CN104784743A - Preparation method for aromatic and bacteriostatic chitosan-based wound dressing - Google Patents
Preparation method for aromatic and bacteriostatic chitosan-based wound dressing Download PDFInfo
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Abstract
The invention discloses a preparation method for aromatic and bacteriostatic chitosan-based wound dressing. The preparation method comprises the following steps: mixing tea tree essential oil, menthol and folium artemisiae argyi essential oil according to a certain proportion to obtain a natural aromatic bacteriostatic agent; coating lipidosome with the natural aromatic bacteriostatic agent to obtain aromatic and bacteriostatic lipidosome; dispersing the aromatic and bacteriostatic lipidosome into a chitosan-sodium alginate-gelatin solution, and performing freeze drying according to certain process to obtain the aromatic and bacteriostatic chitosan-based wound dressing. The aromatic and bacteriostatic chitosan-based wound dressing is of a porous structure and efficient in bacteria capturing effect, lasting, broad-spectrum, efficient and antibacterial, good in slow release and antibacterial performance, hemostasis, water absorption and gas permeability and good in biocompatibility, has certain mint flavor, and has obvious curative effect in large wounds and burns.
Description
Technical field
The invention belongs to medical material tech field, be specifically related to a kind of preparation method of chitosan-based wound dressing of fragrant bacteriostatic.
Background technology
Chitosan is natural polymer biological polyoses de-acetyl chitin product; there is excellent solvent resistance and alkali resistance; good biocompatibility and skin affinity; biocidal property, film property, breathability, water absorption, moisture retention are good; can stop blooding, promote the advantages such as wound healing, can be used as medical material.But because chitosan fragility is large, poor mechanical property, makes it be used alone and is restricted.At present, lot of documents chitosan and other polymer blended modification is had to obtain the dressing membrane of function admirable.
Tea tree ethereal oil, is the oiliness extract that Australia Melaleuca Alternifolia vanes vapor distillation obtains, has special aromatic odor.Tea tree ethereal oil has significant bacteriostatic activity and antimicrobial spectrum scope widely, to common gram positive bacteria, gram negative bacteria and fungus, all there is strong inhibitory action, side effect and the little unique advantage of residual toxicity, have no stimulation to skin compared with chemical antibacterial.Tea tree ethereal oil have purify air, sterilize, immune, anticorrosion, the purposes such as cytotrophy are provided, can as medical dressing antibacterial safely and effectively.
P-Cymene is the extract of leaf from Folium Artemisiae Argyi, stem, and squeezing and pressing method and solvent extraction method refine the volatile flavor of extraction.The attending effectiveness of P-Cymene, blood of regulating the flow of vital energy, warming the meridian arteries and veins, dispelling cold and dampness, pain relieving, antibacterial, antiinflammatory, excitation digestive gland, relieving cough and reducing sputum, short circulation, QI invigorating, promotes immunity.
Menthol, organic compound, colorless needle crystals or granular.For the main component in Herba Menthae and lavender quintessence oil, exist with the state of ester with free.Menthol has 8 kinds of isomers, they in fragrance matter different, levorotatory menthol has Herba Menthae fragrance and has refrigerant effect, and racemization menthol also has refrigerant effect, and other isomer is without refrigerant effect.Can be used as the odorant of toothpaste, perfume, beverage and confection etc.Being pharmaceutically used as excitants, acting on skin or mucosa, having refrigerant itching-relieving action; For oral administration can be used for, has a headache and nose, pharynx, laryngitis etc.
But the oxidation product of quintessence oil can cause skin allergy, therefore plants essential oil and component thereof are encapsulated by liposome technology, prepare the antibacterial with good anti-microbial property of stable in properties.In addition, liposome cannot be detained at large-area skin with suspensions, needs to be fixed in a kind of timbering material to continue to play antibacterial effect.Therefore, quintessence oil liposome is joined in chitin-sodium alginate-gelatin solution, obtain the chitosan-based wound dressing of fragrant bacteriostatic by certain procedures lyophilizing, there is important using value and development prospect.
A kind of chitosan-based electrostatic spinning composite wound dressing and preparation method thereof is disclosed in patent of invention ZL201310574818.X.The method adopts the chitosan nano fiber of method of electrostatic spinning preparation containing plants essential oil to be combined into composite wound dressing with chitosan casting films again.Method is simple to operate, dressing good biocompatibility, environmental friendliness, do not add too much auxiliary agent, organic solvent, to human body skin also nonirritant, there is certain plant fragrance taste, stronger biocidal property, good slow-releasing, to a certain degree can hide the abnormal flavour that wound suppuration produces, can also accelerate to eliminate the nervous of patient, relieving stress, pleasure, meets the spiritual enjoyment of people.Comfortableness also improves greatly, dressing is fitted skin more, is well suited for the treatment of wounds of joint part, the pain that when can reduce the wounded's joint motions, skin stretch is brought.But what this dressing adopted is dissolution type sterilization mechanism, and the release of plant-derived essential oil makes antibacterial action time shorter.And diffuse into wound fluid and may reduce essential oil concentration, the effect of impact sterilization.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of novel processing step of chitosan-based wound dressing of fragrant bacteriostatic, the maintenance fungicidal effectiveness that the chitosan-based wound dressing that the method prepares can be long-term.
For solving the problems of the technologies described above, the technical solution used in the present invention is as follows:
A preparation method for the chitosan-based wound dressing of fragrant bacteriostatic, the method comprises the steps:
(1) by tea tree ethereal oil, menthol and P-Cymene mix and blend at low temperatures, be dissolved in phosphate buffered solution, obtain natural aromatic antibacterial;
(2) with the ratio of every 125mg soybean lecithin and cholesterol gross mass and 10ml natural aromatic antibacterial, thin film aquation legal system is adopted to obtain Liposomal suspensions;
(3) Liposomal suspensions is added pre-configured chitin-sodium alginate-gelatin solution, then add sucrose as stabilizing agent, low temperature fully stirs and obtains homogeneous liquid; Liquid is applied to polyfluortetraethylene plate surface, places 2h and make it launch completely;
(4) polyfluortetraethylene plate scribbling liquid is put into vacuum freezing drying oven,-5 DEG C of pre-freeze 6h, then be cooled to-55 ~-80 DEG C (speed being preferably 5 DEG C/h is cooled to-80 DEG C) with the speed of 1 ~ 10 DEG C/h, evacuation maintains below 0.012mBar again, lyophilization 72 ~ 100h (being preferably 90h), obtains the chitosan-based wound dressing of fragrant bacteriostatic.
In step (1), the mass ratio of described tea tree ethereal oil, menthol and P-Cymene is 1:1:1, and described cryogenic temperature is 4 DEG C, and speed of agitator is 60 revs/min.
In step (1), phosphate buffer solution is prepared as follows and is obtained: sodium chloride 8g/L, potassium chloride 0.2g/L, sodium hydrogen phosphate 1.44g/L, dipotassium hydrogen phosphate 0.24g/L, solvent is water, with hydrochloric acid adjust pH to 6.5, add the Tween 80 that mass fraction is 6%.
In step (1), the mixture of tea tree ethereal oil, menthol and P-Cymene adds phosphate buffer solution with the concentration of 0.2 ~ 2g/100mL, is preferably 1g/100mL.
In step (2), the mass ratio of soybean lecithin and cholesterol is 4:1.
In step (2), described thin film aquation method is: pour in round-bottomed flask after soybean lecithin and cholesterol are dissolved in chloroform, at room temperature revolves steaming to bottle wall and forms the homogeneous thin film of one deck; Phosphate buffer solution 20ml being added natural antibacterial agent in 55 DEG C of ultrasonic water bath is preheated to 55 DEG C, then adds and be covered with in the round-bottomed flask of thin film, and sonic oscillation 10 minutes, supersonic frequency is 400MHz, and frequency of oscillation is 200 revs/min.
In step (3), described chitin-sodium alginate-gelatin solution, is be dissolved in 1%v/v acetic acid aqueous solution by the mixture of chitosan, sodium alginate and gelatin with the concentration of 4g/100mL, stirs at 4 DEG C, adjust pH to 6.5 and get final product; Wherein, the mass ratio of chitosan, sodium alginate and gelatin is 2 ~ 4:1:1 (being preferably 3:1:1), and chitosan mean molecule quantity is 500kDa, and deacetylation is 85%.
In step (3), the volume ratio of Liposomal suspensions and chitin-sodium alginate-gelatin solution is 1:1 ~ 3 (being preferably 1:2).
In step (3), the addition of sucrose counts 2g/100mL with the volume of mixture of Liposomal suspensions and chitin-sodium alginate-gelatin solution.
In step (3), low temperature fully stirs and obtains homogeneous liquid, and cryogenic temperature is 4 ~ 8 DEG C (being preferably 4 DEG C); Speed of agitator is 100 ~ 200 revs/min (being preferably 150 revs/min).
The chitosan-based wound dressing of the fragrant bacteriostatic that the present invention obtains.This wound dressing has lastingly, wide spectrum, efficiently antibacterial effect, possesses good sustained-release antibacterial, hemostatic, water absorption and permeability, good biocompatibility, and with certain mint flavored, has obvious curative effects to large-scale wound and burn.
Beneficial effect: preparation method of the present invention compared with prior art, has the following advantages:
1, the advantage of chitosan and plants essential oil liposome is combined, in conjunction with the anastalsis of chitosan and the fragrant bacteriostatic effect of plants essential oil.Obtained wound dressing anastalsis is obvious, and antibacterial activity is strong, and broad-spectrum antibacterial effect is remarkable; The chitosan dressing of preparation has certain mint flavored, to a certain degree can optimize the environment, purify air, and can also accelerate to eliminate the nervous of people, relieving stress, pleasure, meets the spiritual enjoyment of people.
2, compared with other wound dressings, its preparation technology is relatively simple, and good biocompatibility, meets the theory of green, environmental protection; Replace quintessence oil directly to mix obtained chitosan-based material with liposome technology, keep remarkable antibacterial effect, while lasting release fragranced, more reduce the stimulation that quintessence oil causes human body skin.
3, the chitosan-based wound dressing adopting lyophilizing mode obtained, duct is more, and specific surface area is comparatively large, and quintessence oil liposome is bonded in polymeric media, can not carry out arranging the water absorption and the breathability that affect himself in duct, aroma release time so also can be made more lasting.
4, material can obtain more evenly abundant pore passage structure by program lyophilizing mode than anxious freezing, the antibacterial of surface band negative charge is caught by the exposed absorption of the amino of chitosan positive charge on surface in these ducts, and then utilize quintessence oil liposome to merge, thus kill bacteria, namely catch fusion sterilization mechanism.The defect that the quintessence oil this overcoming patent of invention ZL201310574818.X stripping is diluted by wound fluid, maintenance fungicidal effectiveness that can be long-term.Abundant duct is not had in wound dressing prepared by ZL201310574818.X.
Accompanying drawing explanation
Fig. 1 is the chitosan-based wound dressing A cross-sectional scans Electronic Speculum figure obtained by embodiment 1.
Fig. 2 is the specific surface area of chitosan-based wound dressing of the present invention, in figure, A is the specific surface area of embodiment 1, B is the specific surface area of embodiment 2, C is the specific surface area of embodiment 3, and D is the specific surface area of comparative example 1, and E is the specific surface area of comparative example 2, F is the specific surface area of comparative example 3, and G, H are the specific surface area of commercially available two kinds of dressing.
Fig. 3 is the coagulating effectiveness measurement result of chitosan-based wound dressing of the present invention and commercially available two kinds of dressing, in figure, A is the coagulating effectiveness of embodiment 1, B is the coagulating effectiveness of embodiment 2, C is the coagulating effectiveness of embodiment 3, and D is the coagulating effectiveness of comparative example 1, and E is the coagulating effectiveness of comparative example 2, F is the coagulating effectiveness of comparative example 3, and G, H are the coagulating effectiveness of commercially available two kinds of dressing.
Fig. 4 is the quintessence oil release profiles of chitosan-based wound dressing of the present invention, in figure, A is the quintessence oil release profiles of embodiment 1, B is the quintessence oil release profiles of embodiment 2, C is the quintessence oil release profiles of embodiment 3, D is the quintessence oil release profiles of comparative example 1, and E is the quintessence oil release profiles of comparative example 2, and F is the quintessence oil release profiles of comparative example 3.
Fig. 5 is the instantaneous thalline clearance rate measurement result of chitosan-based wound dressing of the present invention and commercially available two kinds of dressing, in figure, A is the instantaneous thalline clearance rate of embodiment 1, B is the instantaneous thalline clearance rate of embodiment 2, C is the instantaneous thalline clearance rate of embodiment 3, and D is the instantaneous thalline clearance rate of comparative example 1, and E is the instantaneous thalline clearance rate of comparative example 2, F is the instantaneous thalline clearance rate of comparative example 3, and G, H are the instantaneous thalline clearance rate of commercially available two kinds of dressing.
Detailed description of the invention
According to following embodiment, the present invention may be better understood.But those skilled in the art will readily understand, the content described by embodiment only for illustration of the present invention, and should can not limit the present invention described in detail in claims yet.
The mensuration of aroma release time: sample is put into 25 DEG C, air pressure is 1 normal atmosphere, and often spend one week in the environment of humidity 50% and take out mensuration, 5 people carry out subjective assessment, are more than or equal to 3 people and are evaluated as dulcet, then regard as fragrance still in the release stage.
Specific area measuring: adopt specific surface area measuring instrument to measure the specific surface area of dressing.
The mensuration of coagulating effectiveness: the chitosan-based wound dressing of equivalent is put into polypropylene tube, preincubate to 37 DEG C.Utilize the whole blood 0.2ml of citric acid treatment to join in pipe, then add 20 μ l 0.2mol/l calcium chloride solutions.Then hatch at pipe being put into 37 DEG C, 30 revs/min of vibrations, do not have captured erythrocyte 25ml to wash after 10 minutes, measure absorbance at 540nm.
The mensuration of quintessence oil release profiles: utilize the release performance of ultraviolet spectrophotometry to chitosan-based wound dressing to measure.The chitosan-based wound dressing accurately taking 0.1g is placed in 50ml 0.01mol/l pH7.4 phosphate buffer (PBS) vibration.Ultraviolet spectrophotometer is used to be determined at the chitosan film extraction solution absorbance of different time in PBS buffer at 265nm place.Take absorbance as vertical coordinate, the time is abscissa, makes the release profiles of chitosan-based wound dressing.
Instantaneous thalline adsorption experiment: in 24 orifice plates, every hole adds 1.5ml concentration 10
8-10
9cfu/ml Candida albicans bacteria suspension, puts into the disc dressing being cut into diameter 1cm, and vibration 5min, takes out dressing.The cell concentration of remaining liq is calculated with blood counting chamber.
Biocidal property is tested: test strain is escherichia coli, staphylococcus aureus and Candida albicans.First chitosan-based wound dressing is cut into the disk that diameter is about 5mm respectively, and through uviol lamp sterilizing, then draws 0.1mL concentration 10
4-10
5cfu/ml bacteria suspension is coated on solid medium plate, is then attached to various containing on bacterium plate with aseptic nipper gripping chitosan-based lyophilizing diaphragm, is placed on after cultivating 18-24h in the incubator of 37 DEG C, measures antibacterial circle diameter.
Embodiment 1:
A kind of preparation method of chitosan-based wound dressing of fragrant bacteriostatic:
(1) by tea tree ethereal oil, menthol and P-Cymene with mass ratio be 1:1:1 at 4 DEG C with 60 revs/min of stirrings.By 8g sodium chloride, 0.2 potassium chloride g/L, 1.44g sodium hydrogen phosphate, 0.24g dipotassium hydrogen phosphate, joins in 800ml water, and stir and make abundant dissolving, with hydrochloric acid adjust pH to 6.5, supplementing water, to 1000ml, adds 60g Tween 80, obtains phosphate buffer solution.Blend of essential oils is added phosphate buffer solution with the concentration of 1g/100mL and namely obtains natural aromatic antibacterial;
(2) pour in round-bottomed flask after 100mg soybean lecithin and 25mg cholesterol being dissolved in chloroform, at room temperature revolve steaming to bottle wall and form the homogeneous thin film of one deck; In 55 DEG C of ultrasonic water bath, 10ml natural aromatic antibacterial is preheated to 55 DEG C, then adds and be covered with in the round-bottomed flask of thin film, sonic oscillation 10 minutes, supersonic frequency is 400MHz, and frequency of oscillation is 200 revs/min, obtained Liposomal suspensions;
(3) be 500kDa by mean molecule quantity, deacetylation be 85% chitosan, sodium alginate and gelatin mix with mass ratio 3:1:1, be dissolved in 1%v/v acetic acid aqueous solution with the concentration of 4%w/v, stir at 4 DEG C, namely adjust pH to 6.5 obtains chitin-sodium alginate-gelatin solution.With 1:2 volume ratio, Liposomal suspensions is mixed with chitin-sodium alginate-gelatin solution, add the sucrose of cumulative volume 2g/100mL, at 4 DEG C, stir under 150 revs/min and obtain homogeneous liquid; Liquid is applied to polyfluortetraethylene plate surface, places 2h and make it launch completely.
(4) polyfluortetraethylene plate scribbling liquid is put into vacuum freezing drying oven,-5 DEG C of pre-freeze 6h, be then cooled to-80 DEG C with the speed of 5 DEG C/h, then evacuation maintain below 0.012mBar, lyophilization 90h, finally obtains the chitosan-based wound dressing A of fragrant bacteriostatic.
Embodiment 2:
A kind of preparation method of chitosan-based wound dressing of fragrant bacteriostatic:
(1) by tea tree ethereal oil, menthol and P-Cymene with mass ratio be 1:1:1 at 4 DEG C with 60 revs/min of stirrings.By 8g sodium chloride, 0.2 potassium chloride g/L, 1.44g sodium hydrogen phosphate, 0.24g dipotassium hydrogen phosphate, joins in 800ml water, and stir and make abundant dissolving, with hydrochloric acid adjust pH to 6.5, supplementing water, to 1000ml, adds 60g Tween 80, obtains phosphate buffer solution.Blend of essential oils is added phosphate buffer solution with the concentration of 0.2g/100mL and namely obtains natural aromatic antibacterial;
(2) pour in round-bottomed flask after 100mg soybean lecithin and 25mg cholesterol being dissolved in chloroform, at room temperature revolve steaming to bottle wall and form the homogeneous thin film of one deck; In 55 DEG C of ultrasonic water bath, 10ml natural aromatic antibacterial is preheated to 55 DEG C, then adds and be covered with in the round-bottomed flask of thin film, sonic oscillation 10 minutes, supersonic frequency is 400MHz, and frequency of oscillation is 200 revs/min, obtained Liposomal suspensions;
(3) be 500kDa by mean molecule quantity, deacetylation be 85% chitosan, sodium alginate and gelatin mix with mass ratio 2:1:1, be dissolved in 1%v/v acetic acid aqueous solution with the concentration of 4%w/v, stir at 4 DEG C, namely adjust pH to 6.5 obtains chitin-sodium alginate-gelatin solution.With 1:1 volume ratio, Liposomal suspensions is mixed with chitin-sodium alginate-gelatin solution, add the sucrose of cumulative volume 2g/100mL, at 4 DEG C, stir under 150 revs/min and obtain homogeneous liquid; Liquid is applied to polyfluortetraethylene plate surface, places 2h and make it launch completely.
(4) polyfluortetraethylene plate scribbling liquid is put into vacuum freezing drying oven,-5 DEG C of pre-freeze 6h, be then cooled to-55 DEG C with the speed of 1 DEG C/h, then evacuation maintain below 0.012mBar, lyophilization 72h, finally obtains the chitosan-based wound dressing B of fragrant bacteriostatic.
Embodiment 3:
A kind of preparation method of chitosan-based wound dressing of fragrant bacteriostatic:
(1) by tea tree ethereal oil, menthol and P-Cymene with mass ratio be 1:1:1 at 4 DEG C with 60 revs/min of stirrings.By 8g sodium chloride, 0.2 potassium chloride g/L, 1.44g sodium hydrogen phosphate, 0.24g dipotassium hydrogen phosphate, joins in 800ml water, and stir and make abundant dissolving, with hydrochloric acid adjust pH to 6.5, supplementing water, to 1000ml, adds 60g Tween 80, obtains phosphate buffer solution.Blend of essential oils is added phosphate buffer solution with the concentration of 2g/100mL and namely obtains natural aromatic antibacterial;
(2) pour in round-bottomed flask after 100mg soybean lecithin and 25mg cholesterol being dissolved in chloroform, at room temperature revolve steaming to bottle wall and form the homogeneous thin film of one deck; In 55 DEG C of ultrasonic water bath, 10ml natural aromatic antibacterial is preheated to 55 DEG C, then adds and be covered with in the round-bottomed flask of thin film, sonic oscillation 10 minutes, supersonic frequency is 400MHz, and frequency of oscillation is 200 revs/min, obtained Liposomal suspensions;
(3) be 500kDa by mean molecule quantity, deacetylation be 85% chitosan, sodium alginate and gelatin mix with mass ratio 4:1:1, be dissolved in 1%v/v acetic acid aqueous solution with the concentration of 4%w/v, stir at 4 DEG C, namely adjust pH to 6.5 obtains chitin-sodium alginate-gelatin solution.With 1:3 volume ratio, Liposomal suspensions is mixed with chitin-sodium alginate-gelatin solution, add the sucrose of cumulative volume 2g/100mL, at 4 DEG C, stir under 150 revs/min and obtain homogeneous liquid; Liquid is applied to polyfluortetraethylene plate surface, places 2h and make it launch completely.
(4) polyfluortetraethylene plate scribbling liquid is put into vacuum freezing drying oven,-5 DEG C of pre-freeze 6h, be then cooled to-80 DEG C with the speed of 10 DEG C/h, then evacuation maintain below 0.012mBar, lyophilization 100h, finally obtains the chitosan-based wound dressing C of fragrant bacteriostatic.
Comparative example 1:
A kind of preparation method of chitosan-based wound dressing of fragrant bacteriostatic:
(1) by tea tree ethereal oil, menthol and P-Cymene with mass ratio be 1:1:1 at 4 DEG C with 60 revs/min of stirrings.By 8g sodium chloride, 0.2 potassium chloride g/L, 1.44g sodium hydrogen phosphate, 0.24g dipotassium hydrogen phosphate, joins in 800ml water, and stir and make abundant dissolving, with hydrochloric acid adjust pH to 6.5, supplementing water, to 1000ml, adds 60g Tween 80, obtains phosphate buffer solution.Blend of essential oils is added phosphate buffer solution with the concentration of 1g/100mL and namely obtains natural aromatic antibacterial;
(2) be 500kDa by mean molecule quantity, deacetylation be 85% chitosan, sodium alginate and gelatin mix with mass ratio 3:1:1, be dissolved in 1%v/v acetic acid aqueous solution with the concentration of 4%w/v, stir at 4 DEG C, namely adjust pH to 6.5 obtains chitin-sodium alginate-gelatin solution.With 1:2 volume ratio, natural aromatic antibacterial is mixed with chitin-sodium alginate-gelatin solution, add the sucrose of cumulative volume 2g/100mL, at 4 DEG C, stir under 150 revs/min and obtain homogeneous liquid; Liquid is applied to polyfluortetraethylene plate surface, places 2h and make it launch completely.
(3) polyfluortetraethylene plate scribbling liquid is put into vacuum freezing drying oven,-5 DEG C of pre-freeze 6h, be then cooled to-80 DEG C with the speed of 5 DEG C/h, then evacuation maintain below 0.012mBar, lyophilization 90h, finally obtains the chitosan-based wound dressing D of fragrant bacteriostatic.
Comparative example 2:
A kind of preparation method of chitosan-based wound dressing of fragrant bacteriostatic:
(1) by tea tree ethereal oil, menthol and P-Cymene with mass ratio be 1:1:1 at 4 DEG C with 60 revs/min of stirrings.By 8g sodium chloride, 0.2 potassium chloride g/L, 1.44g sodium hydrogen phosphate, 0.24g dipotassium hydrogen phosphate, joins in 800ml water, and stir and make abundant dissolving, with hydrochloric acid adjust pH to 6.5, supplementing water, to 1000ml, adds 60g Tween 80, obtains phosphate buffer solution.Blend of essential oils is added phosphate buffer solution with the concentration of 1g/100mL and namely obtains natural aromatic antibacterial;
(2) pour in round-bottomed flask after 100mg soybean lecithin and 25mg cholesterol being dissolved in chloroform, at room temperature revolve steaming to bottle wall and form the homogeneous thin film of one deck; In 55 DEG C of ultrasonic water bath, 10ml natural aromatic antibacterial is preheated to 55 DEG C, then adds and be covered with in the round-bottomed flask of thin film, sonic oscillation 10 minutes, supersonic frequency is 400MHz, and frequency of oscillation is 200 revs/min, obtained Liposomal suspensions;
(3) be 500kDa by mean molecule quantity, deacetylation be 85% chitosan, sodium alginate and gelatin mix with mass ratio 3:1:1, be dissolved in 1%v/v acetic acid aqueous solution with the concentration of 4%w/v, stir at 4 DEG C, namely adjust pH to 6.5 obtains chitin-sodium alginate-gelatin solution.With 1:2 volume ratio, Liposomal suspensions is mixed with chitin-sodium alginate-gelatin solution, add the sucrose of cumulative volume 2g/100mL, at 4 DEG C, stir under 150 revs/min and obtain homogeneous liquid; Liquid is applied to polyfluortetraethylene plate surface, places 2h and make it launch completely.
(4) dry under the polyfluortetraethylene plate room temperature scribbling liquid, finally obtain the chitosan-based wound dressing E of fragrant bacteriostatic.
Comparative example 3:ZL201310574818.X
A preparation method for chitosan-based electrostatic spinning composite wound dressing, comprises the steps:
(1) mixing and stirring in 0.5ml water by 0.5ml tea tree ethereal oil and 0.1g lecithin, ultrasonic disperse is degassed, obtained quintessence oil emulsion;
(2) by 0.75g chitosan, (viscosity-average molecular weight is 5.0 × 10
5, deacetylation is 80 ~ 85%) be dissolved in the acetic acid solution of 50ml 90wt%, add 1ml glycerol as plasticizer, add 1ml quintessence oil emulsion, stirring at room temperature, to dissolving completely, obtains spinning liquid;
(3) be dissolved in by 1g chitosan in the acetic acid solution of 50ml 2wt%, add 1ml glycerol as plasticizer, stirring at room temperature is to dissolving completely, and obtained film forming liquid, utilizes casting filming therapy to obtain chitosan film, take off for subsequent use;
(4) chitosan film is coated on electrostatic spinning dash receiver, spinning liquid is extracted with 10ml syringe (7# tack pin), be fixed on electrostatic spinning apparatus, fixing electrostatic pressure 20KV, receiving range is 7cm, sample rate is 0.3ml/h, at temperature 25 DEG C, carry out electrospinning, obtains quintessence oil chitin fiber granular layer (Fig. 2 is the stereoscan photograph of quintessence oil chitin fiber granular layer).
(5) after electrostatic spinning completes, then one deck chitosan film is covered on quintessence oil chitin fiber granular layer, first with 50 DEG C of compacting 10s, then with 120 DEG C of compacting 10s, obtain chitosan-based electrostatic spinning composite wound dressing F.
The measurement result of dressing aroma release time is as table 1.
The measurement result of table 1 dressing aroma release time
| Sample | Aroma release time/(week) |
| A | 26 |
| B | 27 |
| C | 32 |
| D | 12 |
| E | 10 |
| F | 27 |
The sample of embodiment 1,2,3 has more lasting aroma release time, can better discharge fragrance when it acts on wound as dressing, hides the issuable abnormal flavour of wound microbes effect, makes patient heart more joyful.
Five kinds obtained by above-described embodiment chitosan-based wound dressings containing plants essential oil and commercially available two kinds of wound dressings, its water absorption measures according to YY/T0471.1-2004 standard, moisture-vapor transmission measures according to YY/T0471.2-2004 standard, and result is as table 2.
The water absorption of table 2 wound dressing and moisture-vapor transmission measurement result
| Sample | Water absorption/(gg -1) | Moisture-vapor transmission/(gm -2·d -1) |
| A | 26.72 | 3886 |
| B | 25.98 | 4100 |
| C | 27.17 | 4220 |
| D | 24.50 | 2073 |
| E | 3.03 | 2004 |
| F | 20.00 | 1886 |
| G | 3.49 | 2034 |
| H | 4.93 | 1987 |
Note: G is that the peaceful skin wound healing of art pastes chitosan Wound dressing, brand Ai Beile, Nanchang Hua Kang medical science and technology company limited of manufacturer; H is chitosan medical film, and brand is safe precious, Guangdong Taibao Science and Technology Medical Supplies Co., Ltd of manufacturer.
The water absorption rate of the chitosan-based wound dressing of the fragrant bacteriostatic obtained by the present invention reaches 26.72 ~ 27.17gg
-1, moisture-vapor transmission reaches 3886 ~ 4220gm
-2d
-1, water suction and permeability are all better than commercially available dressing.Owing to not adopting liposome technology or employing to dry film forming in comparative example 1,2, and the present invention adopts liposome and lyophilizing film forming to cause dressing internal structure to be loose structure (Fig. 1), the dressing specific surface area larger (Fig. 2) that freeze drying technology is obtained, its water absorption, moisture-vapor transmission increase (table 2) greatly, wound can be made to keep the drying of appropriateness, be conducive to wound incrustation.
The coagulating effectiveness of dressing is by A
540nmcharacterize, A
540nmthe hemocyte of less explanation eluting is fewer, i.e. the coagulating effectiveness of dressing is better.Fig. 3 shows, the A of A, B, C that the embodiment of the present invention 1,2,3 is obtained
540nmall be less than 0.05, and D, E of comparative example are between 0.10-0.15, and commercially available chitosan dressing is all greater than 0.2.Therefore, the dressing obtained by the present invention has better coagulating effectiveness.
The wound dressing adopting the technology of the present invention to obtain has preferably derived essential oil slow release effect (Fig. 4), progressively slow releasing in 35 weeks.But D, E in comparative example, release time is shorter, and the most of derived essential oil before 15 weeks in dressing discharges into environment, and its quintessence oil slow release effect is not as good as A, B, C.This means the generation fungistatic effect that A, B, C dressing can be more lasting in medical environment.
The wound dressing adopting the technology of the present invention to obtain has preferably instantaneous thalline clearance rate (Fig. 5).The instantaneous thalline clearance rate of A, B, C is at 90%-95%.And the instantaneous thalline clearance rate of other dressing is all lower than 85%.Especially F, although specific surface area is maximum, excessive porosity can cause the seepage of thalline, declines to thalline crown_interception.This means that A, B, C dressing can retain more thalline in medical environment within the shorter time.
The antibacterial test result of dressing is as table 3.
The antibacterial test result of table 3 dressing
Chitosan-based wound dressing containing quintessence oil all has certain bacteriostatic activity.But adopt its bacteriostasis of chitosan dressing of the technology of the present invention more outstanding, and commercially available chitosan-based wound dressing effect is faint, substantially can not suppress microbial growth.
Claims (10)
1. a preparation method for the chitosan-based wound dressing of fragrant bacteriostatic, it is characterized in that, the method comprises the steps:
(1) by tea tree ethereal oil, menthol and P-Cymene mix and blend at low temperatures, be dissolved in phosphate buffered solution, obtain natural aromatic antibacterial;
(2) with the ratio of every 125mg soybean lecithin and cholesterol gross mass and 10ml natural aromatic antibacterial, thin film aquation legal system is adopted to obtain Liposomal suspensions;
(3) Liposomal suspensions is added pre-configured chitin-sodium alginate-gelatin solution, then add sucrose as stabilizing agent, low temperature fully stirs and obtains homogeneous liquid; Liquid is applied to polyfluortetraethylene plate surface, places 2h and make it launch completely;
(4) polyfluortetraethylene plate scribbling liquid is put into vacuum freezing drying oven,-5 DEG C of pre-freeze 6h, be then cooled to-55 ~-80 DEG C with the speed of 1 ~ 10 DEG C/h, then evacuation maintain below 0.012mBar, lyophilization 72 ~ 100h, obtains the chitosan-based wound dressing of fragrant bacteriostatic.
2. the preparation method of the chitosan-based wound dressing of fragrant bacteriostatic according to claim 1, it is characterized in that, in step (1), the mass ratio of described tea tree ethereal oil, menthol and P-Cymene is 1:1:1, described cryogenic temperature is 4 DEG C, and speed of agitator is 60 revs/min.
3. the preparation method of the chitosan-based wound dressing of fragrant bacteriostatic according to claim 1, it is characterized in that, in step (1), phosphate buffer solution is prepared as follows and is obtained: sodium chloride 8g/L, potassium chloride 0.2g/L, sodium hydrogen phosphate 1.44g/L, dipotassium hydrogen phosphate 0.24g/L, solvent is water, with hydrochloric acid adjust pH to 6.5, adds the Tween 80 that mass fraction is 6%.
4. the preparation method of the chitosan-based wound dressing of fragrant bacteriostatic according to claim 1, it is characterized in that, in step (1), the mixture of tea tree ethereal oil, menthol and P-Cymene adds phosphate buffer solution with the concentration of 0.2 ~ 2g/100mL.
5. the preparation method of the chitosan-based wound dressing of fragrant bacteriostatic according to claim 1, is characterized in that, in step (2), the mass ratio of soybean lecithin and cholesterol is 4:1.
6. the preparation method of the chitosan-based wound dressing of fragrant bacteriostatic according to claim 1 or 5, it is characterized in that, in step (2), described thin film aquation method is: pour in round-bottomed flask after soybean lecithin and cholesterol are dissolved in chloroform, at room temperature revolves steaming to bottle wall and forms the homogeneous thin film of one deck; Phosphate buffer solution 20ml being added natural antibacterial agent in 55 DEG C of ultrasonic water bath is preheated to 55 DEG C, then adds and be covered with in the round-bottomed flask of thin film, and sonic oscillation 10 minutes, supersonic frequency is 400MHz, and frequency of oscillation is 200 revs/min.
7. the preparation method of the chitosan-based wound dressing of fragrant bacteriostatic according to claim 1, it is characterized in that, in step (3), described chitin-sodium alginate-gelatin solution, that the mixture of chitosan, sodium alginate and gelatin is dissolved in 1%v/v acetic acid aqueous solution with the concentration of 4g/100mL, stir at 4 DEG C, adjust pH to 6.5 and get final product; Wherein, the mass ratio of chitosan, sodium alginate and gelatin is 2 ~ 4:1:1, and chitosan mean molecule quantity is 500kDa, and deacetylation is 85%.
8. the preparation method of the chitosan-based wound dressing of the fragrant bacteriostatic according to claim 1 or 7, is characterized in that, in step (3), the volume ratio of Liposomal suspensions and chitin-sodium alginate-gelatin solution is 1:1 ~ 3.
9. the preparation method of the chitosan-based wound dressing of the fragrant bacteriostatic according to claim 1 or 7, it is characterized in that, in step (3), the addition of sucrose counts 2g/100mL with the volume of mixture of Liposomal suspensions and chitin-sodium alginate-gelatin solution.
10. the preparation method of the chitosan-based wound dressing of the fragrant bacteriostatic according to claim 1 or 7, is characterized in that, in step (3), low temperature fully stirs and obtains homogeneous liquid, and cryogenic temperature is 4 ~ 8 DEG C; Speed of agitator is 100 ~ 200 revs/min.
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Effective date of registration: 20191223 Address after: 250101 Room 203, building 1, No. 2000, Airport Road, Yaoqiang street, high tech Zone, Jinan City, Shandong Province Patentee after: Jinan Kele Pharmaceutical Co., Ltd Address before: 226019 Jiangsu city of Nantong province sik Road No. 9 Patentee before: Nantong University |
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