CN101507830A - Hydrocolloid for dressing and preparation method thereof - Google Patents
Hydrocolloid for dressing and preparation method thereof Download PDFInfo
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- CN101507830A CN101507830A CNA2009100612098A CN200910061209A CN101507830A CN 101507830 A CN101507830 A CN 101507830A CN A2009100612098 A CNA2009100612098 A CN A2009100612098A CN 200910061209 A CN200910061209 A CN 200910061209A CN 101507830 A CN101507830 A CN 101507830A
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Abstract
The invention discloses a hydrocolloid for dressings, and a preparation method thereof. The hydrocolloid comprises carboxymethyl chitosan, sodium alginate, glycerol, isopropanol, carboxymethyl chitosan quaternary ammonium salt and water, wherein the mass ratio of the carboxymethyl chitosan to the sodium alginate to the glycerol to the isopropanol to the carboxymethyl chitosan quaternary ammonium salt is 0.8-2.5:0.1-1.0:3.0-5.0:0.9-3.0:0.1-1.0; the water accounts for 35 to 55 percent of the hydrocolloid by mass; and the carboxymethyl chitosan quaternary ammonium salt is a mixture of high-molecular-weight carboxymethyl chitosan quaternary ammonium salt and low-molecular-weight carboxymethyl chitosan quaternary ammonium salt, wherein the mass percentage content of the high-molecular-weight carboxymethyl chitosan quaternary ammonium salt is 50 to 90 percent. The preparation method comprises the steps of mixing the carboxymethyl chitosan, the sodium alginate, the glycerol, the isopropanol and the carboxymethyl chitosan quaternary ammonium salt in the mass ratio of 0.8-2.5:0.1-1.0:3.0-5.0:0.9-3.0:0.1-1.0 with purified water, stirring and filtering the mixture, performing foam removal, obtaining a gel solution and baking the gel solution for 8 to 16 hours at a temperature of between 60 and 80 DEG C.
Description
Technical field
The present invention relates to a kind of hydrocolloid that is used for dressing and preparation method thereof, belong to field of medical products, also belong to technical field of biological material.
Background technology
Desirable dressing should have following characteristics: (1) can absorb a large amount of transudates and noxious substance, also can keep certain form and intensity when moistening; (2) can keep the enough humidity of wound, reasonable resistance bacterium property and bacteriostasis are arranged; (3) more change dressings to the wound not damaged; (4) excellent storage stability preferably has the degradable performance, and garbage does not produce pollution to environment.
The hydrocolloid of biologically active since can create moist healing environment with and the character of semipermeable membrane, particularly obtained using widely in the dressing at medical supplies.Compare with traditional dressing, the dressing that utilizes hydrocolloid to make has following advantage: healing is very fast, adhesion wound when changing dressings, be convenient to nurse operation, and the working time, the antibacterial that obviously shorten the nurse can not see through, alleviate wound pain, reduce dressing change frequency.The hydrocolloid that uses in the dressing generally is to be primary raw material with cellulosic derivant sodium carboxymethyl cellulose in the market, but cellulosic function ratio is more single, can not satisfy the requirement of complicated wound surface for wound dressing.
Chitosan is the unique alkaline polysaccharide in the natural polysaccharide, has many special physicochemical character and physiological function.Different molecular weight ranges chitosan the activity of blood is had different character (anticoagulant property is arranged during low-molecular-weight, the coagulant courage and uprightness are arranged during high molecular).Carboxymethyl chitosan and carboxymethyl chitosan quaternary ammonium salt are the derivants of chitosan, have and the chitosan similar biological, and contain a large amount of hydrophilic radicals in the molecule, compare with chitosan, water solublity strengthens greatly, in addition, carboxymethyl chitosan quaternary ammonium salt has good bacteriostasis property, has important use in fields such as biology, medical science and is worth.
Domestic have some producers to utilize the chitosan or derivatives thereof for the feedstock production hydrocolloid and then come production dressing, though the hydrocolloid that obtains like this can partly keep the activity of chitosan, but be difficult to form moistening healing environment at wound with the dressing that it is made, though perhaps can form moist environment, but mechanical property is relatively poor, cracked easily during use, inconvenient nurse uses, and also can bring misery to patient when changing.
Summary of the invention
The objective of the invention is to remedy the deficiencies in the prior art, provide a kind of can be used in dressing can form the wet union environment at wound, have hydrocolloid of bacteriostasis property, stability and mechanical property preferably and preparation method thereof again.
For achieving the above object, the technical solution used in the present invention is: a kind of hydrocolloid that is used for dressing, this hydrocolloid comprises carboxymethyl chitosan, sodium alginate, glycerol, isopropyl alcohol, carboxymethyl chitosan quaternary ammonium salt and water, wherein the mass ratio of carboxymethyl chitosan, sodium alginate, glycerol, isopropyl alcohol and carboxymethyl chitosan quaternary ammonium salt is 0.8～2.5:0.1～1.0:3.0～5.0:0.9～3.0:0.1～1.0, and the quality percentage composition of water is 35～55% of a hydrocolloid quality; The molecular weight of carboxymethyl chitosan is 1000,000～2000,000, and deacetylation is 90%～99%, and the carboxy methylation degree is that the substitution value of 0.5～1.5,6 hydroxyls is 0.5～1.0; Sodium alginate order number is 60～200 orders, and viscosity is 50～400mpas, and pH value is 3.0～9.0; Carboxymethyl chitosan quaternary ammonium salt is the mixture of high molecular carboxymethyl chitosan quaternary ammonium salt and low-molecular-weight carboxymethyl chitosan quaternary ammonium salt, and wherein the quality percentage composition of high molecular carboxymethyl chitosan quaternary ammonium salt is 50～90%; The molecular weight of high molecular carboxymethyl chitosan quaternary ammonium salt is 10,000～50,000, deacetylation is 90～99%, and the carboxy methylation degree is 0.5～1.5, quaternized substitution value is 0.7～2.0, the molecular weight 1000～10,000 of low-molecular-weight carboxymethyl chitosan quaternary ammonium salt, deacetylation is 90～99%, the carboxy methylation degree is 0.5～1.5, and quaternized substitution value is 0.7～1.5.
The dry state tensile strength of described hydrocolloid is greater than 85MPa, and the hygrometric state tensile strength is greater than 30MPa; The water free breaking elongation rate is less than 5%, and the hygrometric state elongation at break is less than 23%.
The present invention also provides the above-mentioned preparation method that is used for the hydrocolloid of dressing, comprises following concrete steps:
(1) in mass ratio the ratio of 0.8～2.5:0.1～1.0:3.0～5.0:0.9～3.0:0.1～1.0 with carboxymethyl chitosan, sodium alginate, glycerol, isopropyl alcohol and carboxymethyl chitosan quaternary ammonium salt, mix with pure water, the quality of pure water is carboxymethyl chitosan and sodium alginate gross mass 20～50 times, fully stir then and make it mix homogeneously, obtain coagulant liquid after filtration, the deaeration; Wherein, the molecular weight of carboxymethyl chitosan is 1000,000～2000,000, and deacetylation is 90～99%, and the carboxy methylation degree is that the substitution value of 0.5～1.5,6 hydroxyls is 0.5～1.0; Sodium alginate order number is 60～200 orders, and viscosity is 50～400mpas, and pH value is 3.0～9.0; Carboxymethyl chitosan quaternary ammonium salt is the mixture of high molecular carboxymethyl chitosan quaternary ammonium salt and low-molecular-weight carboxymethyl chitosan quaternary ammonium salt, and wherein the quality percentage composition of high molecular carboxymethyl chitosan quaternary ammonium salt is 50～90%; The molecular weight of high molecular carboxymethyl chitosan quaternary ammonium salt is 10,000～50,000, deacetylation is 90～99%, and the carboxy methylation degree is 0.5～1.5, quaternized substitution value is 0.7～2.0, the molecular weight 1000～10,000 of low-molecular-weight carboxymethyl chitosan quaternary ammonium salt, deacetylation is 90～99%, the carboxy methylation degree is 0.5～1.5, and quaternized substitution value is 0.7～1.5;
(2) coagulant liquid was obtained hydrocolloid in 8～16 hours in 60～80 ℃ of bakings.
Pour the coagulant liquid that above-mentioned steps (1) obtains in the mould curtain coating or coating film forming, then in 60～80 ℃ of bakings 8～16 hours, obtain membranaceous hydrocolloid after the demoulding, cover non-woven fabrics or polyurethane film in the one side of this membranaceous hydrocolloid, another side covers goes up release paper, and cutting then, packing, sterilizing to obtain dressing.
Filter described in the above-mentioned steps (1) is to be 5～7 * 10 at pressure
5Vacuum filtration under the condition of handkerchief.
Stirring described in the above-mentioned steps (1) is to adopt shearing mulser to stir, and whipping temp is 10～30 ℃, and mixing time is 1～4 hour.
Deaeration described in the above-mentioned steps (1) is to be 7～9 * 10 at pressure
5Vacuum deaerator under the condition of handkerchief.
Above-mentioned mould is the mould with polytetrafluoroethylene anti-stick coating, and coating layer thickness is 45 ± 5 μ m.
Described one side at membranaceous hydrocolloid covers non-woven fabrics or polyurethane film, and another side covers goes up release paper, is to adopt the step-by-step movement laminating machine to cover non-woven fabrics or polyurethane film in the one side of membranaceous hydrocolloid, and another side covers goes up release paper.
The present invention has the following advantages:
Since in the aqueous solution carboxymethyl chitosan and carboxymethyl chitosan quaternary ammonium salt can form a large amount of O----H and two kinds of hydrogen bonds of N----H with sodium alginate, so they can strengthen mutual gelation reaction after fully mixing, and improve the mechanical property of hydrocolloid.The cells of microorganisms wall has negative charge mostly, and high-molecular weight carboxymethyl chitosan quaternary ammonium salt has a large amount of positive charges after the ionization in water, can be adsorbed in the microorganism surface, stops nutrient substance to enter in the cell, thereby causes microorganism depleted and die; Low-molecular-weight carboxymethyl chitosan quaternary ammonium salt then can enter in the cell, influences the transcription of DNA, makes microbial death.Therefore the hydrocolloid that obtains of the present invention can be brought into play the cooperative effect of carboxymethyl chitosan, carboxymethyl chitosan quaternary ammonium salt and sodium alginate, make the hydrocolloid that obtains to keep the biological activity and the medical performance of raw material itself, have good moisture pick-up properties and bacteriostasis property again, all can reach 1 μ g/ml the minimal inhibitory concentration of staphylococcus aureus, bacillus subtilis, Pseudomonas aeruginosa, Candida albicans, Aspergillus niger.Can absorb a large amount of Wound exudates with its dressing of making, improve speed of wound healing, protect from infection the wound surface spread of germs and the infection that causes, regulate immunity, promote the wound blood coagulation.
2. adjust the water content and the mechanical property of hydrocolloid among the present invention by the ratio of control glycerol and sodium alginate, make its stable performance, keep moisture not lose for a long time, the dressing that utilizes this hydrocolloid to make at room temperature can be preserved 2 years at least.The dry state tensile strength of this hydrocolloid is greater than 85MPa, and the hygrometric state tensile strength is greater than 30MPa; The water free breaking elongation rate is less than 5%, and the hygrometric state elongation at break is less than 23%, makes and can avoid behind the dressing owing to crackedly cause secondary to be changed to patient bringing misery, except that general wound, also be applicable to force parts such as pressure ulcer, joint.
3. adopt shearing mulser to stir, can guarantee that raw material fully dissolves, homogenize in water; Adopt vacuum deaerator and vacuum bakeout, when improving the quality of products, shortened the production time greatly.
4. technology of the present invention is simple, is easy to large-scale production, and cost is low, is easy to promote, and does not adopt any noxious substance, and is little to the influence of ecological environment.
5. when this hydrocolloid being used for production dressing,, can effectively solve the viscous problem of hydrocolloid and mould owing to adopt mould with anti-stick coating.
The specific embodiment
The invention will be further described below by specific embodiment, and its purpose is to help to understand content of the present invention better, but the protection domain that these embodiment do not limit the present invention in any way.
Embodiment 1
Getting molecular weight is 1000,000～2000,000, deacetylation is 90%, the carboxy methylation degree is that the substitution value of 0.5,6 hydroxyl is 0.5 carboxymethyl chitosan 1.8kg, gets 100 orders, viscosity is 400mpas, pH value is 7.0 sodium alginate 0.5kg, glycerol 4kg, isopropyl alcohol 1kg, molecular weight is 10,000～50,000, deacetylation is 90%, the carboxy methylation degree is 0.5, quaternized substitution value is 0.7 carboxymethyl chitosan quaternary ammonium salt 0.3Kg, and molecular weight is 1000～10,000, deacetylation is 90%, the carboxy methylation degree is 0.5, and quaternized substitution value is 0.7 carboxymethyl chitosan quaternary ammonium salt 0.05Kg, adds in the pure water of 60kg, adopt shearing mulser to stir and made it mix homogeneously in 2 hours, 5 * 10 in 20 ℃
5Vacuum filtration under the condition of handkerchief, 7 * 10
5Obtain coagulant liquid behind the vacuum deaerator under the handkerchief condition, coagulant liquid was obtained hydrocolloid in 8～16 hours 60 ℃ of bakings.Comprise carboxymethyl chitosan, sodium alginate, glycerol, isopropyl alcohol, carboxymethyl chitosan quaternary ammonium salt and water in this hydrocolloid, the quality percentage composition of water is 35% of a hydrocolloid quality.
Embodiment 2
Getting molecular weight is 1000,000～2000,000, deacetylation is 95%, the carboxy methylation degree is that the substitution value of 0.9,6 hydroxyl is 0.8 carboxymethyl chitosan 1.5kg, gets 100 orders, viscosity is 300mpas, pH value is 8.0 sodium alginate 1.0kg, glycerol 6kg, isopropyl alcohol 1kg, molecular weight is 10,000～50,000, deacetylation is 95%, the carboxy methylation degree is 0.7, quaternized substitution value is 1.0 carboxymethyl chitosan quaternary ammonium salt 0.5Kg, and molecular weight is 1000～10,000, deacetylation is 95%, the carboxy methylation degree is 0.7, and quaternized substitution value is 1.0 carboxymethyl chitosan quaternary ammonium salt 0.3Kg, adds in the pure water of 80kg, adopt shearing mulser to stir and made it mix homogeneously in 4 hours, 6 * 10 in 10 ℃
5Vacuum filtration under the condition of handkerchief, 8 * 10
5Vacuum deaerator obtains coagulant liquid under the handkerchief condition, and coagulant liquid was obtained hydrocolloid in 16 hours 70 ℃ of bakings.Comprise carboxymethyl chitosan, sodium alginate, glycerol, isopropyl alcohol, carboxymethyl chitosan quaternary ammonium salt and water in this hydrocolloid, the quality percentage composition of water is 40% of a hydrocolloid quality.
Embodiment 3
Getting molecular weight is 1000,000～2000,000, deacetylation is 98%, the carboxy methylation degree is that the substitution value of 1.5,6 hydroxyls is 1.0 carboxymethyl chitosan 0.8kg, gets 200 orders, viscosity is 400mpas, pH value is 8.5 sodium alginate 0.5kg, glycerol 4kg, isopropyl alcohol 1kg, molecular weight is 10,000～50,000, deacetylation is 99%, the carboxy methylation degree is 1.5, quaternized substitution value is 2.0 carboxymethyl chitosan quaternary ammonium salt 0.2Kg, and molecular weight is 1000～10,000, deacetylation is 99%, the carboxy methylation degree is 1.5, and quaternized substitution value is 1.5 carboxymethyl chitosan quaternary ammonium salt 0.1Kg, adds in the pure water of 60kg, adopt shearing mulser to stir and made it mix homogeneously in 1 hour, 7 * 10 in 30 ℃
5Vacuum filtration under the condition of handkerchief, 9 * 10
5Obtain coagulant liquid behind the vacuum deaerator under the handkerchief condition, coagulant liquid was obtained hydrocolloid in 16 hours 60 ℃ of bakings.Comprise carboxymethyl chitosan, sodium alginate, glycerol, isopropyl alcohol, carboxymethyl chitosan quaternary ammonium salt and water in this hydrocolloid, the quality percentage composition of water is 55% of a hydrocolloid quality.
Pour the coagulant liquid that obtains after the deaeration in the mould curtain coating or coating film forming, 60～80 ℃ of bakings 8～16 hours, obtain membranaceous hydrocolloid after the demoulding, cover non-woven fabrics or polyurethane film in the one side of this membranaceous hydrocolloid then, another side covers goes up release paper, and cutting then, packing, sterilizing to obtain dressing.
Hydrocolloid of the present invention has good bacteriostasis property, and its experiment the results are shown in Table 1.
The bacteriostatic experiment result of table 1 hydrocolloid of the present invention
Annotate :+expression has colony growth, the aseptic length of being born of-expression.
Claims (9)
1. hydrocolloid that is used for dressing, it is characterized in that: this hydrocolloid comprises carboxymethyl chitosan, sodium alginate, glycerol, isopropyl alcohol, carboxymethyl chitosan quaternary ammonium salt and water, wherein the mass ratio of carboxymethyl chitosan, sodium alginate, glycerol, isopropyl alcohol and carboxymethyl chitosan quaternary ammonium salt is 0.8～2.5:0.1～1.0:3.0～5.0:0.9～3.0:0.1～1.0, and the quality percentage composition of water is 35～55% of a hydrocolloid quality; The molecular weight of carboxymethyl chitosan is 1000,000～2000,000, and deacetylation is 90%～99%, and the carboxy methylation degree is that the substitution value of 0.5～1.5,6 hydroxyls is 0.5～1.0; Sodium alginate order number is 60～200 orders, and viscosity is 50～400mpas, and pH value is 3.0～9.0; Carboxymethyl chitosan quaternary ammonium salt is the mixture of high molecular carboxymethyl chitosan quaternary ammonium salt and low-molecular-weight carboxymethyl chitosan quaternary ammonium salt, and wherein the quality percentage composition of high molecular carboxymethyl chitosan quaternary ammonium salt is 50～90%; The molecular weight of high molecular carboxymethyl chitosan quaternary ammonium salt is 10,000～50,000, deacetylation is 90～99%, and the carboxy methylation degree is 0.5～1.5, quaternized substitution value is 0.7～2.0, the molecular weight 1000～10,000 of low-molecular-weight carboxymethyl chitosan quaternary ammonium salt, deacetylation is 90～99%, the carboxy methylation degree is 0.5～1.5, and quaternized substitution value is 0.7～1.5.
2. the hydrocolloid that is used for dressing according to claim 1 is characterized in that: the dry state tensile strength of described hydrocolloid is greater than 85MPa, and the hygrometric state tensile strength is greater than 30MPa; The water free breaking elongation rate is less than 5%, and the hygrometric state elongation at break is less than 23%.
3. preparation method that is used for the hydrocolloid of dressing according to claim 1 is characterized in that comprising following concrete steps:
(1) in mass ratio the ratio of 0.8～2.5:0.1～1.0:3.0～5.0:0.9～3.0:0.1～1.0 with carboxymethyl chitosan, sodium alginate, glycerol, isopropyl alcohol, carboxymethyl chitosan quaternary ammonium salt, mix with pure water, the quality of pure water is carboxymethyl chitosan and sodium alginate gross mass 20～50 times, fully stir then and make it mix homogeneously, obtain coagulant liquid after filtration, the deaeration; Wherein, the molecular weight of carboxymethyl chitosan is 1000,000～2000,000, and deacetylation is 90～99%, and the carboxy methylation degree is that the substitution value of 0.5～1.5,6 hydroxyls is 0.5～1.0; Sodium alginate order number is 60～200 orders, and viscosity is 50～400mpas, and pH value is 3.0～9.0; Carboxymethyl chitosan quaternary ammonium salt is the mixture of high molecular carboxymethyl chitosan quaternary ammonium salt and low-molecular-weight carboxymethyl chitosan quaternary ammonium salt, and wherein the quality percentage composition of high molecular carboxymethyl chitosan quaternary ammonium salt is 50～90%; The molecular weight of high molecular carboxymethyl chitosan quaternary ammonium salt is 10,000～50,000, deacetylation is 90～99%, and the carboxy methylation degree is 0.5～1.5, quaternized substitution value is 0.7～2.0, the molecular weight of low-molecular-weight carboxymethyl chitosan quaternary ammonium salt is 1000～10,000, and deacetylation is 90～99%, the carboxy methylation degree is 0.5～1.5, and quaternized substitution value is 0.7～1.5;
(2) coagulant liquid was obtained hydrocolloid in 8～16 hours in 60～80 ℃ of bakings.
4. according to the described preparation method that is used for the hydrocolloid of dressing of claim 3, it is characterized in that: pour the coagulant liquid that step (1) obtains in the mould curtain coating or coating film forming, then in 60～80 ℃ of bakings 8～16 hours, obtain membranaceous hydrocolloid after the demoulding, cover non-woven fabrics or polyurethane film in the one side of this membranaceous hydrocolloid, another side covers goes up release paper, and cutting then, packing, sterilizing to obtain dressing.
5. according to the described preparation method that is used for the hydrocolloid of dressing of claim 3, it is characterized in that: stirring described in the step (1) is to adopt shearing mulser to stir, and whipping temp is 10～30 ℃, and mixing time is 1～4 hour.
6. according to the described preparation method that is used for the hydrocolloid of dressing of claim 3, it is characterized in that: filtering described in the step (1) is to be 5～7 * 10 at pressure
5Vacuum filtration under the condition of handkerchief.
7. according to the described preparation method that is used for the hydrocolloid of dressing of claim 3, it is characterized in that: deaeration described in the step (1) is to be 7～9 * 10 at pressure
5Vacuum deaerator under the condition of handkerchief.
8. according to the described preparation method that is used for the hydrocolloid of dressing of claim 4, it is characterized in that: described mould is the mould with polytetrafluoroethylene anti-stick coating, and coating layer thickness is 45 ± 5 μ m.
9. according to the described preparation method that is used for the hydrocolloid of dressing of claim 4, it is characterized in that: described one side at membranaceous hydrocolloid covers non-woven fabrics or polyurethane film, another side covers goes up release paper, be to adopt the step-by-step movement laminating machine to cover non-woven fabrics or polyurethane film in the one side of membranaceous hydrocolloid, another side covers goes up release paper.
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