CN112516373B - Surgical hemostatic cotton containing polyvinyl alcohol and preparation method thereof - Google Patents
Surgical hemostatic cotton containing polyvinyl alcohol and preparation method thereof Download PDFInfo
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- A61L24/00—Surgical adhesives or cements; Adhesives for colostomy devices
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- A61L24/00—Surgical adhesives or cements; Adhesives for colostomy devices
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- 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
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- A61L24/00—Surgical adhesives or cements; Adhesives for colostomy devices
- A61L24/04—Surgical adhesives or cements; Adhesives for colostomy devices containing macromolecular materials
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- A61L24/00—Surgical adhesives or cements; Adhesives for colostomy devices
- A61L24/04—Surgical adhesives or cements; Adhesives for colostomy devices containing macromolecular materials
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- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/20—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing organic materials
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- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
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- 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
- A61L2300/412—Tissue-regenerating or healing or proliferative agents
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Abstract
The invention is applicable to the technical field of medical treatment, and provides a surgical hemostatic cotton containing polyvinyl alcohol and a preparation method thereof, wherein the hemostatic cotton comprises the following raw materials in parts by weight: 26-37 parts of polyvinyl alcohol, 18-28 parts of aldehyde dextran, 15-27 parts of chitosan compound, 8-13 parts of lysine, 3-5 parts of casein, 1-4 parts of plasticizer, 1-3 parts of antioxidant and 2-4 parts of penetration enhancer; the aldehyde group glucan and the chitosan compound are compounded, and then the aldehyde group glucan and the chitosan compound are matched with the polyvinyl alcohol to play a role in synergy, so that the blood adsorbability, the blood coagulation performance and the antibacterial performance are greatly improved.
Description
Technical Field
The invention belongs to the field of medical treatment, and particularly relates to a surgical hemostatic cotton containing polyvinyl alcohol and a preparation method thereof.
Background
Blood is one of the important components of the human body, accounting for about 8% of the adult body weight, corresponding to 70-80 ml of blood per kg of body weight, and about 5L of blood for an adult (about 70 kg). It undertakes the material exchange of all tissues and organs of the human body, and if the amount of bleeding exceeds more than 30% of the total blood in a short time, the human body will die due to excessive blood loss. In the death incidents such as traffic accidents, natural disasters, war and the like, most of the accidents are caused by uncontrollable bleeding, so that effective hemostasis has an important function for saving the lives of patients, and the application of hemostatic materials cannot be avoided if the effective hemostasis is realized.
At present, after various artery and vein puncture and catheter extraction operations in hospitals, compression hemostasis is needed to be carried out on wounds. The most widely applied compression hemostasis mode in hospitals is that medical staff adopt gauze to perform compression hemostasis. Medical personnel superimpose gauze over the wound and then use bandages or straps to secure. Such a way of operation has drawbacks: firstly, the bandage or the bandage does not have extensibility and viscosity, and can not automatically give compression force, so that after the bandage or the bandage is fixed, the compression force can be lost if the bandage or the bandage is not tightly bound, and gauze can possibly move if a patient moves; secondly, the gauze has poor blood absorption performance, is easy to infect wounds and realizes the compression of the wounds only by the compression force given by bandages or bands.
At present, the rapid hemostatic materials include zeolite, gelatin, collagen, polysaccharides, polypeptides, polyvinyl alcohol, graphene and the like. These materials vary in origin and in hemostatic mechanisms, but they are generally classified into 3 types: the first category, which accelerates the physiological process of hemostasis by rapidly increasing the concentration of factors involved in coagulation in the blood in the vicinity of the wound (either physically or chemically) within a short time; the second, direct activation or involvement in the coagulation system by the material itself or released factors; third, the vessels are physically sealed by strong adhesion.
However, when acute bleeding or surgical bleeding is encountered, the hemostasis speed and the hemostasis amount of the common hemostatic material cannot meet the requirement of emergency treatment during massive rapid bleeding, and meanwhile, the common hemostatic material has a common antibacterial treatment effect on wounds.
Disclosure of Invention
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The embodiment of the invention is realized in such a way that the surgical hemostatic cotton containing polyvinyl alcohol comprises the following raw materials in parts by weight: 26-37 parts of polyvinyl alcohol, 18-28 parts of aldehyde dextran, 15-27 parts of chitosan compound, 8-13 parts of lysine, 3-5 parts of casein, 1-4 parts of plasticizer, 1-3 parts of antioxidant and 2-4 parts of penetration enhancer;
the chitosan complex is prepared by the following method:
dissolving 2.00g of chitosan in 350ml of 1% acetic acid solution, stirring for 1h, neutralizing with 0.1mol/ml NaOH solution to generate a transparent colloid, filtering with a floxacin funnel, washing residual NaOH with sufficient distilled water, drying, and fully grinding the product;
adding 1.00g of treated chitosan into a 100ml flask, adding 50ml of N, N-dimethylformamide aqueous solution, vigorously stirring for 24h, transferring the flask into a heat collection type constant temperature magnetic stirrer, controlling the temperature to be 70 ℃, dropwise adding 50ml of N, N-dimethylformamide solution (epoxy group; chitosan amino =1: 1.5) containing 1.9g of epoxy thiacalixarene into the flask, reacting for 24h, evaporating the solvent under reduced pressure, washing residues with a small amount of trichloromethane and distilled water, drying in vacuum to obtain a final product, and fully grinding the product.
As a further scheme of the invention: the feed comprises the following raw materials in parts by weight: 28-35 parts of polyvinyl alcohol, 20-26 parts of aldehyde dextran, 17-25 parts of chitosan compound, 8-12 parts of lysine, 3-4 parts of casein, 2-4 parts of plasticizer, 2-3 parts of antioxidant and 2-4 parts of permeation enhancer.
As a further scheme of the invention: the feed comprises the following raw materials in parts by weight: 30-34 parts of polyvinyl alcohol, 20-22 parts of aldehyde dextran, 20-23 parts of chitosan compound, 10-12 parts of lysine, 3-4 parts of casein, 3-4 parts of plasticizer, 2-3 parts of antioxidant and 3-4 parts of permeation enhancer.
As a further scheme of the invention: the feed comprises the following raw materials in parts by weight: 32 parts of polyvinyl alcohol, 20 parts of aldehyde dextran, 22 parts of chitosan compound, 11 parts of lysine, 4 parts of casein, 4 parts of plasticizer, 2 parts of antioxidant and 3 parts of penetration enhancer.
As a further scheme of the invention: the aldehyde dextran is prepared by the following method: oxidizing glucan in an aqueous solution by sodium periodate under a dark condition, and reacting for 18-30 h at room temperature; adding the reaction solution into a 9-14 kDa dialysis bag for dialysis for 4-10 times, and freeze-drying to obtain aldehyde group glucan, wherein the aldehyde group content is 15% -95%; the molecular weight of the glucan is 20kDa to 150 kDa.
A preparation method of surgical hemostatic cotton containing polyvinyl alcohol comprises the following steps:
1) preparing raw materials in parts by weight: 26-37 parts of polyvinyl alcohol, 18-28 parts of aldehyde dextran, 15-27 parts of chitosan compound, 8-13 parts of lysine, 3-5 parts of casein, 1-4 parts of plasticizer, 1-3 parts of antioxidant and 2-4 parts of penetration enhancer;
2) compounding aldehyde group glucan and a chitosan compound to form a mixed solution A;
3) dissolving polyvinyl alcohol and lysine in water, adding casein, and heating and stirring to obtain a mixed solution B;
4) adding the mixed solution A into the mixed solution B, continuously stirring, and slowly adding a plasticizer, an antioxidant and a penetration enhancer to obtain a mixed solution C;
5) and pouring the mixed solution C into a mold, pre-freezing, freeze-drying until the sol is freeze-dried, swelling, and freeze-drying again to obtain the porous hemostatic cotton.
As a further scheme of the invention: in the step 3), the heating temperature is 30-40 ℃.
As a further scheme of the invention: in the step 5), the swelling process comprises the following steps: and (3) soaking the sol sample after freeze drying in a calcium chloride solution, wherein the concentration of the calcium chloride solution is 0-0.05 g/ml, and the swelling multiple is 30-200 times.
According to the surgical hemostatic cotton containing polyvinyl alcohol, the aldehyde group glucan has excellent antibacterial and wound healing promoting performances due to the aldehyde group structure; in the chitosan compound, chitosan and epoxy thiacalixarene are subjected to crosslinking reaction, so that the adsorbability is greatly improved; the aldehyde group glucan and the chitosan compound are compounded, and then the aldehyde group glucan and the chitosan compound are matched with the polyvinyl alcohol to play a role in synergy, so that the blood adsorbability, the blood coagulation performance and the antibacterial performance are greatly improved.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The medical grade polyvinyl alcohol is an extremely safe high molecular organic matter, has no toxicity or side effect on a human body, has good biocompatibility, and can be particularly used for hemostasis on wound dressings.
The aldehyde group structure of the aldehyde group glucan has excellent antibacterial and wound healing promoting performances; in the chitosan compound, chitosan and epoxy thiacalixarene are subjected to crosslinking reaction, so that the adsorbability is greatly improved; after the aldehyde group glucan and the chitosan compound are compounded, the wound healing promoting performance is greatly improved.
In the embodiment of the invention, the surgical hemostatic cotton containing polyvinyl alcohol comprises the following raw materials in parts by weight: 26-37 parts of polyvinyl alcohol, 18-28 parts of aldehyde dextran, 15-27 parts of chitosan compound, 8-13 parts of lysine, 3-5 parts of casein, 1-4 parts of plasticizer, 1-3 parts of antioxidant and 2-4 parts of penetration enhancer;
the chitosan complex is prepared by the following method:
dissolving 2.00g of chitosan in 350ml of 1% acetic acid solution, stirring for 1h, neutralizing with 0.1mol/ml NaOH solution to generate a transparent colloid, filtering with a floxacin funnel, washing residual NaOH with sufficient distilled water, drying, and fully grinding the product;
adding 1.00g of treated chitosan into a 100ml flask, adding 50ml of N, N-dimethylformamide aqueous solution, vigorously stirring for 24h, transferring the flask into a heat collection type constant temperature magnetic stirrer, controlling the temperature to be 70 ℃, dropwise adding 50ml of N, N-dimethylformamide solution (epoxy group; chitosan amino =1: 1.5) containing 1.9g of epoxy thiacalixarene into the flask, reacting for 24h, evaporating the solvent under reduced pressure, washing residues with a small amount of trichloromethane and distilled water, drying in vacuum to obtain a final product, and fully grinding the product.
The invention also provides a preparation method of the surgical hemostatic cotton containing the polyvinyl alcohol, which comprises the following steps:
1) preparing raw materials in parts by weight: 26-37 parts of polyvinyl alcohol, 18-28 parts of aldehyde dextran, 15-27 parts of chitosan compound, 8-13 parts of lysine, 3-5 parts of casein, 1-4 parts of plasticizer, 1-3 parts of antioxidant and 2-4 parts of penetration enhancer;
2) compounding aldehyde group glucan and a chitosan compound to form a mixed solution A;
3) dissolving polyvinyl alcohol and lysine in water, adding casein, and heating and stirring to obtain a mixed solution B;
4) adding the mixed solution A into the mixed solution B, continuously stirring, and slowly adding a plasticizer, an antioxidant and a penetration enhancer to obtain a mixed solution C;
5) and pouring the mixed solution C into a mold, pre-freezing, freeze-drying until the sol is freeze-dried, swelling, and freeze-drying again to obtain the porous hemostatic cotton.
The technical effects of the hemostatic cotton for operation containing polyvinyl alcohol of the present invention will be further described with reference to the following specific examples, but the specific implementation methods mentioned in these examples are only illustrative and explanatory of the technical solution of the present invention, and do not limit the implementation scope of the present invention, and all modifications and substitutions based on the above principles should be within the protection scope of the present invention.
Example 1
Dissolving 2.00g of chitosan in 350ml of 1% acetic acid solution, stirring for 1h, neutralizing with 0.1mol/ml NaOH solution to generate a transparent colloid, filtering with a floxacin funnel, washing residual NaOH with sufficient distilled water, drying, and fully grinding the product; adding 1.00g of treated chitosan into a 100ml flask, adding 50ml of N, N-dimethylformamide aqueous solution, violently stirring for 24h, moving the flask into a heat collection type constant temperature magnetic stirrer, controlling the temperature to be 70 ℃, dropwise adding 50ml of N, N-dimethylformamide solution (epoxy group; chitosan amino =1: 1.5) containing 1.9g of epoxy thiacalixarene into the flask, reacting for 24h, evaporating the solvent under reduced pressure, washing residues with a small amount of trichloromethane and distilled water, drying in vacuum to obtain a final product, and fully grinding the product to obtain a chitosan compound for later use; oxidizing glucan in an aqueous solution by sodium periodate under a dark condition, and reacting for 18-30 h at room temperature; adding the reaction solution into a 9-14 kDa dialysis bag for dialysis for 4-10 times, and freeze-drying to obtain aldehyde group glucan for later use; preparing raw materials in parts by weight: 26 parts of polyvinyl alcohol, 18 parts of aldehyde dextran, 15 parts of chitosan compound, 8 parts of lysine, 3 parts of casein, 1 part of ethylene glycol, 1 part of chitin and 2 parts of peppermint oil; compounding aldehyde group glucan and a chitosan compound to form a mixed solution A; dissolving polyvinyl alcohol and lysine in water, adding casein, and heating and stirring to obtain a mixed solution B; adding the mixed solution A into the mixed solution B, continuously stirring, and slowly adding a plasticizer, chitin and peppermint oil to obtain a mixed solution C; and pouring the mixed solution C into a mold, pre-freezing, freeze-drying until the sol is freeze-dried, swelling, and freeze-drying again to obtain the porous hemostatic cotton.
Example 2
Dissolving 2.00g of chitosan in 350ml of 1% acetic acid solution, stirring for 1h, neutralizing with 0.1mol/ml NaOH solution to generate a transparent colloid, filtering with a floxacin funnel, washing residual NaOH with sufficient distilled water, drying, and fully grinding the product; adding 1.00g of treated chitosan into a 100ml flask, adding 50ml of N, N-dimethylformamide aqueous solution, violently stirring for 24h, moving the flask into a heat collection type constant temperature magnetic stirrer, controlling the temperature to be 70 ℃, dropwise adding 50ml of N, N-dimethylformamide solution (epoxy group; chitosan amino =1: 1.5) containing 1.9g of epoxy thiacalixarene into the flask, reacting for 24h, evaporating the solvent under reduced pressure, washing residues with a small amount of trichloromethane and distilled water, drying in vacuum to obtain a final product, and fully grinding the product to obtain a chitosan compound for later use; oxidizing glucan in an aqueous solution by sodium periodate under a dark condition, and reacting for 18-30 h at room temperature; adding the reaction solution into a 9-14 kDa dialysis bag for dialysis for 4-10 times, and freeze-drying to obtain aldehyde group glucan for later use; preparing raw materials in parts by weight: 37 parts of polyvinyl alcohol, 28 parts of aldehyde dextran, 27 parts of chitosan compound, 13 parts of lysine, 5 parts of casein, 4 parts of sodium lactate, 3 parts of chitin and 4 parts of olive oil; compounding aldehyde group glucan and a chitosan compound to form a mixed solution A; dissolving polyvinyl alcohol and lysine in water, adding casein, and heating and stirring to obtain a mixed solution B; adding the mixed solution A into the mixed solution B, continuously stirring, and slowly adding a plasticizer, chitin and olive oil to obtain a mixed solution C; and pouring the mixed solution C into a mold, pre-freezing, freeze-drying until the sol is freeze-dried, swelling, and freeze-drying again to obtain the porous hemostatic cotton.
Example 3
Dissolving 2.00g of chitosan in 350ml of 1% acetic acid solution, stirring for 1h, neutralizing with 0.1mol/ml NaOH solution to generate a transparent colloid, filtering with a floxacin funnel, washing residual NaOH with sufficient distilled water, drying, and fully grinding the product; adding 1.00g of treated chitosan into a 100ml flask, adding 50ml of N, N-dimethylformamide aqueous solution, violently stirring for 24h, moving the flask into a heat collection type constant temperature magnetic stirrer, controlling the temperature to be 70 ℃, dropwise adding 50ml of N, N-dimethylformamide solution (epoxy group; chitosan amino =1: 1.5) containing 1.9g of epoxy thiacalixarene into the flask, reacting for 24h, evaporating the solvent under reduced pressure, washing residues with a small amount of trichloromethane and distilled water, drying in vacuum to obtain a final product, and fully grinding the product to obtain a chitosan compound for later use; oxidizing glucan in an aqueous solution by sodium periodate under a dark condition, and reacting for 18-30 h at room temperature; adding the reaction solution into a 9-14 kDa dialysis bag for dialysis for 4-10 times, and freeze-drying to obtain aldehyde group glucan for later use; preparing raw materials in parts by weight: 28 parts of polyvinyl alcohol, 20 parts of aldehyde dextran, 17 parts of chitosan compound, 8 parts of lysine, 3 parts of casein, 2 parts of sorbitol, 2 parts of chitin, and 2 parts of borneol and peppermint oil; compounding aldehyde group glucan and a chitosan compound to form a mixed solution A; dissolving polyvinyl alcohol and lysine in water, adding casein, and heating and stirring to obtain a mixed solution B; adding the mixed solution A into the mixed solution B, continuously stirring, and slowly adding a plasticizer, chitin, borneol and peppermint oil to obtain a mixed solution C; and pouring the mixed solution C into a mold, pre-freezing, freeze-drying until the sol is freeze-dried, swelling, and freeze-drying again to obtain the porous hemostatic cotton.
Example 4
Dissolving 2.00g of chitosan in 350ml of 1% acetic acid solution, stirring for 1h, neutralizing with 0.1mol/ml NaOH solution to generate a transparent colloid, filtering with a floxacin funnel, washing residual NaOH with sufficient distilled water, drying, and fully grinding the product; adding 1.00g of treated chitosan into a 100ml flask, adding 50ml of N, N-dimethylformamide aqueous solution, violently stirring for 24h, moving the flask into a heat collection type constant temperature magnetic stirrer, controlling the temperature to be 70 ℃, dropwise adding 50ml of N, N-dimethylformamide solution (epoxy group; chitosan amino =1: 1.5) containing 1.9g of epoxy thiacalixarene into the flask, reacting for 24h, evaporating the solvent under reduced pressure, washing residues with a small amount of trichloromethane and distilled water, drying in vacuum to obtain a final product, and fully grinding the product to obtain a chitosan compound for later use; oxidizing glucan in an aqueous solution by sodium periodate under a dark condition, and reacting for 18-30 h at room temperature; adding the reaction solution into a 9-14 kDa dialysis bag for dialysis for 4-10 times, and freeze-drying to obtain aldehyde group glucan for later use; preparing raw materials in parts by weight: 35 parts of polyvinyl alcohol, 26 parts of aldehyde dextran, 25 parts of chitosan compound, 12 parts of lysine, 4 parts of casein, 4 parts of plasticizer prepared from ethylene glycol, sodium lactate and sorbitol, 3 parts of chitin, and 4 parts of borneol and peppermint oil; compounding aldehyde group glucan and a chitosan compound to form a mixed solution A; dissolving polyvinyl alcohol and lysine in water, adding casein, and heating and stirring to obtain a mixed solution B; adding the mixed solution A into the mixed solution B, continuously stirring, and slowly adding a plasticizer, chitin, borneol and peppermint oil to obtain a mixed solution C; and pouring the mixed solution C into a mold, pre-freezing, freeze-drying until the sol is freeze-dried, swelling, and freeze-drying again to obtain the porous hemostatic cotton.
Example 5
Dissolving 2.00g of chitosan in 350ml of 1% acetic acid solution, stirring for 1h, neutralizing with 0.1mol/ml NaOH solution to generate a transparent colloid, filtering with a floxacin funnel, washing residual NaOH with sufficient distilled water, drying, and fully grinding the product; adding 1.00g of treated chitosan into a 100ml flask, adding 50ml of N, N-dimethylformamide aqueous solution, violently stirring for 24h, moving the flask into a heat collection type constant temperature magnetic stirrer, controlling the temperature to be 70 ℃, dropwise adding 50ml of N, N-dimethylformamide solution (epoxy group; chitosan amino =1: 1.5) containing 1.9g of epoxy thiacalixarene into the flask, reacting for 24h, evaporating the solvent under reduced pressure, washing residues with a small amount of trichloromethane and distilled water, drying in vacuum to obtain a final product, and fully grinding the product to obtain a chitosan compound for later use; oxidizing glucan in an aqueous solution by sodium periodate under a dark condition, and reacting for 18-30 h at room temperature; adding the reaction solution into a 9-14 kDa dialysis bag for dialysis for 4-10 times, and freeze-drying to obtain aldehyde group glucan for later use; preparing raw materials in parts by weight: 30 parts of polyvinyl alcohol, 20 parts of aldehyde dextran, 20 parts of chitosan compound, 10 parts of lysine, 3 parts of casein, 3 parts of plasticizer prepared from ethylene glycol and sodium lactate, 2 parts of chitin, 3 parts of hydroxypropyl-beta-cyclodextrin and 3 parts of borneol; compounding aldehyde group glucan and a chitosan compound to form a mixed solution A; dissolving polyvinyl alcohol and lysine in water, adding casein, and heating and stirring to obtain a mixed solution B; adding the mixed solution A into the mixed solution B, continuously stirring, and slowly adding a plasticizer, chitin, hydroxypropyl-beta-cyclodextrin and borneol to obtain a mixed solution C; and pouring the mixed solution C into a mold, pre-freezing, freeze-drying until the sol is freeze-dried, swelling, and freeze-drying again to obtain the porous hemostatic cotton.
Example 6
Dissolving 2.00g of chitosan in 350ml of 1% acetic acid solution, stirring for 1h, neutralizing with 0.1mol/ml NaOH solution to generate a transparent colloid, filtering with a floxacin funnel, washing residual NaOH with sufficient distilled water, drying, and fully grinding the product; adding 1.00g of treated chitosan into a 100ml flask, adding 50ml of N, N-dimethylformamide aqueous solution, violently stirring for 24h, moving the flask into a heat collection type constant temperature magnetic stirrer, controlling the temperature to be 70 ℃, dropwise adding 50ml of N, N-dimethylformamide solution (epoxy group; chitosan amino =1: 1.5) containing 1.9g of epoxy thiacalixarene into the flask, reacting for 24h, evaporating the solvent under reduced pressure, washing residues with a small amount of trichloromethane and distilled water, drying in vacuum to obtain a final product, and fully grinding the product to obtain a chitosan compound for later use; oxidizing glucan in an aqueous solution by sodium periodate under a dark condition, and reacting for 18-30 h at room temperature; adding the reaction solution into a 9-14 kDa dialysis bag for dialysis for 4-10 times, and freeze-drying to obtain aldehyde group glucan for later use; preparing raw materials in parts by weight: 34 parts of polyvinyl alcohol, 22 parts of aldehyde dextran, 23 parts of chitosan compound, 12 parts of lysine, 4 parts of casein, 4 parts of plasticizer made of sodium lactate and sorbitol, 3 parts of hinokitiol and 4 parts of borneol; compounding aldehyde group glucan and a chitosan compound to form a mixed solution A; dissolving polyvinyl alcohol and lysine in water, adding casein, and heating and stirring to obtain a mixed solution B; adding the mixed solution A into the mixed solution B, continuously stirring, and slowly adding a plasticizer, hinokitiol and borneol to obtain a mixed solution C; and pouring the mixed solution C into a mold, pre-freezing, freeze-drying until the sol is freeze-dried, swelling, and freeze-drying again to obtain the porous hemostatic cotton.
Example 7
Dissolving 2.00g of chitosan in 350ml of 1% acetic acid solution, stirring for 1h, neutralizing with 0.1mol/ml NaOH solution to generate a transparent colloid, filtering with a floxacin funnel, washing residual NaOH with sufficient distilled water, drying, and fully grinding the product; adding 1.00g of treated chitosan into a 100ml flask, adding 50ml of N, N-dimethylformamide aqueous solution, violently stirring for 24h, moving the flask into a heat collection type constant temperature magnetic stirrer, controlling the temperature to be 70 ℃, dropwise adding 50ml of N, N-dimethylformamide solution (epoxy group; chitosan amino =1: 1.5) containing 1.9g of epoxy thiacalixarene into the flask, reacting for 24h, evaporating the solvent under reduced pressure, washing residues with a small amount of trichloromethane and distilled water, drying in vacuum to obtain a final product, and fully grinding the product to obtain a chitosan compound for later use; oxidizing glucan in an aqueous solution by sodium periodate under a dark condition, and reacting for 18-30 h at room temperature; adding the reaction solution into a 9-14 kDa dialysis bag for dialysis for 4-10 times, and freeze-drying to obtain aldehyde group glucan for later use; preparing raw materials in parts by weight: 32 parts of polyvinyl alcohol, 20 parts of aldehyde dextran, 22 parts of chitosan compound, 11 parts of lysine, 4 parts of casein, 4 parts of plasticizer prepared from sodium lactate and sorbitol, 2 parts of chitin and 3 parts of hydroxypropyl-beta-cyclodextrin; compounding aldehyde group glucan and a chitosan compound to form a mixed solution A; dissolving polyvinyl alcohol and lysine in water, adding casein, and heating and stirring to obtain a mixed solution B; adding the mixed solution A into the mixed solution B, continuously stirring, and slowly adding a plasticizer, chitin and hydroxypropyl-beta-cyclodextrin to obtain a mixed solution C; and pouring the mixed solution C into a mold, pre-freezing, freeze-drying until the sol is freeze-dried, swelling, and freeze-drying again to obtain the porous hemostatic cotton.
Comparative example 1
Dissolving 2.00g of chitosan in 350ml of 1% acetic acid solution, stirring for 1h, neutralizing with 0.1mol/ml NaOH solution to generate a transparent colloid, filtering with a floxacin funnel, washing residual NaOH with sufficient distilled water, drying, and fully grinding the product; adding 1.00g of treated chitosan into a 100ml flask, adding 50ml of N, N-dimethylformamide aqueous solution, violently stirring for 24h, moving the flask into a heat collection type constant temperature magnetic stirrer, controlling the temperature to be 70 ℃, dropwise adding 50ml of N, N-dimethylformamide solution (epoxy group; chitosan amino =1: 1.5) containing 1.9g of epoxy thiacalixarene into the flask, reacting for 24h, evaporating the solvent under reduced pressure, washing residues with a small amount of trichloromethane and distilled water, drying in vacuum to obtain a final product, and fully grinding the product to obtain a chitosan compound for later use; preparing raw materials in parts by weight: 32 parts of polyvinyl alcohol, 22 parts of chitosan compound, 11 parts of lysine, 4 parts of casein, 4 parts of plasticizer, 2 parts of antioxidant and 3 parts of penetration enhancer; dissolving polyvinyl alcohol and lysine in water, adding casein, and heating and stirring to obtain a mixed solution B; adding the chitosan compound into the mixed solution B, continuously stirring, and slowly adding a plasticizer, an antioxidant and a penetration enhancer to obtain a mixed solution C; and pouring the mixed solution C into a mold, pre-freezing, freeze-drying until the sol is freeze-dried, swelling, and freeze-drying again to obtain the porous hemostatic cotton.
Comparative example 2
Oxidizing glucan in an aqueous solution by sodium periodate under a dark condition, and reacting for 18-30 h at room temperature; adding the reaction solution into a 9-14 kDa dialysis bag for dialysis for 4-10 times, and freeze-drying to obtain aldehyde group glucan for later use; preparing raw materials in parts by weight: 32 parts of polyvinyl alcohol, 20 parts of aldehyde dextran, 11 parts of lysine, 4 parts of casein, 4 parts of plasticizer, 2 parts of antioxidant and 3 parts of penetration enhancer; dissolving polyvinyl alcohol and lysine in water, adding casein, and heating and stirring to obtain a mixed solution B; adding aldehyde dextran into the mixed solution B, continuously stirring, and slowly adding a plasticizer, an antioxidant and a penetration enhancer to obtain a mixed solution C; and pouring the mixed solution C into a mold, pre-freezing, freeze-drying until the sol is freeze-dried, swelling, and freeze-drying again to obtain the porous hemostatic cotton.
Comparative example 3
Preparing raw materials in parts by weight: 32 parts of polyvinyl alcohol, 11 parts of lysine, 4 parts of casein, 4 parts of plasticizer, 2 parts of antioxidant and 3 parts of penetration enhancer; dissolving polyvinyl alcohol and lysine in water, adding casein, and heating and stirring to obtain a mixed solution B; continuously stirring the mixed solution B, and slowly adding a plasticizer, an antioxidant and a penetration enhancer to obtain a mixed solution C; and pouring the mixed solution C into a mold, pre-freezing, freeze-drying until the sol is freeze-dried, swelling, and freeze-drying again to obtain the porous hemostatic cotton.
Experimental example 1
The bactericidal performance and the blood coagulation performance of the hemostatic sponges prepared in examples 1-7 and comparative examples 1-3 were tested, and the specific results are shown in table 1.
TABLE 1
As can be seen from Table 1, the hemostatic cotton prepared in examples 1-7 of the present invention can effectively improve the blood adsorption of the product, promote blood coagulation, and provide the product with excellent antibacterial property by adding the aldehyde dextran and the chitosan complex for compounding; the best results of example 7 can be seen by comparing examples 1-7; compared with the experimental data of example 7, comparative example 1, comparative example 2 and comparative example 3, the test proves that the aldehyde group glucan and the chitosan compound are singly added into the hemostatic cotton, and the blood adsorbability, the blood coagulation performance and the antibacterial performance are effectively enhanced.
In conclusion, the aldehyde group structure of the aldehyde glucan has excellent antibacterial and wound healing promoting performances; in the chitosan compound, chitosan and epoxy thiacalixarene are subjected to crosslinking reaction, so that the adsorbability is greatly improved; after the aldehyde group glucan and the chitosan compound are compounded, the aldehyde group glucan and the chitosan compound are matched with polyvinyl alcohol to play a role in synergy, so that the blood adsorbability, the blood coagulation performance and the antibacterial performance are greatly improved.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (9)
1. The surgical hemostatic cotton containing polyvinyl alcohol is characterized by comprising the following raw materials in parts by weight: 26-37 parts of polyvinyl alcohol, 18-28 parts of aldehyde dextran, 15-27 parts of chitosan compound, 8-13 parts of lysine, 3-5 parts of casein, 1-4 parts of plasticizer, 1-3 parts of antioxidant and 2-4 parts of penetration enhancer;
the chitosan complex is prepared by the following method:
dissolving 2.00g of chitosan in 350ml of 1% acetic acid solution, stirring for 1h, neutralizing with 0.1mol/ml NaOH solution to generate a transparent colloid, filtering with a floxacin funnel, washing residual NaOH with sufficient distilled water, drying, and fully grinding the product;
adding 1.00g of treated chitosan into a 100ml flask, adding 50ml of N, N-dimethylformamide aqueous solution, vigorously stirring for 24h, transferring the flask into a heat collection type constant-temperature magnetic stirrer, controlling the temperature to be 70 ℃, and dropwise adding 50ml of N, N-dimethylformamide solution containing 1.9g of epoxy thiacalix arene into the flask, wherein the epoxy group: reacting for 24h, removing the solvent by reduced pressure evaporation, washing the residue with a small amount of chloroform and distilled water, drying in vacuum to obtain the final product, and fully grinding the product.
2. The hemostatic cotton containing polyvinyl alcohol for operation as claimed in claim 1, which comprises the following raw materials by weight: 28-35 parts of polyvinyl alcohol, 20-26 parts of aldehyde dextran, 17-25 parts of chitosan compound, 8-12 parts of lysine, 3-4 parts of casein, 2-4 parts of plasticizer, 2-3 parts of antioxidant and 2-4 parts of permeation enhancer.
3. The hemostatic cotton containing polyvinyl alcohol for operation as claimed in claim 1, which comprises the following raw materials by weight: 30-34 parts of polyvinyl alcohol, 20-22 parts of aldehyde dextran, 20-23 parts of chitosan compound, 10-12 parts of lysine, 3-4 parts of casein, 3-4 parts of plasticizer, 2-3 parts of antioxidant and 3-4 parts of permeation enhancer.
4. The hemostatic cotton containing polyvinyl alcohol for operation as claimed in claim 1, which comprises the following raw materials by weight: 32 parts of polyvinyl alcohol, 20 parts of aldehyde dextran, 22 parts of chitosan compound, 11 parts of lysine, 4 parts of casein, 4 parts of plasticizer, 2 parts of antioxidant and 3 parts of penetration enhancer.
5. The hemostatic sponge according to claim 1, wherein said aldehyde dextran is prepared by the following method: oxidizing glucan in an aqueous solution by sodium periodate under a dark condition, and reacting for 18-30 h at room temperature; adding the reaction solution into a 9-14 kDa dialysis bag for dialysis for 4-10 times, and freeze-drying to obtain aldehyde group glucan, wherein the aldehyde group content is 15% -95%; the molecular weight of the glucan is 20kDa to 150 kDa.
6. The hemostatic cotton containing polyvinyl alcohol for operation as claimed in claim 1, wherein the plasticizer is one or more of ethylene glycol, sodium lactate and sorbitol; the antioxidant is chitin or hinokitiol; the penetration enhancer is one or more of hydroxypropyl-beta-cyclodextrin, Borneolum Syntheticum, oleum Menthae Dementholatum or oleum Olivarum.
7. The method for preparing hemostatic cotton containing polyvinyl alcohol for operation as claimed in any one of claims 1 to 6, comprising the steps of:
1) preparing raw materials in parts by weight: 26-37 parts of polyvinyl alcohol, 18-28 parts of aldehyde dextran, 15-27 parts of chitosan compound, 8-13 parts of lysine, 3-5 parts of casein, 1-4 parts of plasticizer, 1-3 parts of antioxidant and 2-4 parts of penetration enhancer;
2) compounding aldehyde group glucan and a chitosan compound to form a mixed solution A;
3) dissolving polyvinyl alcohol and lysine in water, adding casein, and heating and stirring to obtain a mixed solution B;
4) adding the mixed solution A into the mixed solution B, continuously stirring, and slowly adding a plasticizer, an antioxidant and a penetration enhancer to obtain a mixed solution C;
5) and pouring the mixed solution C into a mold, pre-freezing, freeze-drying until the sol is freeze-dried, swelling, and freeze-drying again to obtain the porous hemostatic cotton.
8. The method for preparing hemostatic cotton for operation containing polyvinyl alcohol according to claim 7, wherein the heating temperature in step 3) is 30 ℃ to 40 ℃.
9. The method for preparing hemostatic cotton for operation with polyvinyl alcohol as claimed in claim 7, wherein the swelling process in step 5) comprises: and (3) soaking the sol sample after freeze drying in a calcium chloride solution, wherein the concentration of the calcium chloride solution is 0-0.05 g/ml, and the swelling multiple is 30-200 times.
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