CN104042791A - Antibacterial modified chitosan foaming agent and preparation method thereof - Google Patents
Antibacterial modified chitosan foaming agent and preparation method thereof Download PDFInfo
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Abstract
The invention relates to an antibacterial modified chitosan foaming agent and a preparation method thereof. The preparation method of the antibacterial modified chitosan foaming agent comprises the steps of preparing modified chitosan, extracting white tea, preparing a complex solution containing chitosan, preparing a corn protein complex solution and preparing an antibacterial modified chitosan foaming agent. The antibacterial modified chitosan foaming agent has antibacterial ability more than 99% on staphylococcus aureus, escherichia coli, streptococcus, candida albicans or pseudomonas aeruginosa and shows good bacteriostatic ability. The antibacterial modified chitosan foaming agent can be applied to treatment on bacterial vaginitis, colpomycosis and mixed vaginitis and can be widely applied.
Description
[technical field]
The invention belongs to medical drugs technical field.More specifically, the present invention relates to a kind of antibacterial modified chitose foaming agent, also relate to the preparation method of described antibacterial modified chitose foaming agent
[background technology]
Vaginitis is the common genitals's inflammation of a kind of women, and in married woman, crowd over half suffers from vaginitis in various degree, clinically vaginitis is probably divided into kind more than ten, specifically comprises bacterial vaginitis, trichomonal vaginitis, monilial vaginitis, senile vaginitis, infant vaginitis, candidiasis vaginitis, viral HSV, HPv vaginitis, gonococcal vaginitis, desquamative inflammatory vaginitis, nonspecific vaginitis, Tuberculous vaginitis, Drug vaginitis, radioactivity vaginitis, ulcer of vagina is acute, anaphylaxis vaginitis, chronic vaginitis, burn worm property vaginitis and mixed vaginitis etc., more common and be mainly bacterial vaginitis to the more serious vaginitis of women's health hazard ratio, trichomonal vaginitis and monilial vaginitis, be embodied in pudendum convulsion and itch, heating, scorching hot, leucorrhoea grow in quantity abnormal flavour, the symptoms such as discomfort are common gynecological diseases, frequently-occurring disease, serious harm WomanHealth, brings inconvenience to patient's work and life.
Vaginitis outward manifestation is mainly local disease, thus in its treatment measure substantially taking external treatment as main, it is auxiliary that treatment by oral administration of medicines is taken medicine.In external treatment, work out in recent years many new methods and developed many therapeutant dosage forms, as washing liquid, vaginal suppository, vaginal tablet, powder, paste, unguentum and capsule, membrane etc.Washing liquid is mainly external, can not contact with focus for a long time, therefore can not effectively bring into play drug effect, can only serve as daily health caring medication; Unguentum, vaginal tablet and vaginal suppository are slow in intravaginal onset, cannot fully contact with focus, and medicine disperses inhomogeneous, when use, will directly use hand operated, easily pollutes medicine, causes cross infection, in addition, returns patient and brings foreign body sensation.
In view of there is in use inconvenience in above healing potion, have that contact area is little, assimilation effect is bad, easily cause the deficiencies such as cross infection, people have developed new dosage form-foam, foam has overcome the shortcoming of above-mentioned dosage form, can make medicine be uniformly distributed in intravaginal, fully contact with vaginal mucosa wrinkle skirt, absorb rapidly good effect.
At present, people have carried out broad research to foam, for example CN101380447A discloses a kind of chitose foaming agent that is used for the treatment of gynaecopathia and preparation method thereof, and this chitose foaming agent is compound formulated by chitosan, manna oligosaccharide, benzalkonium chloride, aloe, Oleum Curcumae, triclosan, NPE, Cortex cocois radicis oil base alkanolamide, PEG400, sodium lauryl sulphate, dodecyl alcohol ether ammonium sulfate, tween, triethanolamine, purified water and the third butane etc.; CN102872160A discloses a kind of for scalding the nano silver foam agent of burn, ulcer wound disinfection, and described nano silver foam agent is made up of wither joint agent and propellant of nanometer silver sol solution, chitosan, solubilizing agent, wetting agent, thickening agent, antiseptic, foaming agent, Fungicidal substance, refrigerant material, pH; CN102895256A discloses chitosan plural gel foam of the dual contraceptive efficacy of a kind of women's of being applicable to barrier spermicidal and preparation method thereof, and it is made up of chitosan gel rubber substrate and surfactant, ancillary drug, cosolvent, Acidifier, foaming agent, foam stabiliser, solvent and propellant.
There is following technological deficiency in these technology: one, they all use treib gasaerosoles such as comprising propane, butane or iso-butane, halogenated hydrocarbons, two, add medicines dressing wide in variety, complex manufacturing process; Though three taking chitosan as host matrix, all adds other antimicrobial component, as compositions such as triclosan, nanometer silver, Borneolum Syntheticum, Mentholums.State Food and Drug Administration expressly provides at present, should eliminate gradually CFC class material as pharmaceutic adjuvant aerosol for external use, in addition, propellant can have certain zest to vagina, therefore, research and develop a kind of vaginal foam of making simple, safety, environmental protection extremely urgent.
In addition, have not yet to see about utilizing chitosan to prepare the patent of foam as primary raw material.At present the chitosan of application is to be mainly polymer chitosan, does not also see by chitin modified, controls its molecular weight and deacetylation and improve the relevant report of foam antibacterial action.
The object of the invention is to overcome the shortcoming existing in prior art, solve problems such as lacking at present the environmental protection of pure chitosan class, efficient foam agent, manufacture method complexity, a kind of preparation method of modified chitosan anti-bacteria foam is proposed, the foam obtaining has trickle foaming structure, antibacterial wide spectrum is effective, can promote focus cellular-restoring, and preparation and application method is simple, can be advantageously used in various colpitic treatment, the nursing etc. of clinical gynecological.
[summary of the invention]
[technical problem that will solve]
The object of this invention is to provide a kind of antibacterial modified chitose foaming agent.
Another object of the present invention is to provide the preparation method of described antibacterial modified chitose foaming 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 modified chitose foaming agent.
The step of this antibacterial modified chitose foaming agent preparation method is as follows:
A, prepare modification of chitosan
By deacetylation 70%, molecular weight 30 × 10
4～60 × 10
4the chitosan of Da is dissolved in by weight in 1～2% aqueous acetic acid, and the solution obtaining carries out supersound process in ultrasonic washing unit, then carries out classification with polyvinylidene fluoride (PVDF) ultrafiltration membrane, dry, obtains the chitosan of molecular weight 500～1000Da; This chitosan is added to by weight in 40～50% potassium hydroxide aqueous solutions, under the condition of 110～120 DEG C of temperature, process 15～20min, then neutralize, filtration, distilled water wash, be dried with 1.0～3.0N aqueous hydrochloric acid solution, obtain the modification of chitosan of deacetylation 98～99%, molecular weight 500～1000Da;
B, Ramulus et Folium Mussaendae Pubescentis extract
Take 15～25 weight portion Ramulus et Folium Mussaendae Pubescentis, toward wherein adding 80～120 weight portion distilled water, then at 95～100 DEG C of temperature, extract 25～35min, filter, remove tea grounds, the filtrate standardize solution obtaining, to 100 weight portions, is obtained containing tea polyphenols, caffeine, theophylline, Ramulus et Folium Mussaendae Pubescentis extracting solution tannic acid, that concentration is 0.016～0.024g/ml;
C, prepare chitosan-containing composite solution
The modification of chitosan that 2～10 weight portions are prepared in steps A is dissolved in glacial acetic acid aqueous solution, then add 0.2～1.2 weight portion polysorbas20, 0.2～1.2 weight portion Tween 80, 0.3～0.8 weight portion dodecanol polyethenoxy ether sodium sulfate and 0.5～1.5 weight portion sodium lauryl sulphate, the Ramulus et Folium Mussaendae Pubescentis extracting solution that adds again 1.5～2.5 weight portions to prepare at step B after dissolving, 0.05～0.15 weight portion pi-allyl triphenyl bromide phosphine and 0.30～0.50 weight portion ascorbyl palmitate, continue to stir, after dissolving, obtain a kind of composite solution of chitosan-containing,
D, preparation are containing corn protein composite solution
0.1～1.0 weight portion corn protein, 0.2～1.2 weight portion agarose, 0.1～0.3 weight portion sorbitol, 0.01～0.09 weight portion chondroitin sulfate are dissolved in 18～42 weight portion distilled water, obtain a kind of composite solution containing corn protein;
E, prepare antibacterial modified chitose foaming agent
Take 4～8 weight portion glycerol, add water, stir, then add the composite solution of the chitosan-containing that 25～35 weight portions obtain at step C and the composite solution containing corn protein that 30～40 weight portions obtain at step D, stir, obtain described antibacterial modified chitose foaming agent.
A preferred embodiment of the invention, in steps A, dissolves 5～15min under the condition of deacetylation 70% chitosan low whipping speed 250～350rpm in aqueous acetic acid.
According to another kind of preferred implementation of the present invention, in steps A, supersound process 35～45min under the condition that the solution obtaining is 200W at supersonic frequency 22kHz and ultrasonic power.
According to another kind of preferred implementation of the present invention, in step B, the weight ratio of Ramulus et Folium Mussaendae Pubescentis and distilled water is 18～22:90～110.
According to another kind of preferred implementation of the present invention, in step C, described glacial acetic acid aqueous solution is by 0.1～0.3 weight portion glacial acetic acid and the preparation of 18～22 weight portion distilled water.
According to another kind of preferred implementation of the present invention, in step C, the weight ratio of polysorbas20, Tween 80, dodecanol polyethenoxy ether sodium sulfate and sodium lauryl sulphate is 0.5～0.8:0.5～0.8:0.4～0.6:0.8～1.2.
According to another kind of preferred implementation of the present invention, in step C, the weight ratio of Ramulus et Folium Mussaendae Pubescentis extracting solution, pi-allyl triphenyl bromide phosphine and ascorbyl palmitate is 1.8～2.2:0.08～0.12:0.36～0.42.
According to another kind of preferred implementation of the present invention, in step D, the weight ratio of corn protein, agarose, sorbitol and chondroitin sulfate is 0.3～0.7:0.4～1.0:0.15～0.25:0.03～0.08.
According to another kind of preferred implementation of the present invention, in step e, the composite solution of glycerol, chitosan-containing is 5～6:28～32:32～38 with the weight ratio of the composite solution containing corn protein.
The invention still further relates to the antibacterial modified chitose foaming agent that adopts described preparation method to obtain.Described antibacterial modified chitose foaming agent all reaches more than 99% the antibacterial ability of staphylococcus aureus, escherichia coli, streptococcus, Candida albicans or bacillus pyocyaneus.
The present invention will be described below in more detail.
The present invention relates to a kind of preparation method of antibacterial modified chitose foaming agent.
The step of this preparation method is as follows:
A, prepare modification of chitosan
By deacetylation 70%, molecular weight 30 × 10
4～60 × 10
4the chitosan of Da is dissolved in by weight in 1～2% aqueous acetic acid, and the solution obtaining carries out supersound process in ultrasonic washing unit, then carries out classification with polyvinylidene fluoride (PVDF) ultrafiltration membrane, dry, obtains the chitosan of molecular weight 500～1000Da; This chitosan is added to by weight in 40～50% potassium hydroxide aqueous solutions, under the condition of 110～120 DEG C of temperature, process 15～20min, then neutralize, filtration, distilled water wash, be dried with 1.0～3.0N aqueous hydrochloric acid solution, obtain the modification of chitosan of deacetylation 98～99%, molecular weight 500～1000Da;
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.Antibacterial modified chitose foaming agent main body of the present invention is natural product chitosan, and it has improved the biological safety of described foam, meanwhile, avoids using propellant, so improved the safety in utilization of described foam, is conducive to environmental protection.
In this step, under the condition of the chitosan of deacetylation 70% low whipping speed 250～350rpm in aqueous acetic acid, dissolve 5～15min, obtain chitosan aqueous acetic acid.
The chitosan that the present invention uses is product sold in the market, for example by Jinan Haidebei Marine Organism Engineering Co., Ltd. with trade name food pharmaceutical grade chitosan product sold.
In this step, adopt hyperfiltration process by deacetylation 70%, molecular weight 30 × 10
4～60 × 10
4da high molecular weight chitosan prepares the chitosan of molecular weight 500～1000Da.
In the present invention, the object of ultrasonic waves for cleaning processing is to allow high molecular weight chitosan aqueous acetic acid carry out ultrasonic Treatment 30～50 minutes under the condition of ultrasonic frequency 20～25kHz and power 180～220W, obtains low-molecular weight chitoglycan complex solution.Preferably, supersound process 35～45min under the condition that high molecular weight chitosan aqueous acetic acid is 200W at supersonic frequency 22kHz and ultrasonic power.
The ultrasonic washing unit that the present invention uses is product sold in the market, for example by Changzhou You Da ultrasonic equipment company limited with trade name YD1008 ultrasonic washing unit product sold.
The present invention is by molecule hyperfiltration technique; by chitosan classification; the chitosan with best molecular level scope that intercepting molecular weight is 500～1000; then by again deacetylated; the modification of chitosan that obtains high deacetylized, low-molecular-weight, narrow molecular weight distribution, improves broad-spectrum antibacterial property energy greatly.
Normally a kind of hydrophobicity ultrafilter membrane with good any biological inert, chemical stability, heat stability of polyvinylidene fluoride (PVDF) ultrafiltration membrane.
Carrying out classification with polyvinylidene fluoride (PVDF) ultrafiltration membrane is that a kind of chitosan molecule that molecular weight is greater than to 500～1000Da is held back, and the operation that the chitosan molecule that allows molecular weight be less than 500～1000Da is passed through.The molecular weight of chitosan adopts conventional gel permeation chromatography method to measure and obtains.
The performance of the polyvinylidene fluoride (PVDF) ultrafiltration membrane that the present invention uses is as follows: thickness 110-150 μ m, Unit Weight 3.3-5.1mg/cm
2, porosity 72-78%, intensity be greater than 60pst.
The polyvinylidene fluoride (PVDF) ultrafiltration membrane that the present invention uses is product sold in the market, for example by KENKER company of the U.S. with trade name polyvinylidene fluoride film product sold.
After classification, dry is to allow the chitosan molecule part that the molecular weight collected is 500～1000Da under temperature 60 C condition, be dried to water content lower than 6% in hot-air dry equipment.
Then, the chitosan molecule that is 500～1000Da to obtained molecular weight is carried out modification with alkali, i.e. further deacetylated processing.
In this modification procedure, the object of washing is to remove salt and other impurity that neutralization produces.Dry object is to remove moisture, and the equipment that this drying steps uses is with previously described identical, and baking temperature condition is also with previously described identical.
B, Ramulus et Folium Mussaendae Pubescentis extract
Take 15～25 weight portion Ramulus et Folium Mussaendae Pubescentis, toward wherein adding 80～120 weight portion distilled water, then at 95～100 DEG C of temperature, extract 25～35min, filter, remove tea grounds, by the filtrate standardize solution obtaining to 100 weight portions, the Ramulus et Folium Mussaendae Pubescentis extracting solution that the concentration that obtains containing tea polyphenols, caffeine, theophylline, tannic acid etc. is 0.016～0.024g/ml;
Ramulus et Folium Mussaendae Pubescentis be a kind of after harvesting without completing or kneading, only, through the tea shining or the dry machining of slow fire obtains, its polyphenols equal size is higher.The diseases such as Ramulus et Folium Mussaendae Pubescentis has the effects such as eliminating inflammation and expelling toxin, clearing heat and moistening lung, suppressing the hyperactive liver benefit blood, blood pressure lowering fat reducing, allaying tiredness, uncomfortable, the digestive functional disturbance that especially excessive, greasy too much to tobacco and wine, liver-fire is excessively prosperous to be caused have the health-care effect of uniqueness, ethereality.
In the present invention, if Ramulus et Folium Mussaendae Pubescentis is less than 95 DEG C by the temperature of distilled water extraction, can make to extract not exclusively; If Ramulus et Folium Mussaendae Pubescentis higher than 100 DEG C, there will be the oxidized problem of Polyphenols by the temperature of distilled water extraction; Therefore, to be 95～100 DEG C by the temperature of distilled water extraction be suitable to Ramulus et Folium Mussaendae Pubescentis.
The Ramulus et Folium Mussaendae Pubescentis that the present invention uses is product sold in the market, for example by Fujian Pinpinxiang Tea Industry Co., Ltd. with trade name Fuding white tea product sold.
Preferably, the weight ratio of Ramulus et Folium Mussaendae Pubescentis and distilled water is 18～22:90～110.
C, prepare chitosan-containing composite solution
The modification of chitosan that 2～10 weight portions are prepared in steps A is dissolved in glacial acetic acid aqueous solution, then add 0.2～1.2 weight portion polysorbas20, 0.2～1.2 weight portion Tween 80, 0.3～0.8 weight portion dodecanol polyethenoxy ether sodium sulfate and 0.5～1.5 weight portion sodium lauryl sulphate, the Ramulus et Folium Mussaendae Pubescentis extracting solution that adds again 1.5～2.5 weight portions to prepare at step B after dissolving, 0.05～0.15 weight portion pi-allyl triphenyl bromide phosphine and 0.30～0.50 weight portion ascorbyl palmitate, continue to stir, after dissolving, obtain a kind of composite solution of chitosan-containing,
Described glacial acetic acid aqueous solution is by 0.1～0.3 weight portion glacial acetic acid and the preparation of 18～22 weight portion distilled water.
In this step, using polysorbas20, Tween 80, dodecanol polyethenoxy ether sodium sulfate and sodium lauryl sulphate is in order to make antibacterial modified chitose foaming agent of the present invention have good spumescence.
The weight ratio of polysorbas20, Tween 80, dodecanol polyethenoxy ether sodium sulfate and sodium lauryl sulphate is 0.5～0.8:0.5～0.8:0.4～0.6:0.8～1.2, preferably 0.55～0.74:0.58～0.72:0.45～0.55:0.88～1.12.
Polysorbas20, Tween 80, dodecanol polyethenoxy ether sodium sulfate and the sodium lauryl sulphate that the present invention uses is all product sold in the market, for example by Guangdong Run Hua Chemical Co., Ltd. with trade name polysorbas20, Tween 80 product sold, the dodecanol polyethenoxy ether sodium sulfate of being sold with trade name AES-2EO by Shanghai Xian Jie Chemical Industry Science Co., Ltd, sodium lauryl sulphate by Shanghai You Yang Industrial Co., Ltd. with trade name K12 sale.
In addition, the present invention is by adding a small amount of phosphorus-containing compound, regulate the foaming effect of anion surfactant and non-ionic surface active agent, make foam finer and smoother, stable, diffusion power promotes greatly, can in vaginitis, evenly spread without propellant, and in vagina, effect is rapider, the efficient general medicines such as also dark people's vaginal mucosa fold deep, fornix portion and cervix uteri mouth that disperse are difficult to the place arriving, and are conducive to same pathogen contact and also produce rapidly antibacterial, bactericidal action.
Antibacterial modified chitose foaming agent of the present invention is by containing the synergism of amino chitosan and phosphorus-containing compound, Ramulus et Folium Mussaendae Pubescentis extract, there is 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 are all had to more than 99% kill efficiency, greatly improve anti-microbial property.
Preferably, the weight ratio of Ramulus et Folium Mussaendae Pubescentis extracting solution, pi-allyl triphenyl bromide phosphine and ascorbyl palmitate is 1.8～2.2:0.08～0.12:0.36～0.42.
D, preparation are containing corn protein composite solution
0.1～1.0 weight portion corn protein, 0.2～1.2 weight portion agarose, 0.1～0.3 weight portion sorbitol, 0.01～0.09 weight portion chondroitin sulfate are dissolved in 18～42 weight portion distilled water, obtain a kind of composite solution containing corn protein;
The corn protein that the present invention uses is product sold in the market, for example by Li Tong bio tech ltd, Shandong with trade name Zein powder product sold.
Agarose is a kind of linear polymer, and its basic structure is by 3 of β-D-galactose of 1,3 link and the link of Isosorbide-5-Nitrae position, the long-chain polymer that 6-inner ether-L-galactose alternately couples together.Agar pectin is by many less molecular heterogeneous mixture.Agarose is generally heated to more than 90 DEG C and dissolves in water, and temperature forms the gel of good semi-solid while dropping to 35-40 DEG C.The agarose that the present invention uses is product sold in the market, for example by Fujian Ming Fu agar company limited with trade name agar powder product sold.
The sorbitol (Sorbitol) that the present invention uses is product sold in the market, for example by Shouguang, Shandong Hua Tian sugar alcohol company limited with trade name Neosorb product sold.
Chondroitin sulfate is a covalently bound class glycosaminoglycans that forms Dan Baiduotang proteoglycan PG on protein, and chondroitin sulfate is present in from nematicide to people except in exophytic all biologies, is bringing into play many important physiological functions.The chondroitin sulfate that the present invention uses is product sold in the market, for example by Anhui Kebao Biology Engineering Co., Ltd with trade name chondroitin sulfate product sold.
Antibacterial modified chitose foaming agent of the present invention contains ascorbyl palmitate, sorbitol, zein and chondroitin sulfate; they can either play the effect of stable foam; protection vaginal wall cell membrane be can also play, reparation and the growth of infection process cell accelerated to be subject to.
Preferably, the weight ratio of corn protein, agarose, sorbitol and chondroitin sulfate is 0.3～0.7:0.4～1.0:0.15～0.25:0.03～0.08.
E, prepare antibacterial modified chitose foaming agent
Take 4～8 weight portion glycerol, add water, stir, then add the composite solution of the chitosan-containing that 25～35 weight portions obtain at step C and the composite solution containing corn protein that 30～40 weight portions obtain at step D, stir, obtain described antibacterial modified chitose foaming agent.
According to the present invention, glycerol when being described scope containing the amount of the composite solution of corn protein, if the amount of the composite solution of chitosan-containing is less than 25 weight portions, there will be anti-microbial property to decline; If the amount of the composite solution of chitosan-containing is greater than 35 weight portions, there will be solution viscosity problems of too; Therefore, the amount of the composite solution of chitosan-containing is that 25～35 weight portions are rational.Similarly, when the amount of the composite solution of glycerol and chitosan-containing is described scope, if be less than 30 weight portions containing the amount of the composite solution of corn protein, can make foam stability decline; Be greater than 40 weight portions if contain the amount of the composite solution of corn protein, can be affected by anti-microbial property; Therefore, the amount of the composite solution of chitosan-containing is that 30～40 weight portions are rational.
Preferably, the composite solution of glycerol, chitosan-containing is 5～6:28～32:32～38 with the weight ratio of the composite solution containing corn protein.
The invention still further relates to the antibacterial modified chitose foaming agent that adopts described preparation method to obtain.Antibacterial modified chitose foaming agent all reaches more than 99% the antibacterial ability of staphylococcus aureus, escherichia coli, streptococcus, Candida albicans or bacillus pyocyaneus.
Antibacterial modified chitose foaming agent of the present invention can be applied to treatment bacterial vaginitis, colpitis mycotica and mixed vaginitis etc., applies very extensive.
Antibacterial modified chitose foaming agent of the present invention detects and analyzes through the antibacterial detection method of national standard (GB/T16886), antibacterial ability to staphylococcus aureus, escherichia coli, streptococcus, Candida albicans or bacillus pyocyaneus etc. all reaches more than 99%, demonstrates good bacteriostasis.
[beneficial effect]
The invention has the beneficial effects as follows:
1, antibacterial modified chitose foaming agent main body of the present invention adopts natural product chitosan, has improved the biological safety of foam, meanwhile, avoids using propellant, has improved safety in utilization and environmental protection.
2, the present invention adopts molecule hyperfiltration technique by chitosan classification, intercepts the chitosan of molecular weight 500-1000, then by deacetylated, obtains the modification of chitosan of high deacetylized, low-molecular-weight, narrow molecular weight distribution, greatly improves broad-spectrum antibacterial property energy.
3, the antibacterial modified chitose foaming agent that prepared by the present invention is by containing the synergism of amino chitosan and phosphorus-containing compound, Ramulus et Folium Mussaendae Pubescentis extract, there is 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 are all had to more than 99% kill efficiency, greatly improve anti-microbial property.
4, the present invention is by adding a small amount of phosphorus-containing compound, regulate the foaming effect of anion surfactant and non-ionic surface active agent, make foam finer and smoother, stable, diffusion power promotes greatly, can in vaginitis, evenly spread without propellant, in vagina, effect is rapider, efficient disperse and the general medicine such as dark people's vaginal mucosa fold deep, fornix portion and cervix uteri mouth is difficult to the place arriving, is conducive to same pathogen contact and produces rapidly antibacterial, bactericidal action.
5, the present invention passes through to increase ascorbyl palmitate, sorbitol, and zein and chondroitin sulfate, can either play the effect of stable foam, more can play protection vaginal wall cell membrane, accelerates to be subject to reparation and the growth of infection process cell.
[detailed description of the invention]
Can understand better the present invention by following embodiment.
Embodiment 1: prepare antibacterial modified chitose foaming agent
The implementation step of this embodiment is as follows:
A, prepare modification of chitosan
By sold with trade name food pharmaceutical grade chitosan by Jinan Haidebei Marine Organism Engineering Co., Ltd., deacetylation 70%, molecular weight 30 × 10
4the chitosan of Da, in 2% aqueous acetic acid by weight, under the condition of low whipping speed 250rpm, dissolve 15min, the solution obtaining is in the ultrasonic washing unit of being sold with trade name YD1008 ultrasonic washing unit by Changzhou You Da ultrasonic equipment company limited, under the condition of ultrasonic frequency 20kHz and power 200W, carry out ultrasonic Treatment 45 minutes, use again the polyvinylidene fluoride (PVDF) ultrafiltration membrane of being sold with trade name polyvinylidene fluoride film by KENKER company of the U.S. to carry out classification, dry under temperature 60 C condition in hot-air dry equipment, obtain the chitosan of molecular weight 900Da, this chitosan is added to by weight in 50% potassium hydroxide aqueous solution, under the condition of 116 DEG C of temperature, process 17min, then neutralize, filtration, distilled water wash, in drying equipment similar to the above, under temperature 60 C condition, be dried with 2.0N aqueous hydrochloric acid solution, obtain the modification of chitosan of deacetylation 98%, molecular weight 500Da,
B, Ramulus et Folium Mussaendae Pubescentis extract
Take the Ramulus et Folium Mussaendae Pubescentis that 15 weight portions are sold with trade name Fuding white tea by Fujian Pinpinxiang Tea Industry Co., Ltd., toward wherein adding 90 weight portion distilled water, then at 95 DEG C of temperature, extract 35min, filter, remove tea grounds, the filtrate standardize solution obtaining, to 100 weight portions, is obtained to the Ramulus et Folium Mussaendae Pubescentis extracting solution that the mixture concentrations such as tea polyphenols and caffeine, theophylline, tannic acid are 0.016g/ml;
C, prepare chitosan-containing composite solution
The modification of chitosan that 8 weight portions are prepared in steps A is dissolved in the glacial acetic acid aqueous solution by 0.2 weight portion glacial acetic acid and the preparation of 18 weight portion distilled water, then add 1.0 weight portion polysorbas20s, 0.6 weight portion Tween 80, the sodium lauryl sulphate that the dodecanol polyethenoxy ether sodium sulfate that 0.3 weight portion is sold with trade name AES-2EO by Shanghai Xian Jie Chemical Industry Science Co., Ltd and 1.5 weight portions are sold with trade name K12 by Shanghai You Yang Industrial Co., Ltd., the Ramulus et Folium Mussaendae Pubescentis extracting solution that adds again 2.1 weight portions to prepare at step B after dissolving, the ascorbyl palmitate that the pi-allyl triphenyl bromide phosphine that 0.15 weight portion is prepared according to Ji'nan University's CN102020675B patented technology and 0.38 weight portion are sold with trade name L-AA Palmitate by Shaanxi Sen Fu natural product company limited, continue to stir, after dissolving, obtain a kind of composite solution of chitosan-containing,
D, preparation are containing corn protein composite solution
The corn protein that 0.1 weight portion is sold with trade name Zein powder by Li Tong bio tech ltd, Shandong, the agarose that 0.5 weight portion is sold with trade name agar powder by Fujian Ming Fu agar company limited, the sorbitol that 0.2 weight portion is sold with trade name Neosorb by Shouguang, Shandong Hua Tian sugar alcohol company limited, the chondroitin sulfate that 0.06 weight portion is sold with trade name chondroitin sulfate by Anhui Kebao Biology Engineering Co., Ltd are dissolved in 42 weight portion distilled water, obtain a kind of composite solution containing corn protein;
E, prepare antibacterial modified chitose foaming agent
Take 4 weight portion glycerol, add water, stir, then add the composite solution of the chitosan-containing that 32 weight portions obtain at step C and the composite solution containing corn protein that 40 weight portions obtain at step D, stir, obtain described antibacterial modified chitose foaming agent.
The antibacterial detection method of national standard of describing according to this description detects Analysis deterrmination, and antibacterial modified chitose foaming agent prepared by the present embodiment all reaches 99.4% to the antibacterial ability of staphylococcus aureus, escherichia coli, streptococcus, bacillus pyocyaneus.
Embodiment 2: prepare antibacterial modified chitose foaming agent
The implementation step of this embodiment is as follows:
A, prepare modification of chitosan
By sold with trade name food pharmaceutical grade chitosan by Jinan Haidebei Marine Organism Engineering Co., Ltd., deacetylation 70%, molecular weight 40 × 10
4the chitosan of Da, in 1% aqueous acetic acid by weight, under the condition of low whipping speed 280rpm, dissolve 8min, the solution obtaining is in the ultrasonic washing unit of being sold with trade name YD1008 ultrasonic washing unit by Changzhou You Da ultrasonic equipment company limited, under the condition of ultrasonic frequency 22kHz and power 180W, carry out ultrasonic Treatment 30 minutes, use again the polyvinylidene fluoride (PVDF) ultrafiltration membrane of being sold with trade name polyvinylidene fluoride film by KENKER company of the U.S. to carry out classification, dry under temperature 60 C condition in hot-air dry equipment, obtain the chitosan of molecular weight 500Da, this chitosan is added to by weight in 40% potassium hydroxide aqueous solution, under the condition of 110 DEG C of temperature, process 20min, then neutralize, filtration, distilled water wash, in drying equipment similar to the above, under temperature 60 C condition, be dried with 1.0N aqueous hydrochloric acid solution, obtain the modification of chitosan of deacetylation 99%, molecular weight 650Da,
B, Ramulus et Folium Mussaendae Pubescentis extract
Take the Ramulus et Folium Mussaendae Pubescentis that 18 weight portions are sold with trade name Fuding white tea by Fujian Pinpinxiang Tea Industry Co., Ltd., toward wherein adding 110 weight portion distilled water, then at 100 DEG C of temperature, extract 25min, filter, remove tea grounds, the filtrate standardize solution obtaining, to 100 weight portions, is obtained to the Ramulus et Folium Mussaendae Pubescentis extracting solution that the mixture concentrations such as tea polyphenols and caffeine, theophylline, tannic acid are 0.019g/ml;
C, prepare chitosan-containing composite solution
The modification of chitosan that 2 weight portions are prepared in steps A is dissolved in the glacial acetic acid aqueous solution by 0.1 weight portion glacial acetic acid and the preparation of 20 weight portion distilled water, then add 0.2 weight portion polysorbas20, 0.2 weight portion Tween 80, the sodium lauryl sulphate that the dodecanol polyethenoxy ether sodium sulfate that 0.4 weight portion is sold with trade name AES-2EO by Shanghai Xian Jie Chemical Industry Science Co., Ltd and 1.2 weight portions are sold with trade name K12 by Shanghai You Yang Industrial Co., Ltd., the Ramulus et Folium Mussaendae Pubescentis extracting solution that adds again 1.5 weight portions to prepare at step B after dissolving, the ascorbyl palmitate that the pi-allyl triphenyl bromide phosphine that 0.05 weight portion is prepared according to Ji'nan University's CN102020675B patented technology and 0.30 weight portion are sold with trade name L-AA Palmitate by Shaanxi Sen Fu natural product company limited, continue to stir, after dissolving, obtain a kind of composite solution of chitosan-containing,
D, preparation are containing corn protein composite solution
The corn protein that 0.4 weight portion is sold with trade name Zein powder by Li Tong bio tech ltd, Shandong, the agarose that 0.2 weight portion is sold with trade name agar powder by Fujian Ming Fu agar company limited, the sorbitol that 0.2 weight portion is sold with trade name Neosorb by Shouguang, Shandong Hua Tian sugar alcohol company limited, the chondroitin sulfate that 0.01 weight portion is sold with trade name chondroitin sulfate by Anhui Kebao Biology Engineering Co., Ltd are dissolved in 18 weight portion distilled water, obtain a kind of composite solution containing corn protein;
E, prepare antibacterial modified chitose foaming agent
Take 8 weight portion glycerol, add water, stir, then add the composite solution of the chitosan-containing that 25 weight portions obtain at step C and the composite solution containing corn protein that 30 weight portions obtain at step D, stir, obtain described antibacterial modified chitose foaming agent.
The antibacterial detection method of national standard of describing according to this description detects Analysis deterrmination, and antibacterial modified chitose foaming agent prepared by the present embodiment all reaches 99.3% to the antibacterial ability of staphylococcus aureus, escherichia coli, streptococcus, bacillus pyocyaneus.
Embodiment 3: prepare antibacterial modified chitose foaming agent
The implementation step of this embodiment is as follows:
A, prepare modification of chitosan
By sold with trade name food pharmaceutical grade chitosan by Jinan Haidebei Marine Organism Engineering Co., Ltd., deacetylation 70%, molecular weight 50 × 10
4the chitosan of Da, in 1% aqueous acetic acid by weight, under the condition of low whipping speed 320rpm, dissolve 12min, the solution obtaining is in the ultrasonic washing unit of being sold with trade name YD1008 ultrasonic washing unit by Changzhou You Da ultrasonic equipment company limited, under the condition of ultrasonic frequency 24kHz and power 220W, carry out ultrasonic Treatment 50 minutes, use again the polyvinylidene fluoride (PVDF) ultrafiltration membrane of being sold with trade name polyvinylidene fluoride film by KENKER company of the U.S. to carry out classification, dry under temperature 60 C condition in hot-air dry equipment, obtain the chitosan of molecular weight 800Da, this chitosan is added to by weight in 42% potassium hydroxide aqueous solution, under the condition of 114 DEG C of temperature, process 19min, then neutralize, filtration, distilled water wash, in drying equipment similar to the above, under temperature 60 C condition, be dried with 2.5N aqueous hydrochloric acid solution, obtain the modification of chitosan of deacetylation 98%, molecular weight 820Da,
B, Ramulus et Folium Mussaendae Pubescentis extract
Take the Ramulus et Folium Mussaendae Pubescentis that 22 weight portions are sold with trade name Fuding white tea by Fujian Pinpinxiang Tea Industry Co., Ltd., toward wherein adding 80 weight portion distilled water, then at 98 DEG C of temperature, extract 32min, filter, remove tea grounds, the filtrate standardize solution obtaining, to 100 weight portions, is obtained to the Ramulus et Folium Mussaendae Pubescentis extracting solution that the mixture concentrations such as tea polyphenols and caffeine, theophylline, tannic acid are 0.024g/ml;
C, prepare chitosan-containing composite solution
The modification of chitosan that 6 weight portions are prepared in steps A is dissolved in the glacial acetic acid aqueous solution by 0.2 weight portion glacial acetic acid and the preparation of 22 weight portion distilled water, then add 0.6 weight portion polysorbas20, 1.0 weight portion Tween 80s, the sodium lauryl sulphate that the dodecanol polyethenoxy ether sodium sulfate that 0.6 weight portion is sold with trade name AES-2EO by Shanghai Xian Jie Chemical Industry Science Co., Ltd and 0.9 weight portion are sold with trade name K12 by Shanghai You Yang Industrial Co., Ltd., the Ramulus et Folium Mussaendae Pubescentis extracting solution that adds again 1.8 weight portions to prepare at step B after dissolving, the ascorbyl palmitate that the pi-allyl triphenyl bromide phosphine that 0.07 weight portion is prepared according to Ji'nan University's CN102020675B patented technology and 0.44 weight portion are sold with trade name L-AA Palmitate by Shaanxi Sen Fu natural product company limited, continue to stir, after dissolving, obtain a kind of composite solution of chitosan-containing,
D, preparation are containing corn protein composite solution
The corn protein that 0.8 weight portion is sold with trade name Zein powder by Li Tong bio tech ltd, Shandong, the agarose that 0.9 weight portion is sold with trade name agar powder by Fujian Ming Fu agar company limited, the sorbitol that 0.1 weight portion is sold with trade name Neosorb by Shouguang, Shandong Hua Tian sugar alcohol company limited, the chondroitin sulfate that 0.03 weight portion is sold with trade name chondroitin sulfate by Anhui Kebao Biology Engineering Co., Ltd are dissolved in 28 weight portion distilled water, obtain a kind of composite solution containing corn protein;
E, prepare antibacterial modified chitose foaming agent
Take 5 weight portion glycerol, add water, stir, then add the composite solution of the chitosan-containing that 28 weight portions obtain at step C and the composite solution containing corn protein that 32 weight portions obtain at step D, stir, obtain described antibacterial modified chitose foaming agent.
The antibacterial detection method of national standard of describing according to this description detects Analysis deterrmination, and antibacterial modified chitose foaming agent prepared by the present embodiment all reaches 99.8% to the antibacterial ability of staphylococcus aureus, escherichia coli, streptococcus, bacillus pyocyaneus.
Embodiment 4: prepare antibacterial modified chitose foaming agent
The implementation step of this embodiment is as follows:
A, prepare modification of chitosan
By sold with trade name food pharmaceutical grade chitosan by Jinan Haidebei Marine Organism Engineering Co., Ltd., deacetylation 70%, molecular weight 60 × 10
4the chitosan of Da, in 2% aqueous acetic acid by weight, under the condition of low whipping speed 350rpm, dissolve 5min, the solution obtaining is in the ultrasonic washing unit of being sold with trade name YD1008 ultrasonic washing unit by Changzhou You Da ultrasonic equipment company limited, under the condition of ultrasonic frequency 25kHz and power 180W, carry out ultrasonic Treatment 35 minutes, use again the polyvinylidene fluoride (PVDF) ultrafiltration membrane of being sold with trade name polyvinylidene fluoride film by KENKER company of the U.S. to carry out classification, dry under temperature 60 C condition in hot-air dry equipment, obtain the chitosan of molecular weight 1000Da, this chitosan is added to by weight in 47% potassium hydroxide aqueous solution, under the condition of 120 DEG C of temperature, process 15min, then neutralize, filtration, distilled water wash, in drying equipment similar to the above, under temperature 60 C condition, be dried with 3.0N aqueous hydrochloric acid solution, obtain the modification of chitosan of deacetylation 99%, molecular weight 1000Da,
B, Ramulus et Folium Mussaendae Pubescentis extract
Take the Ramulus et Folium Mussaendae Pubescentis that 25 weight portions are sold with trade name Fuding white tea by Fujian Pinpinxiang Tea Industry Co., Ltd., toward wherein adding 120 weight portion distilled water, then at 100 DEG C of temperature, extract 26min, filter, remove tea grounds, the filtrate standardize solution obtaining, to 100 weight portions, is obtained to the Ramulus et Folium Mussaendae Pubescentis extracting solution that the mixture concentrations such as tea polyphenols and caffeine, theophylline, tannic acid are 0.021g/ml;
C, prepare chitosan-containing composite solution
The modification of chitosan that 10 weight portions are prepared in steps A is dissolved in the glacial acetic acid aqueous solution by 0.3 weight portion glacial acetic acid and the preparation of 20 weight portion distilled water, then add 1.2 weight portion polysorbas20s, 1.2 weight portion Tween 80s, the sodium lauryl sulphate that the dodecanol polyethenoxy ether sodium sulfate that 0.8 weight portion is sold with trade name AES-2EO by Shanghai Xian Jie Chemical Industry Science Co., Ltd and 0.5 weight portion are sold with trade name K12 by Shanghai You Yang Industrial Co., Ltd., the Ramulus et Folium Mussaendae Pubescentis extracting solution that adds again 2.5 weight portions to prepare at step B after dissolving, the ascorbyl palmitate that the pi-allyl triphenyl bromide phosphine that 0.12 weight portion is prepared according to Ji'nan University's CN102020675B patented technology and 0.50 weight portion are sold with trade name L-AA Palmitate by Shaanxi Sen Fu natural product company limited, continue to stir, after dissolving, obtain a kind of composite solution of chitosan-containing,
D, preparation are containing corn protein composite solution
The corn protein that 1.0 weight portions are sold with trade name Zein powder by Li Tong bio tech ltd, Shandong, the agarose that 1.2 weight portions are sold with trade name agar powder by Fujian Ming Fu agar company limited, the sorbitol that 0.3 weight portion is sold with trade name Neosorb by Shouguang, Shandong Hua Tian sugar alcohol company limited, the chondroitin sulfate that 0.09 weight portion is sold with trade name chondroitin sulfate by Anhui Kebao Biology Engineering Co., Ltd are dissolved in 37 weight portion distilled water, obtain a kind of composite solution containing corn protein;
E, prepare antibacterial modified chitose foaming agent
Take 7 weight portion glycerol, add water, stir, then add the composite solution of the chitosan-containing that 35 weight portions obtain at step C and the composite solution containing corn protein that 36 weight portions obtain at step D, stir, obtain described antibacterial modified chitose foaming agent.
The antibacterial detection method of national standard of describing according to this description detects Analysis deterrmination, and antibacterial modified chitose foaming agent prepared by the present embodiment all reaches 99.4% to the antibacterial ability of staphylococcus aureus, escherichia coli, streptococcus, bacillus pyocyaneus.
Embodiment 5: prepare antibacterial modified chitose foaming agent
The implementation step of this embodiment is as follows:
A, prepare modification of chitosan
By sold with trade name food pharmaceutical grade chitosan by Jinan Haidebei Marine Organism Engineering Co., Ltd., deacetylation 70%, molecular weight 40 × 10
4the chitosan of Da, in 1% aqueous acetic acid by weight, under the condition of low whipping speed 350rpm, dissolve 15min, the solution obtaining is in the ultrasonic washing unit of being sold with trade name YD1008 ultrasonic washing unit by Changzhou You Da ultrasonic equipment company limited, under the condition of ultrasonic frequency 22kHz and power 220W, carry out ultrasonic Treatment 35 minutes, use again the polyvinylidene fluoride (PVDF) ultrafiltration membrane of being sold with trade name polyvinylidene fluoride film by KENKER company of the U.S. to carry out classification, dry under temperature 60 C condition in hot-air dry equipment, obtain the chitosan of molecular weight 900Da, this chitosan is added to by weight in 41% potassium hydroxide aqueous solution, under the condition of 110 DEG C of temperature, process 19min, then neutralize, filtration, distilled water wash, in drying equipment similar to the above, under temperature 60 C condition, be dried with 3.0N aqueous hydrochloric acid solution, obtain the modification of chitosan of deacetylation 98%, molecular weight 650Da,
B, Ramulus et Folium Mussaendae Pubescentis extract
Take the Ramulus et Folium Mussaendae Pubescentis that 23 weight portions are sold with trade name Fuding white tea by Fujian Pinpinxiang Tea Industry Co., Ltd., toward wherein adding 120 weight portion distilled water, then at 96 DEG C of temperature, extract 28min, filter, remove tea grounds, the filtrate standardize solution obtaining, to 100 weight portions, is obtained to the Ramulus et Folium Mussaendae Pubescentis extracting solution that the mixture concentrations such as tea polyphenols and caffeine, theophylline, tannic acid are 0.022g/ml;
C, prepare chitosan-containing composite solution
The modification of chitosan that 10 weight portions are prepared in steps A is dissolved in the glacial acetic acid aqueous solution by 0.2 weight portion glacial acetic acid and the preparation of 20 weight portion distilled water, then add 0.8 weight portion polysorbas20, 1.2 weight portion Tween 80s, the sodium lauryl sulphate that the dodecanol polyethenoxy ether sodium sulfate that 0.3 weight portion is sold with trade name AES-2EO by Shanghai Xian Jie Chemical Industry Science Co., Ltd and 1.1 weight portions are sold with trade name K12 by Shanghai You Yang Industrial Co., Ltd., the Ramulus et Folium Mussaendae Pubescentis extracting solution that adds again 1.9 weight portions to prepare at step B after dissolving, the ascorbyl palmitate that the pi-allyl triphenyl bromide phosphine that 0.13 weight portion is prepared according to Ji'nan University's CN102020675B patented technology and 0.39 weight portion are sold with trade name L-AA Palmitate by Shaanxi Sen Fu natural product company limited, continue to stir, after dissolving, obtain a kind of composite solution of chitosan-containing,
D, preparation are containing corn protein composite solution
The corn protein that 0.6 weight portion is sold with trade name Zein powder by Li Tong bio tech ltd, Shandong, the agarose that 1.0 weight portions are sold with trade name agar powder by Fujian Ming Fu agar company limited, the sorbitol that 0.3 weight portion is sold with trade name Neosorb by Shouguang, Shandong Hua Tian sugar alcohol company limited, the chondroitin sulfate that 0.04 weight portion is sold with trade name chondroitin sulfate by Anhui Kebao Biology Engineering Co., Ltd are dissolved in 30 weight portion distilled water, obtain a kind of composite solution containing corn protein;
E, prepare antibacterial modified chitose foaming agent
Take 5 weight portion glycerol, add water, stir, then add the composite solution of the chitosan-containing that 35 weight portions obtain at step C and the composite solution containing corn protein that 40 weight portions obtain at step D, stir, obtain described antibacterial modified chitose foaming agent.
The antibacterial detection method of national standard of describing according to this description detects Analysis deterrmination, and antibacterial modified chitose foaming agent prepared by the present embodiment all reaches 99.2% to the antibacterial ability of staphylococcus aureus, escherichia coli, streptococcus, bacillus pyocyaneus.
Embodiment 6: prepare antibacterial modified chitose foaming agent
The implementation step of this embodiment is as follows:
A, prepare modification of chitosan
By sold with trade name food pharmaceutical grade chitosan by Jinan Haidebei Marine Organism Engineering Co., Ltd., deacetylation 70%, molecular weight 60 × 10
4the chitosan of Da, in 2% aqueous acetic acid by weight, under the condition of low whipping speed 300rpm, dissolve 6min, the solution obtaining is in the ultrasonic washing unit of being sold with trade name YD1008 ultrasonic washing unit by Changzhou You Da ultrasonic equipment company limited, under the condition of ultrasonic frequency 20kHz and power 190W, carry out ultrasonic Treatment 50 minutes, use again the polyvinylidene fluoride (PVDF) ultrafiltration membrane of being sold with trade name polyvinylidene fluoride film by KENKER company of the U.S. to carry out classification, dry under temperature 60 C condition in hot-air dry equipment, obtain the chitosan of molecular weight 1000Da, this chitosan is added to by weight in 50% potassium hydroxide aqueous solution, under the condition of 112 DEG C of temperature, process 18min, then neutralize, filtration, distilled water wash, in drying equipment similar to the above, under temperature 60 C condition, be dried with 3.0N aqueous hydrochloric acid solution, obtain the modification of chitosan of deacetylation 98%, molecular weight 680Da,
B, Ramulus et Folium Mussaendae Pubescentis extract
Take the Ramulus et Folium Mussaendae Pubescentis that 24 weight portions are sold with trade name Fuding white tea by Fujian Pinpinxiang Tea Industry Co., Ltd., toward wherein adding 120 weight portion distilled water, then at 96 DEG C of temperature, extract 29min, filter, remove tea grounds, the filtrate standardize solution obtaining, to 100 weight portions, is obtained to the Ramulus et Folium Mussaendae Pubescentis extracting solution that the mixture concentrations such as tea polyphenols and caffeine, theophylline, tannic acid are 0.020g/ml;
C, prepare chitosan-containing composite solution
The modification of chitosan that 8 weight portions are prepared in steps A is dissolved in the glacial acetic acid aqueous solution by 0.16 weight portion glacial acetic acid and the preparation of 22 weight portion distilled water, then add 1.2 weight portion polysorbas20s, 0.8 weight portion Tween 80, the sodium lauryl sulphate that the dodecanol polyethenoxy ether sodium sulfate that 0.4 weight portion is sold with trade name AES-2EO by Shanghai Xian Jie Chemical Industry Science Co., Ltd and 1.0 weight portions are sold with trade name K12 by Shanghai You Yang Industrial Co., Ltd., the Ramulus et Folium Mussaendae Pubescentis extracting solution that adds again 2.5 weight portions to prepare at step B after dissolving, the ascorbyl palmitate that the pi-allyl triphenyl bromide phosphine that 0.15 weight portion is prepared according to Ji'nan University's CN102020675B patented technology and 0.38 weight portion are sold with trade name L-AA Palmitate by Shaanxi Sen Fu natural product company limited, continue to stir, after dissolving, obtain a kind of composite solution of chitosan-containing,
D, preparation are containing corn protein composite solution
The corn protein that 0.8 weight portion is sold with trade name Zein powder by Li Tong bio tech ltd, Shandong, the agarose that 1.2 weight portions are sold with trade name agar powder by Fujian Ming Fu agar company limited, the sorbitol that 0.25 weight portion is sold with trade name Neosorb by Shouguang, Shandong Hua Tian sugar alcohol company limited, the chondroitin sulfate that 0.04 weight portion is sold with trade name chondroitin sulfate by Anhui Kebao Biology Engineering Co., Ltd are dissolved in 30 weight portion distilled water, obtain a kind of composite solution containing corn protein;
E, prepare antibacterial modified chitose foaming agent
Take 7 weight portion glycerol, add water, stir, then add the composite solution of the chitosan-containing that 26 weight portions obtain at step C and the composite solution containing corn protein that 32 weight portions obtain at step D, stir, obtain described antibacterial modified chitose foaming agent.
The antibacterial detection method of national standard of describing according to this description detects Analysis deterrmination, and antibacterial modified chitose foaming agent prepared by the present embodiment all reaches more than 99.5% the antibacterial ability of staphylococcus aureus, escherichia coli, streptococcus, bacillus pyocyaneus.
Comparative example 1: prepare antibacterial modified chitose foaming agent
Carry out according to the mode identical with embodiment 1, just this comparative example does not add pi-allyl triphenyl bromide phosphine.
The antibacterial detection method of national standard of describing according to this description detects Analysis deterrmination, and antibacterial modified chitose foaming agent prepared by this comparative example all reaches more than 86.2% the antibacterial ability of staphylococcus aureus, escherichia coli, streptococcus, bacillus pyocyaneus.Compared with the result of implementation of embodiment 1, the antibacterial effect of antibacterial modified chitose foaming agent prepared by this comparative example is obviously lower.
Comparative example 2: prepare antibacterial modified chitose foaming agent
Carry out according to the mode identical with embodiment 2, just this comparative example does not add Ramulus et Folium Mussaendae Pubescentis extracting solution.
The antibacterial detection method of national standard of describing according to this description detects Analysis deterrmination, and antibacterial modified chitose foaming agent prepared by this comparative example all reaches more than 85.8% the antibacterial ability of staphylococcus aureus, escherichia coli, streptococcus, bacillus pyocyaneus.Compared with the result of implementation of embodiment 2, the antibacterial effect of antibacterial modified chitose foaming agent prepared by this comparative example is obviously lower.
Claims (10)
1. a preparation method for antibacterial modified chitose foaming agent, is characterized in that the step of this preparation method is as follows:
A, prepare modification of chitosan
By deacetylation 70%, molecular weight 30 × 10
4～60 × 10
4the chitosan of Da is dissolved in by weight in 1～2% aqueous acetic acid, and the solution obtaining carries out supersound process in ultrasonic washing unit, then carries out classification with polyvinylidene fluoride (PVDF) ultrafiltration membrane, dry, obtains the chitosan of molecular weight 500～1000Da; This chitosan is added to by weight in 40～50% potassium hydroxide aqueous solutions, under the condition of 110～120 DEG C of temperature, process 15～20min, then neutralize, filtration, distilled water wash, be dried with 1.0～3.0N aqueous hydrochloric acid solution, obtain the modification of chitosan of deacetylation 98～99%, molecular weight 500～1000Da;
B, Ramulus et Folium Mussaendae Pubescentis extract
Take 15～25 weight portion Ramulus et Folium Mussaendae Pubescentis, toward wherein adding 80～120 weight portion distilled water, then at 95～100 DEG C of temperature, extract 25～35min, filter, remove tea grounds, the filtrate standardize solution obtaining, to 100 weight portions, is obtained containing Ramulus et Folium Mussaendae Pubescentis extracting solution tea polyphenols, caffeine, theophylline and tannic acid, that concentration is 0.016～0.024g/ml;
C, prepare chitosan-containing composite solution
The modification of chitosan that 2～10 weight portions are prepared in steps A is dissolved in glacial acetic acid aqueous solution, then add 0.2～1.2 weight portion polysorbas20, 0.2～1.2 weight portion Tween 80, 0.3～0.8 weight portion dodecanol polyethenoxy ether sodium sulfate and 0.5～1.5 weight portion sodium lauryl sulphate, the Ramulus et Folium Mussaendae Pubescentis extracting solution that adds again 1.5～2.5 weight portions to prepare at step B after dissolving, 0.05～0.15 weight portion pi-allyl triphenyl bromide phosphine and 0.30～0.50 weight portion ascorbyl palmitate, continue to stir, after dissolving, obtain a kind of composite solution of chitosan-containing,
D, preparation are containing corn protein composite solution
0.1～1.0 weight portion corn protein, 0.2～1.2 weight portion agarose, 0.1～0.3 weight portion sorbitol, 0.01～0.09 weight portion chondroitin sulfate are dissolved in 18～42 weight portion distilled water, obtain a kind of composite solution containing corn protein;
E, prepare antibacterial modified chitose foaming agent
Take 4～8 weight portion glycerol, add water, stir, then add the composite solution of the chitosan-containing that 25～35 weight portions obtain at step C and the composite solution containing corn protein that 30～40 weight portions obtain at step D, stir, obtain described antibacterial modified chitose foaming agent.
2. preparation method according to claim 1, is characterized in that in steps A, under the condition of deacetylation 70% chitosan low whipping speed 250～350rpm in aqueous acetic acid, dissolves 5～15min.
3. preparation method according to claim 1, is characterized in that in steps A, supersound process 35～45min under the condition that the solution obtaining is 200W at supersonic frequency 22kHz and ultrasonic power.
4. preparation method according to claim 1, is characterized in that, in step B, the weight ratio of Ramulus et Folium Mussaendae Pubescentis and distilled water is 18～22:90～110.
5. preparation method according to claim 1, is characterized in that in step C, and described glacial acetic acid aqueous solution is by 0.1～0.3 weight portion glacial acetic acid and the preparation of 18～22 weight portion distilled water.
6. preparation method according to claim 1, is characterized in that in step C, the weight ratio of polysorbas20, Tween 80, dodecanol polyethenoxy ether sodium sulfate and sodium lauryl sulphate is 0.5～0.8:0.5～0.8:0.4～0.6:0.8～1.2.
7. preparation method according to claim 1, is characterized in that in step D, the weight ratio of Ramulus et Folium Mussaendae Pubescentis extracting solution, pi-allyl triphenyl bromide phosphine and ascorbyl palmitate is 1.8～2.2:0.08～0.12:0.36～0.42.
8. preparation method according to claim 1, is characterized in that, in step D, the weight ratio of corn protein, agarose, sorbitol and chondroitin sulfate is 0.3～0.7:0.4～1.0:0.15～0.25:0.03～0.08.
9. preparation method according to claim 1, is characterized in that in step e, and the composite solution of glycerol, chitosan-containing is 5～6:28～32:32～38 with the weight ratio of the composite solution containing corn protein.
10. the antibacterial modified chitose foaming agent obtaining according to preparation method described in any one claim in claim 1-9, is characterized in that it all reaches more than 99% the antibacterial ability of staphylococcus aureus, escherichia coli, streptococcus, Candida albicans or bacillus pyocyaneus.
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| CN107161489A (en) * | 2017-06-21 | 2017-09-15 | 芜湖蓝天工程塑胶有限公司 | Composite antibacterial makrolon crisper and preparation method thereof |
| CN109568647A (en) * | 2017-09-28 | 2019-04-05 | 上海君联医疗设备有限公司 | Foam type chitosan liquid film and preparation method thereof |
| CN109316444A (en) * | 2018-11-09 | 2019-02-12 | 南京道大药业有限公司 | A kind of antibacterial chitose foaming agent and preparation method thereof |
| CN112575581A (en) * | 2020-12-29 | 2021-03-30 | 湖南寐家居科技有限公司 | Antibacterial finishing agent for silk fabric and preparation method thereof |
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