CN109395150A - A kind of degradability medical haemostatic material and preparation method thereof - Google Patents

A kind of degradability medical haemostatic material and preparation method thereof Download PDF

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Publication number
CN109395150A
CN109395150A CN201811253016.8A CN201811253016A CN109395150A CN 109395150 A CN109395150 A CN 109395150A CN 201811253016 A CN201811253016 A CN 201811253016A CN 109395150 A CN109395150 A CN 109395150A
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solution
preparation
parts
gelatin
chitosan
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Inventor
邓连华
曹仁广
张金秋
张植民
朱波涛
肖其柏
肖荣方
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Hengtian Nonwoven Co Ltd Ka Wah
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Hengtian Nonwoven Co Ltd Ka Wah
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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
    • A61L24/00—Surgical adhesives or cements; Adhesives for colostomy devices
    • A61L24/04—Surgical adhesives or cements; Adhesives for colostomy devices containing macromolecular materials
    • A61L24/06—Surgical adhesives or cements; Adhesives for colostomy devices containing macromolecular materials obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • 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
    • A61L24/00—Surgical adhesives or cements; Adhesives for colostomy devices
    • A61L24/001—Use of materials characterised by their function or physical properties
    • A61L24/0015—Medicaments; Biocides
    • 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
    • A61L24/00—Surgical adhesives or cements; Adhesives for colostomy devices
    • A61L24/001—Use of materials characterised by their function or physical properties
    • A61L24/0042—Materials resorbable by the body
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L24/00—Surgical adhesives or cements; Adhesives for colostomy devices
    • A61L24/04—Surgical adhesives or cements; Adhesives for colostomy devices containing macromolecular materials
    • A61L24/08—Polysaccharides
    • 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
    • A61L24/00—Surgical adhesives or cements; Adhesives for colostomy devices
    • A61L24/04—Surgical adhesives or cements; Adhesives for colostomy devices containing macromolecular materials
    • A61L24/10—Polypeptides; Proteins
    • A61L24/104—Gelatin
    • 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
    • D01F8/02—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from cellulose, cellulose derivatives, or proteins
    • 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
    • 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
    • D01F8/16—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one other macromolecular compound obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds as constituent
    • 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
    • D01F8/18—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from other substances
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/322—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
    • D06M13/402—Amides imides, sulfamic acids
    • D06M13/438—Sulfonamides ; Sulfamic acids
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M16/00—Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
    • 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
    • A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
    • A61L2300/10—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing inorganic materials
    • A61L2300/102—Metals or metal compounds, e.g. salts such as bicarbonates, carbonates, oxides, zeolites, silicates
    • A61L2300/104—Silver, e.g. silver sulfadiazine
    • 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
    • A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
    • A61L2300/40—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a specific therapeutic activity or mode of action
    • A61L2300/404—Biocides, antimicrobial agents, antiseptic agents
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L2400/00—Materials characterised by their function or physical properties
    • A61L2400/04—Materials for stopping bleeding
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/02—Natural fibres, other than mineral fibres
    • D06M2101/10—Animal fibres
    • D06M2101/12—Keratin fibres or silk
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/16—Synthetic fibres, other than mineral fibres
    • D06M2101/18—Synthetic fibres consisting of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M2101/24—Polymers or copolymers of alkenylalcohols or esters thereof; Polymers or copolymers of alkenylethers, acetals or ketones
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/16—Synthetic fibres, other than mineral fibres
    • D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M2101/32—Polyesters

Abstract

The invention discloses a kind of preparation method of degradability medical haemostatic material, include the following steps: that (1) mixes polyethylene glycol, hyaluronic acid and deionized water according to a certain volume；(2) solution of step (1) is divided into identical three parts, then gelatin, polylactic acid, chitosan is added in three parts of solvents respectively, stirred, be stirred for after later mixing three parts of solution, ultrasound；(3) gelatin/polylactic acid/chitosan composite ultrafine fiber, vacuum drying is made by electrostatic spinning in the mixed solution for obtaining step (2)；(4) step (3) resulting superfine fibre is added in the solution of silver sulfadiazine and is impregnated, is freeze-dried later, finally in heating platen hot pressing up to the degradability medical haemostatic material.The used raw material of hemostatic material of the present invention is good biocompatibility, biodegradable harmless material, has good bioadhesive, can be good at controlling persistently bleeding for tissue, hemostatic capability is very strong.

Description

A kind of degradability medical haemostatic material and preparation method thereof
Technical field
The invention belongs to medical material tech fields, and in particular to a kind of degradability medical haemostatic material and its preparation side Method.
Background technique
Bio-medical material is a kind of new and high technology material to grow up in the late three decades, wherein hemostatic material also with The accidents such as traffic accident, serious burn and scald and disaster increase the concern for gradually causing medical field.With modern section The high speed development of technology, the research of hemostatic material achieve very fast progress, and various novel hemostatic materials continuously emerge, property Very big promotion can also have been obtained.Currently, common topical hemostatic agent has Fibrin Glue, thrombin powder, gelfoam, collagen Protein sponge, chitosan sponge, oxycellulose, microfibrillar collagen, alginic acid fibre, zeolite, cyanoacrylate vinegar ester, plant Polysaccharide powder etc..Haemostatic effect is definite, easy to use, good biocompatibility, the bio-medical hemostatic material that can control degradation rate The main object paid close attention to and studied as people.
Gelatin is to become white or light by the collagenous portion degradation in the connective tissues such as animal skin, bone, sarolemma, flesh evil spirit Yellow, a kind of translucent, micro-strip gloss colorless and odorless, non-volatility, transparent hard non-crystalline material.Gelatin is as a kind of Natural water-soluble Biodegradable polymer material, advantage be exactly catabolite be easily absorbed without generate inflammation it is anti- It answers.Due to this property, it is usually applied to biomedicine field.Dong Yinsheng in 2016 et al. discloses a kind of containing polyethylene Alcohol-gelatin-carboxyl chitosan composite sponge and preparation method thereof (CN201610803838.3), two used are big, and main material is equal For natural biologic material, the chitosan used for carboxyl chitosan, it is convenient that prepare by solution, does not use the weak acid such as acetic acid, hydrochloric acid, The substance that can cause skin allergy or inflammatory reaction will not be remained.But its crosslinking agent selects glutaraldehyde, has toxicity to human body, deposits In some potential safety problems.Sodium alginate is aoxidized using sodium metaperiodate, makes the hydroxyl of sodium alginate part uronic acid unit Base is transformed into aldehyde radical, can not only improve the solubility property of sodium alginate, the aldehyde radical on simultaneous oxidation sodium alginate can with it is bright Schiff reaction occurs for the amino on glue, forms chemical crosslinking structure.
Electrostatic spinning technique is that one kind can prepare diameter continuously, quickly as l0um-l0nm fiber.It is fine with traditional spinning Dimension is compared, and electrospinning fibre has high-specific surface area, and there is also nanoscale hole holes on many fibers, and porosity is very high, because This filtering material, tissue engineering bracket material field show broad application prospect.Gelatin is soluble in 40 DEG C or more of water shape At aqueous solution, the gelatin fiber being relatively large in diameter can be made in this aqueous solution of wet spinning, for bleeding profusely.But it is single Major diameter gelatin fiber there is also certain defects: if porosity, specific surface area are too small, fibre-forming performance is poor, fibre diameter point Cloth range is wide, the mechanical property of fiber not enough etc., these defects also affect to a certain extent gelatin hemostatic material only Hemorrhagic energy, urgent need are improved.
Summary of the invention
In order to overcome the drawbacks of the prior art, the purpose of the present invention is to provide one kind to have excellent performance, haemostatic effect is obvious Gelatin-compounded hemostatic material and preparation method thereof.
To achieve the above object, the technical solution used in the present invention are as follows:
A kind of preparation method of degradability medical haemostatic material, includes the following steps:
(1) preparation of mixed solvent: by polyethylene glycol, hyaluronic acid and deionized water 1-3:2-5:10-20 by volume It is mixed；
(2) solution of step (1) is divided into identical three parts, is then respectively added to gelatin, polylactic acid, chitosan In three parts of solvents, and 35-45 DEG C at a temperature of stir 2-4 hours respectively, later will three parts of solution mix after be stirred for, surpass Sound 1-2 hours；
(3) gelatin/polylactic acid/chitosan composite superfine is made by electrostatic spinning in the mixed solution for obtaining step (2) Fiber is dried in vacuo 12 hours in 60-90 DEG C, spare；
(4) step (3) resulting superfine fibre is added in the solution of silver sulfadiazine and impregnates 1-5 hours, later Freeze-drying, finally in heating platen hot pressing 20-40min up to the degradability medical haemostatic material.
Preferably, in step (2) in three parts of solution the mass concentration of gelatin, polylactic acid and chitosan be respectively 5-10%, 0.5-1.5%, 0.5-1%.
Preferably, the injection rate of electrostatic spinning is 50-80 μ L/min, voltage 20-24KV, spinning nozzle in step (3) Electrospinning is carried out away from receiving device 15-25cm.
Preferably, the solution of the silver sulfadiazine is that silver sulfadiazine is added in glycerol to be configured to solution, Wherein the mass fraction of silver sulfadiazine is 0.1-2%.
Preferably, the temperature being freeze-dried in step (4) is -20 to -5 DEG C, and the vacuum degree of freeze-drying is 100- 300Pa, dry time are 12h.
Preferably, the hot pressing temperature in step (4) is 35-50 DEG C.
In addition, the degradability medical haemostatic material that the method is prepared is also claimed in the present invention, wherein described Hemostatic material is 40-60nm, length 0.5-2mm, specific surface area 40-60m in threadiness, the diameter of fiber2/ g, porosity Reach 90% or more.
Compared with prior art, the invention has the benefit that
(1) present invention using polyethylene glycol, hyaluronic acid and deionized water double solvents replace aqueous solvent, mainly because The dissolubility of gelatin, polylactic acid and chitosan in water can be improved in addition for polyethylene glycol and hyaluronic acid, is effectively improved The spinnability of mixed solution, conducive to superfine fiber is formed, to obtain the gelatin-compounded hemostatic material haveing excellent performance；
(2) present invention is modified gelatin using a small amount of polylactic acid and chitosan, can enhance to a certain extent bright The adhesive of glue and biological tissue, is bonded conducive to it with tissue, quick-acting haemostatic powder, and another aspect chitosan can effectively change The anthemorrhagic speed of kind gelatin, polylactic acid can improve the mechanical performance of gelatin to a certain extent, improve in comprehensive performance The anthemorrhagic performance of gelatin；
(3) present invention has the silver sulfadiazine of excellent antibacterial performance on fiber on dipping, effectively increases hemostasis The antibiotic property of material avoids the infection of the germ in hemostasis；
(4) the used raw material of hemostatic material of the present invention is good biocompatibility, biodegradable harmless material, is had Good bioadhesive can be good at controlling persistently bleeding for tissue, and hemostatic capability is very strong.
Specific embodiment
Attached drawing 1 be the degradability medical haemostatic material of the present embodiment microscope under schematic diagram.
Specific embodiment
The technical scheme in the embodiments of the invention will be clearly and completely described below, it is clear that described implementation Example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common Technical staff's every other embodiment obtained without making creative work belongs to the model that the present invention protects It encloses.
Embodiment 1
A kind of preparation method of degradability medical haemostatic material, includes the following steps:
(1) preparation of mixed solvent: by polyethylene glycol, hyaluronic acid and deionized water, 1:2:10 is mixed by volume It closes；
(2) solution of step (1) is divided into identical three parts, is then respectively added to gelatin, polylactic acid, chitosan In three parts of solvents, and 40 DEG C at a temperature of stir 3 hours respectively, later will three parts of solution mix after be stirred for, ultrasound 1.5 Hour；Wherein, the mass concentration of gelatin, polylactic acid and chitosan is respectively 8%, 1%, 0.5% in three parts of solution；
(3) gelatin/polylactic acid/chitosan composite superfine is made by electrostatic spinning in the mixed solution for obtaining step (2) Fiber is dried in vacuo 12 hours in 80 DEG C, spare；The injection rate of electrostatic spinning is 60 μ L/min, voltage 22KV, spinning nozzle Electrospinning is carried out away from receiving device 20cm；
(4) step (3) resulting superfine fibre is added in the flamazine salting liquid that mass fraction is 0.8% and is soaked Bubble 2 hours, later -10 DEG C of freeze-drying 12h, finally in heating platen hot pressing 30min up to the degradability medical haemostatic Material.
Embodiment 2
A kind of preparation method of degradability medical haemostatic material, includes the following steps:
(1) preparation of mixed solvent: by polyethylene glycol, hyaluronic acid and deionized water, 2:5:15 is mixed by volume It closes；
(2) solution of step (1) is divided into identical three parts, is then respectively added to gelatin, polylactic acid, chitosan In three parts of solvents, and 40 DEG C at a temperature of stir 3 hours respectively, later will three parts of solution mix after be stirred for, ultrasound 1.5 Hour；Wherein, the mass concentration of gelatin, polylactic acid and chitosan is respectively 7%, 1%, 0.5% in three parts of solution；
(3) gelatin/polylactic acid/chitosan composite superfine is made by electrostatic spinning in the mixed solution for obtaining step (2) Fiber is dried in vacuo 12 hours in 80 DEG C, spare；The injection rate of electrostatic spinning is 60 μ L/min, voltage 22KV, spinning nozzle Electrospinning is carried out away from receiving device 20cm；
(4) step (3) resulting superfine fibre is added in the flamazine salting liquid that mass fraction is 0.7% and is soaked Bubble 2 hours, later -10 DEG C of freeze-drying 12h, finally in heating platen hot pressing 30min up to the degradability medical haemostatic Material.
Embodiment 3
A kind of preparation method of degradability medical haemostatic material, includes the following steps:
(1) preparation of mixed solvent: by polyethylene glycol, hyaluronic acid and deionized water, 1:4:12 is mixed by volume It closes；
(2) solution of step (1) is divided into identical three parts, is then respectively added to gelatin, polylactic acid, chitosan In three parts of solvents, and 40 DEG C at a temperature of stir 3 hours respectively, later will three parts of solution mix after be stirred for, ultrasound 1.5 Hour；Wherein, the mass concentration of gelatin, polylactic acid and chitosan is respectively 10%, 1%, 0.5% in three parts of solution；
(3) gelatin/polylactic acid/chitosan composite superfine is made by electrostatic spinning in the mixed solution for obtaining step (2) Fiber is dried in vacuo 12 hours in 80 DEG C, spare；The injection rate of electrostatic spinning is 80 μ L/min, voltage 22KV, spinning nozzle Electrospinning is carried out away from receiving device 20cm；
(4) step (3) resulting superfine fibre is added in the flamazine salting liquid that mass fraction is 1% and is impregnated 2 hours, later -10 DEG C of freeze-drying 12h, finally in heating platen hot pressing 30min up to the degradability medical haemostatic material Material.
Embodiment 4
A kind of preparation method of degradability medical haemostatic material, includes the following steps:
(1) preparation of mixed solvent: by polyethylene glycol, hyaluronic acid and deionized water, 1:5:15 is mixed by volume It closes；
(2) solution of step (1) is divided into identical three parts, is then respectively added to gelatin, polylactic acid, chitosan In three parts of solvents, and 40 DEG C at a temperature of stir 3 hours respectively, later will three parts of solution mix after be stirred for, ultrasound 1.5 Hour；Wherein, the mass concentration of gelatin, polylactic acid and chitosan is respectively 6%, 0.5%, 0.5% in three parts of solution；
(3) gelatin/polylactic acid/chitosan composite superfine is made by electrostatic spinning in the mixed solution for obtaining step (2) Fiber is dried in vacuo 12 hours in 80 DEG C, spare；The injection rate of electrostatic spinning is 60 μ L/min, voltage 22KV, spinning nozzle Electrospinning is carried out away from receiving device 20cm；
(4) step (3) resulting superfine fibre is added in the flamazine salting liquid that mass fraction is 1.2% and is soaked Bubble 2 hours, later -10 DEG C of freeze-drying 12h, finally in heating platen hot pressing 30min up to the degradability medical haemostatic Material.
Embodiment 5
A kind of preparation method of degradability medical haemostatic material, includes the following steps:
(1) preparation of mixed solvent: by polyethylene glycol, hyaluronic acid and deionized water, 1:3:11 is mixed by volume It closes；
(2) solution of step (1) is divided into identical three parts, is then respectively added to gelatin, polylactic acid, chitosan In three parts of solvents, and 40 DEG C at a temperature of stir 3 hours respectively, later will three parts of solution mix after be stirred for, ultrasound 1.5 Hour；Wherein, the mass concentration of gelatin, polylactic acid and chitosan is respectively 9%, 1.5%, 0.5% in three parts of solution；
(3) gelatin/polylactic acid/chitosan composite superfine is made by electrostatic spinning in the mixed solution for obtaining step (2) Fiber is dried in vacuo 12 hours in 80 DEG C, spare；The injection rate of electrostatic spinning is 60 μ L/min, voltage 22KV, spinning nozzle Electrospinning is carried out away from receiving device 20cm；
(4) step (3) resulting superfine fibre is added in the flamazine salting liquid that mass fraction is 1% and is impregnated 2 hours, later -10 DEG C of freeze-drying 12h, finally in heating platen hot pressing 30min up to the degradability medical haemostatic material Material.
Comparative example 1
A kind of preparation method of degradability medical haemostatic material, includes the following steps:
(1) preparation of mixed solvent: by polyethylene glycol and deionized water, 1:10 is mixed by volume；
(2) solution of step (1) is divided into identical three parts, is then respectively added to gelatin, polylactic acid, chitosan In three parts of solvents, and 40 DEG C at a temperature of stir 3 hours respectively, later will three parts of solution mix after be stirred for, ultrasound 1.5 Hour；Wherein, the mass concentration of gelatin, polylactic acid and chitosan is respectively 8%, 1%, 0.5% in three parts of solution；
(3) gelatin/polylactic acid/chitosan composite superfine is made by electrostatic spinning in the mixed solution for obtaining step (2) Fiber is dried in vacuo 12 hours in 80 DEG C, spare；The injection rate of electrostatic spinning is 60 μ L/min, voltage 22KV, spinning nozzle Electrospinning is carried out away from receiving device 20cm；
(4) step (3) resulting superfine fibre is added in the flamazine salting liquid that mass fraction is 0.8% and is soaked Bubble 2 hours, later -10 DEG C of freeze-drying 12h, finally in heating platen hot pressing 30min up to the degradability medical haemostatic Material.
Comparative example 2
A kind of preparation method of degradability medical haemostatic material, includes the following steps:
(1) preparation of mixed solvent: by polyethylene glycol, hyaluronic acid and deionized water, 1:2:10 is mixed by volume It closes；
(2) solution of step (1) is divided into identical two parts, then respectively by gelatin, chitosan be added to two parts it is molten In agent, and 40 DEG C at a temperature of stir 3 hours respectively, later will two parts of solution mix after be stirred for, ultrasound 1.5 hours；Its In, gelatin in two parts of solution, chitosan mass concentration be respectively 8%, 0.5%；
(3) gelatin/polylactic acid/chitosan composite superfine is made by electrostatic spinning in the mixed solution for obtaining step (2) Fiber is dried in vacuo 12 hours in 80 DEG C, spare；The injection rate of electrostatic spinning is 60 μ L/min, voltage 22KV, spinning nozzle Electrospinning is carried out away from receiving device 20cm；
(4) step (3) resulting superfine fibre is added in the flamazine salting liquid that mass fraction is 0.8% and is soaked Bubble 2 hours, later -10 DEG C of freeze-drying 12h, finally in heating platen hot pressing 30min up to the degradability medical haemostatic Material.
The performance of embodiment 1 and comparative example 1-2 material prepared is measured:
(1) measurement method method: taking the material of same size embodiment 1 and comparative example 1-2, observes it and absorbs at room temperature The multiple of pure water；
(2) diameter, the specific surface area, porosity of embodiment 1 and comparative example 1-2 material prepared are measured；
Measurement result such as the following table 1:
(3) clotting index measures:
It extracts rabbit new blood and to be added appropriate anti-coagulants stand-by, embodiment 1 and comparative example 1-2 material are cut into 0.5cm2It lies in beaker, is put into constant temperature 5min in 37 DEG C of water-bath, the blood of 0.1mL is added drop-wise on sample, then 0.02mLCaCl is added dropwise immediately2Solution starts coagulation process, and 37 DEG C of constant temperature of 25mL deionized water are added after 5min and wave 5min, with Removal solution surveys its Abs value in wavelength with ultraviolet specrophotometer at 415nm afterwards.0.1mL blood is diluted with deionized water Abs value after 25mL makees reference value, and clotting index is calculated as follows: BC=100 × Abs sample/Abs reference.
Clotting index
Embodiment 1 20.5
Comparative example 1 34.1
Comparative example 2 32.9
(4) hemostasis experiment:
New Zealand White Rabbit auricular vein injects 3% yellow Jackets 30mg/kg, after anaesthetizing successfully, successively opens abdomen, exposure liver It is dirty.Make lcm × lcm × 0.5cm bleeding surface of a wound on liver surface, respectively by the hemostasis of the embodiment 1 of suitable size and comparative example 1-2 Material is placed in wound, is pressurizeed on hemostatic material with 50g counterweight, a bleeding is observed every 30s, after removing counterweight L0min no longer bleeding is " hemostasis ", records bleeding stopping period.The quality of hemostatic material before and after being stopped blooding with assay balance accurate weighing, Calculate amount of bleeding.Amount of bleeding (ml)=(weight before weight-hemostasis after hemostasis)/blood specific gravity (1.050g/ml).Calculate bleeding Amount.
n Bleeding stopping period (s) Amount of bleeding (ml)
Embodiment 1 5 32 0.64
Comparative example 1 5 59 1.15
Comparative example 2 5 53 1.01
(5) fungistatic effect measures:
The hemostatic material and existing PVA styptic sponge of embodiment 1 and comparative example 1-2 are subjected to bacteriostasis rate experiment, wherein pressing down Escherichia coli+staphylococcus aureus that bacterium rate uses this field common uses normal condition with medical film to observe object Bag, which is padded in container, carries out Bacteria Culture experiment, and compare its bacteriostasis property.Test result see the table below:
Bacteriostasis rate (incubation time 48h)
Embodiment 1 99.5%
Comparative example 1 99.2%
Comparative example 2 99.3%
Existing PVA styptic sponge 36.4%
It is obvious to a person skilled in the art that invention is not limited to the details of the above exemplary embodiments, Er Qie In the case where without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter From the point of view of which point, the present embodiments are to be considered as illustrative and not restrictive, and the scope of the present invention is by appended power Benefit requires rather than above description limits, it is intended that all by what is fallen within the meaning and scope of the equivalent elements of the claims Variation is included within the present invention.
In addition, it should be understood that although this specification is described in terms of embodiments, but not each embodiment is only wrapped Containing an independent technical solution, this description of the specification is merely for the sake of clarity, and those skilled in the art should It considers the specification as a whole, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art The other embodiments being understood that.

Claims (7)

1. a kind of preparation method of degradability medical haemostatic material, which comprises the steps of:
(1) preparation of mixed solvent: by polyethylene glycol, hyaluronic acid and deionized water, 1-3:2-5:10-20 is carried out by volume Mixing；
(2) solution of step (1) is divided into identical three parts, gelatin, polylactic acid, chitosan is then added to three parts respectively In solvent, and 35-45 DEG C at a temperature of stir 2-4 hours respectively, later will three parts of solution mix after be stirred for, ultrasound 1-2 Hour；
(3) gelatin/polylactic acid/chitosan composite ultrafine fiber is made by electrostatic spinning in the mixed solution for obtaining step (2), It is dried in vacuo 12 hours in 60-90 DEG C, it is spare；
(4) step (3) resulting superfine fibre is added in the solution of silver sulfadiazine and is impregnated 1-5 hours, freezed later It is dry, finally in heating platen hot pressing 20-40min up to the degradability medical haemostatic material.
2. preparation method according to claim 1, which is characterized in that gelatin in three parts of solution in step (2), polylactic acid and The mass concentration of chitosan is respectively 5-10%, 0.5-1.5%, 0.5-1%.
3. -2 described in any item preparation methods according to claim 1, which is characterized in that the injection of electrostatic spinning in step (3) Rate is about 50-80 μ L/min, and voltage 20-24KV, spinning nozzle is away from receiving device 15-25cm progress electrospinning.
4. preparation method according to claim 3, which is characterized in that the solution of the silver sulfadiazine is that sulfanilamide (SN) is phonetic Pyridine silver salt, which is added in glycerol, is configured to solution, and wherein the mass fraction of silver sulfadiazine is 0.1-2%.
5. the preparation method according to claim 4, which is characterized in that the temperature being freeze-dried in step (4) is -20 to -5 DEG C, the vacuum degree of freeze-drying is 100-300Pa, and the dry time is 12h.
6. preparation method according to claim 5, which is characterized in that the hot pressing temperature in step (4) is 35-50 DEG C.
7. the degradability medical haemostatic material that a kind of any one of claim 1-6 the method is prepared, which is characterized in that The hemostatic material is 40-60nm, length 0.5-2mm, specific surface area 40-60m in threadiness, the diameter of fiber2/ g, hole Gap rate reaches 90% or more.
CN201811253016.8A 2018-10-25 2018-10-25 A kind of degradability medical haemostatic material and preparation method thereof Pending CN109395150A (en)

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