CN104042719A - Antibacterial modified chitosan spray and preparation method thereof - Google Patents
Antibacterial modified chitosan spray and preparation method thereof Download PDFInfo
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Abstract
The invention relates to antibacterial modified chitosan spray and a preparation method thereof. The preparation method of the antibacterial modified chitosan spray comprises the steps of preparing modified chitosan, preparing gardenia oil, preparing geniposide, preparing spirulina polysaccharide and spirulina polypeptide and preparing chitosan spray. The antibacterial modified chitosan spray is applied to treatment on male and female pruritus vulvae and fungal infection, bacterial infection, folliculitis and vaginitis, also can be used for treating bedsore and long-term skin inflammation, can be widely applied and has antibacterial ability more than 99% on staphylococcus aureus, escherichia coli, streptococcus, candida albicans, pseudomonas aeruginosa or other fungi.
Description
[technical field]
The invention belongs to medical drugs technical field.More specifically, the present invention relates to a kind of antibacterial modified chitosan spray, also relate to the preparation method of described antibacterial modified chitosan spray,
[background technology]
Chitosan is a kind of shell of Crustacean (Eriocheir sinensis shrimp) and natural alkaline macromolecule polysaccharide of segmental appendage class animal (Blatta seu periplaneta etc.) skeleton of deriving from, there is good biocompatibility, biodegradability and regeneration antibacterial, anticorrosion, that promote endotheliocyte, blood capillary, myocardial cell and neural axon, the premium properties such as hemostasis and promotion wound healing.Research shows, low-molecular weight chitoglycan has human body and easily absorbs, can activated lymphocyte, the physiologically active such as enhancing human body immunity power, antibacterial bacteriostatic, inhibition tumor cell growth, in addition, research is found, deacetylating degree of chitosan is higher, and its effect of removing hydroxy radical, superoxide radical and organic free radical is better.These character make it as natural antibacterial, anti-biotic material, antiseptic, have good application prospect.
Along with automiser spray is gradually improved, ejecting agent continues to bring out, for adapting to the needs of the allegro life style of modern society and clinical practice, it is ripe that the preparation technology of various sprays is tending towards, more extensive in aspect application such as part, whole body therapeutic and environment disinfecteds, fully show its unique advantage, development in recent years is very fast, has become an important branch in current medical instruments field.
Spray only aobvious advantage aspect topical therapeutic, because medicinal liquid can be uniformly distributed in local patient part, and can absorb rapidly and play a role.At present, at treatment burn, to scald effect remarkable, cure rate is all more than 90%.Clinical demand at aspects such as infantile eczema, tinea versicolor, closed bone injuries, beriberi and various dermatitis, gynaecopathia, skin injury and ulcer in body surface, periarthritis, control scar hyperplasias is in rising trend.
At present, people utilize chitosan to prepare spray, for example CN102846655A discloses a kind of antibacterial spray and preparation method thereof, this spray is made by water, chitosan, glycerol, polyhexamethylene guanidine, vitamin E, wherein 0.01% chitosan is difficult to bring into play antibacterial effect, antibacterial main body polyhexamethylene guanidine is a kind of synthetic high molecular polymer, is mainly used in aquatic products because of prevention and the treatment of bacterial various diseases.CN102860567A discloses the fresh-keeping spray of a kind of chitosan, and it is made by, chitosan, edible glue, glacial acetic acid, citric acid and water, but it does not clearly demonstrate molecular weight and the deacetylation of chitosan, does not evaluate its antibacterial, corrosion-resistanting fresh-keeping effect yet.CN102524316B discloses a kind of chitosan-based anti-freezing antibacterial spraying agent for cutting surfaces of rubber trees and preparation method thereof, this spray contains chitosan, tea tree ethereal oil, polyvinyl alcohol, plant growth regulator etc., it does not clearly demonstrate molecular weight and the deacetylation of chitosan equally, does not evaluate its antibacterial effect yet.
In addition, have not yet to see about utilizing chitosan to prepare the patent of foam as primary raw material.The chitosan of application is to be mainly polymer chitosan at present, does not also see by chitin modified, controls the relevant report that its molecular weight and deacetylation improve 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, high-efficiency antimicrobial spray, a kind of preparation method of antibacterial modified chitosan spray is proposed, it is good that the spray obtaining has spray effect, medicinal liquid can be uniformly distributed in patient part, and can absorb rapidly and play a role, antibacterial wide spectrum, can promote focus cytothesis and healing growth, can be applicable to part, the whole body therapeutic of sufferer simultaneously.
[summary of the invention]
[technical problem that will solve]
The object of this invention is to provide a kind of antibacterial modified chitosan spray.
Another object of the present invention is to provide the preparation method of described antibacterial modified chitosan spray.
[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 chitosan spray.
The step of this antibacterial modified chitosan spray preparation method is as follows:
A, prepare modification of chitosan
By deacetylation 80%, molecular weight 20 * 10
4～30 * 10
4the chitosan of Da is dissolved in by weight in 1.0～3.0% aqueous acetic acids, be incorporated as again two t-amyl peroxy things of 1～3 times of chitosan weight, the solution obtaining carries out supersound process in ultrasonic washing unit, obtain low-molecular weight chitoglycan complex solution, pass through polyacrylonitrile ultrafiltration film molecular retention and classification, obtaining molecular weight is the chitosan below 500Da again; This chitosan is added to by weight in 35～45% potassium hydroxide aqueous solutions, under the condition of 105～115 ℃ of temperature, process 10～20min, then with 1.0～3.0N aqueous hydrochloric acid solution, neutralize, filtration, distilled water wash, be dried, obtain deacetylation 99～100%, molecular weight is the modification of chitosan below 500Da;
B, prepare Fructus Gardeniae oil
In 80～120 weight portion Fructus Gardeniae powder, add 700～900 weight portion petroleum hydrocarbons, then in ultrasonic washing unit, carry out supersound extraction, filtration obtains filtrate and filtering residue, described filtering residue then repeats supersound extraction 2～3 times with 500～700 weight portion petroleum ether with the same manner, filtrate merges, adopt heating in water bath mode to remove the petroleum hydrocarbon in merging filtrate under the condition of 60～90 ℃ of temperature, obtain Fructus Gardeniae oil;
C, prepare jasminoidin
In 80～120 weight portion Fructus Gardeniae powder, add 800～1200 weight portions, 70～80% ethanol waters by volume, then in ultrasonic washing unit, carry out supersound extraction, filtration obtains filtrate and filtering residue, described filtering residue then repeats supersound extraction 2～3 times with the same manner, filtrate merges, then under flow velocity is the conditions of 20～30 microlitre/seconds, by nonpolarity macroporous adsorptive resins chromatographic column with at flow velocity, be to pass through polyamide column under the conditions of 30～37 microlitre/seconds, then working concentration 15～25% ethanol water eluting agent are by volume from adsorption column eluting, the eluent obtaining is processed and is obtained jasminoidin in rotary evaporator under the condition of distilling under reduced pressure,
D, prepare spirulina polysaccharide and spirulina polypeptide
Fresh spirulina is processed 12～18 minutes in low temperature biomixer under 4 ℃～6 ℃ cryogenic conditions, the treatment fluid obtaining carries out centrifugal treating through low temperature supercentrifuge again under 4 ℃～6 ℃ conditions of temperature, then use filter at low temperature equipment to filter under the condition of 2 ℃～5 ℃ of temperature, then under the condition of 2 ℃～8 ℃ of temperature, use the permeable membrane that molecular cut off is 10kD to carry out membrane permeation processing, obtain spirulina polysaccharide and spirulina polypeptide;
E, preparation chitosan spray
The modification of chitosan that 2.5～3.2 weight portions are obtained in steps A is dissolved in 6～15 weight portion concentration by weight in 0.8～1.2% aqueous acetic acid, then in resulting solution, add 0.8～1.2 weight portion polysorbate60, 0.8～1.2 weight portion lauroylamidopropyl betaine, mix homogeneously, the jasminoidin that adds again 0.3～0.8 weight portion to obtain at step C, the Fructus Gardeniae oil that 0.1～0.4 weight portion obtains at step B, the spirulina polypeptide that 0.1～0.4 weight portion obtains at step D, the spirulina polysaccharide that 0.1～0.4 weight portion obtains at step D, mix homogeneously, finally add 0.1～0.4 weight portion pi-allyl tributyl bromide phosphine, with distilled water, its gross weight is reached to 100 weight portions, obtain described antibacterial modified chitosan spray.
A preferred embodiment of the invention, in steps A, dissolves 5～15min under the condition of deacetylation 80% 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, described filtering residue is when the 1st supersound extraction, and the weight ratio of Fructus Gardeniae powder and petroleum hydrocarbon is 90～110:750～850; When the 2nd time or the 3rd supersound extraction, the weight ratio of Fructus Gardeniae powder and petroleum hydrocarbon is 90～110:550～650.
According to another kind of preferred implementation of the present invention, in step C, described macroporous adsorbent resin is nonpolar D101, LX-60 or the LX-20 type resin being prepared by styrene and divinylbenzene combined polymerization; Described polyamide is by caprolactam or adipic acid and the synthetic polyphosphazene polymer amide preparing of hexamethylene diamine.
According to another kind of preferred implementation of the present invention, in step C, the eluant of described macroporous adsorptive resins or the eluant of described polyamide column are concentration 18～22% ethanol waters by volume.
According to another kind of preferred implementation of the present invention, in step D, described permeable membrane is the permeable membrane of being prepared by polyether sulfone, Triafol T or regenerated cellulose.
According to another kind of preferred implementation of the present invention, in step D, the rotating speed of described low temperature supercentrifuge is 20000～30000 revs/min.
According to another kind of preferred implementation of the present invention, the weight ratio of modification of chitosan, polysorbate60, lauroylamidopropyl betaine, jasminoidin, Fructus Gardeniae oil, spirulina polypeptide, spirulina polysaccharide and pi-allyl tributyl bromide phosphine is 2.8～3.0:0.85～1.12:0.85～1.12:0.45～0.65:0.15～0.24:0.15～0.26:0.15～0.25:0.15～0.24.
The invention still further relates to the antibacterial modified chitosan spray that adopts described preparation method to obtain.Described antibacterial modified chitosan spray reaches more than 99% the antibacterial ability of staphylococcus aureus, escherichia coli, streptococcus, Candida albicans, bacillus pyocyaneus or other fungus.
The present invention will be described in more detail below
The present invention relates to a kind of preparation method of antibacterial modified chitosan spray.
It is main matrix that pure-natural biological mass shell polysaccharide is take in the present invention, by adjusting its molecular weight, change its deacetylation, be used in conjunction with other synergist again, be aided with the combination that can promote nutrition that histiocyte is repaired and growth regulating adjuvant etc. simultaneously, prepare novel chitosan anti-bacteria spray, aspect the treatment for the treatment of gynaecopathia, skin injury and ulcer in body surface, men and women's property pudendal pruritus, infantile eczema, tinea versicolor, beriberi and various dermatitis etc., solely shown advantage.
The step of modified chitosan anti-bacteria spray preparation method of the present invention is as follows:
A, prepare modification of chitosan
By deacetylation 80%, molecular weight 20 * 10
4～30 * 10
4the chitosan of Da is dissolved in by weight in 1.0～3.0% aqueous acetic acids, be incorporated as again two t-amyl peroxy things of 1～3 times of chitosan weight, the solution obtaining carries out supersound process in ultrasonic washing unit, obtain low-molecular weight chitoglycan complex solution, pass through polyacrylonitrile ultrafiltration film molecular retention and classification, obtaining molecular weight is the chitosan below 500Da again; This chitosan is added to by weight in 35～45% potassium hydroxide aqueous solutions, under the condition of 105～115 ℃ of temperature, process 10～20min, then with 1.0～3.0N aqueous hydrochloric acid solution, neutralize, filtration, distilled water wash, be dried, obtain deacetylation 99～100%, molecular weight is the modification of chitosan below 500Da.
The chemical constitution of chitosan (β-(1 → 4)-2-amino-2-deoxy-D-Glucose), for being with cationic macromolecule alkalescence polysaccharide polymer, is unique positively charged, the cation edible fiber of nature; It has the physicochemical properties such as stable physical property, good dissolubility, hydrophilic hygroscopicity, biological degradability, biocompatibility and film property, caking property, breathability.
In steps A, under the condition of deacetylation 80% chitosan low whipping speed 250～350rpm in aqueous acetic acid, dissolve 5～15min.
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, adding the effect of two t-amyl peroxy things (Di-tert-amyl peroxide) is that effect by peroxide makes chitosan molecule chain produce fracture, form low molecular chitosan, using organic peroxide rather than adopting the object of hydrogen peroxide is to make chain breaking process gentleness controlled, and can not produce uncontrollable chain-breaking reaction.
The two t-amyl peroxy things that the present invention uses are product solds in the market, for example by Taizhou City Hai Xiang Chemical Co., Ltd. with trade name t-amyl peroxy thing product sold.
In the present invention, the object that ultrasonic waves for cleaning is processed 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 is with trade name YD1008 ultrasonic washing unit product sold.
The present invention is by molecule hyperfiltration technique; by chitosan classification; intercepting molecular weight is less than the chitosan of the best molecular level scope of having of 500Da; 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 polyacrylonitrile ultrafiltration film.
With polyacrylonitrile ultrafiltration film, carrying out classification is that a kind of chitosan molecule that molecular weight is greater than to 500Da is held back, and the operation that the chitosan molecule that allows molecular weight be less than 500Da is passed through.The molecular weight of chitosan adopts conventional gel permeation chromatography method to measure and obtains.
The performance of the polyacrylonitrile ultrafiltration film that the present invention uses is as follows: thickness 50-90 μ m, Unit Weight 2.1-3.4mg/cm
2, porosity 75-81%, intensity be greater than 15pst.
The polyacrylonitrile ultrafiltration film that the present invention uses is product sold in the market, for example by Zhaoyuan Jin Huimo Science and Technology Ltd. with trade name UFbIA250-PAN film product sold.
After classification, allow the molecular weight collected be that chitosan molecule part below 500Da is dried to water content lower than 6% in hot-air dry equipment under the condition of temperature 60 C.
Then to resulting molecular weight, be, that chitosan molecule below 500Da 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 is used is with previously described identical, and baking temperature condition is also with previously described identical.
B, prepare Fructus Gardeniae oil
In 80～120 weight portion Fructus Gardeniae powder, add 700～900 weight portion petroleum hydrocarbons, then in ultrasonic washing unit, carry out supersound extraction, filtration obtains filtrate and filtering residue, described filtering residue then repeats supersound extraction 2～3 times with 500～700 weight portion petroleum ether with the same manner, filtrate merges, adopt heating in water bath mode to remove the petroleum hydrocarbon in merging filtrate under the condition of 60～90 ℃ of temperature, obtain Fructus Gardeniae oil;
Fructus Gardeniae powder is product sold in the market, for example by north and south, Guangzhou row prepared slices of Chinese crude drugs company limited with trade name Fructus Gardeniae product sold.The granularity of Fructus Gardeniae powder is generally 60～100 orders.
Petroleum hydrocarbon is also product sold in the market, for example by Guangzhou chemical reagents corporation with trade name petroleum ether product sold.
In this step, with petroleum hydrocarbon, from Fructus Gardeniae powder, extract oil-soluble composition Fructus Gardeniae oil.
In this step, described filtering residue is when the 1st supersound extraction, and the weight ratio of Fructus Gardeniae powder and petroleum hydrocarbon is 90～110:750～850; When the 2nd time or the 3rd supersound extraction, the weight ratio of Fructus Gardeniae powder and petroleum hydrocarbon is 90～110:550～650.
The ultrasonic washing unit that this step is used and supersound process condition thereof as previously described, do not repeat them here.
C, prepare jasminoidin
In 80～120 weight portion Fructus Gardeniae powder, add 800～1200 weight portions, 70～80% ethanol waters by volume, then in ultrasonic washing unit, carry out supersound extraction, filtration obtains filtrate and filtering residue, described filtering residue then repeats supersound extraction 2～3 times with the same manner, filtrate merges, then under flow velocity is the conditions of 20～30 microlitre/seconds, by nonpolarity macroporous adsorptive resins chromatographic column with at flow velocity, be to pass through polyamide column under the conditions of 30～37 microlitre/seconds, then working concentration 15～25% ethanol water eluting agent are by volume from adsorption column eluting, the eluent obtaining is processed and is obtained jasminoidin in rotary evaporator under the condition of distilling under reduced pressure,
The granularity of the Fructus Gardeniae powder that this step is used is generally 60～100 orders.
In this step, with ethanol water, from Fructus Gardeniae powder, extract Alcohol soluble composition jasminoidin.
In this step, the ultrasonic washing unit of use and supersound process condition thereof as previously described, do not repeat them here.
In this step, resulting filtrate is separated jasminoidin and Gardenia Yellow and other impurity by the object that nonpolar macroporous adsorption resin is processed.The macroporous adsorbent resin that the present invention uses is nonpolar D101, LX-60 or the LX-20 type resin being prepared by styrene and divinylbenzene combined polymerization, D101, LX-60, the LX-20 macroporous adsorbent resin for example by Xi'an Sunresin New Materials Co., Ltd., with trade name macroporous resin, sold.
In the present invention, described filtrate was less than for 20 microlitre/seconds by the flow velocity of described resin bed, can affect the delivery time; If described flow velocity was greater than for 30 microlitre/seconds, can make absorption with separated incomplete.Therefore, described flow velocity is that be appropriate 20～30 microlitre/seconds, preferably 22～28 microlitre/seconds, more preferably 24～26 microlitre/seconds.
The effluent of described resin bed is then by polyamide column, and its object is further separated pigment and impurity component, purification of samples.
Described polyamide is by caprolactam or adipic acid and the synthetic polyphosphazene polymer amide preparing of hexamethylene diamine.The polyphosphazene polymer amide that the present invention uses is the polyamide of being sold with trade name polyamide by the biochemical plastic molding and processing plant of Taizhou City of Zhejiang Province road and bridge tetramethyl.
In the present invention, described resin bed effluent was less than for 30 microlitre/seconds by the flow velocity of described polyamide column, can affect the delivery time; If described flow velocity was greater than for 37 microlitre/seconds, can affect separating effect.Therefore, described flow velocity is that be appropriate 30～37 microlitre/seconds, preferably 32～36 microlitre/seconds, more preferably 34～36 microlitre/seconds.
Preferably, the eluant of described macroporous adsorptive resins or the eluant of described polyamide column are concentration 18～22% ethanol waters by volume.
In the rotary evaporator that the eluent obtaining is sold with trade name RE-301 type rotary evaporator in Guangzhou Xing Shuo Instrument Ltd., under the condition of pressure 0.002-0.098MPa, carry out distilling under reduced pressure.
D, prepare spirulina polysaccharide and spirulina polypeptide
Fresh spirulina is processed 12～18 minutes in low temperature biomixer under 4 ℃～6 ℃ cryogenic conditions, the treatment fluid obtaining carries out centrifugal treating through low temperature supercentrifuge again under 4 ℃～6 ℃ conditions of temperature, then use filter at low temperature equipment to filter under the condition of 2 ℃～5 ℃ of temperature, then under the condition of 2 ℃～8 ℃ of temperature, use the permeable membrane that molecular cut off is 10kD to carry out membrane permeation processing, obtain spirulina polysaccharide and spirulina polypeptide;
Spirulina (Spirulinap latensis Geitl.) is a class unicellular lower eukaryote, and prokaryote, by filamentous unicellular or that many cells form, the long 200-500 μ of body m, wide 5-10 μ m, cylindrical, be loose or well-regulated spiral rotary shape bending closely.It has the toxicity that alleviates cancer radiation, chemotherapy, improves immunologic function, reduces the effects such as blood fat.
The low temperature biomixer that the present invention uses is product sold in the market, for example by company of Guangdong Juneng Biology & Technology Co., Ltd. with trade name JN-02C low temperature continuous flow cell disintegrating machine product sold.
In this step, the rotating speed of described low temperature supercentrifuge is 20000～30000 revs/min.The low temperature supercentrifuge that the present invention uses is product sold in the market, for example by company of U.S. Beckman Coulter Inc. with trade name XPN-80 supercentrifuge product sold.
Described filter at low temperature equipment is product sold in the market, for example by Dongguan Long Tian filter plant company limited with trade name LT600 insulation jacket filter product sold.
The permeable membrane that the present invention uses is product sold in the market, for example by Hydranautics with trade name QUALSEP DairyRO series concentrating and separating film product sold.
In this step, it is to carry out under 2 ℃～8 ℃ cryogenic conditions that membrane permeation is processed.
Membrane permeation is processed resulting product and is adopted conventional infrared spectrum, its spirulina polysaccharide of mass spectrometric analysis method Analysis deterrmination and spirulina polypeptide.
E, preparation chitosan spray
The modification of chitosan that 2.5～3.2 weight portions are obtained in steps A is dissolved in 6～15 weight portion concentration by weight in 0.8～1.2% aqueous acetic acid, then in resulting solution, add 0.8～1.2 weight portion polysorbate60, 0.8～1.2 weight portion lauroylamidopropyl betaine, mix homogeneously, the jasminoidin that adds again 0.3～0.8 weight portion to obtain at step C, the Fructus Gardeniae oil that 0.1～0.4 weight portion obtains at step B, the spirulina polypeptide that 0.1～0.4 weight portion obtains at step D, the spirulina polysaccharide that 0.1～0.4 weight portion obtains at step D, mix homogeneously, finally add 0.1～0.4 weight portion pi-allyl tributyl bromide phosphine, with distilled water, its gross weight is reached to 100 weight portions.
Preferably, the weight ratio of modification of chitosan, polysorbate60, lauroylamidopropyl betaine, jasminoidin, Fructus Gardeniae oil, spirulina polypeptide, spirulina polysaccharide and pi-allyl tributyl bromide phosphine is 2.8～3.0:0.85～1.12:0.85～1.12:0.45～0.65:0.15～0.24:0.15～0.26:0.15～0.25:0.15～0.24.
The effect of the polysorbate60 that the present invention uses is to stablize Fructus Gardeniae oil and jasminoidin, makes it can in spray, not occur layering, segregation phenomenon; It is product sold in the market, the polysorbate60 of for example being sold with trade name T-60 by Jiangsu Hai'an Petrochemical Plant.
The effect of the lauroylamidopropyl betaine that the present invention uses is can dispersed spirulina polypeptide and spirulina polysaccharide, makes it there will not be precipitation, and meanwhile, lauroylamidopropyl betaine also can play the effect of further lifting chitosan anti-bacteria usefulness; It is product sold in the market, for example by upper marine Xiang Fine Chemical Co., Ltd with trade name CAB35 product sold.
The invention still further relates to the antibacterial modified chitosan spray that adopts described preparation method to obtain.Antibacterial modified chitose foaming agent of the present invention detects and analyzes through the antibacterial detection method of national standard (GB/T16886), and the antibacterial ability of staphylococcus aureus, escherichia coli, streptococcus, Candida albicans, bacillus pyocyaneus or other fungus is reached more than 99%.
Antibacterial modified chitosan spray main body of the present invention adopts the natural products such as chitosan, jasminoidin, Fructus Gardeniae oil, spirulina polypeptide, spirulina polysaccharide, has improved the biological safety of spray and the environmental protection of production process.
Spray of the present invention is by the collaborative impact of high deacetylized micromolecule chitosan and Fructus Gardeniae extract, spirulina polysaccharide extract, given full play to the antibacterial action of chitosan polysaccharide, greatly improved the whole anti-harmful microorganism effect of spray, antibacterial, virus, fungus have all been had to obvious killing effect.Meanwhile, the extract of Fructus Gardeniae and spirulina has biological activity, can reach the healing and the growth that promote damaged skin, tissue, promotes cellular metabolism, strengthens the resistance against diseases of skin.
The present invention is by adding a small amount of Fructus Gardeniae oil, two kinds of non-ionic surface active agents of polysorbate60 and lauroylamidopropyl betaine, have improved the diffusion performance of product, make effective ingredient in spray more easily and epidermis generation effect, evenly diffusion, performance therapeutic effect.
Spray of the present invention is applied to treat men and women's property pruritus vulvae and fungal infection, courses of infection, and folliculitis, vaginitis, is also applied to the treatment of decubital ulcer and the long-term inflammation of skin etc., applies very extensive.
[beneficial effect]
The invention has the beneficial effects as follows:
The present invention adopts mode that two t-amyl peroxy things combine with ultrasonic technique with degrade chitosan; the inventive method adopts organic peroxide; action temperature and; reduce chitosan oxidation stain; again by molecule hyperfiltration technique; by chitosan classification; intercepting molecular weight is lower than the micromolecule chitosan of 500Da; then by deacetylated; acquisition low-molecular-weight is high deacetylized, the modification of chitosan of narrow molecular weight distribution; its free radical resisting improves greatly with removing free radical ability, and to having improved antiinflammatory ability, the ability to function of pathogenic microorganism also improves greatly.
Antibacterial modified chitosan spray main body of the present invention adopts the natural products such as chitosan, jasminoidin, Fructus Gardeniae oil, spirulina polypeptide, spirulina polysaccharide, has improved the biological safety of spray and the environmental protection of production process.
Spray of the present invention is by the collaborative impact of high deacetylized micromolecule chitosan and Fructus Gardeniae extract, spirulina polysaccharide extract, given full play to the antibacterial action of chitosan polysaccharide, greatly improved the whole anti-harmful microorganism effect of spray, antibacterial, virus, fungus have all been had to obvious killing effect.Meanwhile, the extract of Fructus Gardeniae and spirulina has biological activity, can reach the healing and the growth that promote damaged skin, tissue, promotes cellular metabolism, strengthens the resistance against diseases of skin.
The present invention is by adding a small amount of Fructus Gardeniae oil, two kinds of non-ionic surface active agents of polysorbate60 and lauroylamidopropyl betaine, have improved the diffusion performance of product, make effective ingredient in spray more easily and epidermis generation effect, evenly diffusion, performance therapeutic effect.
Spray of the present invention is applied to treat men and women's property pruritus vulvae and fungal infection, courses of infection, and folliculitis, vaginitis, is also applied to the treatment of decubital ulcer and the long-term inflammation of skin etc., applies very extensive.
Spray of the present invention reaches more than 99% the antibacterial ability of staphylococcus aureus, escherichia coli, streptococcus, Candida albicans, bacillus pyocyaneus or other fungus.
[specific embodiment]
By following embodiment, can understand better the present invention.
Embodiment 1: prepare antibacterial modified chitosan spray
The implementation step of this embodiment is as follows:
A, prepare modification of chitosan
By Jinan Haidebei Marine Organism Engineering Co., Ltd., with trade name food pharmaceutical grade chitosan, sold, deacetylation 80%, molecular weight 20 * 10
4the chitosan of Da, in 1.6% aqueous acetic acid by weight, under the condition of low whipping speed 250rpm, dissolve 5min, be incorporated as again two t-amyl peroxy things of 1.0 times of chitosan weight, 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, supersound process 35min under the condition that is 200W at supersonic frequency 22kHz and ultrasonic power, obtain low-molecular weight chitoglycan complex solution, polyacrylonitrile ultrafiltration film molecular retention and classification through being sold with trade name UFbIA250-PAN film by Zhaoyuan Jin Huimo Science and Technology Ltd. again, obtaining molecular weight is the chitosan below 500Da, this chitosan is added to by weight in 35% potassium hydroxide aqueous solution, under the condition of 105 ℃ of temperature, process 10min, then with 1.6N aqueous hydrochloric acid solution, neutralize, filtration, distilled water wash, under the condition of temperature 60 C, be dried, obtain deacetylation 99%, molecular weight is the modification of chitosan below 500Da,
B, prepare Fructus Gardeniae oil
In 80 weight portion Fructus Gardeniae powder, add 700 weight portion petroleum hydrocarbons, then supersound process 35min under the condition that to be take in the ultrasonic washing unit that trade name YD1008 ultrasonic washing unit sells at supersonic frequency 22kHz and ultrasonic power be 200W by Changzhou You Da ultrasonic equipment company limited, filtration obtains filtrate and filtering residue, described filtering residue then repeats supersound extraction 2 times with 500 weight portion petroleum ether with the same manner, filtrate merges, adopt heating in water bath mode under the condition of temperature 60 C, to remove the petroleum hydrocarbon in merging filtrate, obtain Fructus Gardeniae oil;
C, prepare jasminoidin
In 80 weight portion Fructus Gardeniae powder, add 800 weight portions, 70% ethanol water by volume, then in the ultrasonic washing unit of being sold with trade name YD1008 ultrasonic washing unit by Changzhou You Da ultrasonic equipment company limited, supersound process 35min under the condition that is 200W at supersonic frequency 22kHz and ultrasonic power, filtration obtains filtrate and filtering residue, described filtering residue then repeats supersound extraction 3 times with the same manner, filtrate merges, then at flow velocity, be by the D101 type macroporous adsorptive resins of being sold with trade name macroporous resin by Xi'an Sunresin New Materials Co., Ltd. under the conditions of 26 microlitre/seconds, then under the flow velocity condition of 30 microlitre/seconds, pass through the polyamide column of being sold with trade name polyamide by the biochemical plastic molding and processing plant of Taizhou City of Zhejiang Province road and bridge tetramethyl, then working concentration 15% ethanol water eluting agent is by volume from adsorption column eluting, in the rotary evaporator that the eluent obtaining is sold with trade name RE-301 type rotary evaporator in Guangzhou Xing Shuo Instrument Ltd., under the condition of pressure 0.002-0.098MPa, carry out distilling under reduced pressure and obtain jasminoidin,
D, prepare spirulina polysaccharide and spirulina polypeptide
In the low temperature biomixer that company of fresh spirulina You Guangdong Juneng Biology & Technology Co., Ltd. is sold with trade name JN-02C low temperature continuous flow cell disintegrating machine, under 4 ℃ of cryogenic conditions of temperature, process 12 minutes, the treatment fluid obtaining carries out centrifugal treating through the low temperature supercentrifuge of being sold with trade name XPN-80 supercentrifuge by company of U.S. Beckman Coulter Inc. again under 4 ℃ of conditions of temperature, then use the filter at low temperature equipment of being sold with trade name LT600 insulation jacket filter by Dongguan Long Tian filter plant company limited to filter under the condition of 2 ℃ of temperature, then under the condition of 2 ℃ of temperature, use and by Hydranautics, take the permeable membrane that molecular cut off that trade name QUALSEP DairyRO series concentrating and separating film sells is 10kD and carry out membrane permeation processing, obtain spirulina polysaccharide and spirulina polypeptide,
E, preparation chitosan spray
The modification of chitosan that 2.5 weight portions are obtained in steps A is dissolved in 6 weight portion concentration by weight in 0.8% aqueous acetic acid, then toward the polysorbate60 that adds in resulting solution 0.8 weight portion to be sold with trade name T-60 by Jiangsu Hai'an Petrochemical Plant, the lauroylamidopropyl betaine that 0.8 weight portion is sold with trade name CAB35 by upper marine Xiang Fine Chemical Co., Ltd, mix homogeneously, the jasminoidin that adds again 0.3 weight portion to obtain at step C, the Fructus Gardeniae oil that 0.1 weight portion obtains at step B, the spirulina polypeptide that 0.4 weight portion obtains at step D, the spirulina polysaccharide that 0.2 weight portion obtains at step D, mix homogeneously, finally add 0.1 weight portion pi-allyl tributyl bromide phosphine, with distilled water, its gross weight is reached to 100 weight portions.
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 99.0% to the antibacterial ability of staphylococcus aureus, escherichia coli, streptococcus, bacillus pyocyaneus.
Embodiment 2: prepare antibacterial modified chitosan spray
The implementation step of this embodiment is as follows:
A, prepare modification of chitosan
By Jinan Haidebei Marine Organism Engineering Co., Ltd., with trade name food pharmaceutical grade chitosan, sold, deacetylation 80%, molecular weight 24 * 10
4the chitosan of Da, in 3.0% aqueous acetic acid by weight, under the condition of low whipping speed 320rpm, dissolve 5min, be incorporated as again two t-amyl peroxy things of 1.6 times of chitosan weight, 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, supersound process 38min under the condition that is 200W at supersonic frequency 22kHz and ultrasonic power, obtain low-molecular weight chitoglycan complex solution, polyacrylonitrile ultrafiltration film molecular retention and classification through being sold with trade name UFbIA250-PAN film by Zhaoyuan Jin Huimo Science and Technology Ltd. again, obtaining molecular weight is the chitosan below 500Da, this chitosan is added to by weight in 40% potassium hydroxide aqueous solution, under the condition of 105 ℃ of temperature, process 12min, then with 3.0N aqueous hydrochloric acid solution, neutralize, filtration, distilled water wash, under the condition of temperature 60 C, be dried, obtain deacetylation 100%, molecular weight is the modification of chitosan below 500Da,
B, prepare Fructus Gardeniae oil
In 110 weight portion Fructus Gardeniae powder, add 800 weight portion petroleum hydrocarbons, then supersound process 45min under the condition that to be take in the ultrasonic washing unit that trade name YD1008 ultrasonic washing unit sells at supersonic frequency 22kHz and ultrasonic power be 200W by Changzhou You Da ultrasonic equipment company limited, filtration obtains filtrate and filtering residue, described filtering residue then repeats supersound extraction 3 times with 500 weight portion petroleum ether with the same manner, filtrate merges, adopt heating in water bath mode under the condition of temperature 70 C, to remove the petroleum hydrocarbon in merging filtrate, obtain Fructus Gardeniae oil;
C, prepare jasminoidin
In 100 weight portion Fructus Gardeniae powder, add 1060 weight portions, 75% ethanol water by volume, then in the ultrasonic washing unit of being sold with trade name YD1008 ultrasonic washing unit by Changzhou You Da ultrasonic equipment company limited, supersound process 45min under the condition that is 200W at supersonic frequency 22kHz and ultrasonic power, filtration obtains filtrate and filtering residue, described filtering residue then repeats supersound extraction 2 times with the same manner, filtrate merges, then at flow velocity, be by the LX-60 type resin macroporous adsorptive resins of being sold with trade name macroporous resin by Xi'an Sunresin New Materials Co., Ltd. under the conditions of 20 microlitre/seconds, then under the flow velocity condition of 32 microlitre/seconds, pass through the polyamide column of being sold with trade name polyamide by the biochemical plastic molding and processing plant of Taizhou City of Zhejiang Province road and bridge tetramethyl, then working concentration 22% ethanol water eluting agent is by volume from adsorption column eluting, in the rotary evaporator that the eluent obtaining is sold with trade name RE-301 type rotary evaporator in Guangzhou Xing Shuo Instrument Ltd., under the condition of pressure 0.002-0.098MPa, carry out distilling under reduced pressure and obtain jasminoidin,
D, prepare spirulina polysaccharide and spirulina polypeptide
In the low temperature biomixer that company of fresh spirulina You Guangdong Juneng Biology & Technology Co., Ltd. is sold with trade name JN-02C low temperature continuous flow cell disintegrating machine, under 5 ℃ of cryogenic conditions, process 15 minutes, the treatment fluid obtaining carries out centrifugal treating through the low temperature supercentrifuge of being sold with trade name XPN-80 supercentrifuge by company of U.S. Beckman Coulter Inc. again under 4 ℃ of conditions of temperature, then use the filter at low temperature equipment of being sold with trade name LT600 insulation jacket filter by Dongguan Long Tian filter plant company limited to filter under the condition of 3 ℃ of temperature, then under the condition of 5 ℃ of temperature, use and by Hydranautics, take the permeable membrane that molecular cut off that trade name QUALSEP DairyRO series concentrating and separating film sells is 10kD and carry out membrane permeation processing, obtain spirulina polysaccharide and spirulina polypeptide,
E, preparation chitosan spray
The modification of chitosan that 3.2 weight portions are obtained in steps A is dissolved in 14 weight portion concentration by weight in 1.0% aqueous acetic acid, then toward the polysorbate60 that adds in resulting solution 0.9 weight portion to be sold with trade name T-60 by Jiangsu Hai'an Petrochemical Plant, the lauroylamidopropyl betaine that 0.9 weight portion is sold with trade name CAB35 by upper marine Xiang Fine Chemical Co., Ltd, mix homogeneously, the jasminoidin that adds again 0.5 weight portion to obtain at step C, the Fructus Gardeniae oil that 0.3 weight portion obtains at step B, the spirulina polypeptide that 0.2 weight portion obtains at step D, the spirulina polysaccharide that 0.4 weight portion obtains at step D, mix homogeneously, finally add 0.1 weight portion pi-allyl tributyl bromide phosphine, with distilled water, its gross weight is reached to 100 weight portions.
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 99.6% to the antibacterial ability of staphylococcus aureus, escherichia coli, streptococcus, bacillus pyocyaneus.
Embodiment 3: prepare antibacterial modified chitosan spray
The implementation step of this embodiment is as follows:
A, prepare modification of chitosan
By Jinan Haidebei Marine Organism Engineering Co., Ltd., with trade name food pharmaceutical grade chitosan, sold, deacetylation 80%, molecular weight 24 * 10
4the chitosan of Da, in 3.0% aqueous acetic acid by weight, under the condition of low whipping speed 350rpm, dissolve 10min, be incorporated as again two t-amyl peroxy things of 2.0 times of chitosan weight, 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, supersound process 40min under the condition that is 200W at supersonic frequency 22kHz and ultrasonic power, obtain low-molecular weight chitoglycan complex solution, polyacrylonitrile ultrafiltration film molecular retention and classification through being sold with trade name UFbIA250-PAN film by Zhaoyuan Jin Huimo Science and Technology Ltd. again, obtaining molecular weight is the chitosan below 500Da, this chitosan is added to by weight in 38% potassium hydroxide aqueous solution, under the condition of 110 ℃ of temperature, process 18min, then with 1.0N aqueous hydrochloric acid solution, neutralize, filtration, distilled water wash, under the condition of temperature 60 C, be dried, obtain deacetylation 99%, molecular weight is the modification of chitosan below 500Da,
B, prepare Fructus Gardeniae oil
In 100 weight portion Fructus Gardeniae powder, add 840 weight portion petroleum hydrocarbons, then supersound process 42min under the condition that to be take in the ultrasonic washing unit that trade name YD1008 ultrasonic washing unit sells at supersonic frequency 22kHz and ultrasonic power be 200W by Changzhou You Da ultrasonic equipment company limited, filtration obtains filtrate and filtering residue, described filtering residue then repeats supersound extraction 3 times with 700 weight portion petroleum ether with the same manner, filtrate merges, adopt heating in water bath mode under the condition of temperature 60 C, to remove the petroleum hydrocarbon in merging filtrate, obtain Fructus Gardeniae oil;
C, prepare jasminoidin
In 95 weight portion Fructus Gardeniae powder, add 880 weight portions, 75% ethanol water by volume, then in the ultrasonic washing unit of being sold with trade name YD1008 ultrasonic washing unit by Changzhou You Da ultrasonic equipment company limited, supersound process 45min under the condition that is 200W at supersonic frequency 22kHz and ultrasonic power, filtration obtains filtrate and filtering residue, described filtering residue then repeats supersound extraction 2 times with the same manner, filtrate merges, then at flow velocity, be by the LX-20 type resin macroporous adsorptive resins of being sold with trade name macroporous resin by Xi'an Sunresin New Materials Co., Ltd. under the conditions of 24 microlitre/seconds, then under the flow velocity condition of 34 microlitre/seconds, pass through the polyamide column of being sold with trade name polyamide by the biochemical plastic molding and processing plant of Taizhou City of Zhejiang Province road and bridge tetramethyl, then working concentration 18% ethanol water eluting agent is by volume from adsorption column eluting, in the rotary evaporator that the eluent obtaining is sold with trade name RE-301 type rotary evaporator in Guangzhou Xing Shuo Instrument Ltd., under the condition of pressure 0.002-0.098MPa, carry out distilling under reduced pressure and obtain jasminoidin,
D, prepare spirulina polysaccharide and spirulina polypeptide
In the low temperature biomixer that company of fresh spirulina You Guangdong Juneng Biology & Technology Co., Ltd. is sold with trade name JN-02C low temperature continuous flow cell disintegrating machine, under 4 ℃ of cryogenic conditions, process 18 minutes, the treatment fluid obtaining carries out centrifugal treating through the low temperature supercentrifuge of being sold with trade name XPN-80 supercentrifuge by company of U.S. Beckman Coulter Inc. again under 6 ℃ of conditions of temperature, then use the filter at low temperature equipment of being sold with trade name LT600 insulation jacket filter by Dongguan Long Tian filter plant company limited to filter under the condition of 2 ℃ of temperature, then under the condition of 3 ℃ of temperature, use and by Hydranautics, take the permeable membrane that molecular cut off that trade name QUALSEP DairyRO series concentrating and separating film sells is 10kD and carry out membrane permeation processing, obtain spirulina polysaccharide and spirulina polypeptide,
E, preparation chitosan spray
The modification of chitosan that 3.2 weight portions are obtained in steps A is dissolved in 14 weight portion concentration by weight in 1.0% aqueous acetic acid, then toward the polysorbate60 that adds in resulting solution 0.8 weight portion to be sold with trade name T-60 by Jiangsu Hai'an Petrochemical Plant, the lauroylamidopropyl betaine that 0.9 weight portion is sold with trade name CAB35 by upper marine Xiang Fine Chemical Co., Ltd, mix homogeneously, the jasminoidin that adds again 0.5 weight portion to obtain at step C, the Fructus Gardeniae oil that 0.2 weight portion obtains at step B, the spirulina polypeptide that 0.4 weight portion obtains at step D, the spirulina polysaccharide that 0.1 weight portion obtains at step D, mix homogeneously, finally add 0.4 weight portion pi-allyl tributyl bromide phosphine, with distilled water, its gross weight is reached to 100 weight portions.
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 chitosan spray
The implementation step of this embodiment is as follows:
A, prepare modification of chitosan
By Jinan Haidebei Marine Organism Engineering Co., Ltd., with trade name food pharmaceutical grade chitosan, sold, deacetylation 80%, molecular weight 26 * 10
4the chitosan of Da, in 2.5% aqueous acetic acid by weight, under the condition of low whipping speed 250rpm, dissolve 8min, be incorporated as again two t-amyl peroxy things of 2.0 times of chitosan weight, 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, supersound process 40min under the condition that is 200W at supersonic frequency 22kHz and ultrasonic power, obtain low-molecular weight chitoglycan complex solution, polyacrylonitrile ultrafiltration film molecular retention and classification through being sold with trade name UFbIA250-PAN film by Zhaoyuan Jin Huimo Science and Technology Ltd. again, obtaining molecular weight is the chitosan below 500Da, this chitosan is added to by weight in 42% potassium hydroxide aqueous solution, under the condition of 115 ℃ of temperature, process 10min, then with 1.0N aqueous hydrochloric acid solution, neutralize, filtration, distilled water wash, under the condition of temperature 60 C, be dried, obtain deacetylation 99%, molecular weight is the modification of chitosan below 500Da,
B, prepare Fructus Gardeniae oil
In 120 weight portion Fructus Gardeniae powder, add 860 weight portion petroleum hydrocarbons, then supersound process 42min under the condition that to be take in the ultrasonic washing unit that trade name YD1008 ultrasonic washing unit sells at supersonic frequency 22kHz and ultrasonic power be 200W by Changzhou You Da ultrasonic equipment company limited, filtration obtains filtrate and filtering residue, described filtering residue then repeats supersound extraction 3 times with 700 weight portion petroleum ether with the same manner, filtrate merges, adopt heating in water bath mode under the condition of temperature 60 C, to remove the petroleum hydrocarbon in merging filtrate, obtain Fructus Gardeniae oil;
C, prepare jasminoidin
In 90 weight portion Fructus Gardeniae powder, add 920 weight portions, 80% ethanol water by volume, then in the ultrasonic washing unit of being sold with trade name YD1008 ultrasonic washing unit by Changzhou You Da ultrasonic equipment company limited, supersound process 42min under the condition that is 200W at supersonic frequency 22kHz and ultrasonic power, filtration obtains filtrate and filtering residue, described filtering residue then repeats supersound extraction 3 times with the same manner, filtrate merges, then at flow velocity, be by the D101 type resin macroporous adsorptive resins of being sold with trade name macroporous resin by Xi'an Sunresin New Materials Co., Ltd. under the conditions of 30 microlitre/seconds, then under the flow velocity condition of 36 microlitre/seconds, pass through the polyamide column of being sold with trade name polyamide by the biochemical plastic molding and processing plant of Taizhou City of Zhejiang Province road and bridge tetramethyl, then working concentration 18% ethanol water eluting agent is by volume from adsorption column eluting, in the rotary evaporator that the eluent obtaining is sold with trade name RE-301 type rotary evaporator in Guangzhou Xing Shuo Instrument Ltd., under the condition of pressure 0.002-0.098MPa, carry out distilling under reduced pressure and obtain jasminoidin,
D, prepare spirulina polysaccharide and spirulina polypeptide
In the low temperature biomixer that company of fresh spirulina You Guangdong Juneng Biology & Technology Co., Ltd. is sold with trade name JN-02C low temperature continuous flow cell disintegrating machine, under 6 ℃ of cryogenic conditions, process 18 minutes, the treatment fluid obtaining carries out centrifugal treating through the low temperature supercentrifuge of being sold with trade name XPN-80 supercentrifuge by company of U.S. Beckman Coulter Inc. again under 5 ℃ of conditions of temperature, then use the filter at low temperature equipment of being sold with trade name LT600 insulation jacket filter by Dongguan Long Tian filter plant company limited to filter under the condition of 3 ℃ of temperature, then under the condition of 2 ℃ of temperature, use and by Hydranautics, take the permeable membrane that molecular cut off that trade name QUALSEP DairyRO series concentrating and separating film sells is 10kD and carry out membrane permeation processing, obtain spirulina polysaccharide and spirulina polypeptide,
E, preparation chitosan spray
The modification of chitosan that 2.8 weight portions are obtained in steps A is dissolved in 10 weight portion concentration by weight in 1.1% aqueous acetic acid, then toward the polysorbate60 that adds in resulting solution 1.2 weight portions to be sold with trade name T-60 by Jiangsu Hai'an Petrochemical Plant, the lauroylamidopropyl betaine that 1.0 weight portions are sold with trade name CAB35 by upper marine Xiang Fine Chemical Co., Ltd, mix homogeneously, the jasminoidin that adds again 0.8 weight portion to obtain at step C, the Fructus Gardeniae oil that 0.4 weight portion obtains at step B, the spirulina polypeptide that 0.2 weight portion obtains at step D, the spirulina polysaccharide that 0.3 weight portion obtains at step D, mix homogeneously, finally add 0.2 weight portion pi-allyl tributyl bromide phosphine, with distilled water, its gross weight is reached to 100 weight portions.
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 99.1% to the antibacterial ability of staphylococcus aureus, escherichia coli, streptococcus, bacillus pyocyaneus.
Embodiment 5: prepare antibacterial modified chitosan spray
The implementation step of this embodiment is as follows:
A, prepare modification of chitosan
By Jinan Haidebei Marine Organism Engineering Co., Ltd., with trade name food pharmaceutical grade chitosan, sold, deacetylation 80%, molecular weight 24 * 10
4the chitosan of Da, in 1.6% aqueous acetic acid by weight, under the condition of low whipping speed 270rpm, dissolve 10min, be incorporated as again two t-amyl peroxy things of 2.5 times of chitosan weight, 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, supersound process 42min under the condition that is 200W at supersonic frequency 22kHz and ultrasonic power, obtain low-molecular weight chitoglycan complex solution, polyacrylonitrile ultrafiltration film molecular retention and classification through being sold with trade name UFbIA250-PAN film by Zhaoyuan Jin Huimo Science and Technology Ltd. again, obtaining molecular weight is the chitosan below 500Da, this chitosan is added to by weight in 45% potassium hydroxide aqueous solution, under the condition of 105 ℃ of temperature, process 12min, then with 3.0N aqueous hydrochloric acid solution, neutralize, filtration, distilled water wash, under the condition of temperature 60 C, be dried, obtain deacetylation 100%, molecular weight is the modification of chitosan below 500Da,
B, prepare Fructus Gardeniae oil
In 105 weight portion Fructus Gardeniae powder, add 820 weight portion petroleum hydrocarbons, then supersound process 45min under the condition that to be take in the ultrasonic washing unit that trade name YD1008 ultrasonic washing unit sells at supersonic frequency 22kHz and ultrasonic power be 200W by Changzhou You Da ultrasonic equipment company limited, filtration obtains filtrate and filtering residue, described filtering residue then repeats supersound extraction 2 times with 500 weight portion petroleum ether with the same manner, filtrate merges, adopt heating in water bath mode under the condition of temperature 70 C, to remove the petroleum hydrocarbon in merging filtrate, obtain Fructus Gardeniae oil;
C, prepare jasminoidin
In 100 weight portion Fructus Gardeniae powder, add 1000 weight portions, 75% ethanol water by volume, then in the ultrasonic washing unit of being sold with trade name YD1008 ultrasonic washing unit by Changzhou You Da ultrasonic equipment company limited, supersound process 45min under the condition that is 200W at supersonic frequency 22kHz and ultrasonic power, filtration obtains filtrate and filtering residue, described filtering residue then repeats supersound extraction 3 times with the same manner, filtrate merges, then at flow velocity, be by the LX-60 type resin macroporous adsorptive resins of being sold with trade name macroporous resin by Xi'an Sunresin New Materials Co., Ltd. under the conditions of 25 microlitre/seconds, then under the flow velocity condition of 37 microlitre/seconds, pass through the polyamide column of being sold with trade name polyamide by the biochemical plastic molding and processing plant of Taizhou City of Zhejiang Province road and bridge tetramethyl, then working concentration 20% ethanol water eluting agent is by volume from adsorption column eluting, in the rotary evaporator that the eluent obtaining is sold with trade name RE-301 type rotary evaporator in Guangzhou Xing Shuo Instrument Ltd., under the condition of pressure 0.002-0.098MPa, carry out distilling under reduced pressure and obtain jasminoidin,
D, prepare spirulina polysaccharide and spirulina polypeptide
In the low temperature biomixer that company of fresh spirulina You Guangdong Juneng Biology & Technology Co., Ltd. is sold with trade name JN-02C low temperature continuous flow cell disintegrating machine, under 6 ℃ of cryogenic conditions, process 18 minutes, the treatment fluid obtaining carries out centrifugal treating through the low temperature supercentrifuge of being sold with trade name XPN-80 supercentrifuge by company of U.S. Beckman Coulter Inc. again under 5 ℃ of conditions of temperature, then use the filter at low temperature equipment of being sold with trade name LT600 insulation jacket filter by Dongguan Long Tian filter plant company limited to filter under the condition of 3 ℃ of temperature, then under the condition of 2 ℃ of temperature, use and by Hydranautics, take the permeable membrane that molecular cut off that trade name QUALSEP DairyRO series concentrating and separating film sells is 10kD and carry out membrane permeation processing, obtain spirulina polysaccharide and spirulina polypeptide,
E, preparation chitosan spray
The modification of chitosan that 2.6 weight portions are obtained in steps A is dissolved in 10 weight portion concentration by weight in 1.1% aqueous acetic acid, then toward the polysorbate60 that adds in resulting solution 1.0 weight portions to be sold with trade name T-60 by Jiangsu Hai'an Petrochemical Plant, the lauroylamidopropyl betaine that 1.0 weight portions are sold with trade name CAB35 by upper marine Xiang Fine Chemical Co., Ltd, mix homogeneously, the jasminoidin that adds again 0.3 weight portion to obtain at step C, the Fructus Gardeniae oil that 0.4 weight portion obtains at step B, the spirulina polypeptide that 0.1 weight portion obtains at step D, the spirulina polysaccharide that 0.2 weight portion obtains at step D, mix homogeneously, finally add 0.3 weight portion pi-allyl tributyl bromide phosphine, with distilled water, its gross weight is reached to 100 weight portions.
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 6: prepare antibacterial modified chitosan spray
The implementation step of this embodiment is as follows:
A, prepare modification of chitosan
By Jinan Haidebei Marine Organism Engineering Co., Ltd., with trade name food pharmaceutical grade chitosan, sold, deacetylation 80%, molecular weight 24 * 10
4the chitosan of Da, in 1.6% aqueous acetic acid by weight, under the condition of low whipping speed 270rpm, dissolve 10min, be incorporated as again two t-amyl peroxy things of 2.5 times of chitosan weight, 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, supersound process 42min under the condition that is 200W at supersonic frequency 22kHz and ultrasonic power, obtain low-molecular weight chitoglycan complex solution, polyacrylonitrile ultrafiltration film molecular retention and classification through being sold with trade name UFbIA250-PAN film by Zhaoyuan Jin Huimo Science and Technology Ltd. again, obtaining molecular weight is the chitosan below 500Da, this chitosan is added to by weight in 35% potassium hydroxide aqueous solution, under the condition of 105 ℃ of temperature, process 12min, then with 3.0N aqueous hydrochloric acid solution, neutralize, filtration, distilled water wash, under the condition of temperature 60 C, be dried, obtain deacetylation 99%, molecular weight is the modification of chitosan below 500Da,
B, prepare Fructus Gardeniae oil
In 90 weight portion Fructus Gardeniae powder, add 900 weight portion petroleum hydrocarbons, then supersound process 35min under the condition that to be take in the ultrasonic washing unit that trade name YD1008 ultrasonic washing unit sells at supersonic frequency 22kHz and ultrasonic power be 200W by Changzhou You Da ultrasonic equipment company limited, filtration obtains filtrate and filtering residue, described filtering residue then repeats supersound extraction 2 times with 500 weight portion petroleum ether with the same manner, filtrate merges, adopt heating in water bath mode to remove the petroleum hydrocarbon in merging filtrate under the condition of 90 ℃ of temperature, obtain Fructus Gardeniae oil;
C, prepare jasminoidin
In 120 weight portion Fructus Gardeniae powder, add 1200 weight portions, 74% ethanol water by volume, then in the ultrasonic washing unit of being sold with trade name YD1008 ultrasonic washing unit by Changzhou You Da ultrasonic equipment company limited, supersound process 38min under the condition that is 200W at supersonic frequency 22kHz and ultrasonic power, filtration obtains filtrate and filtering residue, described filtering residue then repeats supersound extraction 2 times with the same manner, filtrate merges, then at flow velocity, be by the LX-20 type resin macroporous adsorptive resins of being sold with trade name macroporous resin by Xi'an Sunresin New Materials Co., Ltd. under the conditions of 23 microlitre/seconds, then under the flow velocity condition of 35 microlitre/seconds, pass through the polyamide column of being sold with trade name polyamide by the biochemical plastic molding and processing plant of Taizhou City of Zhejiang Province road and bridge tetramethyl, then working concentration 25% ethanol water eluting agent is by volume from adsorption column eluting, in the rotary evaporator that the eluent obtaining is sold with trade name RE-301 type rotary evaporator in Guangzhou Xing Shuo Instrument Ltd., under the condition of pressure 0.002-0.098MPa, carry out distilling under reduced pressure and obtain jasminoidin,
D, prepare spirulina polysaccharide and spirulina polypeptide
In the low temperature biomixer that company of fresh spirulina You Guangdong Juneng Biology & Technology Co., Ltd. is sold with trade name JN-02C low temperature continuous flow cell disintegrating machine, under 4 ℃ of cryogenic conditions, process 14 minutes, the treatment fluid obtaining carries out centrifugal treating through the low temperature supercentrifuge of being sold with trade name XPN-80 supercentrifuge by company of U.S. Beckman Coulter Inc. again under 6 ℃ of conditions of temperature, then use the filter at low temperature equipment of being sold with trade name LT600 insulation jacket filter by Dongguan Long Tian filter plant company limited to filter under the condition of 5 ℃ of temperature, then under the condition of 8 ℃ of temperature, use and by Hydranautics, take the permeable membrane that molecular cut off that trade name QUALSEP DairyRO series concentrating and separating film sells is 10kD and carry out membrane permeation processing, obtain spirulina polysaccharide and spirulina polypeptide,
E, preparation chitosan spray
The modification of chitosan that 3.0 weight portions are obtained in steps A is dissolved in 8 weight portion concentration by weight in 1.0% aqueous acetic acid, then toward the polysorbate60 that adds in resulting solution 1.1 weight portions to be sold with trade name T-60 by Jiangsu Hai'an Petrochemical Plant, the lauroylamidopropyl betaine that 1.2 weight portions are sold with trade name CAB35 by upper marine Xiang Fine Chemical Co., Ltd, mix homogeneously, the jasminoidin that adds again 0.4 weight portion to obtain at step C, the Fructus Gardeniae oil that 0.1 weight portion obtains at step B, the spirulina polypeptide that 0.4 weight portion obtains at step D, the spirulina polysaccharide that 0.3 weight portion obtains at step D, mix homogeneously, finally add 0.2 weight portion pi-allyl tributyl bromide phosphine, with distilled water, its gross weight is reached to 100 weight portions.
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 99.6% to the antibacterial ability of staphylococcus aureus, escherichia coli, streptococcus, bacillus pyocyaneus.
Claims (10)
1. a preparation method for antibacterial modified chitosan spray, is characterized in that the step of this preparation method is as follows:
A, prepare modification of chitosan
By deacetylation 80%, molecular weight 20 * 10
4～30 * 10
4the chitosan of Da is dissolved in by weight in 1.0～3.0% aqueous acetic acids, be incorporated as again two t-amyl peroxy things of 1～3 times of chitosan weight, the solution obtaining carries out supersound process in ultrasonic washing unit, obtain low-molecular weight chitoglycan complex solution, pass through polyacrylonitrile ultrafiltration film molecular retention and classification, obtaining molecular weight is the chitosan below 500Da again; This chitosan is added to by weight in 35～45% potassium hydroxide aqueous solutions, under the condition of 105～115 ℃ of temperature, process 10～20min, then with 1.0～3.0N aqueous hydrochloric acid solution, neutralize, filtration, distilled water wash, be dried, obtain deacetylation 99～100%, molecular weight is the modification of chitosan below 500Da;
B, prepare Fructus Gardeniae oil
In 80～120 weight portion Fructus Gardeniae powder, add 700～900 weight portion petroleum hydrocarbons, then in ultrasonic washing unit, carry out supersound extraction, filtration obtains filtrate and filtering residue, described filtering residue then repeats supersound extraction 2～3 times with 500～700 weight portion petroleum ether with the same manner, filtrate merges, adopt heating in water bath mode to remove the petroleum hydrocarbon in merging filtrate under the condition of 60～90 ℃ of temperature, obtain Fructus Gardeniae oil;
C, prepare jasminoidin
In 80～120 weight portion Fructus Gardeniae powder, add 800～1200 weight portions, 70～80% ethanol waters by volume, then in ultrasonic washing unit, carry out supersound extraction, filtration obtains filtrate and filtering residue, described filtering residue then repeats supersound extraction 2～3 times with the same manner, filtrate merges, then under being the conditions of 20～30 microlitre/seconds, flow velocity passes through polyamide column by nonpolarity macroporous adsorptive resins chromatographic column with under the flow velocity condition of 30～37 microlitre/seconds, then working concentration 15～25% ethanol water eluting agent are by volume from adsorption column eluting, the eluent obtaining is processed and is obtained jasminoidin in rotary evaporator under the condition of distilling under reduced pressure,
D, prepare spirulina polysaccharide and spirulina polypeptide
Fresh spirulina is processed 12～18 minutes in low temperature biomixer under 4 ℃～6 ℃ cryogenic conditions, the treatment fluid obtaining carries out centrifugal treating through low temperature supercentrifuge again under 4 ℃～6 ℃ conditions of temperature, then use filter at low temperature equipment to filter under the condition of 2 ℃～5 ℃ of temperature, then under the condition of 2 ℃～8 ℃ of temperature, use the permeable membrane that molecular cut off is 10kD to carry out membrane permeation processing, obtain spirulina polysaccharide and spirulina polypeptide;
E, preparation chitosan spray
The modification of chitosan that 2.5～3.2 weight portions are obtained in steps A is dissolved in 6～15 weight portion concentration by weight in 0.8～1.2% aqueous acetic acid, then in resulting solution, add 0.8～1.2 weight portion polysorbate60, 0.8～1.2 weight portion lauroylamidopropyl betaine, mix homogeneously, the jasminoidin that adds again 0.3～0.8 weight portion to obtain at step C, the Fructus Gardeniae oil that 0.1～0.4 weight portion obtains at step B, the spirulina polypeptide that 0.1～0.4 weight portion obtains at step D, the spirulina polysaccharide that 0.1～0.4 weight portion obtains at step D, mix homogeneously, finally add 0.1～0.4 weight portion pi-allyl tributyl bromide phosphine, with distilled water, its gross weight is reached to 100 weight portions.
2. preparation method according to claim 1, is characterized in that in steps A, under the condition of deacetylation 80% 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, and described filtering residue is when the 1st supersound extraction, and the weight ratio of Fructus Gardeniae powder and petroleum hydrocarbon is 90～110:750～850; When the 2nd time or the 3rd supersound extraction, the weight ratio of Fructus Gardeniae powder and petroleum hydrocarbon is 90～110:550～650.
5. preparation method according to claim 1, is characterized in that in step C, and described macroporous adsorbent resin is nonpolar D101, LX-60 or the LX-20 type resin being prepared by styrene and divinylbenzene combined polymerization; Described polyamide is by caprolactam or adipic acid and the synthetic polyphosphazene polymer amide preparing of hexamethylene diamine.
6. preparation method according to claim 1, is characterized in that in step C, and the eluant of described macroporous adsorptive resins or the eluant of described polyamide column are concentration 18～22% ethanol waters by volume.
7. preparation method according to claim 1, is characterized in that in step C, and described permeable membrane is the permeable membrane of being prepared by polyether sulfone, Triafol T or regenerated cellulose.
8. preparation method according to claim 1, is characterized in that in step D, and the rotating speed of described low temperature supercentrifuge is 20000～30000 revs/min.
9. preparation method according to claim 1, is characterized in that the weight ratio of modification of chitosan, polysorbate60, lauroylamidopropyl betaine, jasminoidin, Fructus Gardeniae oil, spirulina polypeptide, spirulina polysaccharide and pi-allyl tributyl bromide phosphine is 2.8～3.0:0.85～1.12:0.85～1.12:0.45～0.65:0.15～0.24:0.15～0.26:0.15～0.25:0.15～0.24.
10. the antibacterial modified chitosan spray obtaining according to preparation method described in any one claim in claim 1-9, is characterized in that it reaches more than 99% the antibacterial ability of staphylococcus aureus, escherichia coli, escherichia coli, streptococcus, Candida albicans, bacillus pyocyaneus or other fungus.
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| CN104707129A (en) * | 2015-03-27 | 2015-06-17 | 严锋 | Ionic polymer based antibacterial spray |
| CN104957190A (en) * | 2015-07-01 | 2015-10-07 | 荆永正 | Sterilizing agent for livestock breeding as well as preparation method and application thereof |
| CN105418779A (en) * | 2015-09-10 | 2016-03-23 | 周玥 | Spirulina polysaccharide extraction process and applications thereof |
| CN105670335A (en) * | 2015-12-31 | 2016-06-15 | 江门市林业科学研究所 | Method for two-pot two stage countercurrent dynamic extraction of gardenia yellow pigment |
| CN106974290A (en) * | 2017-05-22 | 2017-07-25 | 福建海唯美海洋生物科技有限公司 | A kind of health-preserving food for preventing and treating intractable oral cavity ulcer |
| CN110050825A (en) * | 2019-05-24 | 2019-07-26 | 邓光 | Nutrition blueberry dried fruit and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104707129A (en) * | 2015-03-27 | 2015-06-17 | 严锋 | Ionic polymer based antibacterial spray |
| CN104957190A (en) * | 2015-07-01 | 2015-10-07 | 荆永正 | Sterilizing agent for livestock breeding as well as preparation method and application thereof |
| CN105418779A (en) * | 2015-09-10 | 2016-03-23 | 周玥 | Spirulina polysaccharide extraction process and applications thereof |
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