CN1348820A - Coremia-resisting wound protecting film and its prepn - Google Patents

Coremia-resisting wound protecting film and its prepn Download PDF

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Publication number
CN1348820A
CN1348820A CN 01134165 CN01134165A CN1348820A CN 1348820 A CN1348820 A CN 1348820A CN 01134165 CN01134165 CN 01134165 CN 01134165 A CN01134165 A CN 01134165A CN 1348820 A CN1348820 A CN 1348820A
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film
solution
additive
antibacterial
coremia
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CN1187098C (en
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张幼珠
吴徵宇
田保中
王建民
徐帼英
廖镇江
贾生贤
朱德安
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Suzhou University
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Suzhou University
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Abstract

The present invention relates to medical material for covering wound surface. Natural silk is used as main membrane forming material, adding antibacterial agent and additive, with hydrostomia method to coat layer by layer. Then it is dried to obtain the invented protective membrane for wound surface. Said protective membrane not only is aseptic, non-toxic, no irritation and sensitization, but also possesses good tissue compatibity and is adhesive with wound surface.

Description

A kind of Coremia-resisting wound protecting film and preparation method thereof
The present invention relates to the medical material that a kind of wound surface covers, particularly a kind ofly be main material of preparing, contain Wound surface protection film of antibacterial and preparation method thereof with fibroin albumen.
Before the present invention makes, publication number is the Chinese invention patent " a kind of Wound surface protection film and preparation method thereof " of CN1121836, disclosing a kind of is main film forming raw material with silkworm silk, the Wound surface protection film that adjuvants such as adding additive are prepared from, the process for preparing this Wound surface protection film is: earlier silkworm silk is heated in degumming liquid, slough the sericin of silkworm silk periphery, obtain fibroin albumen; Then, with the fibroin albumen heating for dissolving in solvent after the oven dry, make silk fibroin protein solution; Again silk fibroin protein solution is dialysed, filtered, carry out purification processing, obtain pure silk fibroin protein solution; At last, in pure silk fibroin protein solution, add additive, mix homogeneously; be injected in the film die, with promptly getting fibroin protein film behind 40~60 ℃ of hot blast dryings, fibroin protein film is processed into certain specification on demand after; packing, sterilization promptly get the Wound surface protection film finished product.The Wound surface protection film that makes with said method; good permeable, steam permeability reach and the performances such as bonding force of wound surface though have; but can't treat infective wound surface because of no bactericidal action, limit the use of clinically in early stage nothing and infect wound surface and aseptic operation wound surface, as skin donor site.
The objective of the invention is to overcome the deficiency that Wound surface protection film in the prior art exists no bactericidal action, provide a kind of both good, have Wound surface protection film of bactericidal action and preparation method thereof again with human compatibility.
The technology implementation scheme that realizes the object of the invention is: a kind of Coremia-resisting wound protecting film, by being that the fibroin albumen that raw material is made is that filmogen, antibacterial and additive are formed with silkworm silk, the content of fibroin albumen is 80~90%, described antibacterial is one or more in phenols, quaternary ammonium salt, sulfonamides and the organic nitrogen, and content is 1~5%; Described additive is by hygroscopic agent, and cross-linking agent is formed, and content of crosslinking agent is 10~15%, and wherein, hygroscopic agent is a kind of several in propanol, propylene glycol, glycerol, ethylene glycol, Polyethylene Glycol, the glyceryl monostearate; Cross-linking agent is one or more in citric acid, lactic acid, ethylenediaminetetraacetic acid, the epoxide.
The method for preparing described Coremia-resisting wound protecting film, be earlier silkworm silk is come unstuck, dissolving, dialysis, filtration, purification process, obtain carrying out again behind the pure silk fibroin protein solution processing of following steps:
A. antibacterial is dissolved in the polar solvent in 1: 10~30 ratio, makes antimicrobial;
B. the additive that hygroscopic agent and cross-linking agent are formed is dissolved in the normal saline in 1: 5~20 ratio, makes additive solution;
C. with pure silk fibroin protein solution and antimicrobial, additive solution uniform mixing, make and be mixed into coating solution;
D. with pure silk fibroin protein solution or the coating solution system of being mixed into film, make the counterdie that thickness is 0.002~0.006mm after the drying;
E. on counterdie, adopt the sialorrhea method will be mixed into coating solution and drip, be coated with fabric film; repeat this step 10~60 times behind the drying and forming-film; be prepared into the Coremia-resisting wound protecting film that thickness is 0.02~0.06mm, wherein the content of antibacterial is 0.1~1.0 milligram in every square centimeter of fibroin protein film.
Above-described one-tenth membrane drying process is a hot-air seasoning, and baking temperature is 30~40 ℃.
Coremia-resisting wound protecting film provided by the present invention owing to be primary raw material with silkworm silk, therefore, with human body have the favorable tissue compatibility, permeable steam permeability and with the bonding force of wound surface; Especially in film, contain a certain amount of antibacterial, therefore, wound surface is had good sterilization and anti-infectious function; Also because adopted the processing method of layering sialorrhea, coating film forming, smooth smooth, the thickness homogeneous of finished film makes antibacterial being evenly distributed in Wound surface protection film, and can effectively control the release of antibacterial.
Because fibroin albumen is quite pure native protein, the aminoacid of fibroin albumen is formed with the collagen protein that constitutes human body skin bigger similarity, and thus, Wound surface protection film and the human body made with it have the good tissue compatibility, aseptic, nontoxic, and to skin non-stimulated and sensitization; It also have good permeable steam permeability and with the bonding force of wound surface.In Coremia-resisting wound protecting film, contain antibacterial and additive, used antibacterial is the non-antibiotic class, its has a broad antifungal spectrum, the common staphylococcus aureus of infective wound surface, escherichia coli and bacillus pyocyaneus are had good killing action, and little to the human body side effect, toxicity is low, skin is had no stimulation, have good light, heat stability, good with the filmogen compatibility, separately performance is independent of each other after the mixing; Adopt the film build method of substep sialorrhea coating, antibacterial is evenly distributed in protecting film, and can control the release of antibacterial, initial release concentration is bigger, so that release concentration surpasses its minimum bactericidal concentration and has good bactericidal action, subsequently, the antibacterial in the protecting film discharges sustainably, keeps the effect of long period; Simultaneously, because the sialorrhea coating film forming is thin, therefore, drying and forming-film has at a lower temperature guaranteed the bactericidal effect of antibacterial.The outward appearance of this Coremia-resisting wound protecting film is translucent, and thickness is even, and is pliable and tough, smooth, smooth, meet water do not dissolve, not damaged, use very convenient.
Coremia-resisting wound protecting film of the present invention and preparation method thereof can be further specified by following examples:
Embodiment one:
1,1 kilogram of silkworm silk being put into 30 liters of concentration is 0.05% aqueous sodium carbonate, boils 0.5 hour, and the sericin of most silkworm silk periphery is taken off in reprocessing three times, obtains fibroin;
2, with exsiccant fibroin, be 1: 8: 2 calcium chloride, water, alcoholic solution with 6 liters of mol ratios, become silk fibroin protein solution 78 ± 2 ℃ of following heating for dissolving;
3, with the cellophane membrane dialysis, the fibroin albumen mixed solution of gained is dialysed to deionized water, to remove calcium chloride, ethanol, reuse multilamellar absorbent carbasus filters, and makes pure silk fibroin protein solution;
4,25 gram sulfonamides antibacterial are dissolved in 500 ml physiological salines, make antimicrobial;
5, the ratio of 70 gram glycerol in 1: 5 is dissolved in the normal saline, the ratio of 15 gram citric acids in 1: 10 is dissolved in the normal saline, and then, makes additive solution above-mentioned two kinds of solution mixing and stirring;
6, will be added in the container by step 1~3 prepared pure silk fibroin solution, and add the antimicrobial that step 4 makes, and stir after one hour, the additive solution that again step 5 is made adds, and at room temperature stirs half an hour, makes and is mixed into coating solution;
7, with pure silk fibroin solution film forming on the one-tenth film container,, be processed into the counterdie that thickness is 0.003mm with 50 ℃ hot blast drying;
8, adopt the sialorrhea method to drip on counterdie and be mixed into coating solution, coating evenly behind the drying and forming-film, repeats this step 20 times in 35 ℃ hot blast, make the fibroin protein film that contains antibacterial;
9, the fibroin protein film that will contain antibacterial after moisture equilibrium at dry side is cut into 10 * 20 centimetres 2Specification, about 0.04 millimeter of thickness is packed and is sealed on the high frequency sealing machine with the double-layer plastic bag, with the gamma-ray irradiation sterilization, is finished product then.
With the principle of layering coating film forming, can adjust the thickness of film as required.
Embodiment two:
1,0.5 kilogram of leftover bits and pieces silkworm silk being put into 15 liters of concentration is 0.05% aqueous sodium carbonate, boils 0.5 hour, and the sericin of most silkworm silk periphery is taken off in reprocessing three times, obtains fibroin;
2, be 1: 8: 2 calcium chloride, water, alcoholic solution with exsiccant fibroin with 3 liters of mol ratios, become the fibroin albumen mixed solution 78 ± 2 ℃ of following heating for dissolving;
3, with the cellulose membrane dialysis, the fibroin albumen mixed solution of gained is dialysed to deionized water, to remove calcium chloride, ethanol, reuse multilamellar absorbent carbasus filters, and makes pure silk fibroin protein solution;
4,10 gram organic nitrogens and 5 gram sulfonamides antibacterial being dissolved in 300 ml concns is in 5% the glycerol solvent, to make antimicrobial;
5,20 gram glyceryl monostearates and 10 gram lactic acid all are dissolved in the normal saline respectively in 1: 10 ratio, and then, make additive solution above-mentioned two kinds of solution mixing and stirring;
6, will be added in the container by step 1~3 prepared pure silk fibroin solution, and add the antimicrobial that step 4 makes then, and stir after one hour, the additive solution that again step 5 is made adds, and at room temperature stirs half an hour, makes and is mixed into coating solution;
7, the prepared coating solution film forming in becoming film container that is mixed into,, be processed into the counterdie that thickness is 0.002mm with 40 ℃ hot blast drying;
8, adopting the sialorrhea method to drip on counterdie and be mixed into coating solution, after coating is even, is drying and forming-film in 35 ℃ the hot blast in temperature, and the duplicate step 40 of laying equal stress on time makes the fibroin protein film that contains antibacterial;
9, the fibroin protein film that will contain antibacterial after moisture equilibrium at dry side is cut into 10 * 20cm 2Specification, the about 0.05mm of thickness packs and seals on the high frequency sealing machine with the double-layer plastic bag, with the gamma-ray irradiation sterilization, is finished product then.
All can to obtain with silkworm silk be primary raw material, contain the fibroin Wound surface protection film of antibacterial by above embodiment one, two described process operations, and wherein fibroin albumen content is 80~90%, contains 0.1~1.0 milligram of antibacterial on every square centimeter of fibroin protein film.
The Wound surface protection film of made of the present invention has been used over one hundred routine patient's wound surface clinically at burn, clinical practice shows, aseptic nontoxic, no skin irritation of this protecting film and sensitization, have good pliability, permeable steam permeability and with the bonding force of wound surface, can alleviate wound pain; This protecting film has antibiotic and quickens the effect of wound healing, therefore can be used for the treatment of infective wound surface and deep ii degree burn wound surface, and curative effect is good.Table 1 is the contrast of Coremia-resisting wound protecting film of the present invention and prior art fibroin Wound surface protection film technical specification, and result of use can be done concrete statement by table 1.Table 1
Figure A0113416500101
Annotate: in the table "+" number expression effectively, "-" number expression is invalid.

Claims (3)

1. Coremia-resisting wound protecting film, by being that the fibroin albumen that raw material is made is that filmogen, antibacterial and additive are formed with silkworm silk, the content of fibroin albumen is 80~90%, it is characterized in that: described antibacterial is one or more in phenols, quaternary ammonium salt, sulfonamides and the organic nitrogen, and content is 1~5%; Described additive is by hygroscopic agent, and cross-linking agent is formed, and hygroscopic agent is one or more in propanol, propylene glycol, glycerol, ethylene glycol, Polyethylene Glycol, the glyceryl monostearate; Cross-linking agent is one or more in citric acid, lactic acid, ethylenediaminetetraacetic acid, the epoxide, and additive level is 10~15%.
2. method for preparing Coremia-resisting wound protecting film as claimed in claim 1, earlier with silkworm silk through come unstuck, dissolving, dialysis, filtration, purification process, obtain pure silk fibroin protein solution after, it is characterized in that carrying out again the processing of following steps:
A. antibacterial is dissolved in the polar solvent in 1: 10~30 ratio, makes antimicrobial;
B. the additive that hygroscopic agent and cross-linking agent are formed is dissolved in the normal saline in 1: 5~20 ratio, makes additive solution;
C. pure silk fibroin solution and antimicrobial, additive solution are uniformly mixed to form and are mixed into coating solution;
D. with pure silk fibroin solution or the coating solution system of being mixed into film, make the counterdie that thickness is 0.002~0.006mm after the drying;
E. on counterdie, adopt the sialorrhea method will be mixed into coating solution and drip, be coated with fabric film; repeat this step 10~60 times behind the drying and forming-film; be prepared into the Coremia-resisting wound protecting film that thickness is 0.02~0.06mm, wherein the content of antibacterial is 0.1~1.0 milligram in every square centimeter of fibroin protein film.
3. the method for preparing Coremia-resisting wound protecting film according to claim 2 is characterized in that: the dry hot-air seasoning that adopts, baking temperature is 30~40 ℃.
CNB011341653A 2001-11-10 2001-11-10 Coremia-resisting wound protecting film and its prepn Expired - Fee Related CN1187098C (en)

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Cited By (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100342924C (en) * 2004-10-13 2007-10-17 苏州苏豪生物材料科技有限公司 Skin substitute and its preparation method
CN100371027C (en) * 2004-12-02 2008-02-27 华子昂 Biological sterilizeld sanitary napkins and functional biological material therefor
CN101053670B (en) * 2007-04-03 2011-02-02 浙江理工大学 Silk fibroin and polymeric lactic acid compound film and its preparation method
CN102133425A (en) * 2011-03-13 2011-07-27 苏州大学 Tussah silk fibroin film and preparation method thereof
CN102271724A (en) * 2008-10-09 2011-12-07 塔夫茨大学信托人 Modified silk films containing glycerol
CN101545199B (en) * 2009-04-22 2011-12-21 苏州大学 Antibiosis processing method of silk fiber or fabric thereof
CN102319448A (en) * 2011-09-16 2012-01-18 华中科技大学 Antibacterial aquagel material for preparing medical wound dressing and preparation method thereof
US8476483B2 (en) 2006-12-13 2013-07-02 Unicharm Corporation Antibacterial sheet and absorbent article
CN107308490A (en) * 2017-06-07 2017-11-03 常州市天宁区鑫发织造有限公司 A kind of preparation method of liquid antibiotic wound-protecting film
CN108316018A (en) * 2018-03-15 2018-07-24 南通纺织丝绸产业技术研究院 A kind of preparation method of fibroin albumen/chitosan functional solution
CN108478850A (en) * 2018-02-01 2018-09-04 束河医疗科技江苏有限公司 A kind of regenerated silk fibroin hydrogel bandage and the preparation method and application thereof
CN110448715A (en) * 2019-09-03 2019-11-15 西南大学 A kind of preparation method of the medical dressing containing curcumin based on fibroin albumen
CN115105634A (en) * 2022-06-27 2022-09-27 西北有色金属研究院 Process for preparing composite coating with timeliness for orthopedics department
CN115233445A (en) * 2022-08-25 2022-10-25 浙江理工大学 Method for visible light catalytic anti-bacterial durable finishing of real silk

Cited By (18)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100342924C (en) * 2004-10-13 2007-10-17 苏州苏豪生物材料科技有限公司 Skin substitute and its preparation method
CN100371027C (en) * 2004-12-02 2008-02-27 华子昂 Biological sterilizeld sanitary napkins and functional biological material therefor
US8476483B2 (en) 2006-12-13 2013-07-02 Unicharm Corporation Antibacterial sheet and absorbent article
CN101562970B (en) * 2006-12-13 2013-07-10 尤妮佳股份有限公司 Antibacterial sheet and absorbent article
CN101053670B (en) * 2007-04-03 2011-02-02 浙江理工大学 Silk fibroin and polymeric lactic acid compound film and its preparation method
CN102271724A (en) * 2008-10-09 2011-12-07 塔夫茨大学信托人 Modified silk films containing glycerol
CN102271724B (en) * 2008-10-09 2015-10-14 塔夫茨大学信托人 Modification cortina containing glycerol
US10493179B2 (en) 2008-10-09 2019-12-03 Trustees Of Tufts College Modified silk films containing glycerol
CN101545199B (en) * 2009-04-22 2011-12-21 苏州大学 Antibiosis processing method of silk fiber or fabric thereof
CN102133425A (en) * 2011-03-13 2011-07-27 苏州大学 Tussah silk fibroin film and preparation method thereof
CN102319448A (en) * 2011-09-16 2012-01-18 华中科技大学 Antibacterial aquagel material for preparing medical wound dressing and preparation method thereof
CN107308490A (en) * 2017-06-07 2017-11-03 常州市天宁区鑫发织造有限公司 A kind of preparation method of liquid antibiotic wound-protecting film
CN108478850A (en) * 2018-02-01 2018-09-04 束河医疗科技江苏有限公司 A kind of regenerated silk fibroin hydrogel bandage and the preparation method and application thereof
CN108316018A (en) * 2018-03-15 2018-07-24 南通纺织丝绸产业技术研究院 A kind of preparation method of fibroin albumen/chitosan functional solution
CN110448715A (en) * 2019-09-03 2019-11-15 西南大学 A kind of preparation method of the medical dressing containing curcumin based on fibroin albumen
CN115105634A (en) * 2022-06-27 2022-09-27 西北有色金属研究院 Process for preparing composite coating with timeliness for orthopedics department
CN115105634B (en) * 2022-06-27 2023-09-19 西北有色金属研究院 Process for preparing composite coating with timeliness for orthopedics
CN115233445A (en) * 2022-08-25 2022-10-25 浙江理工大学 Method for visible light catalytic anti-bacterial durable finishing of real silk

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