CN104225600B - A kind of preparation method of the Wound antibiotic breast containing hexagonal mesoporous silicon - Google Patents
A kind of preparation method of the Wound antibiotic breast containing hexagonal mesoporous silicon Download PDFInfo
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- CN104225600B CN104225600B CN201410461057.1A CN201410461057A CN104225600B CN 104225600 B CN104225600 B CN 104225600B CN 201410461057 A CN201410461057 A CN 201410461057A CN 104225600 B CN104225600 B CN 104225600B
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- mesoporous silicon
- hexagonal mesoporous
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- microemulsion
- chlorhexidine acetate
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Abstract
The invention discloses the preparation method of a kind of Wound antibiotic containing hexagonal mesoporous silicon breast.The method includes the preparation process of hexagonal mesoporous silicon load chlorhexidine acetate, the preparation process containing nano silver antimicrobials microemulsion and adds the step that pH adjusting agent is compounding.Containing multiple antimicrobial component in the present invention, there is the strongest broad-spectrum sterilization and antibacterial effect, utilize the construction features of mesoporous silicon simultaneously, the Antibacterial Constituents of load can be played stability and the slow-releasing improving it, make this antibacterial breast have long acting antibiotic effect.In addition mesoporous silicon can also improve the cohesiveness of emulsion, makes sense of touch good, to no skin irritation, has no side effect.
Description
Technical field
The invention belongs to sterilizing sterilization field, be specifically related to the preparation of a kind of Wound antibiotic containing hexagonal mesoporous silicon breast
Method.
Background technology
Skin is our human body outermost one Rotating fields, is the maximum organ of human body.It is effector, is again
Neural sensory receptor.Skin covers whole body, is human body first barrier, various tissues and device in protective
Official is from the invasion and attack of mechanicalness, physical property, chemical and pathogenic microorganism.Therefore damage is received when skin, very
Easily cause the infection of microorganism, and then cause various complication, health is worked the mischief.So skin is hindered
The sterilization sterilizing of mouth is critically important.
General hospital uses ethanol and iodine class disinfectant to wound disinfection sterilization.Owing to both materials can only
Eliminate a part of antibacterial or virus, and lasts is inconspicuous, in use can carry to patient simultaneously
Carry out obvious sensation of pricking.Substantial amounts of clinical verification shows, the bacterial micro-organism of about 80% grow epidermis with
In and the gauffer of skin inside.The merit of most bacterial micro-organism is killed owing to ethanol and iodine class disinfectant do not penetrate
Can, therefore use the ethanol of routine and iodine class disinfectant not to reach the most far away the effect that long-acting, broad-spectrum disinfecting is antibacterial
Really, it is difficult to the cleaning keeping wound skin is aseptic.
The most hexagonal mesoporous silicon is not used as the report of slow controlled release antibiotic breast.
Summary of the invention
Present invention aims to the deficiencies in the prior art, it is provided that a kind of Wound antibiotic containing hexagonal mesoporous silicon
The preparation method of breast.
The preparation method of a kind of Wound antibiotic breast containing hexagonal mesoporous silicon, comprises the following steps:
(1) preparation of hexagonal mesoporous silicon load chlorhexidine acetate:
Weigh chlorhexidine acetate to be dissolved in dehydrated alcohol in the vial being placed in sealing, add hexagonal mesoporous
Silicon, puts in the shaking table of 32~35 DEG C 6~8h, centrifugal after being then washed with deionized 3~5 times, finally will
The precipitation obtained is placed in 50~70 DEG C of baking ovens 24~48h, standby in final product is put into dry device;
(2) preparation containing nano silver antimicrobials microemulsion:
Being dissolved in dehydrated alcohol by nano silver antimicrobials, be subsequently adding tween 80, isopropyl palmitate mixes
And stir 3~5min, and then it is added dropwise over deionized water, after being added dropwise to complete, mixed liquor stirring 8~12h,
To the microemulsion containing nano silver antimicrobials;
(3) the compounding of the hexagonal mesoporous silicon of chlorhexidine acetate and microemulsion it is loaded with:
Weigh and step (1) is loaded with the hexagonal mesoporous silicon of chlorhexidine acetate and microemulsion prepared by step (2)
With homogenizer high-speed stirred 15~30min under the conditions of 6000~8000rpm after liquid mixing, add pH adjusting agent
Regulation pH is 5~7, finally gives the Wound antibiotic breast containing hexagonal mesoporous silicon.
In said method, described in step (1), chlorhexidine acetate concentration in dehydrated alcohol is
0.002~0.0035g/ml;The mass ratio of chlorhexidine acetate and mesoporous silicon is 2~3:1.
In said method, described in step (2) containing nano silver microemulsion liquid based on 100g, its composition bag as follows:
Nanometer silver 100~150 μ g, dehydrated alcohol 20~30g, tween 80 20~30g, isopropyl palmitate 5~10g,
Remaining is deionized water.
In said method, the load hexagonal mesoporous silicon of chlorhexidine acetate described in step (3), microemulsion mix
The mass ratio closed is 1:50~80.
In said method, the pH adjusting agent described in step (3) is citric acid, tartaric acid, phosphoric acid, hydrogen
More than one in potassium oxide or triethanolamine.
Compared with prior art, it is an advantage of the current invention that:
(1) chlorhexidine acetate Antibacterial Constituents is loaded with the loose structure of hexagonal mesoporous silicon, can be to activity
Composition carries out slow controlled release, improves its stability, reduces the zest to skin;The most hexagonal mesoporous silicon can change
The cohesiveness of kind emulsion, makes sense of touch good, has no side effect.
(2) the antibacterial breast of the present invention contains multiple antimicrobial component, has the strongest broad-spectrum antibacterial bactericidal action;
(3) preparation method of the present invention is simple, and equipment is simple, and production cost is low.
Accompanying drawing explanation
Fig. 1 is that bacterium Ruzhong chlorhexidine acetate has carried out release in vitro design sketch.
Specific embodiment
Following example will be further illustrated the preferred embodiment belonging in the scope of the invention, but the present invention
Claimed scope is not limited in embodiment.
Embodiment 1
(1) preparation of hexagonal mesoporous silicon load chlorhexidine acetate:
Weigh 2g chlorhexidine acetate to be dissolved in 1000ml dehydrated alcohol in the vial being placed in sealing, add
The hexagonal mesoporous silicon of 1g, puts into 6h in the shaking table of 32 DEG C, centrifugal, finally after being then washed with deionized 3 times
The precipitation obtained is placed on 24h in 50 DEG C of baking ovens, standby in final product is put into dry device.
(2) preparation containing nano silver antimicrobials microemulsion:
100 μ g nano silver antimicrobials are dissolved in 25g dehydrated alcohol, are subsequently adding 25g tween 80,
5g isopropyl palmitate mixes and is slowly stirred 3min, is then added dropwise over deionized water to microemulsion gross mass
For 100g, after being added dropwise to complete, mixed liquor stirring 8h, obtain the microemulsion containing nano silver antimicrobials.
(3) the compounding of the hexagonal mesoporous silicon of chlorhexidine acetate and microemulsion it is loaded with:
Weigh 1g in step (1) and be loaded with the hexagonal mesoporous silicon of chlorhexidine acetate and prepared by 50g step (2)
Microemulsion mixing after by homogenizer high-speed stirred 15min under the conditions of 6000rpm, add 0.05g hydroxide
Potassium regulation pH is 6.1, finally gives containing hexagonal mesoporous silicon Wound antibiotic breast.
Embodiment 2
(1) preparation of hexagonal mesoporous silicon load chlorhexidine acetate:
Weigh 3.5g chlorhexidine acetate to be dissolved in 1000ml dehydrated alcohol in the vial being placed in sealing, add
Enter the hexagonal mesoporous silicon of 1.4g, put into 8h in the shaking table of 35 DEG C, centrifugal after being then washed with deionized 3 times,
Finally the precipitation obtained is placed on 36h in 70 DEG C of baking ovens, standby in final product is put into dry device.
(2) preparation containing nano silver antimicrobials microemulsion:
150 μ g nano silver antimicrobials are dissolved in 30g dehydrated alcohol, are subsequently adding 30g tween 80,
5g isopropyl palmitate mixes and is slowly stirred 5min, is then added dropwise over deionized water to microemulsion gross mass
For 100g, after being added dropwise to complete, mixed liquor stirring 12h, obtain the microemulsion containing nano silver antimicrobials.
(3) the compounding of the hexagonal mesoporous silicon of chlorhexidine acetate and microemulsion it is loaded with:
Weigh 1g in step (1) and be loaded with the hexagonal mesoporous silicon of chlorhexidine acetate and prepared by 80g step (2)
Microemulsion mixing after by homogenizer high-speed stirred 15min under the conditions of 6000rpm, add 0.05g tri-ethanol
Amine regulation pH is 6.5, finally gives containing hexagonal mesoporous silicon Wound antibiotic breast.
Embodiment 3
(1) preparation of hexagonal mesoporous silicon load chlorhexidine acetate:
Weigh 3g chlorhexidine acetate to be dissolved in 1000ml dehydrated alcohol in the vial being placed in sealing, add
The hexagonal mesoporous silicon of 1g, puts into 8h in the shaking table of 35 DEG C, centrifugal, finally after being then washed with deionized 3 times
The precipitation obtained is placed on 48h in 60 DEG C of baking ovens, standby in final product is put into dry device.
(2) preparation containing nano silver antimicrobials microemulsion:
150 μ g nano silver antimicrobials are dissolved in 20g dehydrated alcohol, are subsequently adding 20g tween 80,
5g isopropyl palmitate mixes and is slowly stirred 5min, is then added dropwise over deionized water to microemulsion gross mass
For 100g, after being added dropwise to complete, mixed liquor stirring 10h, obtain the microemulsion containing nano silver antimicrobials.
(3) the compounding of the hexagonal mesoporous silicon of chlorhexidine acetate and microemulsion it is loaded with:
Weigh 1g in step (1) and be loaded with the hexagonal mesoporous silicon of chlorhexidine acetate and prepared by 70g step (2)
Microemulsion mixing after by homogenizer high-speed stirred 15min under the conditions of 6000rpm, add 0.05g citric acid
Regulation pH is 5.8, finally gives containing hexagonal mesoporous silicon Wound antibiotic breast.
Embodiment 4
(1) preparation of hexagonal mesoporous silicon load chlorhexidine acetate:
Weigh 3g chlorhexidine acetate to be dissolved in 1000ml dehydrated alcohol in the vial being placed in sealing, add
The hexagonal mesoporous silicon of 1.2g, puts into 8h in the shaking table of 37 DEG C, centrifugal after being then washed with deionized 3 times,
After the precipitation obtained is placed on 48h in 60 DEG C of baking ovens, standby in final product is put into dry device.
(2) preparation containing nano silver antimicrobials microemulsion:
150 μ g nano silver antimicrobials are dissolved in 30g dehydrated alcohol, are subsequently adding 30g tween 80,
8g isopropyl palmitate mixes and is slowly stirred 5min, is then added dropwise over deionized water to microemulsion gross mass
For 100g, after being added dropwise to complete, mixed liquor stirring 12h, obtain the microemulsion containing nano silver antimicrobials.
(3) the compounding of the hexagonal mesoporous silicon of chlorhexidine acetate and microemulsion it is loaded with:
Weigh 1g in step (1) and be loaded with the hexagonal mesoporous silicon of chlorhexidine acetate and prepared by 50g step (2)
Microemulsion mixing after by homogenizer high-speed stirred 15min under the conditions of 8000rpm, add 0.05g phosphoric acid and adjust
Joint pH is 5.7, finally gives containing hexagonal mesoporous silicon Wound antibiotic breast.
Carrying out antibacterial effect test with the Wound antibiotic breast of embodiment 1 preparation below, other embodiments 2~4 are with real
Execute example 1 and test effect basic simlarity, illustrate the most one by one.
One, the present invention is containing minimal inhibitory concentration test (MIC) of hexagonal mesoporous silicon Wound antibiotic breast:
Testing according to Ministry of Public Health disinfection technology standard (2002 editions) 2.1.7.3, its result of the test is listed in table 1
In.
Table 1 is containing the minimal inhibitory concentration result of the test of hexagonal mesoporous silicon Wound antibiotic breast
General minimal inhibitory concentration is less than 800ppm it can be assumed that material has anti-microbial property, and the present invention's is anti-as can be seen from the above table
Bacterium breast minimal inhibitory concentration is all far smaller than 800ppm, i.e. demonstrates good bacteriostatic activity.
Two, stability test
, there is not lamination in Wound antibiotic containing the hexagonal mesoporous silicon breast of the present invention centrifugal 5min under 4500rpm rotating speed;
Place under the conditions of 25 DEG C, 35 DEG C and 40 DEG C simultaneously and all keep intact for one month, lamination does not occurs;
Measure the content of wherein chlorhexidine acetate, during 15d, content respectively when 1d, 15d and 30d with ultraviolet spectrophotometry
Have dropped 0.5%, during 30d, content have dropped 2%;
More than experiment demonstrates the antibacterial breast of the present invention and has good stability.
Three, release test
With ultraviolet spectrophotometry, the antibacterial Ruzhong chlorhexidine acetate of the present invention is carried out extracorporeal releasing experiment, releasing effect such as figure
Shown in 1.As seen from Figure 1, the release of the antibacterial breast Dichlorodiphenyl Acetate chlorhexidine of the present invention is up to 12h.
Claims (5)
1. the preparation method of the Wound antibiotic breast containing hexagonal mesoporous silicon, it is characterised in that comprise the following steps:
(1) preparation of hexagonal mesoporous silicon load chlorhexidine acetate:
Weigh chlorhexidine acetate to be dissolved in dehydrated alcohol in the vial being placed in sealing, add hexagonal mesoporous silicon, put into 6 ~ 8h in the shaking table of 32 ~ 35 DEG C, then it is centrifuged after being washed with deionized 3 ~ 5 times, finally the precipitation obtained is placed on 24 ~ 48h in 50 ~ 70 DEG C of baking ovens, standby in final product is put into dry device;
(2) preparation containing nano silver antimicrobials microemulsion:
Being dissolved in dehydrated alcohol by nano silver antimicrobials, be subsequently adding tween 80, isopropyl palmitate is mixed and stirred for 3 ~ 5min, is then added dropwise over deionized water, after being added dropwise to complete, and mixed liquor stirring 8 ~ 12h, obtain the microemulsion containing nano silver antimicrobials;
(3) the compounding of the hexagonal mesoporous silicon of chlorhexidine acetate and microemulsion it is loaded with:
Weigh and step (1) is loaded with the hexagonal mesoporous silicon of chlorhexidine acetate and after microemulsion mixing prepared by step (2) with homogenizer high-speed stirred 15 ~ 30min under the conditions of 6000 ~ 8000rpm, adding pH adjusting agent regulation pH is 5 ~ 7, finally gives the Wound antibiotic breast containing hexagonal mesoporous silicon.
The preparation method of a kind of Wound antibiotic breast containing hexagonal mesoporous silicon the most according to claim 1, it is characterised in that described in step (1), chlorhexidine acetate concentration in dehydrated alcohol is 0.002 ~ 0.0035g/ml;The mass ratio of chlorhexidine acetate and mesoporous silicon is 2 ~ 3:1.
The preparation method of a kind of Wound antibiotic breast containing hexagonal mesoporous silicon the most according to claim 1, it is characterized in that, described in step (2) containing nano silver microemulsion liquid based on 100g, its composition bag as follows: nanometer silver 100 ~ 150 μ g, dehydrated alcohol 20 ~ 30g, tween 80 20 ~ 30g, isopropyl palmitate 5 ~ 10g, remaining be deionized water.
The preparation method of a kind of Wound antibiotic breast containing hexagonal mesoporous silicon the most according to claim 1, it is characterised in that the load hexagonal mesoporous silicon of chlorhexidine acetate described in step (3), the mass ratio of microemulsion mixing are 1:50 ~ 80.
The preparation method of a kind of Wound antibiotic breast containing hexagonal mesoporous silicon the most according to claim 1, it is characterised in that the pH adjusting agent described in step (3) is more than one in citric acid, tartaric acid, phosphoric acid, potassium hydroxide or triethanolamine.
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Citations (2)
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CN103520019A (en) * | 2013-09-27 | 2014-01-22 | 华南理工大学 | Preparation method of beautifying, sun-blocking and isolating emulsion containing hexagonal meso-porous silicon |
CN103705415A (en) * | 2013-12-13 | 2014-04-09 | 华南理工大学 | Epidermal repair emulsion of meso-porous silicon carrying epidermal growth factor and preparation method thereof |
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CN103520019A (en) * | 2013-09-27 | 2014-01-22 | 华南理工大学 | Preparation method of beautifying, sun-blocking and isolating emulsion containing hexagonal meso-porous silicon |
CN103705415A (en) * | 2013-12-13 | 2014-04-09 | 华南理工大学 | Epidermal repair emulsion of meso-porous silicon carrying epidermal growth factor and preparation method thereof |
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"复方纳米银抗菌乳液杀菌效果的研究";魏坤等;《中国消毒学杂志》;20100915;第27卷(第5期);521-523 * |
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