CN104711702B - There is the collagen aggregation composite type medical fiber of antibacterial/bacteria resistance function - Google Patents

There is the collagen aggregation composite type medical fiber of antibacterial/bacteria resistance function Download PDF

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CN104711702B
CN104711702B CN201510127304.9A CN201510127304A CN104711702B CN 104711702 B CN104711702 B CN 104711702B CN 201510127304 A CN201510127304 A CN 201510127304A CN 104711702 B CN104711702 B CN 104711702B
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collagen
aggregation
collagen aggregation
sodium
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CN104711702A (en
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但卫华
刘新华
但年华
龚居霞
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Sichuan University
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Abstract

The invention discloses a kind of collagen aggregation composite type medical fiber with antibacterial/bacteriostasis efficacy, be characterized in collagen aggregation as raw material, supercritical CO2For medium, using epoxy propanesulfonate or anhydride is modifying agent, obtains acid-soluble collagen aggregation;Again with carboxymethyl cellulose as raw material, employing sodium metaperiodate is oxidant, obtains dialdehyde carboxymethyl cellulose;Then by acid-soluble collagen aggregation, dialdehyde carboxymethyl cellulose sodium is organic with chitin mixes, and the technological process such as the most agitated, standing and defoaming, spinning has prepared collagen aggregation composite type medical fiber.This fibrous material has had the splendid antibacterial/bacteriostatic activity of the good biology performance of collagen aggregation, biodegradable, mechanical property and chitin, antiinflammatory/promotion wound healing effect concurrently, properties is substantially better than the collagen-based complex fiber material prepared with common collagen for raw material, can be as biological dressing, hemostatic material, absorbable suture, medical cosmetic material etc..

Description

There is the collagen aggregation composite type medical fiber of antibacterial/bacteria resistance function
Technical field
The present invention relates to a kind of collagen aggregation composite type medical fiber with antibacterial/bacteria resistance function, belonged to biological Field of medical materials.
Background technology
Collagen has been found to as the splendid bio-medical material of combination property, and it is raw with other natural/synthesis macromolecules Collagen group composite material prepared by thing medical material organic composite, focus that always collagen research field is widely explored and difficulty Point, collagen and composite thereof have been made into the different dosage forms such as gel, solution, sponge, granule, fiber and biomembrane, extensively Be applied to the biomedical sectors such as tissue engineering bracket, biological dressing, hemostatic material, suture.Particularly by collagen Or its composite becomes medical function fiber by wet spinning preparation, paid close attention to widely by researchers especially, the most Having some medical fibre launch, the trade name of as the most first in Hunan medical high-tech protein line company limited exploitation " good is repaiied Pure natural sub-thread collagen sutures " Surgical Absorbable Suture, it is simply that prepared by wet spinning animal tendon collagen Form.In recent years, more occur in that the report of the substantial amounts of Patents about collagen-based composite medical fiber, but Wei Hua etc. are with glue Former and chitosan is raw material, organic blended, has been prepared the collagen-chitin composite medical of superior performance by wet spinning Fiber (but defend China, and Zhou Wenchang, Zeng Rui etc. Chinese invention patent. ZL 200410022640.9);Chen Wu bravely waits and is also prepared for Collagen-polyvinyl composite fibre, and use metal ion and acetal composite fibre has been carried out modified (Chen Wuyong, Lin Yunzhou, Ye Guangdou, etc. Chinese invention patent. ZL200510020902.2).But, numerous studies show, collagen-based composite fibre Preparation process and properties of product there is also following defect:
1. the spinnability of collagen own is poor, is difficult to spinning;
2. collagen-based composite fibre mechanical strength is the most poor, and biodegradability is too fast can not meet organism metabolism Demand, its structural stability is the most poor simultaneously, is easily affected by external environment.
In order to make up drawbacks described above, it is (main that the composite fibre that wet spinning prepares generally is immersed in acetalation bath by researcher Want composition mostly to be formaldehyde, glutaraldehyde) in modified, cause the biocompatibility of material significantly to decline, and there is potential toxicity, Directly affect the application of material.
It is known that the existing way of collagen is the aggregation of the higher level structure having collagen in organizer, collagen Aggregation is to directly obtain from collagen tissue body, for collagen fiber and the mixture of fibre bundle, is that collagen passes through laterally to assemble With the lateral supermolecule three-dimensional net structure body assembling automatic self assembly.Visible, collagen aggregation is more nearly organizer The form of interior collagen, therefore the spinnability of collagen aggregation, mechanics mechanical performance, biological activity, biodegradability, structure are steady Many performances such as qualitative are all markedly superior to common collagen, itself thus be more suitable for the raw material of wet spinning.But collagen set The collagen Conventional solvents such as body is water insoluble, diluted acid, therefore the present invention is modified to it by epoxy propanesulfonate or anhydride, increases glue The hydrophilic group of former aggregation so that it is become acid-soluble, is more convenient for the subsequent applications of material.Carboxymethyl cellulose is current The cellulose kind that range is the widest in the world, consumption is maximum, has been widely used in food, pharmaceuticals industry, by oxidation Reaction makes its strand expose the dialdehyde carboxymethyl cellulose that aldehyde radical is prepared as, and it is good that it has been sufficiently reserved carboxymethyl cellulose itself Good performance, has hypotoxicity equally, and can with the amino generation schiff base reaction of tropocollagen molecule and produce the effect of effectively crosslinking Really, can substitute, as the biotype cross-linking agent of collagen, the acetalation bath that current collagen-based composite fibre is used completely.Carapace Antibacterial/the bacteriostatic activity of element is relatively strong, it is blended with collagen aggregation, dialdehyde carboxymethyl cellulose, gives full play to the association of storeroom Same-action, can prepare, by wet spinning, the collagen aggregation composite type medical that combination property is superior, have antibacterial/bacteria resistance function Fiber.
Summary of the invention
A kind of collagen collection with antibacterial/bacteriostasis efficacy provided for the deficiencies in the prior art is provided Fit composite type medical fiber.This fibrous material should be that one had both had preferable physical and mechanical properties, suitable biodegradation The premium properties such as performance, biological activity and biocompatibility, can the most effectively stop blooding again, antibacterial/antibacterial, wound healing With the bio-medical material repaired.
For achieving the above object, the present invention adopts the following technical scheme that
(1) preparation of acid-soluble collagen aggregation: take the collagen aggregation of 1~2 weight portions, ground on grinder Grind, be ground into floccule, be then impregnated in the buffer solution that pH is 9.0~11.5 of 1~20 parts by volume, in temperature be Stir 5~10h under conditions of 4~10 DEG C, above-mentioned collagen aggregation is taken out from solution, drains, the most again by above-mentioned collagen Aggregation and the epoxy propanesulfonate of 0.05~0.2 weight portion or anhydride are poured into supercritical carbon dioxide reactor simultaneously, Temperature is 30 DEG C~45 DEG C, pressure is to react 2~48 h under conditions of 8~15Mpa, takes out the collagen collection after crosslinking after terminating Zoarium, is successively immersed in it in PBS and deionized water and repeatedly cleans 5~10h, and final lyophilization is made acid-soluble Collagen aggregation;
(2) preparation of dialdehyde carboxymethyl cellulose sodium: by sodium carboxymethyl cellulose and 20~50 volumes of 1~2 weight portions The Acetic acid-sodium acetate buffer that pH is 3.0~5.0 of part is poured in reactor simultaneously, stirs to clarify under room temperature, then will The sodium metaperiodate of 0.5~2 weight portions is dissolved in the above-mentioned buffer of 1~4 parts by volume, and is slowly poured in reactor, in temperature Degree be 25 DEG C~35 DEG C under conditions of stirring reaction 48~72h, question response terminate after add reaction terminating agent Polyethylene Glycol 0.1~ 1 parts by volume, after being slowly stirred 0.5~1h, then adds the sodium chloride of 2~5 weight portions and 30~100 parts by volume to reactor Acetone, stands and makes Precipitation, removes supernatant, the most by centrifugation, wash, dialyse, lyophilization prepares dialdehyde carboxylic first Base sodium cellulosate;
(3) preparation of collagen aggregation compound spinning mother solution: the procollagen aggregation of 1~2 weight portions is stirred molten Solution, in the acetum of the 0.1~0.5mol/L of 100~200 parts by volume, adds 0.1~0.5 weight portion in above-mentioned solution Dialdehyde carboxymethyl cellulose sodium, at 4~10 DEG C stir 10~24h, obtain composite spinning mother solution A;Again by 1~2 weight portions The same stirring and dissolving of chitin, at the acetum of the 0.1~0.5mol/L of 100~200 parts by volume, obtains composite spinning mother solution B;Be finally 4~6:6~4 to be blended above-mentioned composite spinning mother solution A and composite spinning mother solution B according to volume ratio, temperature be 4~ Under conditions of 10 DEG C, stirring 5~12h, standing and defoaming, obtain wet spinning mother solution;
(4) preparation of collagen aggregation composite type medical fiber: use wet-spinning frame, with mass ratio be 5~9:1~ The sodium sulfate of 5 is solidification liquid with the saturated mixed solution of sodium chloride, at 35~55 DEG C of solidification temperaturies and 0.05~0.3Mpa nitrogen Spray webbing under pressure condition, under suitable pull strength effect, coagulation forming obtains crude fibre, then through graded ethanol substep desalination, Washing repeatedly, 100~150 DEG C of hot-stretch sizing (hot-stretch rate is 90%~150%), dosage are 6~30KGy/h60Co is produced Gamma-rays sterilization, molding packaging, obtain collagen aggregation composite type medical fiber.
In above-mentioned preparation method, the source animal skin of the collagen aggregation in step (1) or tendon be ecology, can Trace to the source;In step (2), sodium carboxymethyl cellulose, epoxy propanesulfonate, anhydride are commercially available, wherein the carboxylic of sodium carboxymethyl cellulose Methyl content is 65%~85%;The diameter of the collagen aggregation composite type medical fiber in step (4) can be according to technological parameter Convert and adjust;Wet-spinning frame used by the present invention is that Shanxi Inst. of Coal Chemistry, Chinese Academy of Sciences produces.
The key performance of the collagen aggregation composite type medical fiber with antibacterial/bacteria resistance function should meet claimed below:
Outward appearance: white or slightly yellow fibrous material;
Content of beary metal :≤10 μ g/g (m/m);
Line density: 1~20 dtex;
Fracture strength: 1~8 cN/dtex;
Elongation at break: 15%~50%;
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.
This technology compared with prior art, has the advantage that
(1) different from the collagen-based composite fibre having been reported, the present invention is with collagen aggregation as raw material, by epoxy third Sodium sulfonate or the more hydrophilic group of anhydride modified introducing, prepared acid-soluble collagen aggregation, with acid-soluble collagen set Body is as the base material of wet spinning, and compared with common collagen, its structure is more nearly the existence configuration of collagen in organizer, Therefore its spinnability, mechanics mechanical performance, biodegradability, biological activity etc. are the most excellent;
(2) present invention homemade dialdehyde carboxymethyl cellulose sodium has the highest chemical reactivity, it is possible to collagen collection Fit generation effectively cross-links, and makes the properties of collagen aggregation improve further, himself biocompatibility, anthemorrhagic performance etc. The most superior, the biological activity of collagen aggregates will not be produced impact, there is not potential toxicity, can substitute completely at present (main component mostly is formaldehyde, glutaraldehyde, can cause the biocompatibility of material in the acetalation bath that collagen-based composite fibre is used Significantly decline, and there is potential toxicity, directly affect the application of material), and dialdehyde carboxymethyl cellulose sodium produces into This is low, it is simple to large-scale promotion uses, and is the excellent Biological cross-linker of a kind of collagen;
(3) at supercritical CO2In fluid condition being chemically crosslinked collagen aggregation, early stage can be as chemical reaction Medium, the later stage again can be the method efficient stable, green as residual, unreacted epoxy propanesulfonate or the solvent of anhydride extraction Colour circle is protected, and advantageously ensures that the biocompatibility of material.
Detailed description of the invention
The present invention is specifically described below by implementing, it is necessary to it is pointed out here that to be that the present embodiment is served only for right The present invention is further described, and it is not intended that limiting the scope of the invention, the person skilled in the art in this field Nonessential improvement and adjustment can be made according to the content of foregoing invention.
Embodiment 1
(1) preparation of acid-soluble collagen aggregation: take the collagen aggregation of 1 weight portion, is ground, powder on grinder It is broken into floccule, is then impregnated in the buffer solution that pH is 9.0 of 1 parts by volume, stir under conditions of temperature is 4 DEG C 5h, takes out above-mentioned collagen aggregation from solution, drains, the most again by above-mentioned collagen aggregation and the ring of 0.05 weight portion Oxygen propanesulfonate is poured into supercritical carbon dioxide reactor simultaneously, temperature be 30 DEG C, pressure be 8Mpa under conditions of react 2h, takes out the collagen aggregation after crosslinking after terminating, it be successively immersed in PBS and deionized water and repeatedly clean 5h, acid-soluble collagen aggregation is made in final lyophilization;
(2) preparation of dialdehyde carboxymethyl cellulose sodium: be by the sodium carboxymethyl cellulose of 1 weight portion and the pH of 20 parts by volume The Acetic acid-sodium acetate buffer of 3.0 is poured in reactor simultaneously, stirs to clarify under room temperature, then by the high iodine of 0.5 weight portion Acid sodium is dissolved in the above-mentioned buffer of 1 parts by volume, and is slowly poured in reactor, and under conditions of temperature is 25 DEG C, stirring is anti- Reaction terminating agent Polyethylene Glycol 0.1 parts by volume is added, after being slowly stirred 0.5h, then to reactor after answering 48h, question response to terminate Add sodium chloride and the acetone of 30 parts by volume of 2 weight portions, stand and make Precipitation, remove supernatant, the most by centrifugation, wash Wash, dialyse, lyophilization prepares dialdehyde carboxymethyl cellulose sodium;
(3) preparation of collagen aggregation compound spinning mother solution: the procollagen aggregation stirring and dissolving of 1 weight portion is existed In the acetum of the 0.5mol/L of 100 parts by volume, in above-mentioned solution, add the dialdehyde carboxymethyl cellulose of 0.1 weight portion Sodium, stirs 10h, obtains composite spinning mother solution A at 4 DEG C;Again by the same stirring and dissolving of chitin of 1 weight portion in 100 parts by volume The acetum of 0.5mol/L, obtain composite spinning mother solution B;Finally by above-mentioned composite spinning mother solution A and composite spinning mother solution B It is that 4:6 is blended according to volume ratio, under conditions of temperature is 4 DEG C, stirs 5h, standing and defoaming, obtains wet spinning mother solution;
(4) preparation of collagen aggregation composite type medical fiber: employing wet-spinning frame, with mass ratio as 5:5 Sodium sulfate is solidification liquid with the saturated mixed solution of sodium chloride, sprays under the conditions of 35 DEG C of solidification temperaturies and 0.05Mpa nitrogen pressure Silk, under suitable pull strength effect, coagulation forming obtains crude fibre, then through graded ethanol substep desalination, washing repeatedly, 100 DEG C hot-stretch sizing (hot-stretch rate is 90%), dosage are 6KGy/h60Gamma-rays sterilization, molding packaging produced by Co, Obtain collagen aggregation composite type medical fiber.
Embodiment 2
(1) preparation of acid-soluble collagen aggregation: take the collagen aggregation of 1.5 weight portions, grinder is ground, It is ground into floccule, is then impregnated in the buffer solution that pH is 10.5 of 15 parts by volume, under conditions of temperature is 5 DEG C Stirring 8h, in toilet, above-mentioned collagen aggregation is taken out from solution, drains, the most again by above-mentioned collagen aggregation with The succinic anhydrides of 0.1 weight portion is poured into supercritical carbon dioxide reactor simultaneously, temperature be 35 DEG C, pressure be 10Mpa's Under the conditions of react 12 h, take out the collagen aggregation after crosslinking after terminating, it be successively immersed in PBS and deionized water In repeatedly clean 8h, acid-soluble collagen aggregation is made in final lyophilization;
(2) preparation of dialdehyde carboxymethyl cellulose sodium: by sodium carboxymethyl cellulose and the pH of 30 parts by volume of 1.5 weight portions Be 4.0 Acetic acid-sodium acetate buffer be poured in reactor simultaneously, stir to clarify under room temperature, then by the high iodine of 1 weight portion Acid sodium is dissolved in the above-mentioned buffer of 2 parts by volume, and is slowly poured in reactor, and under conditions of temperature is 30 DEG C, stirring is anti- Reaction terminating agent Polyethylene Glycol 0.5 parts by volume is added, after being slowly stirred 40min, then to reaction after answering 60h, question response to terminate Still adds sodium chloride and the acetone of 50 parts by volume of 3 weight portions, stands and makes Precipitation, removes supernatant, the most by centrifugation, washes Wash, dialyse, lyophilization prepares dialdehyde carboxymethyl cellulose sodium;
(3) preparation of collagen aggregation compound spinning mother solution: by the procollagen aggregation stirring and dissolving of 1.5 weight portions In the acetum of the 0.2mol/L of 150 parts by volume, in above-mentioned solution, add the dialdehyde carboxymethyl fiber of 0.2 weight portion Element sodium, stirs 15h under conditions of temperature is 6 DEG C, obtains composite spinning mother solution A;Again the chitin of 1.5 weight portions is stirred equally Mix the acetum of the 0.2mol/L being dissolved in 150 parts by volume, obtain composite spinning mother solution B;Finally by above-mentioned Compound spinning screw Liquid A and composite spinning mother solution B is that 5:5 is blended according to volume ratio, stirs 8h, standing and defoaming, obtain under conditions of temperature is 6 DEG C Wet spinning mother solution;
(4) preparation of collagen aggregation composite type medical fiber: use wet-spinning frame, the sulfur with mass ratio as 6:4 Acid sodium is solidification liquid with the saturated mixed solution of sodium chloride, spray webbing under the conditions of 45 DEG C of solidification temperaturies and 0.2Mpa nitrogen pressure, Under suitable pull strength effect, coagulation forming obtains crude fibre, then through graded ethanol substep desalination, washing repeatedly, 120 DEG C Hot-stretch sizing (hot-stretch rate is 120%), dosage are 15KGy/h60Gamma-rays sterilization, molding packaging produced by Co, Obtain collagen aggregation composite type medical fiber.
Embodiment 3
(1) preparation of acid-soluble collagen aggregation: take the collagen aggregation of 2 weight portions, is ground, powder on grinder It is broken into floccule, is then impregnated in the buffer solution that pH is 11.5 of 20 parts by volume, under conditions of temperature is 10 DEG C Stirring 10h, takes out above-mentioned collagen aggregation from solution, drains, the most again by above-mentioned collagen aggregation and 0.2 weight portion Epoxy propanesulfonate be poured into supercritical carbon dioxide reactor simultaneously, temperature be 45 DEG C, pressure be 15Mpa under conditions of anti- Answer 48 h, after terminating, take out the collagen aggregation after crosslinking, it is successively immersed in PBS and deionized water the most clear Washing 10h, acid-soluble collagen aggregation is made in final lyophilization;
(2) preparation of dialdehyde carboxymethyl cellulose sodium: be by the sodium carboxymethyl cellulose of 2 weight portions and the pH of 50 parts by volume The Acetic acid-sodium acetate buffer of 5.0 is poured in reactor simultaneously, stirs to clarify under room temperature, then by the periodic acid of 2 weight portions Sodium is dissolved in the above-mentioned buffer of 4 parts by volume, and, slowly it is poured in reactor, under conditions of temperature is 35 DEG C, stirring is anti- Add reaction terminating agent Polyethylene Glycol 1 parts by volume after answering 72h, question response to terminate, after being slowly stirred 1h, then add to reactor The sodium chloride of 5 weight portions and the acetone of 100 parts by volume, stand and make Precipitation, removes supernatant, the most by centrifugation, washs, thoroughly Analysis, lyophilization prepare dialdehyde carboxymethyl cellulose sodium;
(3) preparation of collagen aggregation compound spinning mother solution: the procollagen aggregation stirring and dissolving of 2 weight portions is existed In the acetum of the 0.1mol/L of 200 parts by volume, in above-mentioned solution, add the dialdehyde carboxymethyl cellulose of 0.5 weight portion Sodium, stirs 24h under conditions of temperature is 10 DEG C, obtains composite spinning mother solution A;Again the chitin of 2 weight portions is stirred equally It is dissolved in the acetum of the 0.1mol/L of 200 parts by volume, obtains composite spinning mother solution B;Finally by above-mentioned composite spinning mother solution A and composite spinning mother solution B is that 6:4 is blended according to volume ratio, stirs 12h, standing and defoaming, obtain under conditions of temperature is 10 DEG C Final spinning mother solution;
(4) preparation of collagen aggregation composite type medical fiber: use wet-spinning frame, the sulfur with mass ratio as 9:1 Acid sodium is solidification liquid with the saturated mixed solution of sodium chloride, spray webbing under the conditions of 55 DEG C of solidification temperaturies and 0.3Mpa nitrogen pressure, Under suitable pull strength effect, coagulation forming obtains crude fibre, then through graded ethanol substep desalination, washing repeatedly, 150 DEG C Hot-stretch sizing (hot-stretch rate is 150%), dosage are 30KGy/h60Gamma-rays sterilization, molding packaging produced by Co, To collagen aggregation composite type medical fiber.

Claims (4)

1. there is the preparation method of the collagen aggregation composite type medical fiber of antibacterial/bacteria resistance function, comprise the steps:
(1) preparation of acid-soluble collagen aggregation: take the collagen aggregation of 1~2 weight portions, is ground, powder on grinder It is broken into floccule, is then impregnated in the buffer solution that pH is 9.0~11.5 of 1~20 parts by volume, is 4~10 in temperature Stir 5~10h under conditions of DEG C, above-mentioned collagen aggregation is taken out from solution, drains, the most again by above-mentioned collagen aggregation It is poured into supercritical carbon dioxide reactor with epoxy propanesulfonate or the anhydride of 0.05~0.2 weight portion simultaneously, is 30 in temperature DEG C~45 DEG C, pressure be to react 2~48h under conditions of 8~15MPa, take out the collagen aggregation after crosslinking after terminating, by it first After be immersed in PBS and deionized water and repeatedly clean 5~10h, acid-soluble collagen aggregation is made in final lyophilization;
(2) preparation of dialdehyde carboxymethyl cellulose sodium: by the sodium carboxymethyl cellulose of 1~2 weight portions and 20~50 parts by volume PH be 3.0~5.0 Acetic acid-sodium acetate buffer be poured in reactor simultaneously, stir to clarify under room temperature, then by 0.5~2 The sodium metaperiodate of weight portion is dissolved in the above-mentioned buffer of 1~4 parts by volume, and is slowly poured in reactor, is 25 in temperature DEG C~35 DEG C under conditions of stirring reaction 48~72h, question response terminate after add reaction terminating agent Polyethylene Glycol 0.1~1 volume Part, after being slowly stirred 0.5~1h, then add sodium chloride and the acetone of 30~100 parts by volume of 2~5 weight portions to reactor, Standing makes Precipitation, removes supernatant, the most by centrifugation, wash, dialyse, lyophilization prepares dialdehyde carboxymethyl fiber Element sodium;
(3) preparation of collagen aggregation compound spinning mother solution: the procollagen aggregation stirring and dissolving of 1~2 weight portions is existed In the acetum of the 0.1~0.5mol/L of 100~200 parts by volume, in above-mentioned solution, add the double of 0.1~0.5 weight portion Aldehyde sodium carboxymethyl cellulose, stirs 10~24h, obtains composite spinning mother solution A at 4~10 DEG C;Again by the carapace of 1~2 weight portions The same stirring and dissolving of element, at the acetum of the 0.1~0.5mol/L of 100~200 parts by volume, obtains composite spinning mother solution B;? After be 4~6:6~4 to be blended above-mentioned composite spinning mother solution A and composite spinning mother solution B according to volume ratio, be 4~10 DEG C in temperature Under conditions of stir 5~12h, standing and defoaming, obtain wet spinning mother solution;
(4) preparation of collagen aggregation composite type medical fiber: use wet-spinning frame, be 5~9:1~5 with mass ratio Sodium sulfate is solidification liquid with the saturated mixed solution of sodium chloride, at 35~55 DEG C of solidification temperaturies and 0.05~0.3MPa nitrogen pressure Under the conditions of spray webbing, under suitable pull strength effect, coagulation forming obtains crude fibre, then through graded ethanol substep desalination, repeatedly Washing, 100~150 DEG C of hot-stretch sizings, hot-stretch rate are 90%~150%, dosage is 6~30KGy/h60γ produced by Co Radiation sterilization sterilizing, molding packaging, obtain collagen aggregation composite type medical fiber;Obtained has antibacterial/bacteria resistance function Collagen aggregation composite type medical fiber consist predominantly of acid-soluble collagen aggregation, dialdehyde carboxymethyl cellulose sodium and carapace Three kinds of bio-medical raw materials of element, its Key Performance Indicator is as follows:
Outward appearance: white or slightly yellow fibrous material;
Content of beary metal :≤10 μ g/g;
Line density: 1~20dtex;
Fracture strength: 1~8cN/dtex;
Elongation at break: 15%~50%;
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.
There is the preparation method of the collagen aggregation composite type medical fiber of antibacterial/bacteria resistance function the most as claimed in claim 1, It is characterized in that described anhydride can be any one of acetic anhydride and succinic anhydrides.
There is the preparation method of the collagen aggregation composite type medical fiber of antibacterial/bacteria resistance function the most as claimed in claim 1, It is characterized in that the described multi-layer aggregation that collagen aggregation is common collagen, be from Corii Sus domestica, pig tendon, Corii Bovis seu Bubali, beef tendon, donkey Any one of skin, Corium Mus or rat-tail tendon extract acquisition.
There is the preparation method of the collagen aggregation composite type medical fiber of antibacterial/bacteria resistance function the most as claimed in claim 1, It is characterized in that described preparation process is all to complete in clean worker-house, the cleanliness factor in clean worker-house is ten thousand grades.
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CN105327389B (en) * 2015-11-23 2018-11-27 四川大学 Cotton-shaped antibacterial anti hemorrhagic material based on collagen aggregates and preparation method thereof
CN109021170B (en) * 2017-06-09 2022-05-17 天津科技大学 Preparation method of salt-resistant nano/micro fibril cellulose gel
CN108210985A (en) * 2018-01-22 2018-06-29 陕西科技大学 A kind of high-strength medical hydrogel based on human-like collagen and preparation method thereof
CN111501121A (en) * 2019-01-31 2020-08-07 华北水利水电大学 Method for preparing collagen fiber by wet spinning
CN110499541B (en) * 2019-07-18 2021-09-14 福建农林大学 High-strength bionic fiber based on collagen liquid crystal in-situ self-assembly and preparation method thereof
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CN115094629A (en) * 2022-08-26 2022-09-23 江苏亨瑞生物医药科技有限公司 Recombinant collagen modified cellulose fiber and preparation method thereof

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JPH06296673A (en) * 1993-04-14 1994-10-25 Mitsubishi Rayon Co Ltd Fiber for hemostatic material
CN1245543C (en) * 2004-05-28 2006-03-15 四川大学 Preparing method for collagen stroma composite medical fibre spinning stoste
CN100535212C (en) * 2006-10-11 2009-09-02 东华大学 Method for preparing collagen protein and chitosan composite nano fibre and film electro static spinning
CN101265621A (en) * 2007-03-13 2008-09-17 成都佰乐金生物科技有限公司 Collagen protein-polyvinyl alcohol-chitosan blending medical fibre and method for making same
CN101450223A (en) * 2007-11-30 2009-06-10 张博 Hemostasia material based on chitosan, collagen and sodium cellulose glycolate and preparation method and use thereof
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