北京理工大学 Method for preparing high-molecular-weight polylactic acid through direct polycondensation and chain extension

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CN1624019A (en) * 2004-10-25 2005-06-08 安徽中人科技有限责任公司 Method for preparing poly (L-lactic acid-glycollic acid)
CN101721739A (en) * 2008-10-10 2010-06-09 陈东 Polymer composite fiber surgical suture line capable of sustaining and controlling release of therapeutic medicaments and preparation method thereof
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