CN104027300A - Antibacterial chitosan gel and preparation method thereof - Google Patents
Antibacterial chitosan gel and preparation method thereof Download PDFInfo
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Abstract
The invention relates to antibacterial chitosan gel and a preparation method of the antibacterial chitosan gel. The preparation method includes the steps of preparing complex liquid containing chitosan, preparing a fibroin ethanol solution, preparing a carrageenan solution, preparing a quaternary phosphonium compound solution, preparing gel and other steps. According to the antibacterial chitosan gel, high-molecular-weight chitosan and low-molecular-weight chitosan compounds are used as main base materials in cooperation with antibiotic synergist, gelatinizing agents, histocyte repairing auxiliary materials and the like for being compounded, and use of other chemicals, biological drugs and other ingredients is avoided; as a result, the safety of the gel is improved, cost is reduced, irritation to patients is reduced, and health restoration of the patients is facilitated. The ability of the prepared antibacterial chitosan gel to resist bacteria such as staphylococcus aureus, coliform bacteria, streptococcus and pseudomonas aeruginosa reaches more than 99 percent, so the antibacterial chitosan gel shows good bacteriostatic ability.
Description
[technical field]
The invention belongs to medical drugs technical field.More specifically, the present invention relates to a kind of antibacterial chitosan gel rubber agent, also relate to the preparation method of described antibacterial chitosan gel rubber agent.
[background technology]
The superior function that macromolecule hydrogel material itself has, as swelling character, viscoelasticity behavior and suitable mechanical strength etc., make it cause the very big interest of numerous researcheres and concern, corresponding preparation is maked rapid progress, is achieved great success with developmental research, its application has penetrated into the every field such as health care, biological medicine, daily-use chemical industry, food, environmental protection, and also in the application to more wide, expands.Particularly good biocompatibility makes again it good in the application prospect of biomedical aspect, as can be used as the embedding, protein electrophorese, contact lenses of tissue filling agent, medicinal slow release agent, enzyme, artificial blood plasma, artificial skin, tissue engineering bracket material etc., and along with the hydrogel of excellent performance is continually developed, biomedical technology level is improved greatly.Much research is verified, chitosan is as the unique alkaline polysaccharide of occurring in nature, there is obvious bactericidal action, under acid condition, the amino in high deacetylized chitosan molecule, with positive charge, can adsorb the antibacterial with negative charge, the life state of interference cell, make cell membrane deformation fracture, inclusions is oozed out, and causes bacterolysis and death.Research is also found, high molecular weight chitosan has excellent gel characteristic, by the special electrostatic force of group in chitosan molecule chain, close hydrophobic interaction and hydrogen bond action, can produce compound with some gellant, formation can keep the colloidal materials of large quantity of moisture, has very strong moisture absorption, performance of keeping humidity, can also provide enough viscosity simultaneously, can be affixed on mucosa, skin etc. and locate and do not come off, can not produce pessimal stimulation and anaphylaxis etc. to human body skin.Therefore, there is at present much research to concentrate on and develop various chitosan gel rubbers applying biological engineering in medicine.
At present, some patents of invention or application for a patent for invention relate to employing chitosan and prepare gel, for example CN101278896B discloses a kind of chitosan nano silver gel agent and application thereof, and it is prepared by nanometer silver, chitosan base polymer, carbomer, Polycarbophil, cellulose, polyvinyl alcohol, Polyethylene Glycol, polyamide, clay, collagen protein, pectin, sulphuric acid, acetic acid, formic acid etc.CN103316033A discloses a kind of gel and uses thereof, and it is prepared by chitosan base polymer, hyalomitome acids material, newborn acid, gel-type vehicle, wetting agent, diluent etc.CN102397474A discloses a kind of Sanguis Draxonis oral gel for the treatment of stress gastric ulcer, and it is prepared by Sanguis Draxonis extract, carbomer, chitosan, sodium carboxymethyl cellulose, diethanolamine etc.CN103520232A discloses a kind of preparation method of gel, and it is prepared by Fructus cnidii extract clathrate, Clindamycin Hydrochloride clathrate, hydroxypropyl cellulose, water, glycerol, chitosan, ethyl hydroxybenzoate alcoholic solution, aqueous sodium persulfate solution etc.In addition, CN102657602 discloses 3,5-hydroxyl-4-isopropyl toluylene chitosan gel rubber agent and preparation method thereof; CN102626524A discloses Chitosangynaecologicsuppository antibacterial gel and preparation method thereof; CN101757071A discloses a kind of Irreversible vagina antibiosis gel preparation and preparation method thereof etc.
There is following technological deficiency in these prior aries: though 1, most gel take chitosan as host matrix, but other medicine of load all, comprising chemicals, bio-pharmaceutical, Chinese herbal medicine or nanometer silver etc., the object that adopts chitosan to make gel dosage form is mainly to make medicine play slow releasing function; 2, generally use synthetic material carbomer etc. as the main material that forms gel; 3, do not use other natural activity biological material that can produce damaged tissue and cytothesis effect, effectiveness and the safety of product are restricted.Therefore, research and develop that a kind of making is simple, safety, environmental protection, and it is significant for clinical treatment to have the Novel pure chitosan gel rubber agent of tissue repair function.
[summary of the invention]
[technical problem that will solve]
The object of this invention is to provide a kind of antibacterial chitosan gel rubber agent.
Another object of the present invention is to provide the preparation method of described antibacterial chitosan gel rubber agent.
[technical scheme]
The present invention is achieved through the following technical solutions.
The present invention relates to a kind of preparation method of antibacterial chitosan gel rubber agent.
The step of this antibacterial chitosan gel rubber agent preparation method is as follows:
A, prepare the complex liquid of chitosan-containing
Glacial acetic acid is mixed homogeneously with distilled water, toward wherein adding molecular weight 60 * 10
4the high molecular weight chitosan of Da, deacetylation 85-95% and molecular weight are lower than 1 * 10
3the low-molecular weight chitoglycan of Da, deacetylation 98-100%, stirring and dissolving, adds polyoxyethylene Pilus Caprae seu Ovis alcohol ether again after homogenize, stir, and obtains a kind of complex liquid of chitosan-containing;
B, prepare fibroin alcoholic solution
Fibroin is added in ethanol water, and stirring and dissolving, obtains a kind of fibroin alcoholic solution;
C, preparation carrageenan solutions
Distilled water is heated to 90～100 ℃ of temperature, then adds carrageenan, stirring and dissolving, obtains a kind of carrageenan solutions;
D, prepare quaternary phosphonium compound solution
Pi-allyl triphenyl bromide phosphine mixes according to weight ratio 1:1.8～2.2 with pi-allyl three amyl group phosphonium chlorides, obtains a kind of mixture; Then described mixture is added in distilled water, after dissolving, adds again sucrose fatty acid ester, stir, obtain a kind of sucrose fatty acid ester quaternary phosphonium compound solution that contains;
E, prepare gel
The fibroin alcoholic solution that the complex liquid of the chitosan-containing that steps A is obtained obtains with step B is mixed homogeneously, again mixed solution is added in the carrageenan solutions that step C obtains, stir, what then add that step D obtains contains sucrose fatty acid ester quaternary phosphonium compound solution, add distilled water, mix homogeneously, obtains described antibacterial chitosan gel rubber agent.
A preferred embodiment of the invention, in steps A, the weight ratio of glacial acetic acid and distilled water is 0.8～1.2:16～22.
According to another kind of preferred implementation of the present invention, in steps A, the weight ratio of described high molecular weight chitosan and described low-molecular weight chitoglycan is 1.8～2.2:2.6～3.4.
According to another kind of preferred implementation of the present invention, in step D, the weight ratio of polyoxyethylene Pilus Caprae seu Ovis alcohol ether and chitosan total amount is 1:4.8～5.2.
According to another kind of preferred implementation of the present invention, in step B, the weight ratio of fibroin and ethanol water is 0.3～0.8:1.6～2.4.
According to another kind of preferred implementation of the present invention, in step B, the concentration of described ethanol water is by volume 80～95%.
According to another kind of preferred implementation of the present invention, in step C, the weight ratio of distilled water and carrageenan is 25～35:0.5～1.8.
According to another kind of preferred implementation of the present invention, in step D, the weight ratio of pi-allyl triphenyl bromide phosphine and pi-allyl three amyl group phosphonium chloride mixture and distilled water is 0.1～0.5:8～12.
According to another kind of preferred implementation of the present invention, in step D, the weight ratio of pi-allyl triphenyl bromide phosphine and pi-allyl three amyl group phosphonium chloride mixture and sucrose fatty acid ester is 0.1～0.5:0.8～1.2.
The invention still further relates to the antibacterial chitosan gel rubber agent that adopts described preparation method to obtain.Described antibacterial chitosan gel rubber agent reaches more than 99% the antibacterial ability of staphylococcus aureus, escherichia coli, streptococcus, Candida albicans or bacillus pyocyaneus.
The present invention will be described in more detail below.
The present invention relates to a kind of preparation method of antibacterial chitosan gel rubber agent.
The step of this antibacterial chitosan gel rubber agent preparation method is as follows:
A, prepare the complex liquid of chitosan-containing
Glacial acetic acid is mixed homogeneously with distilled water, toward wherein adding molecular weight 60 * 10
4the high molecular weight chitosan of Da, deacetylation 85-95% and molecular weight are lower than 1 * 10
3the low-molecular weight chitoglycan of Da, deacetylation 98-100%, stirring and dissolving, adds polyoxyethylene Pilus Caprae seu Ovis alcohol ether again after homogenize, stir, and obtains a kind of complex liquid of chitosan-containing;
In this step, the weight ratio of glacial acetic acid and distilled water is 0.8～1.2:16～22, and preferably, the weight ratio of glacial acetic acid and distilled water is 1.0:18～20.
The chemical constitution of chitosan (β-(1 → 4)-2-amino-2-deoxy-D-Glucose), for being with cationic macromolecule alkalescence polysaccharide polymer, is unique positively charged, the cation edible fiber of nature; It has the physicochemical properties such as stable physical property, good dissolubility, hydrophilic hygroscopicity, biological degradability, biocompatibility and film property, caking property, breathability.
In the present invention, object high molecular weight chitosan and low-molecular weight chitoglycan being used in conjunction with is to utilize the good gelling property of high molecular weight chitosan and the good antibacterial properties of low-molecular weight chitoglycan.
In this step, the weight ratio of described high molecular weight chitosan and described low-molecular weight chitoglycan is 1.8～2.2:2.6～3.4.If the amount of high molecular weight chitosan is too low or when too high, can make the gelling properties of this gel be affected.Similarly, if the amount of low-molecular weight chitoglycan is too low or when too high, can make the anti-microbial property of gel be affected.Therefore, the weight ratio of described high molecular weight chitosan and described low-molecular weight chitoglycan is 1.8～2.2:2.6～3.4, rational, preferably 2.0:2.8～3.2.
The high molecular weight chitosan that the present invention uses and low-molecular weight chitoglycan are product solds in the market, the high molecular weight chitosan of for example being sold with trade name food pharmaceutical grade chitosan by Jinan Haidebei Marine Organism Engineering Co., Ltd., the low-molecular weight chitoglycan that sell with trade name chitosan effluent Bei Bai taste bio tech ltd.
Described polyoxyethylene Pilus Caprae seu Ovis alcohol ether (ethoxylated lanolin alcohol) is made by additive reaction by lanolin alcohol and oxirane.In the present invention, the effect of polyoxyethylene Pilus Caprae seu Ovis alcohol ether is to improve solubilising and the infiltration compatible role improving skin.
In this step, the weight ratio of described polyoxyethylene Pilus Caprae seu Ovis alcohol ether and chitosan total amount (the amount sum of the amount of described high molecular weight chitosan and described low-molecular weight chitoglycan) is 1:4.8～5.2.According to the present invention, if chitosan total amount is less than 4,8, can make the formation effect of gel and antibacterial action decline; If chitosan total amount is greater than 5.2, can make gel decline to the moistening of skin and osmosis effect; Therefore, chitosan total amount is 4.8～5.2nd, appropriate, preferably 1:5.0.
The polyoxyethylene Pilus Caprae seu Ovis alcohol ether that the present invention uses is product sold in the market, for example by Britain standing grain major company with trade name polyoxyethylene Pilus Caprae seu Ovis alcohol ether product sold.
B, prepare fibroin alcoholic solution
Fibroin is added in ethanol water, and stirring and dissolving, obtains a kind of fibroin alcoholic solution.
Fibroin is the natural polymer fibrin extracting from silkworm silk, its content is 70%～80% of silkworm silk amount, it contains 18 seed amino acids, and wherein the amount of glycine (gly), alanine (ala) and serine (ser) is described total amino acid content more than 80%.
In this step, the weight ratio of fibroin and ethanol water is 0.3～0.8:1.6～2.4.The concentration of described ethanol water is by volume 80～95%.
According to the present invention, the amount of fibroin and ethanol water is less than or is all worthless higher than this scope, because fibroin amount height makes to dissolve not exclusively and solution viscosity is higher, measure low do not reach that fibroin plays to the nursing of skin and repairing effect.Preferably, the weight ratio of fibroin and ethanol water is 0.4～0.6:1.8～2.2.
The fibroin that the present invention uses is product sold in the market, for example by Suzhou Bao Sili fibroin fiber Science and Technology Ltd. with trade name fibroin fiber product sold.
C, preparation carrageenan solutions
Distilled water is heated to 90～100 ℃ of temperature, then adds carrageenan, stirring and dissolving, obtains a kind of carrageenan solutions.
Carrageenan (kappa-Carrageenan) is the hydrophilic colloid extracting from the red algae zostera marina such as Eucheuma muricatum (Gmel.) Web.Van Bos., polysaccharide sulfuric ester calcium, potassium, sodium, ammonium salt that it is comprised of galactose and Anhydrogalactose..The carrageenan that the present invention uses is product sold in the market, for example by Beilun In Ningbo Ya Xu Chemical Co., Ltd. with trade name carrageenan product sold.
In this step, the weight ratio of distilled water and carrageenan is 25～35:0.5～1.8.
D, prepare quaternary phosphonium compound solution
Pi-allyl triphenyl bromide phosphine mixes according to weight ratio 1:1.8～2.2 with pi-allyl three amyl group phosphonium chlorides, obtains a kind of mixture; Then described mixture is added in distilled water, after dissolving, adds again sucrose fatty acid ester, stir, obtain a kind of sucrose fatty acid ester quaternary phosphonium compound solution that contains;
In this step, the effect of pi-allyl triphenyl bromide phosphine (Allyltriphenylphosphonium bromide) is by the effect with three phenyl, improves the gelling properties of gel, improves the anti-microbial property of chitosan.
The effect of pi-allyl three amyl group phosphonium chlorides (Allyltriamylphosphoniumchloride) is by the effect of band straight chained alkyl (amyl group) quaternary phosphonium compound, produce cooperative effect with band phenyl quaternary phosphonium compound, greatly promote the gelling property of gel and the anti-microbial property of chitosan.
The effect of sucrose fatty acid ester (Sucrose Fatty Acid Esters) is to play emulsifying and Stabilization as a kind of non-ionic surface active agent, meanwhile, also can further promote antibacterial effect.
The pi-allyl triphenyl bromide phosphine that the present invention uses is product sold in the market, the pi-allyl triphenyl bromide phosphine product of for example preparing according to Ji'nan University's CN102020675B patented technology.
The pi-allyl three amyl group phosphonium chlorides that the present invention uses are product solds in the market, for example by Shanghai flute cypress chemicals technology company limited with trade name pi-allyl three amyl group phosphonium chloride ionic liquid product solds.
The sucrose fatty acid ester that the present invention uses is product sold in the market, for example by Hangzhou Jin Helai food additive company limited with trade name sucrose ester product sold.
In the present invention, the weight ratio of pi-allyl triphenyl bromide phosphine and pi-allyl three amyl group phosphonium chloride mixture and distilled water is 0.1～0.5:8～12.
When the amount of distilled water is 8～12, if the amount of described mixture is less than 0.1, make the Synergistic antimicrobial effect of itself and chitosan influenced; If the amount of described mixture is greater than 0.5, the gelling hardness of gel is undesirable; Therefore, the amount of described mixture is 0.1～0.5th, suitable, and preferably, the weight ratio of pi-allyl triphenyl bromide phosphine and pi-allyl three amyl group phosphonium chloride mixture and distilled water is 0.2～0.4:9～11.
In this step, the weight ratio of pi-allyl triphenyl bromide phosphine and pi-allyl three amyl group phosphonium chloride mixture and sucrose fatty acid ester (Sucrose Fatty Acid Esters) is 0.1～0.5:0.8～1.2.
When the amount of described mixture is 0.1～0.5, if the amount of sucrose fatty acid ester is less than 0.8, emulsifying and Stabilization are bad; If the amount of sucrose fatty acid ester is greater than 1.2, unfavorable to gelling properties; Therefore, the amount of sucrose fatty acid ester is 0.8～1.2nd, suitable, and preferably, the weight ratio of pi-allyl triphenyl bromide phosphine and pi-allyl three amyl group phosphonium chloride mixture and sucrose fatty acid ester is 0.2～0.4:0.9～1.1.
E, prepare gel
The fibroin alcoholic solution that the complex liquid of the chitosan-containing that steps A is obtained obtains with step B is mixed homogeneously, again this mixed solution is added in the carrageenan solutions that step C obtains, stir, what then add that step D obtains contains sucrose fatty acid ester quaternary phosphonium compound solution, add distilled water, mix homogeneously, obtains described antibacterial chitosan gel rubber agent.
Antibacterial chitosan gel rubber agent of the present invention detects and analyzes through the antibacterial detection method of national standard (GB/T16886), prepared antibacterial chitosan gel rubber agent all reaches more than 99% the antibacterial ability of staphylococcus aureus, escherichia coli, streptococcus, bacillus pyocyaneus etc., demonstrates good bacteriostasis.
The present invention is that to take polymer chitosan and low molecular chitosan complex be main matrix, be used in conjunction with the combinations such as Trimethoprim, gellant, histiocyte reparation adjuvant composite, avoid using the compositions such as other chemicals, bio-pharmaceutical and Chinese herbal medicine and nanometer silver, carbomer, improved the safety of gel, also reduce costs simultaneously and reduce the zest to patient, promoting that patient gets well.
The chitosan anti-bacteria gel that adopts the present invention to prepare can be applied to treat bacterial skin infections, men and women's pruritus vulvae, vaginitis, vitamin B1 deficiency, decubital ulcer, skin chronicity ulcer etc.
Chitosan anti-bacteria gel of the present invention can adopt the conventional method known by the technical staff in the art to apply.
[beneficial effect]
The present invention compared with prior art has following beneficial effect:
1, chitosan anti-bacteria gel main body of the present invention is natural product chitosan, does not use other synthetic chemistry or bio-pharmaceutical, Chinese herbal medicine etc., is difficult for producing drug resistance, and biological safety is high;
2, with molecular weight 60 * 10
4the high molecular weight chitosan of Da, as gelled matrix, is used in conjunction with the natural seaweed extracts such as carrageenan, obtains good gelling effect, avoids using the synthetic chemistry materials such as carbomer, has further improved safety and the environmental benefit of product;
3, adopt molecular weight lower than the high deacetylized chitosan of 1000Da low-molecular-weight as antibacterial main body, be used in conjunction with quaternary phosphonium compound as synergist, obtain good antibacterial effect, avoid using other medicines;
4, use fibroin and sucrose-fatty ester complexes etc. to there is the natural activity biological material of damaged tissue and cytothesis effect, can promote patient's function of getting well early;
5, chitosan anti-bacteria gel of the present invention has efficient collaborative anti-harmful microorganism effect, antibacterial, virus, fungus are all had to obvious killing effect, the clinical bacterias such as staphylococcus aureus, hemolytic chain bacterium, bacillus pyocyaneus, Candida albicans and escherichia coli and other harmful fungoid are all had to more than 99% kill efficiency.
[specific embodiment]
By following embodiment, can understand better the present invention.
Embodiment 1: the preparation of chitosan anti-bacteria gel
A, prepare the complex liquid of chitosan-containing
Glacial acetic acid is mixed homogeneously according to weight ratio 0.9:22 with distilled water, according to the weight ratio 1.8:2.6 of high molecular weight chitosan and low-molecular weight chitoglycan, in its glacial acetic acid aqueous solution, add the molecular weight 60 * 10 of being sold with trade name food pharmaceutical grade chitosan by Jinan Haidebei Marine Organism Engineering Co., Ltd.
4the molecular weight 800Da that sell with trade name chitosan the high molecular weight chitosan of Da, deacetylation 88%, effluent Bei Bai taste bio tech ltd, the low-molecular weight chitoglycan of deacetylation 100%, stirring and dissolving, after homogenize, according to the weight ratio 1:4.8 of polyoxyethylene Pilus Caprae seu Ovis alcohol ether and chitosan total amount, add the polyoxyethylene Pilus Caprae seu Ovis alcohol ether of being sold with trade name polyoxyethylene Pilus Caprae seu Ovis alcohol ether by Britain standing grain major company again, stir, obtain a kind of complex liquid of chitosan-containing;
B, prepare fibroin alcoholic solution
According to fibroin and the concentration weight ratio 0.3:1.8 of 80% ethanol water by volume, the fibroin of being sold with trade name fibroin fiber by Suzhou Bao Sili fibroin fiber Science and Technology Ltd. is added in described ethanol water, stirring and dissolving, obtains a kind of fibroin alcoholic solution;
C, preparation carrageenan solutions
Distilled water is heated to 90 ℃ of temperature, then according to the weight ratio 25:1.0 of distilled water and carrageenan, in its distilled water, adds the carrageenan of being sold with trade name carrageenan by Beilun In Ningbo Ya Xu Chemical Co., Ltd., stirring and dissolving, obtains a kind of carrageenan solutions;
D, prepare quaternary phosphonium compound solution
By the pi-allyl triphenyl bromide phosphine product of preparing according to Ji'nan University's CN102020675B patented technology, mixed according to weight ratio 1:1.8 with the pi-allyl three amyl group phosphonium chlorides of being sold with trade name pi-allyl three amyl group phosphonium chloride ionic liquids by Shanghai flute cypress chemicals technology company limited, obtain a kind of mixture; Then according to the weight ratio 0.1:11 of described mixture and distilled water, described mixture is added in distilled water, after dissolving, add again the sucrose fatty acid ester of being sold with trade name sucrose ester by Hangzhou Jin Helai food additive company limited, the weight ratio of wherein said mixture and sucrose fatty acid ester is 0.1:1.1, stir, obtain a kind of sucrose fatty acid ester quaternary phosphonium compound solution that contains;
E, prepare gel
The fibroin alcoholic solution that the complex liquid of the chitosan-containing that steps A is obtained obtains with step B is mixed homogeneously, again this mixed solution is added in the carrageenan solutions that step C obtains, stir, what then add that step D obtains contains sucrose fatty acid ester quaternary phosphonium compound solution, add distilled water, mix homogeneously, obtains described antibacterial chitosan gel rubber agent.
The antibacterial detection method of national standard of describing according to this description detects Analysis deterrmination, and antibacterial chitosan gel rubber agent prepared by the present embodiment all reaches 99.3% to the antibacterial ability of staphylococcus aureus, escherichia coli, streptococcus, bacillus pyocyaneus.
Embodiment 2: the preparation of chitosan anti-bacteria gel
A, prepare the complex liquid of chitosan-containing
Glacial acetic acid is mixed homogeneously according to weight ratio 0.8:16 with distilled water, according to the weight ratio 2.0:3.4 of high molecular weight chitosan and low-molecular weight chitoglycan, in its glacial acetic acid aqueous solution, add the molecular weight 60 * 10 of being sold with trade name food pharmaceutical grade chitosan by Jinan Haidebei Marine Organism Engineering Co., Ltd.
4the molecular weight 900Da that sell with trade name chitosan the high molecular weight chitosan of Da, deacetylation 85%, effluent Bei Bai taste bio tech ltd, the low-molecular weight chitoglycan of deacetylation 98%, stirring and dissolving, after homogenize, according to the weight ratio 1:5.2 of polyoxyethylene Pilus Caprae seu Ovis alcohol ether and chitosan total amount, add the polyoxyethylene Pilus Caprae seu Ovis alcohol ether of being sold with trade name polyoxyethylene Pilus Caprae seu Ovis alcohol ether by Britain standing grain major company again, stir, obtain a kind of complex liquid of chitosan-containing;
B, prepare fibroin alcoholic solution
According to fibroin and the concentration weight ratio 0.4:2.3 of 85% ethanol water by volume, the fibroin of being sold with trade name fibroin fiber by Suzhou Bao Sili fibroin fiber Science and Technology Ltd. is added in described ethanol water, stirring and dissolving, obtains a kind of fibroin alcoholic solution;
C, preparation carrageenan solutions
Distilled water is heated to 92 ℃ of temperature, then according to the weight ratio 30:0.5 of distilled water and carrageenan, in its distilled water, adds the carrageenan of being sold with trade name carrageenan by Beilun In Ningbo Ya Xu Chemical Co., Ltd., stirring and dissolving, obtains a kind of carrageenan solutions;
D, prepare quaternary phosphonium compound solution
By the pi-allyl triphenyl bromide phosphine product of preparing according to Ji'nan University's CN102020675B patented technology, mixed according to weight ratio 1:2.0 with the pi-allyl three amyl group phosphonium chlorides of being sold with trade name pi-allyl three amyl group phosphonium chloride ionic liquids by Shanghai flute cypress chemicals technology company limited, obtain a kind of mixture; Then according to the weight ratio 0.5:8 of described mixture and distilled water, described mixture is added in distilled water, after dissolving, add again the sucrose fatty acid ester of being sold with trade name sucrose ester by Hangzhou Jin Helai food additive company limited, the weight ratio of wherein said mixture and sucrose fatty acid ester is 0.2:0.8, stir, obtain a kind of sucrose fatty acid ester quaternary phosphonium compound solution that contains;
E, prepare gel
The fibroin alcoholic solution that the complex liquid of the chitosan-containing that steps A is obtained obtains with step B is mixed homogeneously, again this mixed solution is added in the carrageenan solutions that step C obtains, stir, what then add that step D obtains contains sucrose fatty acid ester quaternary phosphonium compound solution, add distilled water, mix homogeneously, obtains described antibacterial chitosan gel rubber agent.
The antibacterial detection method of national standard of describing according to this description detects Analysis deterrmination, and antibacterial chitosan gel rubber agent prepared by the present embodiment all reaches 99.6% to the antibacterial ability of staphylococcus aureus, escherichia coli, streptococcus, bacillus pyocyaneus.
Embodiment 3: the preparation of chitosan anti-bacteria gel
A, prepare the complex liquid of chitosan-containing
Glacial acetic acid is mixed homogeneously according to weight ratio 1.2:18 with distilled water, according to the weight ratio 2.2:3.2 of high molecular weight chitosan and low-molecular weight chitoglycan, in its glacial acetic acid aqueous solution, add the molecular weight 60 * 10 of being sold with trade name food pharmaceutical grade chitosan by Jinan Haidebei Marine Organism Engineering Co., Ltd.
4the molecular weight 960Da that sell with trade name chitosan the high molecular weight chitosan of Da, deacetylation 92%, effluent Bei Bai taste bio tech ltd, the low-molecular weight chitoglycan of deacetylation 100%, stirring and dissolving, after homogenize, according to the weight ratio 1:5.0 of polyoxyethylene Pilus Caprae seu Ovis alcohol ether and chitosan total amount, add the polyoxyethylene Pilus Caprae seu Ovis alcohol ether of being sold with trade name polyoxyethylene Pilus Caprae seu Ovis alcohol ether by Britain standing grain major company again, stir, obtain a kind of complex liquid of chitosan-containing;
B, prepare fibroin alcoholic solution
According to fibroin and the concentration weight ratio 0.6:1.6 of 90% ethanol water by volume, the fibroin of being sold with trade name fibroin fiber by Suzhou Bao Sili fibroin fiber Science and Technology Ltd. is added in described ethanol water, stirring and dissolving, obtains a kind of fibroin alcoholic solution;
C, preparation carrageenan solutions
Distilled water is heated to 100 ℃ of temperature, then according to the weight ratio 35:1.8 of distilled water and carrageenan, in its distilled water, adds the carrageenan of being sold with trade name carrageenan by Beilun In Ningbo Ya Xu Chemical Co., Ltd., stirring and dissolving, obtains a kind of carrageenan solutions;
D, prepare quaternary phosphonium compound solution
By the pi-allyl triphenyl bromide phosphine product of preparing according to Ji'nan University's CN102020675B patented technology, mixed according to weight ratio 1:2.2 with the pi-allyl three amyl group phosphonium chlorides of being sold with trade name pi-allyl three amyl group phosphonium chloride ionic liquids by Shanghai flute cypress chemicals technology company limited, obtain a kind of mixture; Then according to the weight ratio 0.4:10 of described mixture and distilled water, described mixture is added in distilled water, after dissolving, add again the sucrose fatty acid ester of being sold with trade name sucrose ester by Hangzhou Jin Helai food additive company limited, the weight ratio of wherein said mixture and sucrose fatty acid ester is 0.5:1.0, stir, obtain a kind of sucrose fatty acid ester quaternary phosphonium compound solution that contains;
E, prepare gel
The fibroin alcoholic solution that the complex liquid of the chitosan-containing that steps A is obtained obtains with step B is mixed homogeneously, again this mixed solution is added in the carrageenan solutions that step C obtains, stir, what then add that step D obtains contains sucrose fatty acid ester quaternary phosphonium compound solution, add distilled water, mix homogeneously, obtains described antibacterial chitosan gel rubber agent.
The antibacterial detection method of national standard of describing according to this description detects Analysis deterrmination, and antibacterial chitosan gel rubber agent prepared by the present embodiment all reaches 99.2% to the antibacterial ability of staphylococcus aureus, escherichia coli, streptococcus, bacillus pyocyaneus.
Embodiment 4: the preparation of chitosan anti-bacteria gel
A, prepare the complex liquid of chitosan-containing
Glacial acetic acid is mixed homogeneously according to weight ratio 1.0:20 with distilled water, according to the weight ratio 1.9:3.0 of high molecular weight chitosan and low-molecular weight chitoglycan, in its glacial acetic acid aqueous solution, add the molecular weight 60 * 10 of being sold with trade name food pharmaceutical grade chitosan by Jinan Haidebei Marine Organism Engineering Co., Ltd.
4the molecular weight 845Da that sell with trade name chitosan the high molecular weight chitosan of Da, deacetylation 95%, effluent Bei Bai taste bio tech ltd, the low-molecular weight chitoglycan of deacetylation 98%, stirring and dissolving, after homogenize, according to the weight ratio 1:4.9 of polyoxyethylene Pilus Caprae seu Ovis alcohol ether and chitosan total amount, add the polyoxyethylene Pilus Caprae seu Ovis alcohol ether of being sold with trade name polyoxyethylene Pilus Caprae seu Ovis alcohol ether by Britain standing grain major company again, stir, obtain a kind of complex liquid of chitosan-containing;
B, prepare fibroin alcoholic solution
According to fibroin and the concentration weight ratio 0.8:2.4 of 95% ethanol water by volume, the fibroin of being sold with trade name fibroin fiber by Suzhou Bao Sili fibroin fiber Science and Technology Ltd. is added in described ethanol water, stirring and dissolving, obtains a kind of fibroin alcoholic solution;
C, preparation carrageenan solutions
Distilled water is heated to 96 ℃ of temperature, then according to the weight ratio 30:1.4 of distilled water and carrageenan, in its distilled water, adds the carrageenan of being sold with trade name carrageenan by Beilun In Ningbo Ya Xu Chemical Co., Ltd., stirring and dissolving, obtains a kind of carrageenan solutions;
D, prepare quaternary phosphonium compound solution
By the pi-allyl triphenyl bromide phosphine product of preparing according to Ji'nan University's CN102020675B patented technology, mixed according to weight ratio 1:2.0 with the pi-allyl three amyl group phosphonium chlorides of being sold with trade name pi-allyl three amyl group phosphonium chloride ionic liquids by Shanghai flute cypress chemicals technology company limited, obtain a kind of mixture; Then according to the weight ratio 0.2:12 of described mixture and distilled water, described mixture is added in distilled water, after dissolving, add again the sucrose fatty acid ester of being sold with trade name sucrose ester by Hangzhou Jin Helai food additive company limited, the weight ratio of wherein said mixture and sucrose fatty acid ester is 0.4:1.2, stir, obtain a kind of sucrose fatty acid ester quaternary phosphonium compound solution that contains;
E, prepare gel
The fibroin alcoholic solution that the complex liquid of the chitosan-containing that steps A is obtained obtains with step B is mixed homogeneously, again this mixed solution is added in the carrageenan solutions that step C obtains, stir, what then add that step D obtains contains sucrose fatty acid ester quaternary phosphonium compound solution, add distilled water, mix homogeneously, obtains described antibacterial chitosan gel rubber agent.
The antibacterial detection method of national standard of describing according to this description detects Analysis deterrmination, and antibacterial chitosan gel rubber agent prepared by the present embodiment all reaches 99.6% to the antibacterial ability of staphylococcus aureus, escherichia coli, streptococcus, bacillus pyocyaneus.
Embodiment 5: the preparation of chitosan anti-bacteria gel
A, prepare the complex liquid of chitosan-containing
Glacial acetic acid is mixed homogeneously according to weight ratio 0.9:16 with distilled water, according to the weight ratio 2.2:3.0 of high molecular weight chitosan and low-molecular weight chitoglycan, in its glacial acetic acid aqueous solution, add the molecular weight 60 * 10 of being sold with trade name food pharmaceutical grade chitosan by Jinan Haidebei Marine Organism Engineering Co., Ltd.
4the molecular weight 900Da that sell with trade name chitosan the high molecular weight chitosan of Da, deacetylation 88%, effluent Bei Bai taste bio tech ltd, the low-molecular weight chitoglycan of deacetylation 100%, stirring and dissolving, after homogenize, according to the weight ratio 1:4.9 of polyoxyethylene Pilus Caprae seu Ovis alcohol ether and chitosan total amount, add the polyoxyethylene Pilus Caprae seu Ovis alcohol ether of being sold with trade name polyoxyethylene Pilus Caprae seu Ovis alcohol ether by Britain standing grain major company again, stir, obtain a kind of complex liquid of chitosan-containing;
B, prepare fibroin alcoholic solution
According to fibroin and the concentration weight ratio 0.4:2.4 of 80% ethanol water by volume, the fibroin of being sold with trade name fibroin fiber by Suzhou Bao Sili fibroin fiber Science and Technology Ltd. is added in described ethanol water, stirring and dissolving, obtains a kind of fibroin alcoholic solution;
C, preparation carrageenan solutions
Distilled water is heated to 92 ℃ of temperature, then according to the weight ratio 35:1.4 of distilled water and carrageenan, in its distilled water, adds the carrageenan of being sold with trade name carrageenan by Beilun In Ningbo Ya Xu Chemical Co., Ltd., stirring and dissolving, obtains a kind of carrageenan solutions;
D, prepare quaternary phosphonium compound solution
By the pi-allyl triphenyl bromide phosphine product of preparing according to Ji'nan University's CN102020675B patented technology, mixed according to weight ratio 1:1.8 with the pi-allyl three amyl group phosphonium chlorides of being sold with trade name pi-allyl three amyl group phosphonium chloride ionic liquids by Shanghai flute cypress chemicals technology company limited, obtain a kind of mixture; Then according to the weight ratio 0.5:10 of described mixture and distilled water, described mixture is added in distilled water, after dissolving, add again the sucrose fatty acid ester of being sold with trade name sucrose ester by Hangzhou Jin Helai food additive company limited, the weight ratio of wherein said mixture and sucrose fatty acid ester is 0.2:1.2, stir, obtain a kind of sucrose fatty acid ester quaternary phosphonium compound solution that contains;
E, prepare gel
The fibroin alcoholic solution that the complex liquid of the chitosan-containing that steps A is obtained obtains with step B is mixed homogeneously, again this mixed solution is added in the carrageenan solutions that step C obtains, stir, what then add that step D obtains contains sucrose fatty acid ester quaternary phosphonium compound solution, add distilled water, mix homogeneously, obtains described antibacterial chitosan gel rubber agent.
The antibacterial detection method of national standard of describing according to this description detects Analysis deterrmination, and antibacterial chitosan gel rubber agent prepared by the present embodiment all reaches 99.8% to the antibacterial ability of staphylococcus aureus, escherichia coli, streptococcus, bacillus pyocyaneus.
Embodiment 6: the preparation of chitosan anti-bacteria gel
A, prepare the complex liquid of chitosan-containing
Glacial acetic acid is mixed homogeneously according to weight ratio 1.2:20 with distilled water, according to the weight ratio 1.8:3.4 of high molecular weight chitosan and low-molecular weight chitoglycan, in its glacial acetic acid aqueous solution, add the molecular weight 60 * 10 of being sold with trade name food pharmaceutical grade chitosan by Jinan Haidebei Marine Organism Engineering Co., Ltd.
4the molecular weight 845Da that sell with trade name chitosan the high molecular weight chitosan of Da, deacetylation 92%, effluent Bei Bai taste bio tech ltd, the low-molecular weight chitoglycan of deacetylation 100%, stirring and dissolving, after homogenize, according to the weight ratio 1:4.8 of polyoxyethylene Pilus Caprae seu Ovis alcohol ether and chitosan total amount, add the polyoxyethylene Pilus Caprae seu Ovis alcohol ether of being sold with trade name polyoxyethylene Pilus Caprae seu Ovis alcohol ether by Britain standing grain major company again, stir, obtain a kind of complex liquid of chitosan-containing;
B, prepare fibroin alcoholic solution
According to fibroin and the concentration weight ratio 0.6:1.6 of 85% ethanol water by volume, the fibroin of being sold with trade name fibroin fiber by Suzhou Bao Sili fibroin fiber Science and Technology Ltd. is added in described ethanol water, stirring and dissolving, obtains a kind of fibroin alcoholic solution;
C, preparation carrageenan solutions
Distilled water is heated to 90 ℃ of temperature, then according to the weight ratio 30:1.0 of distilled water and carrageenan, in its distilled water, adds the carrageenan of being sold with trade name carrageenan by Beilun In Ningbo Ya Xu Chemical Co., Ltd., stirring and dissolving, obtains a kind of carrageenan solutions;
D, prepare quaternary phosphonium compound solution
By the pi-allyl triphenyl bromide phosphine product of preparing according to Ji'nan University's CN102020675B patented technology, mixed according to weight ratio 1:2.2 with the pi-allyl three amyl group phosphonium chlorides of being sold with trade name pi-allyl three amyl group phosphonium chloride ionic liquids by Shanghai flute cypress chemicals technology company limited, obtain a kind of mixture; Then according to the weight ratio 0.2:11 of described mixture and distilled water, described mixture is added in distilled water, after dissolving, add again the sucrose fatty acid ester of being sold with trade name sucrose ester by Hangzhou Jin Helai food additive company limited, the weight ratio of wherein said mixture and sucrose fatty acid ester is 0.2:1.0, stir, obtain a kind of sucrose fatty acid ester quaternary phosphonium compound solution that contains;
E, prepare gel
The fibroin alcoholic solution that the complex liquid of the chitosan-containing that steps A is obtained obtains with step B is mixed homogeneously, again this mixed solution is added in the carrageenan solutions that step C obtains, stir, what then add that step D obtains contains sucrose fatty acid ester quaternary phosphonium compound solution, add distilled water, mix homogeneously, obtains described antibacterial chitosan gel rubber agent.
The antibacterial detection method of national standard of describing according to this description detects Analysis deterrmination, and antibacterial chitosan gel rubber agent prepared by the present embodiment all reaches 99.5% to the antibacterial ability of staphylococcus aureus, escherichia coli, streptococcus, bacillus pyocyaneus.
Claims (10)
1. a preparation method for antibacterial chitosan gel rubber agent, is characterized in that the step of this preparation method is as follows:
A, prepare the complex liquid of chitosan-containing
Glacial acetic acid is mixed homogeneously with distilled water, toward wherein adding molecular weight 60 * 10
4the high molecular weight chitosan of Da, deacetylation 85-95% and molecular weight are lower than 1 * 10
3the low-molecular weight chitoglycan of Da, deacetylation 98-100%, stirring and dissolving, adds polyoxyethylene Pilus Caprae seu Ovis alcohol ether again after homogenize, stir, and obtains a kind of complex liquid of chitosan-containing;
B, prepare fibroin alcoholic solution
Fibroin is added in ethanol water, and stirring and dissolving, obtains a kind of fibroin alcoholic solution;
C, preparation carrageenan solutions
Distilled water is heated to 90～100 ℃ of temperature, then adds carrageenan, stirring and dissolving, obtains a kind of carrageenan solutions;
D, prepare quaternary phosphonium compound solution
Pi-allyl triphenyl bromide phosphine mixes according to weight ratio 1:1.8～2.2 with pi-allyl three amyl group phosphonium chlorides, obtains a kind of mixture; Then described mixture is added in distilled water, after dissolving, adds again sucrose fatty acid ester, stir, obtain a kind of sucrose fatty acid ester quaternary phosphonium compound solution that contains;
E, prepare gel
The fibroin alcoholic solution that the complex liquid of the chitosan-containing that steps A is obtained obtains with step B is mixed homogeneously, again mixed solution is added in the carrageenan solutions that step C obtains, stir, what then add that step D obtains contains sucrose fatty acid ester quaternary phosphonium compound solution, add distilled water, mix homogeneously, obtains described antibacterial chitosan gel rubber agent.
2. preparation method according to claim 1, is characterized in that in steps A, and the weight ratio of glacial acetic acid and distilled water is 0.8～1.2:16～22.
3. preparation method according to claim 1, is characterized in that in steps A, and the weight ratio of described high molecular weight chitosan and described low-molecular weight chitoglycan is 1.8～2.2:2.6～3.4.
4. preparation method according to claim 1, is characterized in that in steps A, and the weight ratio of polyoxyethylene Pilus Caprae seu Ovis alcohol ether and chitosan total amount is 1:4.8～5.2.
5. preparation method according to claim 1, is characterized in that, in step B, the weight ratio of fibroin and ethanol water is 0.3～0.8:1.6～2.4.
6. preparation method according to claim 1 or 5, is characterized in that in step C, and the concentration of described ethanol water is by volume 80～95%.
7. preparation method according to claim 1, is characterized in that, in step C, the weight ratio of distilled water and carrageenan is 25～35:0.5～1.8.
8. preparation method according to claim 1, is characterized in that in step D, and the weight ratio of pi-allyl triphenyl bromide phosphine and pi-allyl three amyl group phosphonium chloride mixture and distilled water is 0.1～0.5:8～12.
9. preparation method according to claim 1, is characterized in that in step D, and the weight ratio of pi-allyl triphenyl bromide phosphine and pi-allyl three amyl group phosphonium chloride mixture and sucrose fatty acid ester is 0.1～0.5:0.8～1.2.
10. the antibacterial chitosan gel rubber agent that preparation method obtains according to claim 1, is characterized in that it reaches more than 99% the antibacterial ability of staphylococcus aureus, escherichia coli, streptococcus, Candida albicans or bacillus pyocyaneus.
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| CN107715102A (en) * | 2017-10-19 | 2018-02-23 | 关亚玲 | A kind of preparation method of the thimerosal comprising fibroin |
| CN108904780A (en) * | 2018-08-24 | 2018-11-30 | 湖南金朋医疗器械有限公司 | A kind of gynaecological gel and preparation method thereof |
| WO2019110325A1 (en) | 2017-12-05 | 2019-06-13 | Universita' Degli Studi Di Roma "La Sapienza" | Composition for use in the finishing, preservation, restoration of manufactures |
| CN112370464A (en) * | 2019-12-27 | 2021-02-19 | 青岛博智汇力生物科技有限公司 | Marine oligosaccharide composition for treating beriberi |
| CN114652621A (en) * | 2022-03-31 | 2022-06-24 | 宁德师范学院 | Chitosan and silicon oxide composite hydrogel with high ethanol content |
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