CN105885063B - A kind of preparation method of the medical temperature-sensitive hydrogel containing nano silver - Google Patents
A kind of preparation method of the medical temperature-sensitive hydrogel containing nano silver Download PDFInfo
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Abstract
The preparation method of the invention discloses a kind of medical temperature-sensitive hydrogel containing nano silver, is mainly prepared by following raw materials according, is mass parts：Chitosan fine powder 20, silver nitrate 0.01.Products made thereby of the present invention has the characteristics that nano silver and chitosan and advantage; not only has nanometer silver antimicrobial; it is also equipped with chitosan and promotes cell growth; it reduces scar to generate, dispersant and protective agent of the chitosan as nano silver, make in the distribution temperature-sensitive hydrogel system of nano silver uniformly, stable; and the temperature-sensitive hydrogel containing nano silver has good moisturizing, gas permeability; and it is degradable, bio-compatibility is good, safety and low toxicity.
Description
Technical field
The present invention relates to medical material fields, more particularly to a kind of preparation of the medical temperature-sensitive hydrogel containing nano silver
Method.
Background technology
Chitosan has degradability, adsorptivity, film forming etc., and since its molecular structure contains a large amount of amino and hydroxyl
The groups such as base, are easily modified by sulphation, and the chitosan derivatives of different structure and function are generated, such as anticancer, antibacterial, controlled release, anti-freezing
The biological functions such as blood activity, have been widely used in biomedicine field.Wherein chitin biodressing has good
Gas and moisture retention can prevent water loss, can absorb wound fluid, have good biocidal property, prevent from infecting, only
Blood promotes wound healing.It also has good biocompatibility, biological degradability and film forming simultaneously, not only meets wound
The condition having required for mouth dressing, and there is excellent characteristic in terms of wound reparation, different clinical purposes can be made
Medical dressing.Nano silver is a kind of emerging functional material, since the pattern, grain size and stability etc. of nano silver make nano silver
With excellent performance.Its bactericidal effect is hundreds times of common silver, has to a variety of pathogenic microorganisms and inhibits and kill well
The effect of going out to pathogenic bacteria long action time, and not will produce drug resistance.Nowadays antibiotic usage is than wide, the anti-medicine of bacterium
Property it is very strong, people begin to focus on the material that not will produce drug resistance, and chitosan has stronger coordination ability with metal ion, obtain
To composite material both can possess simultaneously the advantages of.Temperature sensitive type water gel refers to being generated with the variation of ambient temperature
The intellectual material of stimulating responsive.The also controllable drug release of temperature-sensitive hydrogel, the shortcomings that changing conventional medicament such as drug effect is short, medicine
Object concentration cannot control, and can also perceive ambient temperature, discharge drug automatically, can control drug concentration well, make lesion
The drug concentration at position is constantly in Valid concentration.
101927030 A of publication No. CN（Application number 201010253355.3）Chinese patent literature disclose one kind and contain
Nano silver, zinc, bismuth biological dressing preparation method, be to synthesize chitosan with the method for synthesis in solid state and/or chitosan spreads out
Biological nano silver and zinc, bismuth compound, and be dissolved in solution, qs glycerin, collagen etc. is added, is obtained using casting filming therapy thin
Film dressing, or sponge dressing is obtained by freeze-drying.102492182 A of publication No. CN（Application number
201110402089.0）Chinese patent literature disclose it is a kind of containing the chitosan of rare earth element and/or its derivative biology
Film, preparation method are as follows：（1）Chitosan and/or chitosan derivatives are ground to fine powder；（2）According to chitosan and/
Or the weight ratio 100 of chitosan derivatives and rare earth compound：0.5~10（It is preferred that 100：2~8, more preferable 100：5）, will
Step（1）Gained fine powder and rare earth compound fine powder mixing, fully quickly grind 1~3 hour（It is preferred that 1.5~2.5 hours, more
It is preferred that 2 hours）To get chitosan and/or its derivative RE composite；（3）By step（2）Gained fine powder distilled water or
The glacial acetic acid solution of 0.5-1.2% is configured to the chitosan that mass concentration is 1-4% and/or its derivative RE composite is molten
Liquid；（4）By step（3）Acquired solution, fish gelatin solution and glycerine press certain volume ratio mixing, vacuumize degassing；（5）It will（4）
Gained mixed liquor pours on the cleaned glass plate kept flat, is cast into film, spontaneously dries, both must contain the chitosan of rare earth element with
/ or derivatives thereof biofilm.102358787 A of publication No. CN（Application number 201110311471.0）Chinese patent literature
Disclose a kind of silver-colored, chitosan and/or its derivates nanometer compound solid-phase synthesis, preparation method：（1）By chitosan
And/or chitosan derivatives are ground to fine powder；（2）Silver nitrate is ground into fine powder；（3）By chitosan and/or chitosan
Derivative fine powder and silver nitrate fine powder mixing, are fully ground 1~3 hour, chitosan and/or chitosan derivatives and silver nitrate
Weight ratio be 100：0.0005~0.5；（4）By step（3）Obtained fine powder is further ground 1~6 hour, is exposed to light
24~48 hours are silver, chitosan and/or the chitosan derivatives nano-complex of 1~100nm to get silver granuel diameter under source.
The acid-base value of chitosan/sodium glycero-phosphate gel systems is similar to human body, by the change of drug ratios, can make
The phase transition temperature of the gel systems maintains 37 DEG C or so of human body temperature, therefore using characteristic as the system, develops
Go out a kind of temperature-sensitive hydrogel of anti-inflammatory sterilization.
Invention content
In view of the deficiencies of the prior art, the object of the present invention is to provide a kind of methods simple, product safety contains nanometer
The preparation method of the medical temperature-sensitive hydrogel of silver.
The technical scheme is that:
A kind of medical temperature-sensitive hydrogel containing nano silver, is mainly prepared by following raw materials according, is mass parts：Shell is poly-
Sugared fine powder 20, silver nitrate 0.01；Steps are as follows：
（1）Chitosan fine powder and silver nitrate are taken, is placed in grinder, high speed grinding 1.5-2.5 hours, discharging, ultraviolet lamp
Chitosan nano silver mixture is made in lower irradiation 3-5 hours；
（2）By step（1）Made mixture is dissolved in the aqueous acetic acid of 0.1mol/L, and stirring is to being completely dissolved rear ice bath
To 4-10 DEG C of obtained sample solution, under stirring, then it is added dropwise 56%βPhosphoglycerol sodium water solution, after being added dropwise to complete, then
The disodium phosphate soln of saturation is added dropwise, it is 6.80-7.00 to be adjusted to pH；
（3）By step（2）Products therefrom is put into heating in thermostat water bath, takes out to get hydrogel.
The preparation method, step（1）It is 3000-5000 revs/min to grind rotating speed（Preferably, rotating speed 3500-
4500 revs/min；More preferred, rotating speed is 4000 revs/min）.
The preparation method, step（1）Grinding 1.8-2.2 hours（Preferably, it grinds 2 hours）.
The preparation method, step（1）It is irradiated 3.5-4.5 hours under ultraviolet lamp（Preferably, irradiation 4 is small under ultraviolet lamp
When）.
The preparation method, which is characterized in that step（2）Ice bath is to 5-9 DEG C（Preferably, ice bath is to 7 DEG C）.
The preparation method, step（2）A concentration of 1%-3% of sample solution（Preferably, sample solution is a concentration of
1.5-2.5%；More preferred, a concentration of the 2% of sample solution）.
The preparation method, step（2）56%βThe volume ratio of phosphoglycerol sodium water solution and sample solution is 1:8-12
（Preferably, 56%βThe volume ratio of phosphoglycerol sodium water solution and sample solution is 1:9-11；More preferred, 56%βGlycerine
The volume ratio of sodium phosphate aqueous solution and sample solution is 1:10）.
The preparation method, step（2）Adjusting pH is 6.88-6.92（Preferably, it is 6.90 to adjust pH）.
The preparation method, step（2）Rotating speed under stirring is 1000-1500 revs/min（Preferably, rotating speed
It is 1100-1400 revs/min；More preferred, rotating speed is 1300 revs/min）.
The preparation method, step（3）The temperature of thermostat water bath is 35-39 DEG C（Preferably, temperature is 36-38 DEG C；
More preferred, temperature is 37 DEG C）.
The preparation method, step（3）Heating 2-6 minutes（Preferably, it heats 3-5 minutes；More preferred, heating 4
Minute）.
A kind of medical temperature-sensitive hydrogel containing nano silver provided by the invention is prepared simply, and moisture retention is good.In addition to this,
The excellent results of the present invention are also manifested by：
1, products made thereby of the present invention has the characteristics that nano silver and chitosan and advantage, not only has nanometer silver antimicrobial,
It is also equipped with chitosan and promotes cell growth, reduce the effect that scar generates；
2, dispersant and protective agent of the chitosan as nano silver makes the distribution temperature-sensitive hydrogel of nano silver uniformly, stable
In system；
3, temperature-sensitive hydrogel containing nano silver has good moisturizing, gas permeability, and degradable, and bio-compatibility is good, safety
Low toxicity.
Specific implementation mode
With reference to embodiment and the experimental example technical solution that the present invention will be described in detail, but protection domain is without being limited thereto.
A kind of medical temperature-sensitive hydrogel containing nano silver of embodiment 1, is mainly prepared by following raw materials according（Every part
100g）：20 parts of chitosan fine powder, 0.01 part of silver nitrate.
A kind of preparation method of the medical temperature-sensitive hydrogel containing nano silver is：
（1）Chitosan fine powder and silver nitrate are taken, is placed in grinder, high speed grinding 1.5 hours, rotating speed is 3000 revs/min
Clock discharges, and is irradiated 3 hours under ultraviolet lamp, and chitosan nano silver mixture is made；
（2）By step（1）Made mixture is dissolved in the aqueous acetic acid of 0.1mol/L, and stirring is to being completely dissolved rear ice bath
To 4 DEG C obtained a concentration of 1% of sample solution, in the case where rotating speed is 1000 revs/min of stirring, then it is added dropwise 56%βGlycerine
Sodium phosphate aqueous solution, 56%βThe volume ratio of phosphoglycerol sodium water solution and sample solution is 1:8, after being added dropwise to complete, then it is added dropwise full
The disodium phosphate soln of sum, it is 6.80 to be adjusted to pH；
（3）By step（2）Products therefrom is put into heating 2 minutes in 35 DEG C of thermostat water bath, takes out to get hydrogel.
A kind of medical temperature-sensitive hydrogel containing nano silver of embodiment 2, is mainly prepared by following raw materials according（Every part
200g）：20 parts of chitosan fine powder, 0.01 part of silver nitrate.
A kind of preparation method of the medical temperature-sensitive hydrogel containing nano silver is：
（1）Chitosan fine powder and silver nitrate are taken, is placed in grinder, high speed grinding 2.5 hours, rotating speed is 5000 revs/min
Clock discharges, and is irradiated 5 hours under ultraviolet lamp, and chitosan nano silver mixture is made；
（2）By step（1）Made mixture is dissolved in the aqueous acetic acid of 0.1mol/L, and stirring is to being completely dissolved rear ice bath
To 10 DEG C obtained a concentration of 3% of sample solution, in the case where rotating speed is 1500 revs/min of stirring, then it is added dropwise 56%βIt is sweet
Oleophosphoric acid sodium water solution, 56%βThe volume ratio of phosphoglycerol sodium water solution and sample solution is 1:12, after being added dropwise to complete, then drip
The disodium phosphate soln for adding saturation, it is 7.00 to be adjusted to pH；
（3）By step（2）Products therefrom is put into heating 6 minutes in 39 DEG C of thermostat water bath, takes out to get hydrogel.
A kind of medical temperature-sensitive hydrogel containing nano silver of embodiment 3, is mainly prepared by following raw materials according（Every part
500g）：20 parts of chitosan fine powder, 0.01 part of silver nitrate.
A kind of preparation method of the medical temperature-sensitive hydrogel containing nano silver is：
（1）Chitosan fine powder and silver nitrate are taken, is placed in grinder, high speed grinding 1.8 hours, rotating speed is 3500 revs/min
Clock discharges, and is irradiated 3.5 hours under ultraviolet lamp, and chitosan nano silver mixture is made；
（2）By step（1）Made mixture is dissolved in the aqueous acetic acid of 0.1mol/L, and stirring is to being completely dissolved rear ice bath
To 5 DEG C obtained a concentration of 1.5% of sample solution, in the case where rotating speed is 1100 revs/min of stirring, then it is added dropwise 56%βIt is sweet
Oleophosphoric acid sodium water solution, 56%βThe volume ratio of phosphoglycerol sodium water solution and sample solution is 1:9, after being added dropwise to complete, then it is added dropwise
The disodium phosphate soln of saturation, it is 6.88 to be adjusted to pH；
（3）By step（2）Products therefrom is put into heating 3 minutes in 36 DEG C of thermostat water bath, takes out to get hydrogel.
A kind of medical temperature-sensitive hydrogel containing nano silver of embodiment 4, is mainly prepared by following raw materials according（Every part
1kg）：
20 parts of chitosan fine powder, 0.01 part of silver nitrate.
A kind of preparation method of the medical temperature-sensitive hydrogel containing nano silver is：
（1）Chitosan fine powder and silver nitrate are taken, is placed in grinder, high speed grinding 2.2 hours, rotating speed is 4500 revs/min
Clock discharges, and is irradiated 4.5 hours under ultraviolet lamp, and chitosan nano silver mixture is made；
（2）By step（1）Made mixture is dissolved in the aqueous acetic acid of 0.1mol/L, and stirring is to being completely dissolved rear ice bath
To 9 DEG C obtained a concentration of 2.5% of sample solution, in the case where rotating speed is 1400 revs/min of stirring, then it is added dropwise 56%βIt is sweet
Oleophosphoric acid sodium water solution, 56%βThe volume ratio of phosphoglycerol sodium water solution and sample solution is 1:8, after being added dropwise to complete, then it is added dropwise
The disodium phosphate soln of saturation, it is 6.92 to be adjusted to pH；
（3）By step（2）Products therefrom is put into heating 5 minutes in 38 DEG C of thermostat water bath, takes out to get hydrogel.
A kind of medical temperature-sensitive hydrogel containing nano silver of embodiment 5, is mainly prepared by following raw materials according（Every part
5kg）：
20 parts of chitosan fine powder, 0.01 part of silver nitrate.
A kind of preparation method of the medical temperature-sensitive hydrogel containing nano silver is：
（1）Chitosan fine powder and silver nitrate are taken, is placed in grinder, high speed grinding 2 hours, rotating speed is 4000 revs/min,
It discharges, is irradiated 4 hours under ultraviolet lamp, chitosan nano silver mixture is made；
（2）By step（1）Made mixture is dissolved in the aqueous acetic acid of 0.1mol/L, and stirring is to being completely dissolved rear ice bath
To 7 DEG C obtained a concentration of 2% of sample solution, in the case where rotating speed is 1300 revs/min of stirring, then it is added dropwise 56%βGlycerine
Sodium phosphate aqueous solution, 56%βThe volume ratio of phosphoglycerol sodium water solution and sample solution is 1:10, after being added dropwise to complete, then it is added dropwise
The disodium phosphate soln of saturation, it is 6.90 to be adjusted to pH；
（3）By step（2）Products therefrom is put into heating 4 minutes in 37 DEG C of thermostat water bath, takes out to get hydrogel.
Initial gelatinization time of a kind of medical temperature-sensitive hydrogel containing nano silver of test example present invention gained and antibacterial
Active measurement：
1, the measurement of initial gelatinization time
By step in embodiment 1-5（2）Products made thereby is transferred in centrifuge tube respectively, is put into 37 DEG C of thermostat water baths,
Start timing, tilts or reverse centrifuge tube every 20s, after being inverted 30s, solution no longer flows, and judgement forms gel, when by this
Between be used as the Primogel time, respectively measure record each embodiment initial gelatinization time.
2, Antibacterial Activity
Test strain：1. bacterium：G+ bacteria（G+）：Staphylococcus aureus reference culture ATCC25923
（Liaocheng People's Hospital provides）.Gram-negative bacterium（G-）：Escherichia coli clinical strains, enterobacter cloacae clinic bacterium
Strain, streptococcus pneumonia clinical strains, P. aeruginosa clinical bacterial strain（It is provided by the Liaocheng City hospital of traditional Chinese hospital）, the bloodthirsty bar of influenza
Bacterium clinical strains（It is provided by Liaocheng People's Hospital）；2. fungi：Candida albicans, Candida glabrata（By in Liaocheng City
Hospital is cured to provide）.
Test method：1. to the bacteriostasis of 6 kinds of bacteriums
Each strain of preservation is subjected to activation culture respectively, after growing single bacterium colony, with a little thalline of oese picking in dress
In the test tube for having 9ml sterile salines, shaken well prepares 10 respectively7The suspension of cfu/ml.Aseptically, exist
Add suitable culture medium in the culture dish of 90mm, after solidification plus 100 microlitres of bacterium solutions, coating uniformly, stand 20-30min.It will prepare
Sample, i.e. temperature-sensitive hydrogel, the 0.025% temperature sensitive water-setting containing nano silver containing nano silver of chitosan temperature-sensitive hydrogel, 0.01%
Glue, products made thereby of the present invention（Embodiment 5）, the circle of a diameter of 0.4cm is made respectively, is placed on same solid medium,
It is repeated 6 times, is cultivated for 24 hours in 37 DEG C of constant incubator.Whether there is or not bacterial growths for the contact surface of observation sample and culture medium, and survey
The size for measuring inhibition zone is analyzed using SPSS v11.5 software statistics, and data are with mean ± standard deviation（x±S）It indicates.
2. to the bacteriostasis of 2 kinds of fungies
Each strain of preservation is subjected to activation culture respectively, prepares the bacterium solution of a concentration of 1 × 106cfu/ml respectively, it is other
Operation is same as above, and cultivates 48h in 37 DEG C of constant incubator, and observing the contact surface of sample and culture medium, whether there is or not bacterial growths, measure
The size of inhibition zone.It is analyzed using SPSS software statistics, measurement data is with mean ± standard deviation（±S）It indicates.
Test result：As shown in Table 1, the initial gelatinization time of embodiment 5 is most short, illustrates chitosan crosslinked speed most
Soon.Simultaneously as shown in Table 2, four kinds of samples have certain contact bacteriostasis with fungi with bacterium to experiment and to the suppressions of bacterium
The inhibiting effect used better than to fungi is made, wherein products made thereby of the present invention is superior to other to the bacteriostasis of fungi and bacterium
Three samples, it is seen that with the increase of content of nanometer silver, the bacteriostasis of hydrogel is better, therefore, products made thereby of the present invention
With preferable fungistatic effect.
The initial gelatinization time of the different embodiments of table 1
Contact antibacterial antibacterial circle diameter of 2 each sample of table to bacterium with fungi（± SD, unit：cm）
Note：A：Chitosan temperature-sensitive hydrogel；B：0.01% temperature-sensitive hydrogel containing nano silver；C：0.025% containing nano silver
Temperature-sensitive hydrogel；D：Products made thereby of the present invention（Embodiment 5）.
It should be pointed out that specific implementation mode is the more representational example of the present invention, it is clear that skill of the invention
Art scheme is not limited to the above embodiments, and can also have many variations.Those skilled in the art define public affairs with the present invention
Written description open or according to file is undoubted to be obtained, and this patent scope of the claimed is considered as.
Claims (11)
1. a kind of preparation method of the medical temperature-sensitive hydrogel containing nano silver, which is characterized in that mainly prepared by following raw materials according
It forms, is mass parts：Chitosan fine powder 20, silver nitrate 0.01；Steps are as follows：
（1）Chitosan fine powder and silver nitrate are taken, is placed in grinder, high speed grinding 1.8-2.2 hours, grinding rotating speed is 3000-
It 5000 revs/min, discharges, is irradiated 3.5-4.5 hours under ultraviolet lamp, chitosan nano silver mixture is made；
（2）By step（1）Made mixture is dissolved in the aqueous acetic acid of 0.1mol/L, and stirring is to being completely dissolved rear ice bath to 5-
9 DEG C, sample solution is made, a concentration of 1%-2% of sample solution, under stirring, rotating speed is 1000-1500 revs/min, then
It is added dropwise 56%βPhosphoglycerol sodium water solution, 56%βThe volume ratio of phosphoglycerol sodium water solution and sample solution is 1:8-12,
After being added dropwise to complete, then the disodium phosphate soln of saturation is added dropwise, adjusting pH is 6.88-6.92；
（3）By step（2）Products therefrom is put into heating in thermostat water bath, and temperature is 35-39 DEG C, and constant temperature is extremely after initial gelatinization
Gel is formed, is taken out to get hydrogel.
2. preparation method as described in claim 1, which is characterized in that step（1）It is 3500-4500 revs/min to grind rotating speed.
3. preparation method as described in claim 1, which is characterized in that step（1）It is 4000 revs/min to grind rotating speed.
4. preparation method as described in claim 1, which is characterized in that step（1）Grinding 2 hours.
5. preparation method as described in claim 1, which is characterized in that step（1）It is irradiated 4 hours under ultraviolet lamp.
6. preparation method as described in claim 1, which is characterized in that step（2）Ice bath is to 7 DEG C.
7. preparation method as described in claim 1, which is characterized in that step（2）56%βPhosphoglycerol sodium water solution and sample
The volume ratio of solution is 1:9-11.
8. preparation method as described in claim 1, which is characterized in that step（2）56%βPhosphoglycerol sodium water solution and sample
The volume ratio of solution is 1:10.
9. preparation method as described in claim 1, which is characterized in that step（2）It is 6.90 to adjust pH.
10. preparation method as described in claim 1, which is characterized in that step（2）Under stirring, rotating speed 1100-1400
Rev/min.
11. preparation method as described in claim 1, which is characterized in that step（3）The temperature of thermostat water bath is 37 DEG C.
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| CN107189082B (en) * | 2017-07-22 | 2020-03-24 | 聊城大学 | Preparation method of bletilla striata chitosan-based temperature-sensitive hydrogel |
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| CN102358787B (en) * | 2009-08-11 | 2013-06-05 | 聊城大学 | Solid phase synthesis method of silver and chitosan and/or chitosan derivative nanometer compound |
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