CN108245700A - A kind of hydroxypropyl methyl cellulose chitosan film dressing and preparation method thereof - Google Patents
A kind of hydroxypropyl methyl cellulose chitosan film dressing and preparation method thereof Download PDFInfo
- Publication number
- CN108245700A CN108245700A CN201810060065.3A CN201810060065A CN108245700A CN 108245700 A CN108245700 A CN 108245700A CN 201810060065 A CN201810060065 A CN 201810060065A CN 108245700 A CN108245700 A CN 108245700A
- Authority
- CN
- China
- Prior art keywords
- preparation
- chitosan
- hpmcs
- solution
- methyl cellulose
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
- A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
- A61L15/22—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons containing macromolecular materials
- A61L15/225—Mixtures of macromolecular compounds
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
- A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
- A61L15/42—Use of materials characterised by their function or physical properties
- A61L15/44—Medicaments
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
- A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
- A61L15/42—Use of materials characterised by their function or physical properties
- A61L15/46—Deodorants or malodour counteractants, e.g. to inhibit the formation of ammonia or bacteria
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
- A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
- A61L15/42—Use of materials characterised by their function or physical properties
- A61L15/60—Liquid-swellable gel-forming materials, e.g. super-absorbents
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules
- C08J3/246—Intercrosslinking of at least two polymers
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/20—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing organic materials
- A61L2300/23—Carbohydrates
- A61L2300/232—Monosaccharides, disaccharides, polysaccharides, lipopolysaccharides
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/40—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a specific therapeutic activity or mode of action
- A61L2300/404—Biocides, antimicrobial agents, antiseptic agents
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/40—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a specific therapeutic activity or mode of action
- A61L2300/412—Tissue-regenerating or healing or proliferative agents
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2301/08—Cellulose derivatives
- C08J2301/26—Cellulose ethers
- C08J2301/28—Alkyl ethers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2305/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2301/00 or C08J2303/00
- C08J2305/08—Chitin; Chondroitin sulfate; Hyaluronic acid; Derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2401/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2401/08—Cellulose derivatives
- C08J2401/26—Cellulose ethers
- C08J2401/28—Alkyl ethers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2405/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2401/00 or C08J2403/00
- C08J2405/08—Chitin; Chondroitin sulfate; Hyaluronic acid; Derivatives thereof
Landscapes
- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Epidemiology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Veterinary Medicine (AREA)
- Hematology (AREA)
- Public Health (AREA)
- Dispersion Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Materials For Medical Uses (AREA)
Abstract
The present invention provides a kind of modified hydroxypropyl methyl cellulose chitosan film dressing and preparation method thereof, and preparation method includes：After hydroxypropyl methyl cellulose is fully dissolved, succinic anhydride heating 5 6h of reaction are added, cold filtration is precipitated, and will obtain HPMCS after precipitation cleaning, drying；Chitosan solution is formed after chitosan is fully dissolved, and the pH value of chitosan solution is adjusted between 67, a concentration of 0.01 0.02g/ml of chitosan solution；The HPMCS solution of a concentration of 0.01 0.03g/ml is configured to after HPMCS is dissolved, with the chitosan solution according to volume ratio 1：(1 3) be uniformly mixed, after addition EDC and NHS reagents stirring, centrifugal treating, after cross-linking reaction cleaning to get.The film dressing various aspects performance being prepared by using the above method is more excellent, and should be widely promoted application.
Description
Technical field
The present invention relates to wound dressing production fields, thin in particular to a kind of hydroxypropyl methyl cellulose chitosan
Film dressing and preparation method thereof.
Background technology
Skin is the important organ of human body, is played a protective role to human body.However, the damage of skin can cause it is a series of
Problem.For example, the infecting of wound, the acceleration of metabolism, the loss of excessive moisture and protein, endocrine and immune system
Imbalance, it is serious can be with threat to life.Therefore, after skin barrier is damaged, it usually needs use ideal wound dressing
It is wrapped up to protect wound, prevents the infection of wound and serious dehydration, be provided with the moist environment conducive to wound healing, promoted
Into the healing of wound.
Ideal wound dressing should have the following conditions：Allow to remove extra exudate from wound surface；There is provided one
The microenvironment of a humidity；Wound is protected, avoids germ contamination；The bad stink of wound can be adsorbed；It keeps and promotes wound meat
The normal growth of bud tissue promotes wound healing, preventing from scar；It is permeable, it breathes freely, good biocompatibility；Low adherency is easily replaced,
It avoids bringing secondary damage；Dressing should have certain mechanical strength, and softness is not deformed；The dosage of medical dressing is reduced,
Nursing time is short.
In the prior art, the such as natural or synthetic faciola of traditional dressing, absorbent cotton, gauze etc., have different degrees of
Absorb wound exudate, the effect of protection.Its main function is by absorbing wound exudate, keeping wound dry and preventing from causing a disease
Bacterium enters wound and causes infection.But these traditional dressing it is universal the defects of be：The moistening of wound cannot be kept, extends wound
It heals in face；Granulation tissue is easily grown in dressing mesh, during more change dressings easily and wound adhesion, so as to compromise new growth
Granulation tissue and cause pain；In addition with haemostatic effect it is poor the problem of.
In view of this, it is special to propose the present invention.
Invention content
The first object of the present invention is to provide a kind of preparation method of hydroxypropyl methyl cellulose chitosan film dressing,
After HPMC is changed into succinyl hypromellose (HPMCS) by the preparation method using modified method, then using crosslinking
Agent carries out cross-linking catalyst HPMCS and chitosan (CS), the material after crosslinking are no longer dissolve in water, can but be swollen in water, absorbs
A large amount of moisture, mechanical performance is also more excellent, can overcome all shortcomings of other dressing in the prior art, entire preparation side
Method is easy to operate, and operating condition is mild, and the reagent of use is commercially available common reagent, and source is virtually expanded than wide
The applicable surface of dressing in itself is opened up, should be widely promoted application.
The second object of the present invention is to provide the hydroxypropyl methyl cellulose chitosan that above-mentioned preparation method is prepared
Film dressing, the dressing have suitable gas-premeable in itself, can maintain micro- wet wound climate, prevent wound dehydrates or Seepage
Go out liquid excessive buildup, and a certain amount of oxygen penetration can be allowed, so as to healing acceleration process, the dressing is by using specific preparation
After method crosslinking synthesis, the performance of various aspects is more excellent, suitable for expanding production application.
In order to realize the above-mentioned purpose of the present invention, spy uses following technical scheme：
The present invention provides a kind of preparation methods of hydroxypropyl methyl cellulose chitosan film dressing, specifically include as follows
Step：
(A) after hydroxypropyl methyl cellulose is fully dissolved, addition succinic anhydride heating reaction 5-6h, cold filtration obtains
Precipitation will obtain HPMCS after precipitation cleaning, drying；
(B) form chitosan solution after chitosan is fully dissolved, and by the pH value of chitosan solution adjust to 6-7 it
Between, a concentration of 0.01-0.02g/ml of chitosan solution；
(C) the HPMCS solution of a concentration of 0.01-0.03g/ml is configured to after HPMCS is dissolved, with the chitosan solution
According to volume ratio 1：(1-3) is uniformly mixed, and after addition EDC and NHS reagents stirring, centrifugal treating is cleaned after cross-linking reaction, i.e.,
.
In the prior art, ideal wound dressing should have the following conditions：Allow to remove extra ooze from wound surface
Go out object；One moist microenvironment is provided；Wound is protected, avoids germ contamination；The bad stink of wound can be adsorbed；It keeps simultaneously
Promote the normal growth of wound granulation tissue, promote wound healing, preventing from scar；It is permeable, it breathes freely, good biocompatibility；It is low viscous
It is attached, it easily replaces, avoids bringing secondary damage；Dressing should have certain mechanical strength, and softness is not deformed；Reduce Medical coating
The dosage of material, nursing time are short.
Its main function of traditional dressing is by absorbing wound exudate, keeping wound dry and preventing pathogenic bacteria from entering
Wound causes infection.Studies have found that the wound climate of micro- wet slant acidity can quickly promote wound healing.Wound has anxious
Property, chronic, exudation and the different type such as dry.Wound healing process has several different stages, can be fitted without a kind of dressing
For all wound management.So more and more new pattern compress are developed.These modern dressing are all based on creating
Best healing environment, promotes fibroblast to creep in wound surface, and traditional dressing shortcoming is obvious：It cannot keep
The moistening of wound extends wound healing；Granulation tissue is easily grown in dressing mesh, more change dressings easily and wound adhesion,
It damages the granulation tissue newly grown and causes pain；Haemostatic effect is poor.
The present invention applies in order to solve the above technical problems, providing a kind of modified hydroxypropyl methyl cellulose chitosan film
The preparation method of material, the preparation method be by the way that HPMC is changed into succinyl hypromellose (HPMCS) after, then adopt
Cross-linking catalyst HPMCS and chitosan (CS) are carried out with crosslinking agent, the film dressing being prepared using such method is had both
The dual excellent properties of hydroxypropyl methyl cellulose and chitosan using the mutual supplement with each other's advantages of both materials, have abandoned previous biography
The all defect of system dressing, the marketing for dressing provide new feasible program.
Chitosan (CS) at present has been widely used for biology and medical domain, be with antibacterial, moisture absorption, promote blood coagulation and
The polycation polysaccharide of wound healing effect.Chitosan has effects that good wound promoting healing, being capable of effective stimulus nerve mother
Cell division inhibits fibroblastic growth, mitigates the formation of scar.There is good biocompatibility and biology to drop simultaneously
Xie Xing.(Fan Lihong, Zhao's Zhe are yellow to be managed into grade chitosans/sodium alginate polyelectrolyte sponge and antibacterial functions Wuhan by Fan Lihong etc.
Work college journal, 2006,28 (11):Chitosan/sodium alginate polyelectrolyte sponge 25-28) is prepared for, research finds the sponge
With porous structure and excellent water absorbing properties, different antiseptics can be loaded and show special anti-microbial property.He Lanzhen
Deng (preparation of He Lanzhen, Liu Yi, Yang Dan chitose-gelatine sponge shape wound dressings and performance study Pharmaceutical Biotechnologies
.2006,13 (1):45-48) prepare chitose-gelatine sponge shape wound dressing have porosity, good hydrophilic property, air penetrability and
The features such as water absorption rate is higher, mechanical strength is moderate, and with hemostasis, the dual effect for reducing surface of a wound exudation and wound being avoided to dry
Fruit can play the role of protecting the surface of a wound in wound healing process.Chitosan itself is not soluble in water, making material mechanical strength
It is low, it needs to carry out produced with combination with other materials.More than material is all compound latter made bio-sponge class material, manufacture craft
Complexity, product quality are difficult to control, and are not easy to mass produce.
Hydroxypropyl methyl cellulose (HPMC) is a kind of water-soluble cellulose, has good biocompatibility, water-soluble
And biological degradability, it is widely used in field of medical accessory, but the material is individually in use, meet water or wound fluid meeting
Melt, deformation, it can not be separately as dressing application.
As it can be seen that have the problem of such or such if when two kinds of materials exclusive uses, it is impossible to ensure its material
Performance itself is optimal, and the present invention has been exactly based on specific preparation method, and two kinds of materials are merged well
Film dressing is made, just just compensates for each material the defects of property itself, and be not in the preparation method entirely invented
Simple fusion, is that first hydroxypropyl methyl cellulose is modified after obtaining HPMCS, then carries out interworking with chitosan solution, certainly
The reaction temperature of the pH value of chitosan solution in entire preparation method, hydroxypropyl methyl cellulose and succinic anhydride, time, solution
Concentration, also parameters such as ratio of hydroxypropyl methyl cellulose and chitosan are required to control in suitable proportional region,
Operating procedure only according to the invention is carried out after implementing by step, and the film dressing performance being prepared can just reach the present invention
Index, if which parameter without control in suitable range, may influence whether the comprehensive of the dressing finally obtained
Energy.
In order to further improve the performance of product, each operating parameter of the invention to being arrived involved in entire preparation method
Adjustment is optimized.
Preferably, in step (A), the hydroxypropyl methyl cellulose per 2-10g uses the DMF (fumaric acid two of 25-100ml
Formicester) solvent fully dissolved.
Preferably, in step (A), DMAP (4-dimethylaminopyridine) solvent for adding 0.2-0.8g continues stirring and dissolving
Afterwards, the quality for adding succinic anhydride is 5-10g.
In addition, in the step (A) of the present invention, carry out needing to control certain operating condition during heating reaction, reaction
Temperature is controlled between 70-90 DEG C.
The product of reaction is needed by certain post processing, is filtered and is collected precipitation, and sediment then is used anhydrous second
Ether is rinsed, and HPMCS is obtained after dry.Certainly it is cleaned 2-4 times repeatedly preferably with anhydrous ether.
In the step (B) of the present invention, it is preferable that chitosan solution needs to control in the range of certain pH, adjusts pH
Preferably with a concentration of 1mol/L of the sodium hydroxide solution of 1-2mol/L, more preferably sodium hydroxide solution.
Preferably, in step (C), HPMCS solution is with chitosan solution generally according to 1：(1-3) is uniformly mixed, more preferably
According to volume ratio 1：2 are uniformly mixed, and in addition to this can also be 1：1.5、1：2.5 it waits.
Preferably, (N- maloyls are sub- by addition EDC (1- (3- dimethylamino-propyls) -3- ethyl carbodiimides) and NHS
Amine) reagent stirring time for 4-8min, be more preferably 5min.
Finally, after the stirring of addition EDC and NHS reagents, bubble removing is removed using centrifuge, the time of centrifugation preferably controls
It is more preferably 5min in 4-6min, the rate of centrifugation is preferably controlled in 4000-6000rpm, is more preferably 5000rpm.
After the present invention removes bubble removing by centrifugation, by liquid on a glass, control and carry out cross-linking reaction 6- at 4-5 DEG C
It can be carried out cleaning operation after 12h.
The operating procedure specifically cleaned can carry out in accordance with the following steps：By the sample after the cross-linking reaction in 35-
After being dried under conditions of 40 DEG C, after the sodium hydroxide solution immersion 30-40min for adding 0.1-0.2mol/L, distilled water impregnates again
4-5 times, each 1-2h is finally dried, you can.
Certainly, finally drying generally carries out in an oven, and the film dressing that film must be to the end is taken off after dry 2-3h.
HPMC is changed into succinyl hypromellose (HPMCS) by the present invention by modified method, then using friendship
Join agent and carry out cross-linking catalyst HPMCS and chitosan (CS).Material after crosslinking is no longer dissolved in the water, but can be molten in water
It is swollen, absorb a large amount of moisture.Mechanical experimental results show, under dry or solvent swelling state, compared to pure HPMC films,
CS films and in blend film in proportion, crosslinked film all shows good tensile strength and elongation at break, is especially swollen
The intensity of state.Swelling behavior detection find, all films can in PBS buffer solution Fast-swelling；Compared with pure CS films, own
Cross linking membrane has higher swelling ratio.Vapor and permeability the experimental results showed that, it is suitable that this crosslinked film has
Gas-premeable can maintain micro- wet wound climate, prevent wound dehydrates Huo Seepage from going out liquid excessive buildup, and can allow a certain amount of
Oxygen penetration, so as to healing acceleration process.The detection of these physicochemical properties, above-mentioned performance advantage may indicate that prepared
Obtained film dressing can be used as a kind of suitable wound dressing.
Certainly, the DMAP (dimethylamino naphthyridine) of above-mentioned use can use alchlor, tributylphosphine, pyridine, fourth two
Acid anhydrides replaces, and crosslinking agent EDC can use DCC (dicyclohexylcarbodiimide), DIC (N, N'- diisopropylcarbodiimide) generations
It replaces.
Compared with prior art, beneficial effects of the present invention are：
(1) preparation method of hydroxypropyl methyl cellulose chitosan film dressing of the invention, the preparation method use change
Property means HPMC is changed into succinyl hypromellose (HPMCS) after, then using crosslinking agent carry out cross-linking catalyst
HPMCS and chitosan (CS), the material after crosslinking are no longer dissolve in water, can but be swollen in water, absorb a large amount of moisture, machinery
Performance is also more excellent, can overcome all shortcomings of other dressing in the prior art, and entire preparation method is easy to operate, operation
Mild condition, the reagent of use are commercially available common reagent, and source virtually extends dressing suitable in itself than wide
With face, should be widely promoted application；
(2) the hydroxypropyl methyl cellulose chitosan film dressing being prepared using above-mentioned preparation method, the dressing sheet
Body has suitable gas-premeable, can maintain micro- wet wound climate, prevents wound dehydrates or Seepage from going out liquid excessive buildup, and energy
Allow a certain amount of oxygen penetration, so as to healing acceleration process, after which synthesizes by using the crosslinking of specific preparation method, respectively
The performance of aspect is more excellent, suitable for expanding production application.
Description of the drawings
It, below will be to specific in order to illustrate more clearly of the specific embodiment of the invention or technical solution of the prior art
Embodiment or attached drawing needed to be used in the description of the prior art are briefly described, it should be apparent that, in being described below
Attached drawing is some embodiments of the present invention, for those of ordinary skill in the art, before not making the creative labor
It puts, can also be obtained according to these attached drawings other attached drawings.
Fig. 1 is the crosslinking membrane swelling ratio measurement result figure of the embodiment of the present invention 2；
Fig. 2 is the cross linking membrane moisture-vapor transmission measurement result figure of the embodiment of the present invention 3；
Fig. 3 is the cross linking membrane OTR oxygen transmission rate measurement result figure of the embodiment of the present invention 3.
Specific embodiment
Embodiment of the present invention is described in detail below in conjunction with embodiment, but those skilled in the art will
Understand, the following example is merely to illustrate the present invention, and is not construed as limiting the scope of the invention.It is not specified in embodiment specific
Condition person, the condition suggested according to normal condition or manufacturer carry out.Reagents or instruments used without specified manufacturer is
The conventional products that can be obtained by commercially available purchase.
Embodiment 1
The preparation method of hydroxypropyl methyl cellulose chitosan film dressing is as follows：
1) HPMC powder 2.0g or so is taken, the DMF for adding in 25ml is stirred well to and is completely dissolved；
2) it after HPMC is completely dissolved, adds in 0.2gDMAP and continuing stirring until and is completely dissolved, be slowly added to 10.0g succinic acid
Acid anhydride, is heated to 90 DEG C, and insulation reaction 6h is cooled to room temperature；
3) reaction solution is slowly added into 1000ml anhydrous ethers, filters and collects precipitation, then sediment uses nothing
Then the precipitation being collected into is dried in vacuo to get to HPMCS by water washed with ether 2 times；
4) HPMCS powder 1.0g are weighed, add in a small amount of deionized water, heating stirring is to 50 DEG C, after complete solubilization
It is cooled to room temperature, is settled to 100ml.Chitosan powder 2.0g is weighed, deionized water 60ml is added in, stirs to powder and be completely dispersed
Yu Shuizhong, adding in 1ml acetic acid while stirring is completely dissolved powder, then using the pH of the sodium hydrate regulator solution of 1mol/L
To 6.0, it is finally settled to 100ml；
5) preparation of composite crosslinking film:HPMCS solution and chitosan solution are respectively taken into 50ml, according to 1：1 volume ratio
It is uniformly mixed, then adds in the NHS of the EDC and 1.0g-1.5g of 2.0-4.0g, stirred 5min, use centrifuge 4000rpm
Centrifugation 6min removes bubble removing.Liquid is slowly poured on clean smooth glass plate, is placed in 4 DEG C of refrigerator and continues crosslinking instead
Answer 6h；
6) it cleans：Thick sample will be crosslinked, be positioned in 35 DEG C of oven and dries, then add in 0.1mol/L sodium hydroxides
It is put into distilled water solution and impregnates 5 times, each 1h after aqueous solution covering immersion 30min, until cleaning solution presentation neutrality, at 37 DEG C
Oven in it is dry, take off film to get.
Embodiment 2
The preparation method of hydroxypropyl methyl cellulose chitosan film dressing is as follows：
1) HPMC powder 10.0g or so is taken, the DMF for adding in 100ml is stirred well to and is completely dissolved；
2) it after HPMC is completely dissolved, adds in 0.8gDMAP and continuing stirring until and is completely dissolved, be slowly added to 5.0g succinic acid
Acid anhydride, is heated to 70 DEG C, and insulation reaction 5h is cooled to room temperature；
3) reaction solution is slowly added into 1000ml anhydrous ethers, filters and collects precipitation, then sediment uses nothing
Then the precipitation being collected into is dried in vacuo to get to HPMCS by water washed with ether 4 times；
4) HPMCS powder 3.0g are weighed, add in a small amount of deionized water, heating stirring is to 50 DEG C, after complete solubilization
It is cooled to room temperature, is settled to 100ml.Chitosan powder 1.0g is weighed, deionized water 60ml is added in, stirs to powder and be completely dispersed
Yu Shuizhong, adding in 1ml acetic acid while stirring is completely dissolved powder, then using the pH of the sodium hydrate regulator solution of 2mol/L
To 7.0, it is finally settled to 100ml；
5) preparation of composite crosslinking film:HPMCS solution and chitosan solution are respectively taken into 50ml, according to 1：3 volume ratio
It is uniformly mixed, then adds in the NHS of the EDC and 1.0g-1.5g of 2.0-4.0g, stirred 4min, use centrifuge 6000rpm
Centrifugation 4min removes bubble removing.Liquid is slowly poured on clean smooth glass plate, is placed in 5 DEG C of refrigerator and continues crosslinking instead
Answer 12h；
6) it cleans：Thick sample will be crosslinked, be positioned in 40 DEG C of oven and dries, then add in 0.2mol/L sodium hydroxides
It is put into distilled water solution and impregnates 4 times, each 2h after aqueous solution covering immersion 30min, until cleaning solution presentation neutrality, at 37 DEG C
Oven in it is dry, take off film to get.
Embodiment 3
The preparation method of hydroxypropyl methyl cellulose chitosan film dressing is as follows：
1) HPMC powder 8.0g or so is taken, the DMF for adding in 75ml is stirred well to and is completely dissolved；
2) it after HPMC is completely dissolved, adds in 0.6gDMAP and continuing stirring until and is completely dissolved, be slowly added to 7.0g succinic acid
Acid anhydride, is heated to 80 DEG C, and insulation reaction 5h is cooled to room temperature；
3) reaction solution is slowly added into 1000ml anhydrous ethers, filters and collects precipitation, then sediment uses nothing
Then the precipitation being collected into is dried in vacuo to get to HPMCS by water washed with ether 3 times；
4) HPMCS powder 2.0g are weighed, add in a small amount of deionized water, heating stirring is to 50 DEG C, after complete solubilization
It is cooled to room temperature, is settled to 100ml.Chitosan powder 1.5g is weighed, deionized water 60ml is added in, stirs to powder and be completely dispersed
Yu Shuizhong, adding in 1ml acetic acid while stirring is completely dissolved powder, then using the sodium hydrate regulator solution of 1.5mol/L
PH to 6.0, is finally settled to 100ml；
5) preparation of composite crosslinking film:HPMCS solution and chitosan solution are respectively taken into 50ml, according to 1：2 volume ratio
It is uniformly mixed, then adds in the NHS of the EDC and 1.0g-1.5g of 2.0-4.0g, stirred 8min, use centrifuge 5000rpm
Centrifugation 5min removes bubble removing.Liquid is slowly poured on clean smooth glass plate, is placed in 5 DEG C of refrigerator and continues crosslinking instead
Answer 8h；
6) it cleans：Thick sample will be crosslinked, be positioned in 37 DEG C of oven and dries, then add in 0.15mol/L hydroxides
Sodium water solution covering is put into distilled water solution and impregnates 5 times, each 1.5h after impregnating 35min, until neutrality is presented in cleaning solution,
It is dry in 37 DEG C of oven, take off film to get.
Note：DMAP (dimethylamino naphthyridine) in above-mentioned each embodiment can use alchlor, tributylphosphine, pyrrole
Pyridine, succinic anhydride replace, and crosslinking agent EDC can use DCC (dicyclohexylcarbodiimide), DIC (N, N'- diisopropyl carbon two
Imines) it replaces.
Experimental example 1
Tensile strength and elongation at break：
Good wound dressing must have higher intensity and toughness.Therefore selection tensile strength and elongation at break are made
For Testing index.Dry state HPMCS/CS cross-linked hydrogels film has higher tensile strength than pure HPMCS, under dry state, is crosslinked water
Gel mould has better ductility than pure HPMC and CS films, can adapt to the institutional framework of different parts when pasting in this way.This
Outside, compared to blend film, the tensile strength and fracture elongation of HPMCS/CS cross-linked hydrogel films all significantly improve.In swelling shape
Under state, the mechanical property of HPMCS does not measure, because HPMCS is immersed in PBS solution loses intensity completely soon, and is swollen shape
The tensile strength of pure CS also declines very significantly under state, only 1.57 ± 0.19MPa, and the crosslinking of the embodiment of the present invention 1
HPMCS/CS film the maximum tensile strengths reach 7.84 ± 0.57MPa, and concrete outcome is shown in such as the following table 1.
1 result of the test of table
Experimental example 2
The swelling ratio of the CS films of cross linking membrane and the prior art to the embodiment of the present invention 2 compares, and concrete outcome is shown in attached
Shown in Fig. 1, swelling ratio is capable of the ability of reaction material absorption wound exudate.For wound dressing, good swelling behavior
Dressing can be made quickly to absorb the diffusate of wound, in order to avoid the growth of wound dipping and microorganism.As can be seen from the figure pure shell
Glycan film and cross linking membrane can in PBS Fast-swelling, illustrate that material has good water absorbing properties.By the swelling of blend film
Then rate curve starts to maintain as it can be seen that the swelling ratio of blend film increases sharply over time, and reaches maximum value in 2h
One stable level.
Experimental example 3
The moisture-vapor transmission of cross linking membrane and blank film to the embodiment of the present invention 3 compares, it is generally the case that wound
Moisture-vapor transmission should be moderate, if because vapor penetrate it is too small, may just cause surface of a wound exudate excess accumulation,
And moisture-vapor transmission is excessive, can lead to the over-drying of the surface of a wound, is unfavorable for fibroblastic proliferation and creeps, so as to subtract
The healing rate of slow wound.As known to figure, cross linking membrane is 807g/m in the transmitance of 12h2/ for 24 hours, it is 1245g/m with group control2/
For 24 hours, vapor evaporation 35.18% is reduced；And find that control group is 1518g/m at this time in 60h detections2/ for 24 hours, and cross linking membrane subtracts
Few moisture evaporation 48.49%.Data above illustrates that cross linking membrane is conducive to maintain the wound climate of moistening, and concrete outcome is shown in attached drawing 2.
Experimental example 4
The oxygen light transmittance of the cross linking membrane of the embodiment of the present invention 3 is measured, concrete outcome as shown in Figure 3, is being worked as
Under precondition, the negative control of measure and the OTR oxygen transmission rate of positive control are 9.58mg/L and 12.05mg/L, while cross linking membrane
Oxygen concentration be 11.59mg/L. the result shows that, crosslinked HPMCS/CS aquagel membranes allow oxygen penetration, are suitable for cell again
It is raw, help speed up agglutination.
The cross linking membrane of other embodiment is also passed through into above-mentioned experiment, also obtains identical result of the test.
Although illustrate and describing the present invention with specific embodiment, it will be appreciated that without departing substantially from the present invention's
Many other change and modification can be made in the case of spirit and scope.It is, therefore, intended that in the following claims
Including belonging to all such changes and modifications in the scope of the invention.
Claims (10)
1. a kind of preparation method of modified hydroxypropyl methyl cellulose chitosan film dressing, which is characterized in that including walking as follows
Suddenly：
(A) after hydroxypropyl methyl cellulose is fully dissolved, addition succinic anhydride heating reaction 5-6h, cold filtration is sunk
It forms sediment, HPMCS will be obtained after precipitation cleaning, drying；
(B) it forms chitosan solution after chitosan is fully dissolved, and the pH value of chitosan solution is adjusted between 6-7, shell
A concentration of 0.01-0.02g/ml of glycan solution；
(C) the HPMCS solution of a concentration of 0.01-0.03g/ml is configured to after HPMCS is dissolved, with the chitosan solution according to
Volume ratio 1：(1-3) is uniformly mixed, after addition EDC and NHS reagents stirring, centrifugal treating, after cross-linking reaction cleaning to get.
2. preparation method according to claim 1, which is characterized in that in the step (A), the hydroxypropyl first per 2-10g
Base cellulose is fully dissolved using the DMF solvent of 25-100ml.
3. preparation method according to claim 2, which is characterized in that in the step (A), add the DMAP of 0.2-0.8g
After solvent continues stirring and dissolving, the quality for adding succinic anhydride is 5-10g.
4. preparation method according to claim 3, which is characterized in that in the step (A), heat the temperature control of reaction
Between 70-90 DEG C；
Preferably, after precipitation is cleaned 2-4 times repeatedly using anhydrous ether, vacuum drying obtains HPMCS.
5. preparation method according to claim 1, which is characterized in that in the step (B), it is 1- to adjust pH and use
The sodium hydroxide solution of 2mol/L.
6. preparation method according to claim 1, which is characterized in that in the step (C), HPMCS solution and chitosan
Solution is according to volume ratio 1：2 are uniformly mixed.
7. preparation method according to claim 1, which is characterized in that in the step (C), addition EDC and NHS reagents stir
The time mixed is 4-8min, is more preferably 5min.
8. preparation method according to claim 1, which is characterized in that in the step (C), the rate control of centrifugation exists
4000-6000rpm is more preferably 5000rpm；
Preferably, the time control of centrifugation is more preferably 5min in 4-6min.
9. preparation method according to claim 1, which is characterized in that, will after bubble removing is removed in centrifugation in the step (C)
Liquid on a glass, controls and carries out cross-linking reaction 6-12h at 4-5 DEG C；
Preferably, the method for cleaning includes：After sample after the cross-linking reaction is dried under conditions of 35-40 DEG C, addition
After the sodium hydroxide solution of 0.1-0.2mol/L impregnates 30-40min, distilled water impregnates 4-5 times again, and each 1-2h is finally dried,
.
10. the modification hydroxypropyl methyl cellulose chitosan that claim 1-9 any one of them preparation methods are prepared is thin
Film dressing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810060065.3A CN108245700A (en) | 2018-01-22 | 2018-01-22 | A kind of hydroxypropyl methyl cellulose chitosan film dressing and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810060065.3A CN108245700A (en) | 2018-01-22 | 2018-01-22 | A kind of hydroxypropyl methyl cellulose chitosan film dressing and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108245700A true CN108245700A (en) | 2018-07-06 |
Family
ID=62741682
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810060065.3A Pending CN108245700A (en) | 2018-01-22 | 2018-01-22 | A kind of hydroxypropyl methyl cellulose chitosan film dressing and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108245700A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109224115A (en) * | 2018-11-27 | 2019-01-18 | 大连大学 | A kind of preparation method of chitosan-oxidation microcrystalline cellulose multilayer high porosity medical biologic film |
| CN114410147A (en) * | 2021-12-26 | 2022-04-29 | 南京理工大学 | Preparation method of nano thermite energetic printing ink |
| CN116650356A (en) * | 2023-04-23 | 2023-08-29 | 广州源美生物科技发展有限公司 | Free radical-removing skin care wet tissue and preparation method thereof |
| CN117285724A (en) * | 2022-06-16 | 2023-12-26 | 上海其胜生物制剂有限公司 | Chitosan homogeneous solution and preparation method and application thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102702363A (en) * | 2012-06-01 | 2012-10-03 | 华南理工大学 | Preparation method of hydroxypropyl methylcellulose acetate succinate in novel solvent system |
| CN105273088A (en) * | 2015-11-16 | 2016-01-27 | 泰安瑞泰纤维素有限公司 | Novel technology for preparing hydroxypropyl methyl cellulose derivative |
| CN105288700A (en) * | 2015-11-26 | 2016-02-03 | 西南大学 | Medical thermo-sensitive hydrogel dressing and preparation method thereof |
| EP3216808A1 (en) * | 2016-03-11 | 2017-09-13 | Shin-Etsu Chemical Co., Ltd. | Hypromellose acetate succinate, method for producing the same and composition containing the same |
-
2018
- 2018-01-22 CN CN201810060065.3A patent/CN108245700A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102702363A (en) * | 2012-06-01 | 2012-10-03 | 华南理工大学 | Preparation method of hydroxypropyl methylcellulose acetate succinate in novel solvent system |
| CN105273088A (en) * | 2015-11-16 | 2016-01-27 | 泰安瑞泰纤维素有限公司 | Novel technology for preparing hydroxypropyl methyl cellulose derivative |
| CN105288700A (en) * | 2015-11-26 | 2016-02-03 | 西南大学 | Medical thermo-sensitive hydrogel dressing and preparation method thereof |
| EP3216808A1 (en) * | 2016-03-11 | 2017-09-13 | Shin-Etsu Chemical Co., Ltd. | Hypromellose acetate succinate, method for producing the same and composition containing the same |
| CN107177006A (en) * | 2016-03-11 | 2017-09-19 | 信越化学工业株式会社 | HPMCAS and its production method and the composition containing it |
Non-Patent Citations (3)
| Title |
|---|
| QIONG JIANG ET AL: ""Hypromellose succinate-crosslinked chitosan hydrogel films forpotential wound dressing"", 《INTERNATIONAL JOURNAL OF BIOLOGICAL MACROMOLECULES》 * |
| 姜琼: ""新型复合壳聚糖水凝胶伤口敷料的制备及性能评价"", 《中国博士学位论文全文数据库 工程科技Ι辑》 * |
| 沈纪洋 等: ""羟丙基甲基纤维素丁二酸酯(HPMCS)的制备与性能"", 《高分子通报》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109224115A (en) * | 2018-11-27 | 2019-01-18 | 大连大学 | A kind of preparation method of chitosan-oxidation microcrystalline cellulose multilayer high porosity medical biologic film |
| CN114410147A (en) * | 2021-12-26 | 2022-04-29 | 南京理工大学 | Preparation method of nano thermite energetic printing ink |
| CN117285724A (en) * | 2022-06-16 | 2023-12-26 | 上海其胜生物制剂有限公司 | Chitosan homogeneous solution and preparation method and application thereof |
| CN117285724B (en) * | 2022-06-16 | 2024-04-30 | 上海其胜生物制剂有限公司 | Chitosan homogeneous solution and preparation method and application thereof |
| CN116650356A (en) * | 2023-04-23 | 2023-08-29 | 广州源美生物科技发展有限公司 | Free radical-removing skin care wet tissue and preparation method thereof |
| CN116650356B (en) * | 2023-04-23 | 2024-04-05 | 广州源美生物科技发展有限公司 | Free radical-removing skin care wet tissue and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Zhang et al. | Zn2+-loaded TOBC nanofiber-reinforced biomimetic calcium alginate hydrogel for antibacterial wound dressing | |
| Wang et al. | Preparation of antimicrobial hyaluronic acid/quaternized chitosan hydrogels for the promotion of seawater-immersion wound healing | |
| CN108245700A (en) | A kind of hydroxypropyl methyl cellulose chitosan film dressing and preparation method thereof | |
| CN112300420B (en) | Injectable antibacterial interpenetrating double-network hydrogel and preparation method and application thereof | |
| Cao et al. | A facile and green strategy for the preparation of porous chitosan-coated cellulose composite membranes for potential applications as wound dressing | |
| JP5968447B2 (en) | Chitosan and / or chitin complex with enhanced physical properties and uses thereof | |
| CN111154149A (en) | Hydrogel and preparation method and dressing thereof | |
| CN103055344B (en) | Bacterial cellulose/chitosan composite medical dressing and preparation method thereof | |
| CN110141677B (en) | Local acute hemostasis absorbable material and preparation method thereof | |
| US20050287193A1 (en) | Wound dressing made of chitin and alginate and method for forming the same | |
| CN107118361B (en) | Silk fibroin/carboxymethyl chitosan composite gel and preparation method thereof | |
| CN111690078B (en) | Double-quaternized chitosan derivative, synthetic method thereof, composite sponge biological dressing containing double quaternized chitosan derivative and application of composite sponge biological dressing | |
| CN110507842B (en) | Bacterial cellulose/hyaluronic acid/epsilon-polylysine functional dressing and preparation method thereof | |
| CN109224116A (en) | A kind of the antibacterial anti hemorrhagic medical dressing and preparation method of high-absorbable | |
| CN111053947A (en) | Konjac glucomannan/fish gelatin hydrogel as well as preparation method and application thereof | |
| Cao et al. | Preparation of biodegradable carboxymethyl cellulose/dopamine/Ag NPs cryogel for rapid hemostasis and bacteria-infected wound repair | |
| CN114404648A (en) | Preparation method of degradable antibacterial hemostatic hydrogel for promoting diabetic wound repair | |
| Xiong et al. | Injectable hydrogels of recombinant human collagen type III and chitosan with antibacterial and antioxidative activities for wound healing | |
| Tang et al. | Preparation and characterization of chitosan/sodium cellulose sulfate/silver nanoparticles composite films for wound dressing | |
| WO2017028625A1 (en) | Pleural/meningeal patch and preparation method therefor | |
| Mo et al. | Protamine-grafted carboxymethyl chitosan based hydrogel with adhesive and long-term antibacterial properties for hemostasis and skin wound healing | |
| CN112295009A (en) | Long-acting humidity-controlling antibacterial dressing and preparation method and application thereof | |
| CN111135340B (en) | Biological cellulose composite gel material and application thereof as wound dressing | |
| CN103174017B (en) | Sodium alginate oxide modified chitosan fiber and preparation method and application thereof | |
| CN105820267A (en) | Skin wound repairing preparation as well as preparation method and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20180706 |