CN104436283B - A kind of medical collagen membrane material and preparation method thereof - Google Patents
A kind of medical collagen membrane material and preparation method thereof Download PDFInfo
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- 102000008186 Collagen Human genes 0.000 title claims abstract description 79
- 108010035532 Collagen Proteins 0.000 title claims abstract description 79
- 229920001436 collagen Polymers 0.000 title claims abstract description 79
- 239000000463 material Substances 0.000 title claims abstract description 66
- 239000012528 membrane Substances 0.000 title claims abstract description 54
- 238000002360 preparation method Methods 0.000 title claims abstract description 51
- 241000269799 Perca fluviatilis Species 0.000 claims abstract description 67
- 238000001291 vacuum drying Methods 0.000 claims abstract description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000008367 deionised water Substances 0.000 claims abstract description 16
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 16
- 239000012530 fluid Substances 0.000 claims abstract description 16
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims abstract description 14
- 239000001768 carboxy methyl cellulose Substances 0.000 claims abstract description 14
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims abstract description 14
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims abstract description 14
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 13
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 13
- 239000000203 mixture Substances 0.000 claims abstract description 10
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims abstract description 9
- 238000013019 agitation Methods 0.000 claims abstract description 8
- 238000007598 dipping method Methods 0.000 claims abstract description 8
- 238000005189 flocculation Methods 0.000 claims abstract description 8
- 230000016615 flocculation Effects 0.000 claims abstract description 8
- 238000004108 freeze drying Methods 0.000 claims abstract description 8
- 239000013049 sediment Substances 0.000 claims abstract description 8
- 239000000243 solution Substances 0.000 claims description 34
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 27
- 239000002253 acid Substances 0.000 claims description 25
- 238000000605 extraction Methods 0.000 claims description 21
- 239000000843 powder Substances 0.000 claims description 9
- 239000007864 aqueous solution Substances 0.000 claims description 7
- 238000002386 leaching Methods 0.000 claims description 2
- 238000000034 method Methods 0.000 claims description 2
- 238000005119 centrifugation Methods 0.000 claims 2
- 238000003756 stirring Methods 0.000 abstract description 5
- 239000012567 medical material Substances 0.000 abstract description 3
- -1 shitosan Polymers 0.000 abstract description 2
- 238000001556 precipitation Methods 0.000 description 6
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 5
- 239000012620 biological material Substances 0.000 description 5
- 229910052700 potassium Inorganic materials 0.000 description 5
- 239000011591 potassium Substances 0.000 description 5
- 239000002657 fibrous material Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 210000002318 cardia Anatomy 0.000 description 2
- 238000004113 cell culture Methods 0.000 description 2
- 231100000957 no side effect Toxicity 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 210000002784 stomach Anatomy 0.000 description 2
- 229920002101 Chitin Polymers 0.000 description 1
- 206010018910 Haemolysis Diseases 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 229910001069 Ti alloy Inorganic materials 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 206010052428 Wound Diseases 0.000 description 1
- 208000027418 Wounds and injury Diseases 0.000 description 1
- HZEWFHLRYVTOIW-UHFFFAOYSA-N [Ti].[Ni] Chemical compound [Ti].[Ni] HZEWFHLRYVTOIW-UHFFFAOYSA-N 0.000 description 1
- 230000002052 anaphylactic effect Effects 0.000 description 1
- 239000002473 artificial blood Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000975 bioactive effect Effects 0.000 description 1
- 239000000227 bioadhesive Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 230000023555 blood coagulation Effects 0.000 description 1
- 210000004204 blood vessel Anatomy 0.000 description 1
- 210000001124 body fluid Anatomy 0.000 description 1
- 239000010839 body fluid Substances 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
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- 239000002131 composite material Substances 0.000 description 1
- 239000005548 dental material Substances 0.000 description 1
- 238000000502 dialysis Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003937 drug carrier Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910000939 field's metal Inorganic materials 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 210000003709 heart valve Anatomy 0.000 description 1
- 230000008588 hemolysis Effects 0.000 description 1
- 230000036039 immunity Effects 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000001356 surgical procedure Methods 0.000 description 1
- 210000001519 tissue Anatomy 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000029663 wound healing Effects 0.000 description 1
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Abstract
The invention belongs to field of medical materials, disclose a kind of medical collagen membrane material and preparation method thereof, described medical collagen membrane material comprises that perch collagen is that 14-24 part, polyvinyl alcohol are that 4-8 part, shitosan are that 3-7 part, carboxymethyl cellulose are 5-11 part. Preparation method comprises the following steps: the preparation of (1) perch collagen: perch fish-skin is cleaned by deionized water, vacuum drying, grind, ultrasonic agitation hot dipping is carried, centrifugal, collects upper strata viscous fluid, it is 6.5 that upper strata viscous fluid is adjusted to pH with potassium hydroxide, leave standstill 12h, centrifugal rear collection flocculation sediment, freeze drying; (2) preparation of medical collagen membrane material: get by weight perch collagen, polyvinyl alcohol, shitosan, carboxymethyl cellulose prepared by step (1), after being mixed, above-mentioned each composition adds deionized water, stirring final vacuum is dry, the collagen membrane material for preparing after vacuum drying.
Description
Technical field
The invention belongs to field of medical materials, relate to a kind of medical film material and preparation method thereof, particularly relate to oneMedical collagen membrane material and preparation method thereof.
Background technology
Biomaterial be contact with tissue, body fluid or blood or act on and to human body without toxicity, side effect, solidifyingBlood, not haemolysis, does not cause human body cell sudden change, distortion and canceration, does not cause immunity rejection and anaphylactoid specific function materialMaterial. Nearly thousand kinds of studied biomaterials so far, but only tens of kinds of being widely used. These materials are mainly divided into medicalSynthetic or natural macromolecular material, medical metal material, medical science pottery, medical carbon materials, and their composite etc.Class. There are highly blood coagulation resistant material, bioactive ceramics and glass, titanium or titanium alloy and the memory of titanium nickel in more active research and development fieldAlloy, biologically active slowly-releasing and retouch target drug carrier material, bioadhesive, absorbable biomaterial, chitin and spread outBiological medical application etc. Biomaterial is successfully applied to heart valve prosthesis, artificial blood vessel, artificial B&J, doctorBy conduit, dental material, surgery kinking, slow releasing carrier of medication, dialysis and milipore filter material and the disposable and medical system of the property implantedThe aspects such as product.
Medical collagen membrane material also belongs to the one of biomaterial for medical purpose, and medical collagen membrane material has comparatively clinicallyWide use has more use in wound healing material, timbering material and cell thereof are cultivated, and license notification number isThe patent of invention of CN101264337 discloses a kind of membranaceous porous fibrous material, and its preparation method is mainly by getting after processingAnimal Skin add water to regulate after pH and smash slurry, after processing with stomach cardia, use again acetum processing, carry out frozen drying. Its systemStandby collagen membrane material tensile strength is only less than 3MPa, and elongation at break only has in 200%.
Summary of the invention
The technical problem solving: medical collagen membrane material has larger usage space in biomedical sector, for exampleBe used to prepare the timbering material of Wound dressing material, organizational project, and be used to cell cultivation etc., object of the present invention existsIn provide a kind of biocompatibility better, have no side effect and there is the medical of higher tensile strength and elongation at breakCollagen membrane material and preparation method thereof, the application performance of raising medical collagen membrane material.
Technical scheme: in order to address the above problem, the invention discloses a kind of medical collagen membrane material and preparation method thereof.Described medical collagen membrane material comprises the composition of following weight portion:
Perch collagen 14-24 part,
Polyvinyl alcohol 4-8 part,
Shitosan 3-7 part,
Carboxymethyl cellulose 5-11 part.
Described a kind of medical collagen membrane material, comprises the composition of following weight portion:
Perch collagen 17-20 part,
Polyvinyl alcohol 5-7 part,
Shitosan 4-6 part,
Carboxymethyl cellulose 8-10 part.
Described a kind of medical collagen membrane material, perch collagen is perch fish skin collagen egg prepared by sour formulationIn vain.
A preparation method for medical collagen membrane material, preparation method comprises the following steps:
(1) preparation of perch collagen:
Perch fish-skin and perch are peeled off, after peeling off, perch fish-skin is cleaned by deionized water, clean 3 times, cleanAfter fish-skin is carried out to vacuum drying, after vacuum drying, fish-skin is ground, carry out ultrasonic agitation hot dipping by acid solution and carry, acid solution isThe citric acid solution of 5wt%-8wt%, the weight ratio of acid solution and perch fish-skin powder is 8:1-12:1, hot extraction temperature is 50-60DEG C, ultrasonic power is 100w-200w, extraction time is 3h-4h, after extraction, carry out centrifugal, centrifugal rear collection upper strata viscous fluid, willIt is 6.5 that upper strata viscous fluid is adjusted to pH with potassium hydroxide, leaves standstill 12h, and centrifugal rear collection flocculation sediment carries out precipitation freezing dryAfter dry, prepare perch collagen;
(2) preparation of medical collagen membrane material:
Getting by weight perch collagen prepared by step (1) is that 14-24 part, polyvinyl alcohol are 4-8 part, shitosanFor 3-7 part, carboxymethyl cellulose are 5-11 part, after being mixed, above-mentioned each composition adds the deionized water of 3 times of weight, enterRow stirs, and the aqueous solution is carried out to vacuum drying after being stirred to evenly, is the collagen membrane material of preparation after vacuum drying.
The preparation method of described a kind of medical collagen membrane material, vacuum drying temperature is 55 DEG C, vacuum is 5Pa-200Pa。
The preparation method of described a kind of medical collagen membrane material, the acid solution in perch collagen leaching process isThe citric acid solution of 6wt%.
The preparation method of described a kind of medical collagen membrane material, the weight ratio of acid solution and perch fish-skin powder is 10:1.
In the preparation method of described a kind of medical collagen membrane material, perch collagen is 17-20 part, polyethyleneAlcohol is that 5-7 part, shitosan are that 4-6 part, carboxymethyl cellulose are 8-10 part.
The preparation method of described a kind of medical collagen membrane material, ultrasonic power is 150w.
Beneficial effect: adopted perch collagen as collagen membrane material in medical collagen membrane material of the present inventionMain component, then added polyvinyl alcohol, shitosan, carboxymethyl cellulose. The medical collagen membrane material biology preparingCompatibility is good, produce without irritated situation clinically, has no side effect, and possesses extraordinary tensile strength and extension at breakRate. The preparation method of perch collagen disclosed by the invention is different from the preparation method of traditional collagen, preparationStep is simple, and the recovery rate of the perch collagen preparing is higher, has effectively utilized the money of perch fish-skinSource and improved the intensity of medical collagen membrane material.
Detailed description of the invention
Embodiment 1
(1) preparation of perch collagen:
Perch fish-skin and perch are peeled off, after peeling off, perch fish-skin is cleaned by deionized water, clean 3 times, cleanAfter fish-skin is carried out to vacuum drying, after vacuum drying, fish-skin is ground, carry out ultrasonic agitation hot dipping by acid solution and carry, acid solution is 8wt%Citric acid solution, the weight ratio of acid solution and perch fish-skin powder is 12:1, hot extraction temperature is 60 DEG C, ultrasonic power is100w, extraction time is 3h, carries out centrifugally after extraction, centrifugal rear collection upper strata viscous fluid, by upper strata viscous fluid potassium hydroxideBeing adjusted to pH is 6.5, leaves standstill 12h, and centrifugal rear collection flocculation sediment, carries out precipitation after freeze drying, to prepare perch fishCollagen;
(2) preparation of medical collagen membrane material:
Getting by weight perch collagen prepared by step (1) is that 24Kg, polyvinyl alcohol are that 4Kg, shitosan are3Kg, carboxymethyl cellulose are 11Kg, add the deionized water of 3 times of weight after above-mentioned each composition is mixed, and stirMixing, the aqueous solution is carried out to vacuum drying after being stirred to evenly, is the collagen membrane material of preparation after vacuum drying.
Embodiment 2
(1) preparation of perch collagen:
Perch fish-skin and perch are peeled off, after peeling off, perch fish-skin is cleaned by deionized water, clean 3 times, cleanAfter fish-skin is carried out to vacuum drying, after vacuum drying, fish-skin is ground, carry out ultrasonic agitation hot dipping by acid solution and carry, acid solution is 5wt%Citric acid solution, the weight ratio of acid solution and perch fish-skin powder is 8:1, hot extraction temperature is 50 DEG C, ultrasonic power is 200w,Extraction time is 4h, carries out centrifugally after extraction, and centrifugal rear collection upper strata viscous fluid, is adjusted to upper strata viscous fluid with potassium hydroxidePH is 6.5, leaves standstill 12h, and centrifugal rear collection flocculation sediment, carries out precipitation after freeze drying, to prepare perch fish skin collagenAlbumen;
(2) preparation of medical collagen membrane material:
Getting by weight perch collagen prepared by step (1) is that 14Kg, polyvinyl alcohol are that 8Kg, shitosan are7Kg, carboxymethyl cellulose are 5Kg, add the deionized water of 3 times of weight after above-mentioned each composition is mixed, stir,After being stirred to evenly, the aqueous solution is carried out to vacuum drying, the collagen membrane material for preparing after vacuum drying.
Embodiment 3
(1) preparation of perch collagen:
Perch fish-skin and perch are peeled off, after peeling off, perch fish-skin is cleaned by deionized water, clean 3 times, cleanAfter fish-skin is carried out to vacuum drying, after vacuum drying, fish-skin is ground, carry out ultrasonic agitation hot dipping by acid solution and carry, acid solution is 8wt%Citric acid solution, the weight ratio of acid solution and perch fish-skin powder is 10:1, hot extraction temperature is 60 DEG C, ultrasonic power is100w, extraction time is 3h, carries out centrifugally after extraction, centrifugal rear collection upper strata viscous fluid, by upper strata viscous fluid potassium hydroxideBeing adjusted to pH is 6.5, leaves standstill 12h, and centrifugal rear collection flocculation sediment, carries out precipitation after freeze drying, to prepare perch fishCollagen;
(2) preparation of medical collagen membrane material:
Getting by weight perch collagen prepared by step (1) is that 17Kg, polyvinyl alcohol are that 5Kg, shitosan are4Kg, carboxymethyl cellulose are 10Kg, add the deionized water of 3 times of weight after above-mentioned each composition is mixed, and stirMixing, the aqueous solution is carried out to vacuum drying after being stirred to evenly, is the collagen membrane material of preparation after vacuum drying.
Embodiment 4
(1) preparation of perch collagen:
Perch fish-skin and perch are peeled off, after peeling off, perch fish-skin is cleaned by deionized water, clean 3 times, cleanAfter fish-skin is carried out to vacuum drying, after vacuum drying, fish-skin is ground, carry out ultrasonic agitation hot dipping by acid solution and carry, acid solution is 6wt%Citric acid solution, the weight ratio of acid solution and perch fish-skin powder is 12:1, hot extraction temperature is 55 DEG C, ultrasonic power is150w, extraction time is 3h, carries out centrifugally after extraction, centrifugal rear collection upper strata viscous fluid, by upper strata viscous fluid potassium hydroxideBeing adjusted to pH is 6.5, leaves standstill 12h, and centrifugal rear collection flocculation sediment, carries out precipitation after freeze drying, to prepare perch fishCollagen;
(2) preparation of medical collagen membrane material:
Getting by weight perch collagen prepared by step (1) is that 18Kg, polyvinyl alcohol are that 6Kg, shitosan are5Kg, carboxymethyl cellulose are 9Kg, add the deionized water of 3 times of weight after above-mentioned each composition is mixed, stir,After being stirred to evenly, the aqueous solution is carried out to vacuum drying, the collagen membrane material for preparing after vacuum drying.
Embodiment 5
(1) preparation of perch collagen:
Perch fish-skin and perch are peeled off, after peeling off, perch fish-skin is cleaned by deionized water, clean 3 times, cleanAfter fish-skin is carried out to vacuum drying, after vacuum drying, fish-skin is ground, carry out ultrasonic agitation hot dipping by acid solution and carry, acid solution is 5wt%Citric acid solution, the weight ratio of acid solution and perch fish-skin powder is 8:1, hot extraction temperature is 50 DEG C, ultrasonic power is 200w,Extraction time is 4h, carries out centrifugally after extraction, and centrifugal rear collection upper strata viscous fluid, is adjusted to upper strata viscous fluid with potassium hydroxidePH is 6.5, leaves standstill 12h, and centrifugal rear collection flocculation sediment, carries out precipitation after freeze drying, to prepare perch fish skin collagenAlbumen;
(2) preparation of medical collagen membrane material:
Getting by weight perch collagen prepared by step (1) is that 20Kg, polyvinyl alcohol are that 7Kg, shitosan are6Kg, carboxymethyl cellulose are 8Kg, add the deionized water of 3 times of weight after above-mentioned each composition is mixed, stir,After being stirred to evenly, the aqueous solution is carried out to vacuum drying, the collagen membrane material for preparing after vacuum drying.
Comparative example
License notification number is the patent of invention of CN101264337, with reference to the preparation method of embodiment 1, gets processingAfter Animal Skin add water to regulate after pH and smash slurry, after processing with stomach cardia, use again acetum processing, finally get gel layer and carry out lowAfter temperature freeze drying, it is membranaceous porous fibrous material.
The anti-tensile of the medical collagen membrane material of embodiments of the invention 1 to 5 and the membranaceous porous fibrous material of comparative example is strongDegree and elongation at break are as shown in the table:
Medical collagen membrane material of the present invention on tensile strength and elongation at break all significantly higher than in comparative exampleMembranaceous porous fibrous material, and possess very good biocompatibility, can be used as medical material for many medical science necksIn territory, as tissue engineering material, cell culture material etc.
Claims (6)
1. a preparation method for medical collagen membrane material, preparation method's bag of the medical collagen membrane material described in it is characterized in thatDraw together following steps:
(1) preparation of perch collagen:
Perch fish-skin and perch are peeled off, after peeling off, perch fish-skin is cleaned by deionized water, clean 3 times, will after cleaningFish-skin carries out vacuum drying, after vacuum drying, fish-skin is ground, and carries out ultrasonic agitation hot dipping carry by acid solution, and acid solution is 5wt%-The citric acid solution of 8wt%, the weight ratio of acid solution and perch fish-skin powder is 8:1-12:1, and hot extraction temperature is 50-60 DEG C, superAcoustical power is 100w-200w, and extraction time is 3h-4h, carries out centrifugal after extraction, and collected after centrifugation upper strata viscous fluid, by upper strataIt is 6.5 that viscous fluid potassium hydroxide is adjusted to pH, and leave standstill 12h, collected after centrifugation flocculation sediment, carries out freeze drying by precipitationAfter, prepare perch collagen;
0.060000
Getting by weight perch collagen prepared by step (1) is that 14-24 part, polyvinyl alcohol are that 4-8 part, shitosan are 3-7 parts, carboxymethyl cellulose are 5-11 part, add the deionized water of 3 times of weight after above-mentioned each composition is mixed, and stirMixing, the aqueous solution is carried out to vacuum drying after being stirred to evenly, is the collagen membrane material of preparation after vacuum drying.
2. the preparation method of a kind of medical collagen membrane material according to claim 1, is characterized in that described medical adhesiveIn the preparation method of former membrane material, vacuum drying temperature is 55 DEG C, and vacuum is 5Pa-200Pa.
3. the preparation method of a kind of medical collagen membrane material according to claim 1, is characterized in that described medical adhesiveThe citric acid solution that acid solution in the preparation method of former membrane material in perch collagen leaching process is 6wt%.
4. the preparation method of a kind of medical collagen membrane material according to claim 1, is characterized in that described medical adhesiveIn the preparation method of former membrane material, the weight ratio of acid solution and perch fish-skin powder is 10:1.
5. the preparation method of a kind of medical collagen membrane material according to claim 1, is characterized in that described medical adhesiveIn the preparation method of former membrane material perch collagen be 17-20 part, polyvinyl alcohol be 5-7 part, shitosan be 4-6 part,Carboxymethyl cellulose is 8-10 part.
6. the preparation method of a kind of medical collagen membrane material according to claim 1, is characterized in that described medical adhesiveIn the preparation method of former membrane material, ultrasonic power is 150w.
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| CN106334212A (en) * | 2016-10-09 | 2017-01-18 | 常州亚环环保科技有限公司 | Method for preparing medical tissue glue |
| CN107375248A (en) * | 2017-06-07 | 2017-11-24 | 常州欧康铭化工有限公司 | A kind of wound is with to medicine film |
| CN109265535A (en) * | 2017-07-17 | 2019-01-25 | 大连海洋大学 | The preparation method of collagen |
| CN108653798A (en) * | 2018-06-29 | 2018-10-16 | 中山大学附属第医院 | Composition for hemostasis and medical hemostatic material |
| CN110079098A (en) * | 2019-03-12 | 2019-08-02 | 四川厚诚新材料有限公司 | A kind of multipurpose film of casting method preparation easily takes off material and its application |
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| US7285520B2 (en) * | 2003-12-01 | 2007-10-23 | Kimberly-Clark Worldwide, Inc. | Water disintegratable cleansing wipes |
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| CN102108211A (en) * | 2009-12-28 | 2011-06-29 | 沈阳鑫盛生物科技有限公司 | Chitosan collagen gel and application thereof |
| CN101942204A (en) * | 2010-09-16 | 2011-01-12 | 集美大学 | Production method of collagen membrane |
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