CN106267328A - A kind of preparation method of polycaprolactone abortive calfskin collagen fiber compound hemostatic gel - Google Patents
A kind of preparation method of polycaprolactone abortive calfskin collagen fiber compound hemostatic gel Download PDFInfo
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- CN106267328A CN106267328A CN201610835998.6A CN201610835998A CN106267328A CN 106267328 A CN106267328 A CN 106267328A CN 201610835998 A CN201610835998 A CN 201610835998A CN 106267328 A CN106267328 A CN 106267328A
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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
- A61L24/10—Polypeptides; Proteins
- A61L24/102—Collagen
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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
- A61L24/001—Use of materials characterised by their function or physical properties
- A61L24/0015—Medicaments; Biocides
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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
- A61L24/001—Use of materials characterised by their function or physical properties
- A61L24/0031—Hydrogels or hydrocolloids
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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
- A61L24/001—Use of materials characterised by their function or physical properties
- A61L24/0042—Materials resorbable by the body
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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
- A61L24/046—Surgical adhesives or cements; Adhesives for colostomy devices containing macromolecular materials obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- 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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L89/00—Compositions of proteins; Compositions of derivatives thereof
- C08L89/04—Products derived from waste materials, e.g. horn, hoof or hair
- C08L89/06—Products derived from waste materials, e.g. horn, hoof or hair derived from leather or skin, e.g. gelatin
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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
- 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
- A61L2300/418—Agents promoting blood coagulation, blood-clotting agents, embolising agents
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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
- A61L2400/00—Materials characterised by their function or physical properties
- A61L2400/04—Materials for stopping bleeding
Abstract
The invention discloses the preparation method of a kind of polycaprolactone abortive calfskin collagen fiber compound hemostatic gel, relate to hemostasis gel technical field, comprise the steps: (1) abortive calfskin pretreatment, (2) preparation of collagen fiber Extraction solvent, (3) preparation of collagen fiber solution, (4) preparation of modified collagen fiber solution, the preparation of (5) hemostasis gel.Hemostasis gel of the present invention can directly overlie bleed site, plays haemostatic effect, and hemostasis is rapidly, promotes the reparation of wound surface while effectively reducing amount of bleeding；There is biocompatibility and the biological degradability of excellence simultaneously, safe to use, without any side effects after using.
Description
Technical field:
The present invention relates to hemostasis gel technical field, be specifically related to a kind of polycaprolactone-abortive calfskin collagen fiber compound only
The preparation method of blood clotting glue.
Background technology:
Often bleeding profusely along with wound surface in surgery and trauma operation, so that patient faces great life
Danger, therefore prepare fast and effectively hemostatic material always as the study hotspot of medical field.Traditional hemostatic material exists
The shortcoming that the most portable and sterilization preserves, and hemostasis is almost by mechanism, haemostatic effect is bad.In recent years, people develop
Biological absorbable hemostatic material, wherein Animal Skin Collagen sill is as the good medical material of a kind of biological property, with human body
There is good histocompatibility, biodegradable and have no side effect, the adhesion of cell, propagation and wound can be promoted simultaneously
Compound；And by its distinctive microcellular structure and good adhesiveness, promote the growth diffusion of biotic factor, induce and promote
Enter fibroblastic growth, thus promote the healing of wound.
At present, universal Animal Skin Collagen extracts preparation method and combines extraction method for acid enzyme, mainly includes the pre-place of raw material
Reason, defat, enzymolysis, digestion, saltout, the step such as centrifugal and purification, but there is gained collagen purity and productivity is low, high in cost of production
Problem, and collagen can be made to reduce or lose biomechanical property because dealing with improperly during extracting, thus only affect it
Blood effect.For this problem, our company starts with from the extracting method of collagen, and combines the modification extracting collagen
And the interpolation of auxiliary agent prepares hemostasis gel material, on the basis of low cost, improve haemostatic effect, biocompatibility, biological fall
Solution property and safety in utilization.
Summary of the invention:
The technical problem to be solved is that one is prepared simply, haemostatic effect is good and has superior bio in offer
The preparation method of the polycaprolactone-abortive calfskin collagen fiber compound hemostatic gel of the compatibility and biological degradability.
The technical problem to be solved uses following technical scheme to realize:
The preparation method of a kind of polycaprolactone-abortive calfskin collagen fiber compound hemostatic gel, comprises the steps:
(1) abortive calfskin pretreatment: with purification abortive calfskin of can tracing to the source as raw material, by its fully deployed after wrap up with preservative film
Good, it is placed in-5～0 DEG C of environment freezing 5～8h, then with temperature 5-10 DEG C, the sodium bicarbonate of mass fraction 5% and hexa metaphosphoric acid
Sodium mixed aqueous solution soaks 10～15min, then with sponge brush brushing surface 2～3 times under deionized water shower；
(2) preparation of collagen fiber Extraction solvent: according to the ratio of mol ratio 1.2～1.5:1 by Cyclopropyl Bromide and 2-pyrrole
Pyrrolidone is sufficiently mixed, prior to supersound process 15～30min under supersonic frequency 40kHz, power 50W, then at microwave frequency
Microwave treatment 3～5min under 2450MHz, power 700W, is then heated to reflux state insulated and stirred 30～60min, to be mixed
Solution naturally cools to 5-10 DEG C of deionized water of the weight such as addition after 50-55 DEG C, is sufficiently stirred for rear stratification, phase of fetching water,
Obtain Extraction solvent；
(3) preparation of collagen fiber solution: the abortive calfskin after above-mentioned scrubbing is sent in freezer dryer, is dried to aqueous
Amount, for utilizing onal machine to be ground into the granule that granularity is 2-3mm after 10-15%, adds in above-mentioned made Extraction solvent, fully
Stand 10～15min after dispersion, stand and proceed in ball mill after terminating, be milled to fineness and be less than 50 μm, be subsequently adding quality and divide
The PVP K30 of several 5% and castor oil hydrogenated polyoxyethylene ether mixed aqueous solution, utilize after being sufficiently mixed operating frequency 40Hz,
The Surface Treatment with Plasma machine of power 600W processes 10～15s to gained mixture, and process proceeds to after terminating in 0～5 DEG C of environment
Stand 3～5h, be subsequently added polyacrylic acid and polyethylene glycol oxide, and be heated to reflux state insulated and stirred 15～30min, finally
Crossing 270 mesh sieves, gained filtrate is collagen fiber solution；
(4) preparation of modified collagen fiber solution: add polycaprolactone, poly-second two in above-mentioned made collagen fiber solution
Alcohol 4000 and methionine, in 35～40 DEG C of sealing and standing 1～2h after being uniformly dispersed, be sufficiently mixed, then in microwave frequency
Under 2450MHz, power 700W, microwave treatment 2～3min, is sufficiently mixed again, and utilizes operating frequency 40Hz, power 600W
Surface Treatment with Plasma machine processes 10～15s, and gained mixture cools with the speed of 10～15 DEG C/min under ice-water bath,
Insulated and stirred 10～15min after temperature is down to 0～5 DEG C, obtain modified collagen fiber solution；
(5) preparation of hemostasis gel: in above-mentioned made modified collagen fiber solution add polyglycolic acid, Polycarbophil,
Cystine and haemostatic medicament, be sufficiently mixed after uniformly and be distributed in mould, and utilize gamma-rays sterilization, the most packaged after
Cryopreservation under the conditions of 0～5 DEG C.
In described step (1), sodium bicarbonate is 2～3:1 with the consumption mass ratio of sodium hexameta phosphate.
Abortive calfskin, Extraction solvent, PVP K30, castor oil hydrogenated polyoxyethylene ether, polyacrylic acid in described step (3)
Consumption mass ratio 10～15:40～50:2～3:1～2:0.5～1:0.5～1 with polyethylene glycol oxide.
Through chemical modification before in described step (3), polyacrylic acid uses, its method of modifying is: by polyacrylic acid and cheese ammonia
Acid adds in double weight part ethanol, the post-heating that is uniformly dispersed to reflux state insulated and stirred 10min, add resveratrol and
Disodiumedetate, continues at insulated and stirred 30min under reflux state, after gained mixture naturally cools to 35-40 DEG C
Proceeding to stand in 0-5 DEG C of environment 8h immediately, be then fed in spray dryer, dried gained solid is ground makes powder.
The consumption mass ratio of described polyacrylic acid, tyrosine, resveratrol and disodiumedetate is 10～15:1
～2:3～6:0.5～1.
The consumption mass ratio of collagen fiber solution, polycaprolactone, Macrogol 4000 and methionine in described step (4)
25～30:3～6:1～2:0.5～1.
Modified collagen fiber solution, polyglycolic acid, Polycarbophil, cystine and the use of haemostatic medicament in described step (5)
Amount mass ratio 25～30:2～3:1～2:0.5～1:0.5～1.
Described haemostatic medicament is selected from chemicals or the Chinese medicine extract with hemostasia effect.
The invention has the beneficial effects as follows: the present invention is with purification abortive calfskin of can tracing to the source as raw material, and it is molten that collagen fiber are prepared in extraction
Liquid, and utilize the collagen fiber that polycaprolactone graft modification extracted, and be aided with multiple auxiliary agent and prepare hemostasis gel, this hemostasis
Gel can directly overlie bleed site, plays haemostatic effect, and hemostasis is rapidly, promote wound surface while effectively reducing amount of bleeding
Reparation；There is biocompatibility and the biological degradability of excellence simultaneously, safe to use, make without any poison is secondary after using
With.
Detailed description of the invention:
For the technological means making the present invention realize, creation characteristic, reach purpose and be easy to understand with effect, below knot
Close specific embodiment, the present invention is expanded on further.
Embodiment 1
(1) abortive calfskin pretreatment: with purification abortive calfskin of can tracing to the source as raw material, by its fully deployed after wrap up with preservative film
Good, it is placed in-5～0 DEG C of environment freezing 8h, then with temperature 5-10 DEG C, the sodium bicarbonate of mass fraction 5% and sodium hexameta phosphate
(sodium bicarbonate is 3:1 with the consumption mass ratio of sodium hexameta phosphate) mixed aqueous solution soaks 15min, then under deionized water shower
With sponge brush brushing surface 2 times；
(2) preparation of collagen fiber Extraction solvent: according to the ratio of mol ratio 1.2:1 by Cyclopropyl Bromide and 2-Pyrrolidone
It is sufficiently mixed, prior to supersound process 30min under supersonic frequency 40kHz, power 50W, then at microwave frequency 2450MHz, power
Microwave treatment 5min under 700W, is then heated to reflux state insulated and stirred 60min, and solution to be mixed naturally cools to 50-55
5-10 DEG C of deionized water of the weight such as addition after DEG C, is sufficiently stirred for rear stratification, phase of fetching water, and obtains Extraction solvent；
(3) preparation of collagen fiber solution: 10 parts of abortive calfskins after above-mentioned scrubbing are sent in freezer dryers, be dried to
Water content is to utilize onal machine to be ground into the granule that granularity is 2-3mm after 10-15%, adds above-mentioned made 40 parts of Extraction solvent
In, fully dispersed after stand 15min, stand and proceed in ball mill after terminating, be milled to fineness less than 50 μm, be subsequently adding quality
3 parts of PVP K30s of mark 5% and 1 part of castor oil hydrogenated polyoxyethylene ether mixed aqueous solution, utilize work frequency after being sufficiently mixed
Rate 40Hz, the Surface Treatment with Plasma machine of power 600W process 15s to gained mixture, and process proceeds to 0～5 DEG C of environment after terminating
Middle standing 5h, is subsequently added 0.5 part of polyacrylic acid and 1 part of polyethylene glycol oxide, and is heated to reflux state insulated and stirred 30min,
Finally crossing 270 mesh sieves, gained filtrate is collagen fiber solution；
(4) preparation of modified collagen fiber solution: add 5 parts in above-mentioned made 30 parts of collagen fiber solution and gather in oneself
Ester, 2 parts of Macrogol 4000s and 0.5 part of methionine, in 35～40 DEG C of sealing and standing 2h after being uniformly dispersed, be sufficiently mixed, so
After under microwave frequency 2450MHz, power 700W microwave treatment 3min, be again sufficiently mixed, and utilize operating frequency 40Hz, merit
The Surface Treatment with Plasma machine of rate 600W processes 15s, and gained mixture speed with 10～15 DEG C/min under ice-water bath cools down
Cooling, insulated and stirred 15min after temperature is down to 0～5 DEG C, obtain modified collagen fiber solution；
(5) preparation of hemostasis gel: add in above-mentioned made 25 parts of modified collagen fiber solutions 2 parts of polyglycolic acids, 2 parts
(haemostatic medicament carries selected from the chemicals or Chinese medicine with hemostasia effect for Polycarbophil, 0.5 part of cystine and 1 part of haemostatic medicament
Take thing), be sufficiently mixed after uniformly and be distributed in mould, and utilize gamma-rays sterilization, the most packaged after in 0～5 DEG C of bar
Cryopreservation under part.
Polyacrylic modification: 10 parts of polyacrylic acid and 1 part of tyrosine are added in double weight part ethanol, is uniformly dispersed
Post-heating, to reflux state insulated and stirred 10min, adds 3 parts of resveratrols and 0.5 part of disodiumedetate, continues at
Insulated and stirred 30min under reflux state, gained mixture proceeds to after naturally cooling to 35-40 DEG C stand in 0-5 DEG C of environment immediately
8h, is then fed in spray dryer, and dried gained solid is ground makes powder.
Embodiment 2
(1) abortive calfskin pretreatment: with purification abortive calfskin of can tracing to the source as raw material, by its fully deployed after wrap up with preservative film
Good, it is placed in-5～0 DEG C of environment freezing 5h, then with temperature 5-10 DEG C, the sodium bicarbonate of mass fraction 5% and sodium hexameta phosphate
(sodium bicarbonate is 3:1 with the consumption mass ratio of sodium hexameta phosphate) mixed aqueous solution soaks 15min, then under deionized water shower
With sponge brush brushing surface 2 times；
(2) preparation of collagen fiber Extraction solvent: according to the ratio of mol ratio 1.2:1 by Cyclopropyl Bromide and 2-Pyrrolidone
It is sufficiently mixed, prior to supersound process 30min under supersonic frequency 40kHz, power 50W, then at microwave frequency 2450MHz, power
Microwave treatment 4min under 700W, is then heated to reflux state insulated and stirred 60min, and solution to be mixed naturally cools to 50-55
5-10 DEG C of deionized water of the weight such as addition after DEG C, is sufficiently stirred for rear stratification, phase of fetching water, and obtains Extraction solvent；
(3) preparation of collagen fiber solution: 15 parts of abortive calfskins after above-mentioned scrubbing are sent in freezer dryers, be dried to
Water content is to utilize onal machine to be ground into the granule that granularity is 2-3mm after 10-15%, adds above-mentioned made 50 parts of Extraction solvent
In, fully dispersed after stand 15min, stand and proceed in ball mill after terminating, be milled to fineness less than 50 μm, be subsequently adding quality
2 parts of PVP K30s of mark 5% and 2 parts of castor oil hydrogenated polyoxyethylene ether mixed aqueous solutions, utilize work frequency after being sufficiently mixed
Rate 40Hz, the Surface Treatment with Plasma machine of power 600W process 15s to gained mixture, and process proceeds to 0～5 DEG C of environment after terminating
Middle standing 5h, is subsequently added 0.5 part of polyacrylic acid and 0.5 part of polyethylene glycol oxide, and be heated to reflux state insulated and stirred 15～
30min, finally crosses 270 mesh sieves, and gained filtrate is collagen fiber solution；
(4) preparation of modified collagen fiber solution: add 4 parts in above-mentioned made 25 parts of collagen fiber solution and gather in oneself
Ester, 1 part of Macrogol 4000 and 0.5 part of methionine, in 35～40 DEG C of sealing and standing 2h after being uniformly dispersed, be sufficiently mixed, so
After under microwave frequency 2450MHz, power 700W microwave treatment 3min, be again sufficiently mixed, and utilize operating frequency 40Hz, merit
The Surface Treatment with Plasma machine of rate 600W processes 15s, and gained mixture speed with 10～15 DEG C/min under ice-water bath cools down
Cooling, insulated and stirred 15min after temperature is down to 0～5 DEG C, obtain modified collagen fiber solution；
(5) preparation of hemostasis gel: add in above-mentioned made 30 parts of modified collagen fiber solutions 3 parts of polyglycolic acids, 2 parts
(haemostatic medicament carries selected from the chemicals or Chinese medicine with hemostasia effect for Polycarbophil, 0.5 part of cystine and 1 part of haemostatic medicament
Take thing), be sufficiently mixed after uniformly and be distributed in mould, and utilize gamma-rays sterilization, the most packaged after in 0～5 DEG C of bar
Cryopreservation under part.
Polyacrylic modification: 15 parts of polyacrylic acid and 2 parts of tyrosine are added in double weight part ethanol, is uniformly dispersed
Post-heating, to reflux state insulated and stirred 10min, adds 5 parts of resveratrols and 0.5 part of disodiumedetate, continues at
Insulated and stirred 30min under reflux state, gained mixture proceeds to after naturally cooling to 35-40 DEG C stand in 0-5 DEG C of environment immediately
8h, is then fed in spray dryer, and dried gained solid is ground makes powder.
Hemostasis gel prepared by embodiment 1 and 2 is carried out performance measurement, and result is as follows:
Outward appearance: gel, smooth surface, the impurity being visible by naked eyes；
Moisture :≤80% (wt)；
Gel strength: 100～500g/cm2；
Content of beary metal :≤10 μ g/g (m/m)；
Liposome :≤1% (m/m)；
Ash :≤2% (m/m)；
PH value: >=4.0；
Biological degradability: all degrade in internal January；
Antibacterial/bacteriostasis property: to the bacteriostasis rate of escherichia coli, gold goal bacterium, Candida albicans and bacillus pyocyaneus all >=50%；
Hemolysis rate :≤5%；
Cytotoxicity: cell-cytotoxic reaction is not more than 1 grade；
Sterility test: aseptic；
Sensitization test (STT): without delayed hypersensitivity；
Intradermoreaction is tested: constitutional stimulation index PII < 0.4；
Exogenous DNA content: Residual exogenous DNA amount answers≤10ng/ml (m/v)
Thermal source: without thermal source；
Acute systemic toxicity: without Acute systemic toxicity；
Genetoxic: hereditary-less toxicity；
Gel time :≤30s；
Bleeding stopping period :≤1min.
The ultimate principle of the present invention and principal character and advantages of the present invention have more than been shown and described.The technology of the industry
Personnel, it should be appreciated that the present invention is not restricted to the described embodiments, simply illustrating this described in above-described embodiment and description
The principle of invention, without departing from the spirit and scope of the present invention, the present invention also has various changes and modifications, and these become
Change and improvement both falls within scope of the claimed invention.Claimed scope by appending claims and
Equivalent defines.
Claims (8)
1. the preparation method of polycaprolactone-abortive calfskin collagen fiber compound hemostatic gel, it is characterised in that include walking as follows
Rapid:
(1) abortive calfskin pretreatment: with purification abortive calfskin of can tracing to the source as raw material, by its fully deployed after wrap with preservative film, and
It is placed in-5～0 DEG C of environment freezing 5～8h, then mixes with sodium hexameta phosphate with the sodium bicarbonate of temperature 5-10 DEG C, mass fraction 5%
Aqueous solution soaking 10～15min, then with sponge brush brushing surface 2～3 times under deionized water shower；
(2) preparation of collagen fiber Extraction solvent: according to the ratio of mol ratio 1.2～1.5:1 by Cyclopropyl Bromide and 2-pyrrolidine
Ketone is sufficiently mixed, prior to supersound process 15～30min under supersonic frequency 40kHz, power 50W, then at microwave frequency 2450MHz,
Microwave treatment 3～5min under power 700W, are then heated to reflux state insulated and stirred 30～60min, and solution to be mixed is natural
It is cooled to 5-10 DEG C of deionized water of the weight such as addition after 50-55 DEG C, is sufficiently stirred for rear stratification, phase of fetching water, obtain extraction
Solvent；
(3) preparation of collagen fiber solution: sent in freezer dryer by the abortive calfskin after above-mentioned scrubbing, is dried to water content and is
Utilize onal machine to be ground into the granule that granularity is 2-3mm after 10-15%, add in above-mentioned made Extraction solvent, fully dispersed
Rear standing 10～15min, stands and proceeds in ball mill after terminating, and is milled to fineness and is less than 50 μm, is subsequently adding mass fraction 5%
PVP K30 and castor oil hydrogenated polyoxyethylene ether mixed aqueous solution, utilize operating frequency 40Hz, power after being sufficiently mixed
The Surface Treatment with Plasma machine of 600W processes 10～15s to gained mixture, and process proceeds to stand in 0～5 DEG C of environment 3 after terminating
～5h, it is subsequently added polyacrylic acid and polyethylene glycol oxide, and is heated to reflux state insulated and stirred 15～30min, finally cross 270
Mesh sieve, gained filtrate is collagen fiber solution；
(4) preparation of modified collagen fiber solution: add polycaprolactone, Polyethylene Glycol in above-mentioned made collagen fiber solution
4000 and methionine, in 35～40 DEG C of sealing and standing 1～2h after being uniformly dispersed, it is sufficiently mixed, then in microwave frequency
Under 2450MHz, power 700W, microwave treatment 2～3min, is sufficiently mixed again, and utilizes operating frequency 40Hz, power 600W
Surface Treatment with Plasma machine processes 10～15s, and gained mixture cools with the speed of 10～15 DEG C/min under ice-water bath,
Insulated and stirred 10～15min after temperature is down to 0～5 DEG C, obtain modified collagen fiber solution；
(5) preparation of hemostasis gel: add polyglycolic acid, Polycarbophil, Guang ammonia in above-mentioned made modified collagen fiber solution
Acid and haemostatic medicament, be sufficiently mixed after uniformly and be distributed in mould, and utilize gamma-rays sterilization, the most packaged after in 0
～cryopreservation under the conditions of 5 DEG C.
The preparation method of polycaprolactone the most according to claim 1-abortive calfskin collagen fiber compound hemostatic gel, its feature
It is: in described step (1), sodium bicarbonate is 2～3:1 with the consumption mass ratio of sodium hexameta phosphate.
The preparation method of polycaprolactone the most according to claim 1-abortive calfskin collagen fiber compound hemostatic gel, its feature
It is: abortive calfskin in described step (3), Extraction solvent, PVP K30, castor oil hydrogenated polyoxyethylene ether, polyacrylic acid and poly-
The consumption mass ratio 10～15:40～50:2～3:1～2:0.5～1:0.5～1 of ethylene oxide.
The preparation method of polycaprolactone the most according to claim 1-abortive calfskin collagen fiber compound hemostatic gel, its feature
It is: through chemical modification before in described step (3), polyacrylic acid uses, its method of modifying is: by polyacrylic acid and tyrosine
Adding in double weight part ethanol, the post-heating that is uniformly dispersed, to reflux state insulated and stirred 10min, adds resveratrol and second
Edetate disodium, continues at insulated and stirred 30min under reflux state, and gained mixture is vertical after naturally cooling to 35-40 DEG C
I.e. proceeding to stand in 0-5 DEG C of environment 8h, be then fed in spray dryer, dried gained solid is ground makes powder.
The preparation method of polycaprolactone the most according to claim 4-abortive calfskin collagen fiber compound hemostatic gel, its feature
It is: the consumption mass ratio of described polyacrylic acid, tyrosine, resveratrol and disodiumedetate is 10～15:1～2:
3～6:0.5～1.
The preparation method of polycaprolactone the most according to claim 1-abortive calfskin collagen fiber compound hemostatic gel, its feature
It is: the consumption mass ratio 25 of collagen fiber solution, polycaprolactone, Macrogol 4000 and methionine in described step (4)
～30:3～6:1～2:0.5～1.
The preparation method of polycaprolactone the most according to claim 1-abortive calfskin collagen fiber compound hemostatic gel, its feature
It is: the consumption matter of modified collagen fiber solution, polyglycolic acid, Polycarbophil, cystine and haemostatic medicament in described step (5)
Amount ratio 25～30:2～3:1～2:0.5～1:0.5～1.
The preparation method of polycaprolactone the most according to claim 1-abortive calfskin collagen fiber compound hemostatic gel, its feature
It is: described haemostatic medicament is selected from chemicals or the Chinese medicine extract with hemostasia effect.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107653291A (en) * | 2017-11-15 | 2018-02-02 | 西藏央金生态农牧科技有限公司 | The standby method for hiding Yak-skin Gelatin original albumen and collagen polypeptide of multi-step enzyme method coordinate system |
| CN110393820A (en) * | 2019-09-18 | 2019-11-01 | 上海简逸生物科技有限公司 | A kind of Medical absorbable or the preparation method for being metabolized hemostatic material |
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| JP2002513645A (en) * | 1998-05-07 | 2002-05-14 | ジェンザイム・コーポレーション | Composition comprising a hemostatic compound and a bioabsorbable polymer |
| CN1507358A (en) * | 2001-01-25 | 2004-06-23 | �ο���ҽҩ����˾ | Carrier with solid fibrinogen and solid thrombin |
| CN102939113A (en) * | 2010-04-07 | 2013-02-20 | 巴克斯特国际公司 | Hemostatic sponge |
| US20150151020A1 (en) * | 2012-05-14 | 2015-06-04 | Teijin Limited | Formed sheet product and hemostatic material |
| CN105287997A (en) * | 2015-11-13 | 2016-02-03 | 邢月军 | Hemostatic gel for surgery |
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| JP2002513645A (en) * | 1998-05-07 | 2002-05-14 | ジェンザイム・コーポレーション | Composition comprising a hemostatic compound and a bioabsorbable polymer |
| CN1507358A (en) * | 2001-01-25 | 2004-06-23 | �ο���ҽҩ����˾ | Carrier with solid fibrinogen and solid thrombin |
| CN102939113A (en) * | 2010-04-07 | 2013-02-20 | 巴克斯特国际公司 | Hemostatic sponge |
| US20150151020A1 (en) * | 2012-05-14 | 2015-06-04 | Teijin Limited | Formed sheet product and hemostatic material |
| CN105287997A (en) * | 2015-11-13 | 2016-02-03 | 邢月军 | Hemostatic gel for surgery |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107653291A (en) * | 2017-11-15 | 2018-02-02 | 西藏央金生态农牧科技有限公司 | The standby method for hiding Yak-skin Gelatin original albumen and collagen polypeptide of multi-step enzyme method coordinate system |
| CN110393820A (en) * | 2019-09-18 | 2019-11-01 | 上海简逸生物科技有限公司 | A kind of Medical absorbable or the preparation method for being metabolized hemostatic material |
| CN110393820B (en) * | 2019-09-18 | 2019-12-27 | 上海简逸生物科技有限公司 | Preparation method of medical absorbable or metabolizable hemostatic material |
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| CN106267328B (en) | 2019-04-12 |
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