CN104922053B - A kind of preparation method of chitosan nanoparticles spray-filming agent - Google Patents
A kind of preparation method of chitosan nanoparticles spray-filming agent Download PDFInfo
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- CN104922053B CN104922053B CN201510314637.2A CN201510314637A CN104922053B CN 104922053 B CN104922053 B CN 104922053B CN 201510314637 A CN201510314637 A CN 201510314637A CN 104922053 B CN104922053 B CN 104922053B
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Abstract
The invention provides a kind of preparation method of chitosan nanoparticles spray-filming agent, and the nano-scale chitosan prepared can be evenly dispersed into wherein, allow it well on the application skins based upon bidding surface of a wound, play a part of hemostasis sterilization.The present invention uses two kinds of macromolecule filming materials of PVP and HPMC as spray-filming agent matrix and prepares spray-filming agent, and PVP is safe and non-toxic, there is stronger adhesion to skin, nonirritant, is soluble in polar solvent, there is certain viscosity, good film-forming property；HPMC is dissolved in cold water on a small quantity, good film-forming property, is used in combination generally as adjuvant and other filmogens.Certain proportion ethanol solution is added into the spray-filming agent aqueous solution so that the ejection of spray-filming agent solution is more smooth, and film forming is more uniform.Step（4）It is middle to be mixed again after spray coating solution and the heating of Nano chitosan concentrate, cooled down again after mixing, the technique can further shorten film formation time and drying time, optimize the performance of spray-filming agent.
Description
Technical field
The present invention relates to a kind of preparation of chitosan nanoparticles spray-filming agent, more particularly to a kind of shell for wound site
The preparation of glycan nanoparticle spray-filming agent.
Background technology
The advantages of film, spray patch, is closed in spray-filming agent tying, is prepared into a kind of spraying, is sprayed at skin, mucous membrane affected part
And injured surface, one layer of soluble biofilm is formed, extends medicine in the residence time of affected part, improves drug effect, save other
Dressing, so as to by brand-new physics and the dual antibacterial mechanisms of biology, isolation, kill pathogenic microorganism (including bacterium, fungi and
Virus etc.) form of administration.
Filmogen in spray-filming agent is both a kind of pharmaceutical carrier, can be played the protection surface of a wound by film forming, reduces skin again
Moisture evaporation, promote skin hydration effect and other effects, therefore the selection of filmogen is the key factor that spray-filming agent is successfully prepared.
At present, the filmogen used can be divided mainly into two major classes:Natural polymer filmogen, synthesis macromolecule filming material.Close
3 classes can be divided into according to its polymer monomer molecular structure difference into macromolecule filming material:Polyvinyl alcohol compound;Propylene
Acid copolymer;Cellulose derivative class.In natural high molecular substance, mainly have cellulose, gelatin, chitosan, Bletilla glucomannan,
Starch etc..
Chitin and the bigger chitosan of deacetylation are a kind of polysaccharide with biocompatibility well, can be by human body
Absorb, the artificial skin prepared with the chitosan of high-purity has the function of natural skin, is good artificial skin raw material.Together
When, according to dimensional effect and the principle of skin effect, by various dressing for skin nanosizings, dressing can be made preferably to stick, can had
Effect prevents surface of a wound bleeding and infection, reduces pain, accelerates wound repair.So the nanosizing of chitosan not only remains shell and gathered
The sugared advantageous property of itself, also adds advantageous property possessed by some nanoparticles, by the excellent of both sides for chitosan
Point combines, and has expanded the application of chitosan in itself.
The content of the invention
It is an object of the invention to provide a kind of preparation method of chitosan nanoparticles spray-filming agent, and will can prepare
Good nano-scale chitosan is evenly dispersed into wherein, allows it well on the application skins based upon bidding surface of a wound, plays hemostasis sterilization
Effect.
The present invention is achieved through the following technical solutions：
A kind of preparation method of chitosan nanoparticles spray-filming agent, comprises the following steps：
（1）PVP-k30 6g formation PVP solution soluble in water is taken, separately takes HPMC 0.4g formation HPMC solution soluble in water,
Two parts of solution are mixed again and stirred, 100ml is settled to distilled water, that is, is made into PVP-HPMC mixed solutions；
（2）By step（1）The PVP-HPMC mixed solutions prepared mix with the ethanol solution that volume fraction is 70 ﹪, are made
Coating solution is sprayed, the volume ratio of the two is PVP-HPMC mixed solutions：Volume fraction is 70 ﹪ ethanol solution=1:（1-4）；
（3）Compound concentration is 1mg/ml chitosan solution and 1mg/ml TPP solution respectively, then with TPP solution pair
Chitosan solution is titrated, when the mass ratio of TPP and chitosan is TPP：Chitosan=14:Reach titration end-point when 25, obtain
Nano chitosan turbid, stand, clear liquid removed after turbid precipitation, add deionized water washing, stand and wait it to precipitate again,
Clear liquid is removed again, repeats standing, washing step 3-4 times above, when washing to turbid PH is 5.5-6.5, is produced nanoshell and is gathered
Sugared concentrate, its chitosan content are 5mg/ml；
（4）By step（2）Obtained spray coating solution is heated to 30-35 DEG C, step（3）Obtained Nano chitosan concentrate
50-60 DEG C is heated to, then pours into Nano chitosan concentrate in spray coating solution, then mixed solution is cooled to 10-15 DEG C,
Chitosan nanoparticles spray-filming agent is obtained after standing 1h, wherein the volume ratio of spray coating solution and Nano chitosan concentrate is spray film
Solution：Nano chitosan concentrate=（2-5）：1.
PVP-k30 of the present invention is polyvinylpyrrolidone of the molecular weight between 45000-58000, and HPMC is hydroxyl
Propyl cellulose, TPP are sodium tripolyphosphate.
The present invention uses two kinds of macromolecule filming materials of PVP and HPMC to prepare spray-filming agent, PVP safety as spray-filming agent matrix
It is nontoxic, there is stronger adhesion to skin, it is nonirritant, polar solvent is soluble in, there is certain viscosity, good film-forming property；HPMC is a small amount of
Cold water is dissolved in, good film-forming property, is used in combination generally as adjuvant and other filmogens.Added into the spray-filming agent aqueous solution certain
Ratio ethanol solution so that the ejection of spray-filming agent solution is more smooth, and film forming is more uniform.Step（4）It is middle to spray coating solution and receive
Mixed after rice chitosan concentrate heating, cooled down again after mixing again, the technique can further shorten film formation time and
Drying time, optimize the performance of spray-filming agent.
Advantages of the present invention is as follows：
1. spray-filming agent solution and Nano chitosan concentrate are combined together, make it in skin surface film forming, both can be with
Skin wound is protected by film, has the excellent biological nature hemostasis that can utilize Nano chitosan and promotes wound healing.
Spray-filming agent film formation time and drying time are shorter made from 2., are more convenient to use.
Specific implementation
Embodiment 1：A kind of preparation method of chitosan nanoparticles spray-filming agent, comprises the following steps：
（1）PVP-k30 6g formation PVP solution soluble in water is taken, separately takes HPMC 0.4g formation HPMC solution soluble in water,
Two parts of solution are mixed again and stirred, 100ml is settled to distilled water, that is, is made into PVP-HPMC mixed solutions；
（2）By step（1）The PVP-HPMC mixed solutions prepared mix with the ethanol solution that volume fraction is 70 ﹪, are made
Coating solution is sprayed, the volume ratio of the two is PVP-HPMC mixed solutions：Volume fraction is 70 ﹪ ethanol solution=1:2；
（3）Compound concentration is 1mg/ml chitosan solution and 1mg/ml TPP solution respectively, then with TPP solution pair
Chitosan solution is titrated, when the mass ratio of TPP and chitosan is TPP：Chitosan=14:Reach titration end-point when 25, obtain
Nano chitosan turbid, stand, clear liquid removed after turbid precipitation, add deionized water washing, stand and wait it to precipitate again,
Clear liquid is removed again, repeats standing, washing step 3-4 times above, when washing to turbid PH is 6, produces Nano chitosan concentration
Liquid, its chitosan content are 5mg/ml；
（4）By step（2）Obtained spray coating solution is heated to 33 DEG C, step（3）Obtained Nano chitosan concentrate adds
Then heat is poured into Nano chitosan concentrate in spray coating solution to 55 DEG C, then mixed solution is cooled into 12 DEG C, after standing 1h
Chitosan nanoparticles spray-filming agent is obtained, wherein the volume ratio of spray coating solution and Nano chitosan concentrate is spray coating solution：Receive
Rice chitosan concentrate=3：1.
Embodiment 2：A kind of preparation method of chitosan nanoparticles spray-filming agent, comprises the following steps：
（1）PVP-k30 6g formation PVP solution soluble in water is taken, separately takes HPMC 0.4g formation HPMC solution soluble in water,
Two parts of solution are mixed again and stirred, 100ml is settled to distilled water, that is, is made into PVP-HPMC mixed solutions；
（2）By step（1）The PVP-HPMC mixed solutions prepared mix with the ethanol solution that volume fraction is 70 ﹪, are made
Coating solution is sprayed, the volume ratio of the two is PVP-HPMC mixed solutions：Volume fraction is 70 ﹪ ethanol solution=1:1；
（3）Compound concentration is 1mg/ml chitosan solution and 1mg/ml TPP solution respectively, then with TPP solution pair
Chitosan solution is titrated, when the mass ratio of TPP and chitosan is TPP：Chitosan=14:Reach titration end-point when 25, obtain
Nano chitosan turbid, stand, clear liquid removed after turbid precipitation, add deionized water washing, stand and wait it to precipitate again,
Clear liquid is removed again, repeats standing, washing step 3-4 times above, and when washing to turbid PH is 5.5, it is dense to produce Nano chitosan
Contracting liquid, its chitosan content are 5mg/ml；
（4）By step（2）Obtained spray coating solution is heated to 30 DEG C, step（3）Obtained Nano chitosan concentrate adds
Then heat is poured into Nano chitosan concentrate in spray coating solution to 50 DEG C, then mixed solution is cooled into 10 DEG C, after standing 1h
Chitosan nanoparticles spray-filming agent is obtained, wherein the volume ratio of spray coating solution and Nano chitosan concentrate is spray coating solution：Receive
Rice chitosan concentrate=2：1.
Embodiment 3：A kind of preparation method of chitosan nanoparticles spray-filming agent, comprises the following steps：
（1）PVP-k30 6g formation PVP solution soluble in water is taken, separately takes HPMC 0.4g formation HPMC solution soluble in water,
Two parts of solution are mixed again and stirred, 100ml is settled to distilled water, that is, is made into PVP-HPMC mixed solutions；
（2）By step（1）The PVP-HPMC mixed solutions prepared mix with the ethanol solution that volume fraction is 70 ﹪, are made
Coating solution is sprayed, the volume ratio of the two is PVP-HPMC mixed solutions：Volume fraction is 70 ﹪ ethanol solution=1:4；
（3）Compound concentration is 1mg/ml chitosan solution and 1mg/ml TPP solution respectively, then with TPP solution pair
Chitosan solution is titrated, when the mass ratio of TPP and chitosan is TPP：Chitosan=14:Reach titration end-point when 25, obtain
Nano chitosan turbid, stand, clear liquid removed after turbid precipitation, add deionized water washing, stand and wait it to precipitate again,
Clear liquid is removed again, repeats standing, washing step 3-4 times above, and when washing to turbid PH is 6.5, it is dense to produce Nano chitosan
Contracting liquid, its chitosan content are 5mg/ml；
（4）By step（2）Obtained spray coating solution is heated to 35 DEG C, step（3）Obtained Nano chitosan concentrate adds
Then heat is poured into Nano chitosan concentrate in spray coating solution to 60 DEG C, then mixed solution is cooled into 15 DEG C, after standing 1h
Chitosan nanoparticles spray-filming agent is obtained, wherein the volume ratio of spray coating solution and Nano chitosan concentrate is spray coating solution：Receive
Rice chitosan concentrate=5：1.
Embodiment 4：A kind of preparation method of chitosan nanoparticles spray-filming agent, comprises the following steps：
（1）PVP-k30 6g formation PVP solution soluble in water is taken, separately takes HPMC 0.4g formation HPMC solution soluble in water,
Two parts of solution are mixed again and stirred, 100ml is settled to distilled water, that is, is made into PVP-HPMC mixed solutions；
（2）By step（1）The PVP-HPMC mixed solutions prepared mix with the ethanol solution that volume fraction is 70 ﹪, are made
Coating solution is sprayed, the volume ratio of the two is PVP-HPMC mixed solutions：Volume fraction is 70 ﹪ ethanol solution=1:5；
（3）Compound concentration is 1mg/ml chitosan solution and 1mg/ml TPP solution respectively, then with TPP solution pair
Chitosan solution is titrated, when the mass ratio of TPP and chitosan is TPP：Chitosan=14:Reach titration end-point when 25, obtain
Nano chitosan turbid, stand, clear liquid removed after turbid precipitation, add deionized water washing, stand and wait it to precipitate again,
Clear liquid is removed again, repeats standing, washing step 3-4 times above, and when washing to turbid PH is 6.7, it is dense to produce Nano chitosan
Contracting liquid, its chitosan content are 5mg/ml；
（4）By step（2）Obtained spray coating solution is heated to 40 DEG C, step（3）Obtained Nano chitosan concentrate adds
Then heat is poured into Nano chitosan concentrate in spray coating solution to 48 DEG C, then mixed solution is cooled into 16 DEG C, after standing 1h
Chitosan nanoparticles spray-filming agent is obtained, wherein the volume ratio of spray coating solution and Nano chitosan concentrate is spray coating solution：Receive
Rice chitosan concentrate=6：1.
Embodiment 5：A kind of preparation method of chitosan nanoparticles spray-filming agent, comprises the following steps：
Step（1）、（2）、（3）With embodiment 1；Step（4）It is as follows：
By step（2）Obtained spray coating solution and step（3）Shell is obtained after obtained Nano chitosan concentrate mixing to gather
Sugared nanoparticle spray-filming agent, wherein the volume ratio of spray coating solution and Nano chitosan concentrate is spray coating solution：Nano chitosan
Concentrate=3：1.
Test example：100 university student volunteers are chosen, are randomly divided into 5 experimental groups, every group of 20 people, each experimental group difference
Spray-filming agent made from embodiment 1-5, i.e., be respectively charged into spraying bottle, sprayed with spraying bottle by spray-filming agent made from spraying embodiment 1-5
It is aligned under volunteer's skin of dorsum of hand spray four, sprays away from 10cm, record the average film formation time of each group and average drying time, as a result see
Table 1.
The average film formation time of each group of table 1 and average drying time compare
As it can be seen from table 1 the average film formation time of experimental group corresponding to embodiment 1-3 and average drying time are than reality
It is short to apply experimental group corresponding to example 5, illustrates step（4）The technique of use can further shorten film formation time and drying time, excellent
Change the performance of spray-filming agent.
Claims (2)
- A kind of 1. preparation method of chitosan nanoparticles spray-filming agent, it is characterised in that：Comprise the following steps：（1）PVP-k30 6g formation PVP solution soluble in water is taken, separately takes HPMC 0.4g formation HPMC solution soluble in water, Two parts of solution are mixed again and stirred, 100ml is settled to distilled water, that is, is made into PVP-HPMC mixed solutions；（2）By step（1）The PVP-HPMC mixed solutions prepared mix with the ethanol solution that volume fraction is 70 ﹪, and spray is made Coating solution, the volume ratio of the two are PVP-HPMC mixed solutions：Volume fraction is 70 ﹪ ethanol solution=1:（1-4）；（3）Compound concentration is 1mg/ml chitosan solution and 1mg/ml TPP solution respectively, then with TPP solution pair Chitosan solution is titrated, when the mass ratio of TPP and chitosan is TPP：Chitosan=14:Reach titration end-point when 25, obtain To Nano chitosan turbid, stand, clear liquid is removed after turbid precipitation, add deionized water washing, stand and wait it to sink again Form sediment, then remove clear liquid, repeat standing, washing step 3-4 times above, when washing to turbid PH is 5.5-6.5, produces and receive Rice chitosan concentrate, its chitosan content is 5mg/ml；（4）By step（2）Obtained spray coating solution is heated to 30-35 DEG C, step（3）Obtained Nano chitosan concentrate heating To 50-60 DEG C, then Nano chitosan concentrate is poured into spray coating solution, then mixed solution is cooled to 10-15 DEG C, is stood Chitosan nanoparticles spray-filming agent is obtained after 1h, wherein the volume ratio of spray coating solution and Nano chitosan concentrate is molten for spray film Liquid：Nano chitosan concentrate=（2-5）：1.
- A kind of 2. preparation method of chitosan nanoparticles spray-filming agent as described in claim 1, it is characterised in that：Including such as Lower step：（1）PVP-k30 6g formation PVP solution soluble in water is taken, separately takes HPMC 0.4g formation HPMC solution soluble in water, Two parts of solution are mixed again and stirred, 100ml is settled to distilled water, that is, is made into PVP-HPMC mixed solutions；（2）By step（1）The PVP-HPMC mixed solutions prepared mix with the ethanol solution that volume fraction is 70 ﹪, and spray is made Coating solution, the volume ratio of the two are PVP-HPMC mixed solutions：Volume fraction is 70 ﹪ ethanol solution=1:2；（3）Compound concentration is 1mg/ml chitosan solution and 1mg/ml TPP solution respectively, then with TPP solution pair Chitosan solution is titrated, when the mass ratio of TPP and chitosan is TPP：Chitosan=14:Reach titration end-point when 25, Nano chitosan turbid is obtained, is stood, clear liquid is removed after turbid precipitation, deionized water washing is added, stands and wait it again Precipitation, then clear liquid is removed, standing, washing step 3-4 times above is repeated, when washing to turbid PH is 6, produces nanoshell Glycan concentrate, its chitosan content are 5mg/ml；（4）By step（2）Obtained spray coating solution is heated to 33 DEG C, step（3）Obtained Nano chitosan concentrate is heated to 55 DEG C, then Nano chitosan concentrate is poured into spray coating solution, then mixed solution is cooled to 12 DEG C, obtained after standing 1h To chitosan nanoparticles spray-filming agent, wherein the volume ratio of spray coating solution and Nano chitosan concentrate is spray coating solution：Nanometer Chitosan concentrate=3：1.
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| CN101978954A (en) * | 2010-10-12 | 2011-02-23 | 广东药学院 | Preparation and application of chitosan particles |
| CN102614287A (en) * | 2011-10-20 | 2012-08-01 | 广州中医药大学 | Film-spraying agent for treating acute soft tissue injuries |
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| CN101978954A (en) * | 2010-10-12 | 2011-02-23 | 广东药学院 | Preparation and application of chitosan particles |
| CN102614287A (en) * | 2011-10-20 | 2012-08-01 | 广州中医药大学 | Film-spraying agent for treating acute soft tissue injuries |
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| "医用敷料";赵成如等;《中国医疗器械信息》;20070731;第13卷(第7期);第15-21页 * |
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