CN104042791B - A kind of antibacterial modified chitose foaming agent and preparation method thereof - Google Patents
A kind of antibacterial modified chitose foaming agent and preparation method thereof Download PDFInfo
- Publication number
- CN104042791B CN104042791B CN201410321850.1A CN201410321850A CN104042791B CN 104042791 B CN104042791 B CN 104042791B CN 201410321850 A CN201410321850 A CN 201410321850A CN 104042791 B CN104042791 B CN 104042791B
- Authority
- CN
- China
- Prior art keywords
- weight
- weight portion
- chitosan
- foaming agent
- chitose
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
Landscapes
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The present invention relates to a kind of antibacterial modified chitose foaming agent and preparation method thereof, the method is extracted including preparing modification of chitosan, white tea, prepares chitosan-containing composite solution, prepares composite solution containing corn protein and prepare the steps such as antibacterial modified chitose foaming agent.Antibacterial modified chitose foaming agent of the invention reaches more than 99% to the antibacterial ability of staphylococcus aureus, Escherichia coli, streptococcus, Candida albicans or Pseudomonas aeruginosa etc., shows good bacteriostasis.Antibacterial modified chitose foaming agent of the invention can apply to treatment bacterial vaginitis, colpomycosis and mixed vaginitis etc., using quite varied.
Description
【Technical field】
The invention belongs to medical drugses technical field.More particularly it relates to a kind of antibacterial modified shitosan foam
Agent, further relates to the preparation method of the antibacterial modified chitose foaming agent
【Background technology】
Vaginitis is a kind of common reproductive organs inflammation of women, and in married woman, more than half crowd suffers from different journeys
The vaginitis of degree, vaginitis is clinically probably divided into kind more than ten, specifically includes bacterial vaginitis, trichomonas vaginitis, thought
Pearl bacterium property vaginitis, senile vahinitis, infantile vaginitis, candidiasis vaginitis, viral HSV, HPv vagina
Inflammation, gonococcal vaginitis, desquamative inflammatory vaginitis, nonspecific vaginitis, Tuberculous vaginitis, Drug vaginitis, radioactivity
Vaginitis, ulcer of vagina are acute, anaphylaxis vaginitis, chronic vaginitis, burn worm property vaginitis and mixed vaginitis etc., than
It is more typical and the vaginitis more serious to women's health hazard ratio is mainly bacterial vaginitis, trichomonas vaginitis and thought
Pearl bacterium property vaginitis, be embodied in vulva convulsion itch, generate heat, the symptom such as scorching hot, leucorrhea increasing peculiar smell, discomfort, be common gynaecology
Disease, frequently-occurring disease, serious harm WomanHealth, work and life to patient bring inconvenience.
Vaginitis external manifestation is mainly local disease, so based on being controlled beyond basic on its remedy measures, inside controlling medication
Supplemented by.In external therapy, many new methods have been worked out in recent years and many therapeutant formulations, such as washing lotion, vagina have been developed
Bolt, vaginal tablets, powder, paste, paste and capsule, film etc..Washing lotion is mainly external application, it is impossible to for a long time and focal contact,
Therefore drug effect can not be effectively played, can only be used as daily health caring medication；Paste, vaginal tablets and vaginal plug work in intravaginal
Slowly, it is impossible to be fully contacted with focus, medicine dispersion is uneven, directly to be operated with hand when using, and easily pollutes medicine, causes intersection
Infection, in addition, returning patient brings foreign body sensation.
In view of above healing potion has inconvenience in use, there is that contact area is small, assimilation effect is bad, easy
Cause the deficiencies such as cross-infection, be developed new formulation-foaming agent, foaming agent overcomes the shortcoming of above-mentioned formulation, can make
Medicine is uniformly distributed in intravaginal, is fully contacted with vagina mucosa wrinkle skirt, absorbs rapid, good effect.
At present, people have carried out widely studied to foaming agent, and such as CN101380447A discloses a kind of for treating
Chitose foaming agent of gynecological disease and preparation method thereof, the chitose foaming agent is to prick chlorine by shitosan, mannan-oligosaccharides, benzene
Ammonium, aloe, oil of zedoary turmeric, triclosan, NPE, coconut oil base alkanolamide, PEG400, dodecane
Base sodium sulphate, dodecyl ether sulfate ammonium, tween, triethanolamine, purified water and the third butane etc. be compound to be formulated；
CN102872160A discloses a kind of nano silver foam agent for scalding burn, ulcer wound sterilization, the nano silver foam agent
Be by nano-silver colloid solution, shitosan, solubilizer, wetting agent, thickener, preservative, foaming agent, Fungicidal substance, refrigerant material,
PH withers what section agent and propellant were made；CN102895256A discloses a kind of suitable for the women dual contraceptive efficacy of barrier spermicidal
Chitosan plural gel foaming agent and preparation method thereof, it is by chitosan gel rubber matrix and surfactant, ancillary drug, helps
What solvent, Acidifier, foaming agent, foam stabiliser, solvent and propellant were made.
There is following technological deficiency in these technologies：First, they are all using including propane, butane or iso-butane, halogenated hydrocarbons etc.
Treib gasaerosole, two, addition drug dressing it is wide in variety, complex manufacturing process；Though the 3rd, with shitosan as host matrix, all
Add other antimicrobial components, such as triclosan, Nano Silver, borneol, menthol composition.State Food and Drug Administration's mesh
It is preceding to have expressly provided, CFC class material should be gradually eliminated as pharmaceutic adjuvant aerosol for external use, in addition, propellant can be to the moon
There is certain excitant in road, therefore, research and develop that a kind of to make simple, safe and environment-friendly vaginal foaming agent extremely urgent.
In addition, having not yet to see the patent about preparing foaming agent as primary raw material by the use of shitosan.Application at present
Shitosan be mainly polymer chitosan, also have not seen by chitin modified, controlling its molecular weight and deacetylation
To improve the relevant report of foaming agent antibacterial action.
It is an object of the invention to overcome shortcoming present in prior art, solve to lack at present the environmental protection of pure chitosan class,
The problems such as efficient foam agent, complicated preparation method, propose a kind of preparation method of modified chitosan anti-bacteria foaming agent, the bubble of acquisition
Foam agent has trickle foaming structure, and antibacterial wide spectrum effect is good, and focus cell can be promoted to recover, and the letter of preparation and application method
It is single, treatment, nursing of various vaginitis of clinical gynaecology etc. can be advantageously used in.
【The content of the invention】
[technical problem to be solved]
It is an object of the invention to provide a kind of antibacterial modified chitose foaming agent.
It is a further object to provide the preparation method of the 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 antibacterial modified chitose foaming agent preparation method, is as follows：
A, prepare modification of chitosan
By deacetylation 70%, molecular weight 30 × 104~60 × 104The shitosan of Da is dissolved in 1~2% vinegar by weight
In aqueous acid, the solution for obtaining carries out ultrasonically treated in supersonic wave cleaning machine, then is divided with polyvinylidene fluoride (PVDF) ultrafiltration membrane
Level, dries, and obtains the shitosan of 500~1000Da of molecular weight；This shitosan is added to 40~50% hydroxide by weight
In aqueous solutions of potassium, 15~20min is processed under conditions of 110~120 DEG C of temperature, then entered with 1.0~3.0N aqueous hydrochloric acid solutions
Row neutralize, filtering, distillation water washing, drying, obtain deacetylation 98~99%, 500~1000Da of molecular weight modified shell gather
Sugar；
B, white tea are extracted
15~25 weight portion white teas are weighed, Jia 80 thereto~120 weight portion distilled water, then in 95~100 DEG C of temperature
25~35min of lower extraction, filtering removes tea grounds, and the filtrate constant volume that will be obtained obtains containing tea polyphenols, coffee to 100 weight portions
Coffee because, theophylline, tannic acid, the white tea extract solution that concentration is 0.016~0.024g/ml；
C, prepare chitosan-containing composite solution
2~10 weight portions are dissolved in glacial acetic acid aqueous solution in the modification of chitosan that step A is prepared, are subsequently added into
0.2~1.2 weight portion polysorbas20,0.2~1.2 weight portion Tween 80,0.3~0.8 weight portion dodecanol APEO sulphur
Sour sodium and 0.5~1.5 weight portion lauryl sodium sulfate, add 1.5~2.5 weight portions and are prepared in step B after dissolving
White tea extract solution, 0.05~0.15 weight portion pi-allyl triphenylphosphinebromide and 0.30~0.50 weight portion ascorbic acid palm
Acid esters, continues to stir, and a kind of composite solution of chitosan-containing is obtained after dissolving；
D, preparation composite solution containing corn protein
By 0.1~1.0 parts by weight Corn protein, 0.2~1.2 weight portion agarose, 0.1~0.3 weight portion sorbierite,
0.01~0.09 parts sulfuric acid chondroitin is dissolved in 18~42 weight portion distilled water, obtains a kind of answering containing corn protein
Close solution；
E, prepare antibacterial modified chitose foaming agent
4~8 weight portion glycerine are weighed, water is added, stirred, add what 25~35 weight portions were obtained in step C
The composite solution containing corn protein that the composite solution of chitosan-containing and 30~40 weight portions are obtained in step D, stirs,
Obtain described antibacterial modified chitose foaming agent.
A preferred embodiment of the invention, in step, the shitosan of deacetylation 70% is in aqueous acetic acid
5~15min is dissolved under conditions of middle 250~350rpm of low whipping speed.
Another preferred embodiment of the invention, in step, the solution for obtaining supersonic frequency 22kHz with
Ultrasonic power is ultrasonically treated 35~45min under conditions of 200W.
Another preferred embodiment of the invention, in stepb, the weight ratio of white tea and distilled water is 18~
22：90~110.
Another preferred embodiment of the invention, in step C, described glacial acetic acid aqueous solution be by 0.1~
What 0.3 pbw of glacial acetic acid and 18~22 weight portion distilled water were prepared.
Another preferred embodiment of the invention, in step C, polysorbas20, Tween 80, dodecanol polyoxy second
Alkene ether sodium sulfate is 0.5~0.8 with the weight ratio of lauryl sodium sulfate：0.5~0.8：0.4~0.6：0.8~1.2.
Another preferred embodiment of the invention, in step C, white tea extract solution, pi-allyl triphenyl phosphonium bromide
Phosphine is 1.8~2.2 with the weight ratio of ascorbyl palmitate：0.08~0.12：0.36~0.42.
Another preferred embodiment of the invention, in step D, corn protein, agarose, sorbierite and sulphur
The weight ratio of aching and limp ossein is 0.3~0.7：0.4~1.0：0.15~0.25：0.03~0.08.
Another preferred embodiment of the invention, in step E, glycerine, the composite solution of chitosan-containing with
The weight ratio of the composite solution containing corn protein is 5~6：28~32：32~38.
The invention further relates to the antibacterial modified chitose foaming agent obtained using the preparation method.Described is antibacterial modified
Chitose foaming agent is equal to the antibacterial ability of staphylococcus aureus, Escherichia coli, streptococcus, Candida albicans or Pseudomonas aeruginosa
Reach more than 99%.
The present invention is described in more detail below.
The present invention relates to a kind of preparation method of antibacterial modified chitose foaming agent.
The step of preparation method, is as follows：
A, prepare modification of chitosan
By deacetylation 70%, molecular weight 30 × 104~60 × 104The shitosan of Da is dissolved in 1~2% vinegar by weight
In aqueous acid, the solution for obtaining carries out ultrasonically treated in supersonic wave cleaning machine, then is divided with polyvinylidene fluoride (PVDF) ultrafiltration membrane
Level, dries, and obtains the shitosan of 500~1000Da of molecular weight；This shitosan is added to 40~50% hydroxide by weight
In aqueous solutions of potassium, 15~20min is processed under conditions of 110~120 DEG C of temperature, then entered with 1.0~3.0N aqueous hydrochloric acid solutions
Row neutralize, filtering, distillation water washing, drying, obtain deacetylation 98~99%, 500~1000Da of molecular weight modified shell gather
Sugar；
The chemical constitution of shitosan (β-(1 → 4) -2-amino-2-deoxy-D-Glucose) is the polymeric alkali with cation
Property polysaccharide polymer, be unique positively charged, the cation dietary fibre of nature；It has stable physical property, good molten
The physicochemical property such as Xie Xing, hydrophilic hygroscopicity, biological degradability, biocompatibility and film forming, caking property, gas permeability.The present invention
Antibacterial modified chitose foaming agent main body be natural products shitosan, it improves the biological safety of the foaming agent, together
When, it is to avoid propellant is used, the safety in utilization of the foaming agent is then improve, is conducive to environmental protection.
In this step, the shitosan of deacetylation 70% 250~350rpm of low whipping speed in aqueous acetic acid
Under conditions of dissolve 5~15min, obtain shitosan aqueous acetic acid.
The shitosan that the present invention is used is the product sold in the market, such as by Jinan Hai get Bei marine biotechnologies
The product that Co., Ltd is sold with trade name food pharmaceutical grade shitosan.
In this step, using hyperfiltration process by deacetylation 70%, molecular weight 30 × 104~60 × 104Da macromolecules
Amount shitosan prepares the shitosan of 500~1000Da of molecular weight.
In the present invention, the purpose of ultrasonic wave cleaning treatment is to allow high molecular weight chitosan aqueous acetic acid in ultrasonic wave
Ultrasonication is carried out under conditions of 20~25kHz of frequency and 180~220W of power 30~50 minutes, obtain low-molecular-weight shell and gather
Saccharide complex solution.Preferably, high molecular weight chitosan aqueous acetic acid is 200W's in supersonic frequency 22kHz and ultrasonic power
Under the conditions of ultrasonically treated 35~45min.
The supersonic wave cleaning machine that the present invention is used is the product sold in the market, for example, helped up to ultrasonic wave by Changzhou
The product that equipment Co., Ltd is sold with trade name YD1008 supersonic wave cleaning machines.
Be classified for shitosan by molecule hyperfiltration technique by the present invention, and interception molecular weight is 500~1000 with optimal point
The shitosan of sub- horizontal extent, then by deacetylated again, obtains high deacetylized, low-molecular-weight, narrow molecular weight distribution
Modification of chitosan, greatly improve broad-spectrum antibacterial property energy.
Polyvinylidene fluoride (PVDF) ultrafiltration membrane is typically a kind of with good any biological inert, chemical stability, heat endurance
Hydrophobicity milipore filter.
Carried out being classified with polyvinylidene fluoride (PVDF) ultrafiltration membrane is that a kind of chitosan molecule by molecular weight more than 500~1000Da is cut
Stay, and allow molecular weight to be less than the operation that the chitosan molecule of 500~1000Da passes through.The molecular weight of shitosan is using conventional solidifying
Glue penetration chromatographic process determines what is obtained.
The performance of the polyvinylidene fluoride (PVDF) ultrafiltration membrane that the present invention is used is as follows：110-150 μm of thickness, Unit Weight 3.3-
5.1mg/cm2, porosity 72-78%, intensity be more than 60pst.
The polyvinylidene fluoride (PVDF) ultrafiltration membrane that the present invention is used is the product sold in the market, such as public by U.S. KENKER
Take charge of the product sold with trade name polyvinylidene fluoride film.
In a fractionated, drying be allow collection molecular weight be 500~1000Da chitosan molecule part it is dry in hot-air
Dried to water content under the conditions of temperature 60 C in dry equipment and be less than 6%.
Then, the chitosan molecule that resulting molecular weight is 500~1000Da is modified with alkali, i.e., is further taken off
Acetylation is processed.
In this modification procedure, the purpose of washing is to remove the salt and other impurity for neutralizing and producing.Dry purpose
Be moisture removal, the equipment that this drying steps is used is identical with previously described, drying temperature condition also with above retouch
That states is identical.
B, white tea are extracted
15~25 weight portion white teas are weighed, Jia 80 thereto~120 weight portion distilled water, then in 95~100 DEG C of temperature
25~35min of lower extraction, filtering removes tea grounds, and the filtrate constant volume that will be obtained obtains containing tea polyphenols, coffee to 100 weight portions
Coffee is the white tea extract solution of 0.016~0.024g/ml because of, the concentration of theophylline, tannic acid etc.；
White tea is the tea obtained by one kind passes through solarization or slow fire drying processing after harvesting without finishing or kneading, only, its
Polyphenols equal size is higher.White tea has the work(such as eliminating inflammation and expelling toxin, clearing heat and moistening lung, soothing the liver benefit blood, step-down fat reducing, dispelling fatigue
Effect, especially has unique, spirit to diseases such as excessive drinking and smoking, greasy excessive, the excessively prosperous uncomfortable, digestive functional disturbances for causing of irascibility
Wonderful health-care effect.
In the present invention, if the temperature that white tea distilled water is extracted is less than 95 DEG C, extraction can be made incomplete；If white
The temperature that tea distilled water is extracted is higher than 100 DEG C, then the oxidized problem of Polyphenols occurs；Therefore, white tea distillation water extraction
The temperature for taking is suitable for 95~100 DEG C.
The white tea that the present invention is used is the product sold in the market, for example by Fujian Pinpinxiang Tea Industry Co., Ltd. with
The product of trade name Fuding white tea sale.
Preferably, white tea and the weight ratio of distilled water are 18~22：90~110.
C, prepare chitosan-containing composite solution
2~10 weight portions are dissolved in glacial acetic acid aqueous solution in the modification of chitosan that step A is prepared, are subsequently added into
0.2~1.2 weight portion polysorbas20,0.2~1.2 weight portion Tween 80,0.3~0.8 weight portion dodecanol APEO sulphur
Sour sodium and 0.5~1.5 weight portion lauryl sodium sulfate, add 1.5~2.5 weight portions and are prepared in step B after dissolving
White tea extract solution, 0.05~0.15 weight portion pi-allyl triphenylphosphinebromide and 0.30~0.50 weight portion ascorbic acid palm
Acid esters, continues to stir, and a kind of composite solution of chitosan-containing is obtained after dissolving；
Described glacial acetic acid aqueous solution is prepared by 0.1~0.3 pbw of glacial acetic acid and 18~22 weight portion distilled water.
In this step, polysorbas20, Tween 80, dodecanol polyethenoxy ether sodium sulfate and dodecyl sulphate are used
Sodium is in order that antibacterial modified chitose foaming agent of the invention has good spumescence.
The weight ratio of polysorbas20, Tween 80, dodecanol polyethenoxy ether sodium sulfate and lauryl sodium sulfate 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 lauryl sodium sulfate that the present invention is used are all
It is the product sold in the market, for example, is sold with trade name polysorbas20, Tween 80 by Guangdong Run Hua Chemical Co., Ltd.s
Product, the dodecanol polyethenoxy ether sodium sulfate sold with trade name AES-2EO by Shanghai Xian Jie Chemical Industry Science Co., Ltd,
The lauryl sodium sulfate sold with trade name K12 by Shanghai You Yang Industrial Co., Ltd.s.
In addition, the present invention is lived by adding a small amount of phosphorus-containing compound, regulation anion surfactant with non-ionic surface
Property agent foaming effect, make that foam is finer and smoother, stabilization, diffusion power greatly promotes, can be in vaginitis without propellant
In uniformly spread, act on more rapid in vagina, high efficiency dispersion and deep people's vagina mucosa fold deep, fornix portion and opening of the cervix
Etc. the place that general medicine is difficult to reach, be conducive to same pathogen to contact and produce antibacterial, bactericidal action rapidly.
Antibacterial modified chitose foaming agent of the invention is by the shitosan containing amino and phosphorus-containing compound, Ramulus et Folium Mussaendae Pubescentis extract
Synergy, with efficiently cooperateing with anti-harmful microorganism to act on, obvious killing effect is respectively provided with to bacterium, virus, fungi, it is right
The clinical bacterias such as staphylococcus aureus, hemolytic chain bacterium, Pseudomonas aeruginosa, Candida albicans and Escherichia coli have
More than 99% killing efficiency, is greatly improved anti-microbial property.
Preferably, the weight ratio of white tea extract solution, pi-allyl triphenylphosphinebromide and ascorbyl palmitate be 1.8~
2.2：0.08~0.12：0.36~0.42.
D, preparation composite solution containing corn protein
By 0.1~1.0 parts by weight Corn protein, 0.2~1.2 weight portion agarose, 0.1~0.3 weight portion sorbierite,
0.01~0.09 parts sulfuric acid chondroitin is dissolved in 18~42 weight portion distilled water, obtains a kind of answering containing corn protein
Close solution；
The corn protein that the present invention is used is the product sold in the market, for example, had by the logical biotechnology of Shandong profit
The product that limit company is sold with trade name corn protein powder.
Agarose is a kind of linear polymer, and its basic structure is linked by β-D- galactolipins and the Isosorbide-5-Nitrae position of 1,3 link
The 3,6- inner ether-L- galactolipins alternately long-chain polymer that couples together.Agar pectin is by many smaller molecular compositions
Heterogeneous mixture.Agarose is generally heated to more than 90 DEG C dissolvings in water, and good half is formed when temperature drop is to 35-40 DEG C
The gel of solid-like.The agarose that the present invention is used is the product sold in the market, such as limited by the bright good fortune agar in Fujian
The product that company is sold with trade name agar powder.
The sorbierite (D-sorbite) that the present invention is used is the product sold in the market, such as by Shandong Shouguang Hua Tian
The product that sugar alcohol Co., Ltd is sold with trade name Neosorb.
Chondroitin sulfate is to be covalently attached the class glycosaminoglycan that proteoglycans is formed on protein, and chondroitin sulfate is deposited
Be from nematode to people except it is exophytic it is all biology in, play many important physiological functions.The sulfuric acid that the present invention is used
Chondroitin is the product sold in the market, such as by Anhui Kebao Biology Engineering Co., Ltd with trade name chondroitin sulfate
The product of sale.
Antibacterial modified chitose foaming agent of the invention contains ascorbyl palmitate, sorbierite, zein and sulphur
Aching and limp ossein, they can either play a part of stable foam, additionally it is possible to play protection vaginal wall cell membrane, and quickening is invaded by germ
Contaminate the reparation and growth of cell.
Preferably, the weight ratio of corn protein, agarose, sorbierite 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
4~8 weight portion glycerine are weighed, water is added, stirred, add what 25~35 weight portions were obtained in step C
The composite solution containing corn protein that the composite solution of chitosan-containing and 30~40 weight portions are obtained in step D, stirs,
Obtain described antibacterial modified chitose foaming agent.
According to the present invention, when glycerine is described scope with the amount of the composite solution containing corn protein, if containing shell
The amount of the composite solution of glycan is less than 25 weight portions, then occur that anti-microbial property declines；If the composite solution of chitosan-containing
Amount is more than 35 weight portions, then solution viscosity problems of too occurs；Therefore, the amount of the composite solution of chitosan-containing is 25~35 weights
Amount part is rational.Similarly, when glycerine is described scope with the amount of the composite solution of chitosan-containing, if egg containing corn
The amount of the composite solution of white matter is less than 30 weight portions, then can decline foam stability；If compound molten containing corn protein
The amount of liquid be more than 40 weight portions, then can anti-microbial property be affected；Therefore, the amount of the composite solution of chitosan-containing is 30~40 weights
Amount part is rational.
Preferably, glycerine, the composite solution of chitosan-containing and the weight ratio of the composite solution containing corn protein be 5~
6：28~32：32~38.
The invention further relates to the antibacterial modified chitose foaming agent obtained using the preparation method.Antibacterial modified shitosan
Foaming agent reaches to the antibacterial ability of staphylococcus aureus, Escherichia coli, streptococcus, Candida albicans or Pseudomonas aeruginosa
More than 99%.
Antibacterial modified chitose foaming agent of the invention can apply to treatment bacterial vaginitis, colpomycosis and
Mixed vaginitis etc., using quite varied.
Antibacterial modified chitose foaming agent of the invention is by the antibacterial detection method of national standard (GB/T16886) detection point
Analysis, the antibacterial ability to staphylococcus aureus, Escherichia coli, streptococcus, Candida albicans or Pseudomonas aeruginosa etc. reaches
More than 99%, show good bacteriostasis.
[beneficial effect]
The beneficial effects of the invention are as follows：
1st, antibacterial modified chitose foaming agent main body of the invention uses natural products shitosan, improves the life of foaming agent
Thing security, while, it is to avoid propellant is used, safety in utilization is improve with environmental protection.
2nd, be classified for shitosan using molecule hyperfiltration technique by the present invention, the shitosan of interception molecular weight 500-1000, then
By deacetylated, the modification of chitosan of high deacetylized, low-molecular-weight, narrow molecular weight distribution is obtained, greatly improve antibacterial wide
Spectrality energy.
3rd, antibacterial modified chitose foaming agent prepared by the present invention is by shitosan and phosphorus-containing compound, white tea containing amino
The synergy of extract, with efficiently cooperateing with anti-harmful microorganism to act on, substantially killing is respectively provided with to bacterium, virus, fungi
Effect, it is clinical to staphylococcus aureus, hemolytic chain bacterium, Pseudomonas aeruginosa, Candida albicans and Escherichia coli etc. to cause a disease
Bacterium has more than 99% killing efficiency, and anti-microbial property is greatly improved.
4th, the present invention have adjusted anion surfactant and lived with non-ionic surface by adding a small amount of phosphorus-containing compound
Property agent foaming effect, make that foam is finer and smoother, stabilization, diffusion power greatly promotes, can be in vaginitis without propellant
In uniformly spread, act on more rapid in vagina, high efficiency dispersion and deep people's vagina mucosa fold deep, fornix portion and opening of the cervix
Etc. the place that general medicine is difficult to reach, be conducive to same pathogen to contact and produce antibacterial, bactericidal action rapidly.
5th, the present invention can either be risen by increasing ascorbyl palmitate, sorbierite, zein and chondroitin sulfate
To the effect of stable foam, protection vaginal wall cell membrane can be more played, accelerate reparation and growth by infection process cell.
【Specific embodiment】
The present invention is will be better understood that by following embodiments.
Embodiment 1：Prepare antibacterial modified chitose foaming agent
The implementation steps of the embodiment are as follows：
A, prepare modification of chitosan
By second sold with trade name food pharmaceutical grade shitosan by Jinan Haidebei Marine Organism Engineering Co., Ltd., de-
Acyl degree 70%, molecular weight 30 × 104The shitosan of Da, the low whipping speed 250rpm in 2% aqueous acetic acid by weight
Under the conditions of dissolve 15min, the solution for obtaining by Changzhou You Da ultrasonic equipments Co., Ltd with trade name YD1008 ultrasound
In the supersonic wave cleaning machine of ripple cleaning machine sale, carried out at ultrasonic wave under conditions of ultrasonic frequency 20kHz and power 200W
Reason 45 minutes, then divided with the polyvinylidene fluoride (PVDF) ultrafiltration membrane that trade name polyvinylidene fluoride film is sold with by KENKER companies of the U.S.
Level, dries in hot-air drying equipment under the conditions of temperature 60 C, obtains the shitosan of molecular weight 900Da；This shell is gathered
Sugar is added in 50% potassium hydroxide aqueous solution by weight, and 17min is processed under conditions of 116 DEG C of temperature, then uses 2.0N salt
Aqueous acid is neutralized, filtered, distilled water washing, being done under the conditions of temperature 60 C in drying equipment similar to the above
It is dry, obtain deacetylation 98%, the modification of chitosan of molecular weight 500Da；
B, white tea are extracted
The white tea that 15 weight portions are sold by Fujian Pinpinxiang Tea Industry Co., Ltd. with trade name Fuding white tea is weighed, thereto
Plus 90 weight portion distilled water, 35min then is extracted at 95 DEG C of temperature, filter, tea grounds is removed, the filtrate constant volume that will be obtained is arrived
100 weight portions, obtain the white tea extract solution that the mixture concentration such as tea polyphenols and caffeine, theophylline, tannic acid is 0.016g/ml；
C, prepare chitosan-containing composite solution
8 weight portions are dissolved in by 0.2 pbw of glacial acetic acid and 18 weight portions in the modification of chitosan that step A is prepared
In the glacial acetic acid aqueous solution that distilled water is prepared, 1.0 weight portion polysorbas20s, 0.6 weight portion Tween 80,0.3 weight portion are subsequently added into
The dodecanol polyethenoxy ether sodium sulfate and 1.5 sold with trade name AES-2EO by Shanghai Xian Jie Chemical Industry Science Co., Ltd
The lauryl sodium sulfate that weight portion is sold by Shanghai You Yang Industrial Co., Ltd.s with trade name K12, adds 2.1 weights after dissolving
White tea extract solution, 0.15 weight portion that amount part prepares in step B are according to Ji'nan University's CN102020675B patented technology systems
Standby pi-allyl triphenylphosphinebromide and 0.38 weight portion are by Shaanxi Sen Fu natural products Co., Ltd with trade name L- Vitamin Cs
The ascorbyl palmitate of sour Palmitate sale, continues to stir, and a kind of composite solution of chitosan-containing is obtained after dissolving；
D, preparation composite solution containing corn protein
The zein that 0.1 weight portion is sold by Shandong Li Tong bio tech ltd with trade name corn protein powder
Agarose, 0.2 weight portion that matter, 0.5 weight portion are sold by Fujian Ming Fu agar Co., Ltd with trade name agar powder are by Shandong
Sorbierite, 0.06 weight portion that Shouguang Hua Tian sugar alcohols Co., Ltd is sold with trade name Neosorb are by the precious biology work of Anhui section
Journey Co., Ltd is dissolved in 42 weight portion distilled water with the chondroitin sulfate that trade name chondroitin sulfate is sold, and is obtained one kind and is contained
The composite solution of corn protein；
E, prepare antibacterial modified chitose foaming agent
4 weight portion glycerine are weighed, water is added, stirred, add the chitosan-containing that 32 weight portions are obtained in step C
Composite solution and the composite solution containing corn protein that is obtained in step D of 40 weight portions, stir, obtain described anti-
Bacterium modification of chitosan foaming agent.
Determine that antibacterial manufactured in the present embodiment changes according to the antibacterial detection method detection and analysis of national standard that this specification is described
Property chitose foaming agent reaches to the antibacterial ability of staphylococcus aureus, Escherichia coli, streptococcus, Pseudomonas aeruginosa
99.4%.
Embodiment 2：Prepare antibacterial modified chitose foaming agent
The implementation steps of the embodiment are as follows：
A, prepare modification of chitosan
By second sold with trade name food pharmaceutical grade shitosan by Jinan Haidebei Marine Organism Engineering Co., Ltd., de-
Acyl degree 70%, molecular weight 40 × 104The shitosan of Da, the low whipping speed 280rpm in 1% aqueous acetic acid by weight
Under the conditions of dissolve 8min, the solution for obtaining by Changzhou You Da ultrasonic equipments Co., Ltd with trade name YD1008 ultrasonic waves
In the supersonic wave cleaning machine of cleaning machine sale, ultrasonication is carried out under conditions of ultrasonic frequency 22kHz and power 180W
30 minutes, then divided with the polyvinylidene fluoride (PVDF) ultrafiltration membrane that trade name polyvinylidene fluoride film is sold with by KENKER companies of the U.S.
Level, dries in hot-air drying equipment under the conditions of temperature 60 C, obtains the shitosan of molecular weight 500Da；This shell is gathered
Sugar is added in 40% potassium hydroxide aqueous solution by weight, and 20min is processed under conditions of 110 DEG C of temperature, then uses 1.0N salt
Aqueous acid is neutralized, filtered, distilled water washing, being done under the conditions of temperature 60 C in drying equipment similar to the above
It is dry, obtain deacetylation 99%, the modification of chitosan of molecular weight 650Da；
B, white tea are extracted
The white tea that 18 weight portions are sold by Fujian Pinpinxiang Tea Industry Co., Ltd. with trade name Fuding white tea is weighed, thereto
Plus 110 weight portion distilled water, 25min then is extracted at 100 DEG C of temperature, filter, tea grounds is removed, the filtrate constant volume that will be obtained is arrived
100 weight portions, obtain the white tea extract solution that the mixture concentration such as tea polyphenols and caffeine, theophylline, tannic acid is 0.019g/ml；
C, prepare chitosan-containing composite solution
2 weight portions are dissolved in by 0.1 pbw of glacial acetic acid and 20 weight portions in the modification of chitosan that step A is prepared
In the glacial acetic acid aqueous solution that distilled water is prepared, 0.2 weight portion polysorbas20,0.2 weight portion Tween 80,0.4 weight portion are subsequently added into
The dodecanol polyethenoxy ether sodium sulfate and 1.2 sold with trade name AES-2EO by Shanghai Xian Jie Chemical Industry Science Co., Ltd
The lauryl sodium sulfate that weight portion is sold by Shanghai You Yang Industrial Co., Ltd.s with trade name K12, adds 1.5 weights after dissolving
White tea extract solution, 0.05 weight portion that amount part prepares in step B are according to Ji'nan University's CN102020675B patented technology systems
Standby pi-allyl triphenylphosphinebromide and 0.30 weight portion are by Shaanxi Sen Fu natural products Co., Ltd with trade name L- Vitamin Cs
The ascorbyl palmitate of sour Palmitate sale, continues to stir, and a kind of composite solution of chitosan-containing is obtained after dissolving；
D, preparation composite solution containing corn protein
The zein that 0.4 weight portion is sold by Shandong Li Tong bio tech ltd with trade name corn protein powder
Agarose, 0.2 weight portion that matter, 0.2 weight portion are sold by Fujian Ming Fu agar Co., Ltd with trade name agar powder are by Shandong
Sorbierite, 0.01 weight portion that Shouguang Hua Tian sugar alcohols Co., Ltd is sold with trade name Neosorb are by the precious biology work of Anhui section
Journey Co., Ltd is dissolved in 18 weight portion distilled water with the chondroitin sulfate that trade name chondroitin sulfate is sold, and is obtained one kind and is contained
The composite solution of corn protein；
E, prepare antibacterial modified chitose foaming agent
8 weight portion glycerine are weighed, water is added, stirred, add the chitosan-containing that 25 weight portions are obtained in step C
Composite solution and the composite solution containing corn protein that is obtained in step D of 30 weight portions, stir, obtain described anti-
Bacterium modification of chitosan foaming agent.
Determine that antibacterial manufactured in the present embodiment changes according to the antibacterial detection method detection and analysis of national standard that this specification is described
Property chitose foaming agent reaches to the antibacterial ability of staphylococcus aureus, Escherichia coli, streptococcus, Pseudomonas aeruginosa
99.3%.
Embodiment 3：Prepare antibacterial modified chitose foaming agent
The implementation steps of the embodiment are as follows：
A, prepare modification of chitosan
By second sold with trade name food pharmaceutical grade shitosan by Jinan Haidebei Marine Organism Engineering Co., Ltd., de-
Acyl degree 70%, molecular weight 50 × 104The shitosan of Da, the low whipping speed 320rpm in 1% aqueous acetic acid by weight
Under the conditions of dissolve 12min, the solution for obtaining by Changzhou You Da ultrasonic equipments Co., Ltd with trade name YD1008 ultrasound
In the supersonic wave cleaning machine of ripple cleaning machine sale, carried out at ultrasonic wave under conditions of ultrasonic frequency 24kHz and power 220W
Reason 50 minutes, then divided with the polyvinylidene fluoride (PVDF) ultrafiltration membrane that trade name polyvinylidene fluoride film is sold with by KENKER companies of the U.S.
Level, dries in hot-air drying equipment under the conditions of temperature 60 C, obtains the shitosan of molecular weight 800Da；This shell is gathered
Sugar is added in 42% potassium hydroxide aqueous solution by weight, and 19min is processed under conditions of 114 DEG C of temperature, then uses 2.5N salt
Aqueous acid is neutralized, filtered, distilled water washing, being done under the conditions of temperature 60 C in drying equipment similar to the above
It is dry, obtain deacetylation 98%, the modification of chitosan of molecular weight 820Da；
B, white tea are extracted
The white tea that 22 weight portions are sold by Fujian Pinpinxiang Tea Industry Co., Ltd. with trade name Fuding white tea is weighed, thereto
Plus 80 weight portion distilled water, 32min then is extracted at 98 DEG C of temperature, filter, tea grounds is removed, the filtrate constant volume that will be obtained is arrived
100 weight portions, obtain the white tea extract solution that the mixture concentration such as tea polyphenols and caffeine, theophylline, tannic acid is 0.024g/ml；
C, prepare chitosan-containing composite solution
6 weight portions are dissolved in by 0.2 pbw of glacial acetic acid and 22 weight portions in the modification of chitosan that step A is prepared
In the glacial acetic acid aqueous solution that distilled water is prepared, 0.6 weight portion polysorbas20,1.0 weight portion Tween 80s, 0.6 weight portion are subsequently added into
The dodecanol polyethenoxy ether sodium sulfate and 0.9 sold with trade name AES-2EO by Shanghai Xian Jie Chemical Industry Science Co., Ltd
The lauryl sodium sulfate that weight portion is sold by Shanghai You Yang Industrial Co., Ltd.s with trade name K12, adds 1.8 weights after dissolving
White tea extract solution, 0.07 weight portion that amount part prepares in step B are according to Ji'nan University's CN102020675B patented technology systems
Standby pi-allyl triphenylphosphinebromide and 0.44 weight portion are by Shaanxi Sen Fu natural products Co., Ltd with trade name L- Vitamin Cs
The ascorbyl palmitate of sour Palmitate sale, continues to stir, and a kind of composite solution of chitosan-containing is obtained after dissolving；
D, preparation composite solution containing corn protein
The zein that 0.8 weight portion is sold by Shandong Li Tong bio tech ltd with trade name corn protein powder
Agarose, 0.1 weight portion that matter, 0.9 weight portion are sold by Fujian Ming Fu agar Co., Ltd with trade name agar powder are by Shandong
Sorbierite, 0.03 weight portion that Shouguang Hua Tian sugar alcohols Co., Ltd is sold with trade name Neosorb are by the precious biology work of Anhui section
Journey Co., Ltd is dissolved in 28 weight portion distilled water with the chondroitin sulfate that trade name chondroitin sulfate is sold, and is obtained one kind and is contained
The composite solution of corn protein；
E, prepare antibacterial modified chitose foaming agent
5 weight portion glycerine are weighed, water is added, stirred, add the chitosan-containing that 28 weight portions are obtained in step C
Composite solution and the composite solution containing corn protein that is obtained in step D of 32 weight portions, stir, obtain described anti-
Bacterium modification of chitosan foaming agent.
Determine that antibacterial manufactured in the present embodiment changes according to the antibacterial detection method detection and analysis of national standard that this specification is described
Property chitose foaming agent reaches to the antibacterial ability of staphylococcus aureus, Escherichia coli, streptococcus, Pseudomonas aeruginosa
99.8%.
Embodiment 4：Prepare antibacterial modified chitose foaming agent
The implementation steps of the embodiment are as follows：
A, prepare modification of chitosan
By second sold with trade name food pharmaceutical grade shitosan by Jinan Haidebei Marine Organism Engineering Co., Ltd., de-
Acyl degree 70%, molecular weight 60 × 104The shitosan of Da, the low whipping speed 350rpm in 2% aqueous acetic acid by weight
Under the conditions of dissolve 5min, the solution for obtaining by Changzhou You Da ultrasonic equipments Co., Ltd with trade name YD1008 ultrasonic waves
In the supersonic wave cleaning machine of cleaning machine sale, ultrasonication is carried out under conditions of ultrasonic frequency 25kHz and power 180W
35 minutes, then divided with the polyvinylidene fluoride (PVDF) ultrafiltration membrane that trade name polyvinylidene fluoride film is sold with by KENKER companies of the U.S.
Level, dries in hot-air drying equipment under the conditions of temperature 60 C, obtains the shitosan of molecular weight 1000Da；This shell is gathered
Sugar is added in 47% potassium hydroxide aqueous solution by weight, and 15min is processed under conditions of 120 DEG C of temperature, then uses 3.0N salt
Aqueous acid is neutralized, filtered, distilled water washing, being done under the conditions of temperature 60 C in drying equipment similar to the above
It is dry, obtain deacetylation 99%, the modification of chitosan of molecular weight 1000Da；
B, white tea are extracted
The white tea that 25 weight portions are sold by Fujian Pinpinxiang Tea Industry Co., Ltd. with trade name Fuding white tea is weighed, thereto
Plus 120 weight portion distilled water, 26min then is extracted at 100 DEG C of temperature, filter, tea grounds is removed, the filtrate constant volume that will be obtained is arrived
100 weight portions, obtain the white tea extract solution that the mixture concentration such as tea polyphenols and caffeine, theophylline, tannic acid is 0.021g/ml；
C, prepare chitosan-containing composite solution
10 weight portions are dissolved in by 0.3 pbw of glacial acetic acid and 20 weight in the modification of chitosan that step A is prepared
In the glacial acetic acid aqueous solution that part distilled water is prepared, 1.2 weight portion polysorbas20s, 1.2 weight portion Tween 80s, 0.8 weight are subsequently added into
Part dodecanol polyethenoxy ether sodium sulfate sell with trade name AES-2EO by Shanghai Xian Jie Chemical Industry Science Co., Ltd and
The lauryl sodium sulfate that 0.5 weight portion is sold by Shanghai You Yang Industrial Co., Ltd.s with trade name K12, adds after dissolving
White tea extract solution, 0.12 weight portion that 2.5 weight portions are prepared in step B are according to Ji'nan University CN102020675B patent skills
Pi-allyl triphenylphosphinebromide prepared by art is resisted by Shaanxi Sen Fu natural products Co., Ltd with 0.50 weight portion with trade name L-
The ascorbyl palmitate of bad hematic acid Palmitate sale, continues to stir, and a kind of the compound molten of chitosan-containing is obtained after dissolving
Liquid；
D, preparation composite solution containing corn protein
The zein that 1.0 weight portions are sold by Shandong Li Tong bio tech ltd with trade name corn protein powder
Agarose, 0.3 weight portion that matter, 1.2 weight portions are sold by Fujian Ming Fu agar Co., Ltd with trade name agar powder are by Shandong
Sorbierite, 0.09 weight portion that Shouguang Hua Tian sugar alcohols Co., Ltd is sold with trade name Neosorb are by the precious biology work of Anhui section
Journey Co., Ltd is dissolved in 37 weight portion distilled water with the chondroitin sulfate that trade name chondroitin sulfate is sold, and is obtained one kind and is contained
The composite solution of corn protein；
E, prepare antibacterial modified chitose foaming agent
7 weight portion glycerine are weighed, water is added, stirred, add the chitosan-containing that 35 weight portions are obtained in step C
Composite solution and the composite solution containing corn protein that is obtained in step D of 36 weight portions, stir, obtain described anti-
Bacterium modification of chitosan foaming agent.
Determine that antibacterial manufactured in the present embodiment changes according to the antibacterial detection method detection and analysis of national standard that this specification is described
Property chitose foaming agent reaches to the antibacterial ability of staphylococcus aureus, Escherichia coli, streptococcus, Pseudomonas aeruginosa
99.4%.
Embodiment 5：Prepare antibacterial modified chitose foaming agent
The implementation steps of the embodiment are as follows：
A, prepare modification of chitosan
By second sold with trade name food pharmaceutical grade shitosan by Jinan Haidebei Marine Organism Engineering Co., Ltd., de-
Acyl degree 70%, molecular weight 40 × 104The shitosan of Da, the low whipping speed 350rpm in 1% aqueous acetic acid by weight
Under the conditions of dissolve 15min, the solution for obtaining by Changzhou You Da ultrasonic equipments Co., Ltd with trade name YD1008 ultrasound
In the supersonic wave cleaning machine of ripple cleaning machine sale, carried out at ultrasonic wave under conditions of ultrasonic frequency 22kHz and power 220W
Reason 35 minutes, then divided with the polyvinylidene fluoride (PVDF) ultrafiltration membrane that trade name polyvinylidene fluoride film is sold with by KENKER companies of the U.S.
Level, dries in hot-air drying equipment under the conditions of temperature 60 C, obtains the shitosan of molecular weight 900Da；This shell is gathered
Sugar is added in 41% potassium hydroxide aqueous solution by weight, and 19min is processed under conditions of 110 DEG C of temperature, then uses 3.0N salt
Aqueous acid is neutralized, filtered, distilled water washing, being done under the conditions of temperature 60 C in drying equipment similar to the above
It is dry, obtain deacetylation 98%, the modification of chitosan of molecular weight 650Da；
B, white tea are extracted
The white tea that 23 weight portions are sold by Fujian Pinpinxiang Tea Industry Co., Ltd. with trade name Fuding white tea is weighed, thereto
Plus 120 weight portion distilled water, 28min then is extracted at 96 DEG C of temperature, filter, tea grounds is removed, the filtrate constant volume that will be obtained is arrived
100 weight portions, obtain the white tea extract solution that the mixture concentration such as tea polyphenols and caffeine, theophylline, tannic acid is 0.022g/ml；
C, prepare chitosan-containing composite solution
10 weight portions are dissolved in by 0.2 pbw of glacial acetic acid and 20 weight in the modification of chitosan that step A is prepared
In the glacial acetic acid aqueous solution that part distilled water is prepared, 0.8 weight portion polysorbas20,1.2 weight portion Tween 80s, 0.3 weight are subsequently added into
Part dodecanol polyethenoxy ether sodium sulfate sell with trade name AES-2EO by Shanghai Xian Jie Chemical Industry Science Co., Ltd and
The lauryl sodium sulfate that 1.1 weight portions are sold by Shanghai You Yang Industrial Co., Ltd.s with trade name K12, adds after dissolving
White tea extract solution, 0.13 weight portion that 1.9 weight portions are prepared in step B are according to Ji'nan University CN102020675B patent skills
Pi-allyl triphenylphosphinebromide prepared by art is resisted by Shaanxi Sen Fu natural products Co., Ltd with 0.39 weight portion with trade name L-
The ascorbyl palmitate of bad hematic acid Palmitate sale, continues to stir, and a kind of the compound molten of chitosan-containing is obtained after dissolving
Liquid；
D, preparation composite solution containing corn protein
The zein that 0.6 weight portion is sold by Shandong Li Tong bio tech ltd with trade name corn protein powder
Agarose, 0.3 weight portion that matter, 1.0 weight portions are sold by Fujian Ming Fu agar Co., Ltd with trade name agar powder are by Shandong
Sorbierite, 0.04 weight portion that Shouguang Hua Tian sugar alcohols Co., Ltd is sold with trade name Neosorb are by the precious biology work of Anhui section
Journey Co., Ltd is dissolved in 30 weight portion distilled water with the chondroitin sulfate that trade name chondroitin sulfate is sold, and is obtained one kind and is contained
The composite solution of corn protein；
E, prepare antibacterial modified chitose foaming agent
5 weight portion glycerine are weighed, water is added, stirred, add the chitosan-containing that 35 weight portions are obtained in step C
Composite solution and the composite solution containing corn protein that is obtained in step D of 40 weight portions, stir, obtain described anti-
Bacterium modification of chitosan foaming agent.
Determine that antibacterial manufactured in the present embodiment changes according to the antibacterial detection method detection and analysis of national standard that this specification is described
Property chitose foaming agent reaches to the antibacterial ability of staphylococcus aureus, Escherichia coli, streptococcus, Pseudomonas aeruginosa
99.2%.
Embodiment 6：Prepare antibacterial modified chitose foaming agent
The implementation steps of the embodiment are as follows：
A, prepare modification of chitosan
By second sold with trade name food pharmaceutical grade shitosan by Jinan Haidebei Marine Organism Engineering Co., Ltd., de-
Acyl degree 70%, molecular weight 60 × 104The shitosan of Da, the low whipping speed 300rpm in 2% aqueous acetic acid by weight
Under the conditions of dissolve 6min, the solution for obtaining by Changzhou You Da ultrasonic equipments Co., Ltd with trade name YD1008 ultrasonic waves
In the supersonic wave cleaning machine of cleaning machine sale, ultrasonication is carried out under conditions of ultrasonic frequency 20kHz and power 190W
50 minutes, then divided with the polyvinylidene fluoride (PVDF) ultrafiltration membrane that trade name polyvinylidene fluoride film is sold with by KENKER companies of the U.S.
Level, dries in hot-air drying equipment under the conditions of temperature 60 C, obtains the shitosan of molecular weight 1000Da；This shell is gathered
Sugar is added in 50% potassium hydroxide aqueous solution by weight, and 18min is processed under conditions of 112 DEG C of temperature, then uses 3.0N salt
Aqueous acid is neutralized, filtered, distilled water washing, being done under the conditions of temperature 60 C in drying equipment similar to the above
It is dry, obtain deacetylation 98%, the modification of chitosan of molecular weight 680Da；
B, white tea are extracted
The white tea that 24 weight portions are sold by Fujian Pinpinxiang Tea Industry Co., Ltd. with trade name Fuding white tea is weighed, thereto
Plus 120 weight portion distilled water, 29min then is extracted at 96 DEG C of temperature, filter, tea grounds is removed, the filtrate constant volume that will be obtained is arrived
100 weight portions, obtain the white tea extract solution that the mixture concentration such as tea polyphenols and caffeine, theophylline, tannic acid is 0.020g/ml；
C, prepare chitosan-containing composite solution
8 weight portions are dissolved in by 0.16 pbw of glacial acetic acid and 22 weight in the modification of chitosan that step A is prepared
In the glacial acetic acid aqueous solution that part distilled water is prepared, 1.2 weight portion polysorbas20s, 0.8 weight portion Tween 80,0.4 weight are subsequently added into
Part dodecanol polyethenoxy ether sodium sulfate sell with trade name AES-2EO by Shanghai Xian Jie Chemical Industry Science Co., Ltd and
The lauryl sodium sulfate that 1.0 weight portions are sold by Shanghai You Yang Industrial Co., Ltd.s with trade name K12, adds after dissolving
White tea extract solution, 0.15 weight portion that 2.5 weight portions are prepared in step B are according to Ji'nan University CN102020675B patent skills
Pi-allyl triphenylphosphinebromide prepared by art is resisted by Shaanxi Sen Fu natural products Co., Ltd with 0.38 weight portion with trade name L-
The ascorbyl palmitate of bad hematic acid Palmitate sale, continues to stir, and a kind of the compound molten of chitosan-containing is obtained after dissolving
Liquid；
D, preparation composite solution containing corn protein
The zein that 0.8 weight portion is sold by Shandong Li Tong bio tech ltd with trade name corn protein powder
Agarose, 0.25 weight portion that matter, 1.2 weight portions are sold by Fujian Ming Fu agar Co., Ltd with trade name agar powder are by Shandong
Sorbierite, 0.04 weight portion that Shouguang Hua Tian sugar alcohols Co., Ltd is sold with trade name Neosorb are by the precious biology work of Anhui section
Journey Co., Ltd is dissolved in 30 weight portion distilled water with the chondroitin sulfate that trade name chondroitin sulfate is sold, and is obtained one kind and is contained
The composite solution of corn protein；
E, prepare antibacterial modified chitose foaming agent
7 weight portion glycerine are weighed, water is added, stirred, add the chitosan-containing that 26 weight portions are obtained in step C
Composite solution and the composite solution containing corn protein that is obtained in step D of 32 weight portions, stir, obtain described anti-
Bacterium modification of chitosan foaming agent.
Determine that antibacterial manufactured in the present embodiment changes according to the antibacterial detection method detection and analysis of national standard that this specification is described
Property chitose foaming agent reaches 99.5% to the antibacterial ability of staphylococcus aureus, Escherichia coli, streptococcus, Pseudomonas aeruginosa
More than.
Comparative example 1：Prepare antibacterial modified chitose foaming agent
Carry out according to the same manner as in Example 1, simply the comparative example does not add pi-allyl triphenyl phosphonium bromide
Phosphine.
Determine that prepared by this comparative example anti-according to the antibacterial detection method detection and analysis of national standard that this specification is described
Bacterium modification of chitosan foaming agent reaches to the antibacterial ability of staphylococcus aureus, Escherichia coli, streptococcus, Pseudomonas aeruginosa
More than 86.2%.Compared with the result of implementation of embodiment 1, antibacterial modified chitose foaming agent prepared by this comparative example it is anti-
Bacterium effect is substantially lower.
Comparative example 2：Prepare antibacterial modified chitose foaming agent
Carry out according to the same manner as in Example 2, simply the comparative example does not add white tea extract solution.
Determine that prepared by this comparative example anti-according to the antibacterial detection method detection and analysis of national standard that this specification is described
Bacterium modification of chitosan foaming agent reaches to the antibacterial ability of staphylococcus aureus, Escherichia coli, streptococcus, Pseudomonas aeruginosa
More than 85.8%.Compared with the result of implementation of embodiment 2, antibacterial modified chitose foaming agent prepared by this comparative example it is anti-
Bacterium effect is substantially lower.
Claims (9)
1. a kind of preparation method of antibacterial modified chitose foaming agent, it is characterised in that as follows the step of the preparation method：
A, prepare modification of chitosan
By deacetylation 70%, molecular weight 30 × 104~60 × 104The shitosan of Da is dissolved in 1~2% acetic acid water by weight
In solution, the solution for obtaining is carried out under conditions of being 200W in supersonic frequency 22kHz and ultrasonic power in the supersonic wave cleaning machine
Ultrasonically treated 35~45min, then be classified with polyvinylidene fluoride (PVDF) ultrafiltration membrane, dry, obtain the shell of 500~1000Da of molecular weight
Glycan；This shitosan is added in 40~50% potassium hydroxide aqueous solutions by weight, in 110~120 DEG C of condition of temperature
15~20min of lower treatment, is then neutralized with 1.0~3.0N aqueous hydrochloric acid solutions, is filtered, is distilled water washing, drying, is taken off
The modification of chitosan of acetyl degree 98~99%, 500~1000Da of molecular weight；
B, white tea are extracted
15~25 weight portion white teas are weighed, Jia 80 thereto~120 weight portion distilled water, then carried at 95~100 DEG C of temperature
25~35min is taken, is filtered, remove tea grounds, the filtrate constant volume that will be obtained obtains containing tea polyphenols, coffee to 100 weight portions
Cause, theophylline and tannic acid, the white tea extract solution that concentration is 0.016~0.024g/ml；
C, prepare chitosan-containing composite solution
2~10 weight portions are dissolved in glacial acetic acid aqueous solution in the modification of chitosan that step A is prepared, 0.2 is subsequently added into
~1.2 weight portion polysorbas20s, 0.2~1.2 weight portion Tween 80,0.3~0.8 weight portion dodecanol polyethenoxy ether sodium sulfate
With 0.5~1.5 weight portion lauryl sodium sulfate, added after dissolving 1.5~2.5 weight portions step B prepare it is white
Tea extract, 0.05~0.15 weight portion pi-allyl triphenylphosphinebromide and 0.30~0.50 weight portion vitamin-c palmitate
Ester, continues to stir, and a kind of composite solution of chitosan-containing is obtained after dissolving；
D, preparation composite solution containing corn protein
By 0.1~1.0 parts by weight Corn protein, 0.2~1.2 weight portion agarose, 0.1~0.3 weight portion sorbierite, 0.01
~0.09 parts sulfuric acid chondroitin is dissolved in 18~42 weight portion distilled water, obtains a kind of compound molten containing corn protein
Liquid；
E, prepare antibacterial modified chitose foaming agent
Weigh 4~8 weight portion glycerine, add water, stir, add 25~35 weight portions step C obtain containing shell
The composite solution containing corn protein that the composite solution of glycan and 30~40 weight portions are obtained in step D, stirs, and obtains
Described antibacterial modified chitose foaming agent.
2. preparation method according to claim 1, it is characterised in that in step, the shitosan of deacetylation 70% is in vinegar
5~15min is dissolved in aqueous acid under conditions of 250~350rpm of low whipping speed.
3. preparation method according to claim 1, it is characterised in that in stepb, white tea is with the weight ratio of distilled water
18~22：90~110.
4. preparation method according to claim 1, it is characterised in that in step C, described glacial acetic acid aqueous solution be by
What 0.1~0.3 pbw of glacial acetic acid and 18~22 weight portion distilled water were prepared.
5. preparation method according to claim 1, it is characterised in that in step C, polysorbas20, Tween 80, dodecanol
Polyethenoxy ether sodium sulfate is 0.5~0.8 with the weight ratio of lauryl sodium sulfate：0.5~0.8：0.4~0.6：0.8~
1.2。
6. preparation method according to claim 1, it is characterised in that in step D, white tea extract solution, pi-allyl triphenyl
Bromide phosphine is 1.8~2.2 with the weight ratio of ascorbyl palmitate：0.08~0.12：0.36~0.42.
7. preparation method according to claim 1, it is characterised in that in step D, corn protein, agarose, sorb
Alcohol is 0.3~0.7 with the weight ratio of chondroitin sulfate：0.4~1.0：0.15~0.25：0.03~0.08.
8. preparation method according to claim 1, it is characterised in that in step E, glycerine, chitosan-containing it is compound molten
Liquid is 5~6 with the weight ratio of the composite solution containing corn protein：28~32：32~38.
9. the antibacterial modified chitose foaming agent that the preparation method according to any one of claim 1-8 claim is obtained,
It is characterized in that its antibacterial ability to staphylococcus aureus, Escherichia coli, streptococcus, Candida albicans or Pseudomonas aeruginosa is equal
Reach more than 99%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410321850.1A CN104042791B (en) | 2014-07-07 | 2014-07-07 | A kind of antibacterial modified chitose foaming agent and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410321850.1A CN104042791B (en) | 2014-07-07 | 2014-07-07 | A kind of antibacterial modified chitose foaming agent and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104042791A CN104042791A (en) | 2014-09-17 |
| CN104042791B true CN104042791B (en) | 2017-06-27 |
Family
ID=51496514
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410321850.1A Active CN104042791B (en) | 2014-07-07 | 2014-07-07 | A kind of antibacterial modified chitose foaming agent and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104042791B (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN112575581B (en) * | 2020-12-29 | 2022-05-17 | 湖南寐家居科技有限公司 | Antibacterial finishing agent for silk fabric and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101380447A (en) * | 2008-10-16 | 2009-03-11 | 周小萍 | Chitose foaming agent for treating gynecologic disease and preparation method thereof |
| CN101766188A (en) * | 2008-12-29 | 2010-07-07 | 张子剑 | Chitosan antimicrobial agent |
| CN102113981A (en) * | 2011-01-28 | 2011-07-06 | 武汉耦合医学科技有限责任公司 | Non-rinse pregnant woman perineum medical care gel and preparation method thereof |
| CN102824308A (en) * | 2012-08-31 | 2012-12-19 | 广州润虹医药科技有限公司 | Chitosan antibacterial filming sprayer and preparation method |
| CN103054733A (en) * | 2013-01-29 | 2013-04-24 | 广州拜恩化学科技有限公司 | Chitosan nano-micelle wrappage solution and preparation method thereof |
-
2014
- 2014-07-07 CN CN201410321850.1A patent/CN104042791B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101380447A (en) * | 2008-10-16 | 2009-03-11 | 周小萍 | Chitose foaming agent for treating gynecologic disease and preparation method thereof |
| CN101766188A (en) * | 2008-12-29 | 2010-07-07 | 张子剑 | Chitosan antimicrobial agent |
| CN102113981A (en) * | 2011-01-28 | 2011-07-06 | 武汉耦合医学科技有限责任公司 | Non-rinse pregnant woman perineum medical care gel and preparation method thereof |
| CN102824308A (en) * | 2012-08-31 | 2012-12-19 | 广州润虹医药科技有限公司 | Chitosan antibacterial filming sprayer and preparation method |
| CN103054733A (en) * | 2013-01-29 | 2013-04-24 | 广州拜恩化学科技有限公司 | Chitosan nano-micelle wrappage solution and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104042791A (en) | 2014-09-17 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101278896B (en) | Chitosan nano silver gel agent and uses thereof | |
| CN104257639B (en) | A kind of liniment for Wound treating and preparation method thereof | |
| CN103285028B (en) | Composite antibacterial agent of chitosan and organosilicone quaternary ammonium salt and preparation method of composite antibacterial agent | |
| CN103356738B (en) | Skin disinfection gel and its application | |
| CN104042791B (en) | A kind of antibacterial modified chitose foaming agent and preparation method thereof | |
| CN102824308A (en) | Chitosan antibacterial filming sprayer and preparation method | |
| CN102600494B (en) | Polysaccharide combination and preparation method and application thereof | |
| CN107970488A (en) | A kind of chitin quarternary ammonium salt aquagel antiseptic dressing and preparation method thereof | |
| CN108158995A (en) | A kind of gynaecology's anti-bacteria foaming agent containing chitosan and preparation method thereof | |
| CN104042719B (en) | A kind of antibacterial modified chitosan spray and preparation method thereof | |
| CN107233617A (en) | A kind of wound dressing of liquid chitosan and its preparation and application | |
| CN109646712B (en) | Colloidal sulfur liquid dressing and preparation method thereof | |
| CN106727319A (en) | A kind of gynaecology's foaming agent and preparation method thereof | |
| CN108354880A (en) | A kind of baby child's skin care compositions and methods | |
| CN106947095A (en) | A kind of preparation method for wound healing antibacterial type hydrogel | |
| CN104027300A (en) | Antibacterial chitosan gel and preparation method thereof | |
| JP5933178B2 (en) | Hydrogel of chitosan carboxyalkylamide, process for its preparation, and anhydrous products, dermatological compositions and cosmetic compositions | |
| CN105193705A (en) | Gel containing triclosan | |
| CN104306853A (en) | Chitosan quaternary ammonium salt-rhizoma galangae essential oil compound antibacterial aerosol and preparation method and application thereof | |
| CN107595819B (en) | A kind of Nano diamond modified liquid adhesive bandage and preparation method thereof | |
| CN105193686A (en) | Female care solution and preparation method thereof | |
| CN105126149B (en) | A kind of medical recombination chitosan application | |
| JP5716214B2 (en) | Bread seed-based mixture | |
| CN110090224B (en) | Colloidal dressing for promoting wound healing | |
| CN1969838A (en) | Micro-ecological preparation for treating moniliasis |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |