CN111135302A - Hand-washing-free disinfection gel and preparation method thereof - Google Patents
Hand-washing-free disinfection gel and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the field of disinfection gel, and particularly relates to a hand-washing-free disinfection gel and a preparation method thereof, wherein the hand-washing-free disinfection gel comprises the following components in parts by mass: 0.05 to 5 percent of cationic bactericide, 0.1 to 20 percent of skin-care humectant, 0.1 to 5 percent of thickening agent and the balance of purified water. The invention provides a washing-free hand disinfection gel which takes a cationic bactericide as a main bactericidal component, is compounded with the cationic bactericide through nonionic cellulose ether, has stable performance, can quickly sterilize and inhibit bacteria for a long time, has fresh and cool hand feeling after use, is not sticky, is added with effective skin care components, and can mildly care hands, and a preparation method thereof.
Description
Technical Field
The invention belongs to the field of disinfection gel, and particularly relates to a hand-washing-free disinfection gel and a preparation method thereof.
Background
The prior art and the defects are as follows:
bacterial infection seriously threatens the health of people. Bacteria enter places with dense people streams such as markets, hospitals and schools through various ways, inhabit and breed in the places. Cross-infection is very likely to occur due to the intensive human flow in these areas. For bacteria, the temperature and humidity of human hands are particularly suitable for being used as a hotbed for the growth and propagation of bacteria, and simultaneously, the temperature and humidity provide a transmission medium for various bacteria, which is an important factor for causing bacterial cross infection. The risk of bacterial infection can be reduced to a certain extent by increasing the frequency of hand washing, but the simple hand washing action cannot completely remove pathogenic microorganisms such as bacteria, fungi and the like on hands. And a plurality of pathogenic microorganisms on the hand skin can be killed quickly and effectively by using a proper disinfection product. Hand disinfection is therefore the simplest and most effective means of controlling bacterial cross-contamination.
The cationic bactericide comprises chlorhexidine gluconate, chlorhexidine acetate, polyhexamethylene biguanide hydrochloride, polyhexamethylene guanidine hydrochloride, benzalkonium bromide, benzalkonium chloride, benzethonium chloride, double-chain quaternary ammonium salt and macromolecular quaternary ammonium salt. The cationic bactericide has the advantages of low toxicity, mild bactericidal effect, small skin irritation and the like, has a good bactericidal effect on bacterial propagules, and has a long-acting bactericidal effect.
Ethanol belongs to a medium-level disinfectant, and can quickly kill various microorganisms such as staphylococcus aureus, escherichia coli, candida albicans and the like when the concentration is 60-90%. Ethanol is widely used clinically for disinfection. However, ethanol brings problems of dry skin, chap and the like in the actual use process, and the ethanol has irritation, so that the application of the ethanol as a disinfectant in actual life is limited.
The water type disinfectant is easy to splash and drip in the using process, and the condensation type disinfectant can effectively prevent the splashing and dripping of the disinfectant. Commonly used gel bases are cellulosics and carbomers. If carbomer is used as the gel matrix, the carbomer is anionic, and can directly act with the cationic bactericide to generate an electric neutralization effect so as to cause flocculation and precipitation. If non-ionic cellulose ethers such as hydroxypropyl methyl cellulose or hydroxyethyl cellulose and the like are used as gel matrixes, the gel matrixes are well compounded with cationic bactericides, but cellulose thickeners feel sticky and greasy, so that the application of the gel matrixes in hand-washing-free disinfection gel is greatly limited.
The difficulty and significance for solving the technical problems are as follows:
therefore, based on the problems, the non-washing hand disinfection gel which takes the cationic bactericide as the main bactericidal component, is compounded by the nonionic cellulose ether and the cationic bactericide, has stable performance, can quickly sterilize and inhibit bacteria for a long time, has fresh and non-sticky hand feeling after use, is added with the effective skin care component, and has important practical significance on the hand gentle care and the preparation method thereof.
Disclosure of Invention
The invention aims to solve the technical problems in the prior art and provide the washing-free hand disinfection gel which takes the cationic bactericide as the main bactericidal component, is compounded by the nonionic cellulose ether and the cationic bactericide, has stable performance, fast sterilization and long-acting bacteriostasis, has fresh and non-sticky hand feel after use, is added with the effective skin care component and can mildly care the hands, and the preparation method thereof.
The technical scheme adopted by the invention for solving the technical problems in the prior art is as follows:
the hand-washing-free disinfection gel comprises the following components in parts by mass: 0.05 to 5 percent of cationic bactericide, 0.1 to 20 percent of skin-care humectant, 0.1 to 5 percent of thickening agent and the balance of purified water.
The invention prepares the washing-free hand disinfection gel taking the cationic bactericide as the main bactericidal component by compounding the thickening agent and the cationic bactericide, has stable performance, fast sterilization and long-acting bacteriostasis, has fresh and cool hand feeling without stickiness after use, and simultaneously adds the effective skin care component to carry out mild care on hands.
The invention relates to a hand-washing-free disinfection gel and a preparation method thereof, wherein the gel comprises 0.05-2% of cationic bactericide, 2-10% of skin-care humectant, 0.1-1.5% of thickening agent and the balance of purified water. According to the invention, the thickening agent is pretreated by using the skin-care humectant, so that the thickening agent and the cationic bactericide are prevented from generating precipitation, the hand-washing-free disinfection gel taking the cationic bactericide as a main component is prepared, the hand feeling is fresh and not sticky, common germs such as staphylococcus aureus, pseudomonas aeruginosa, escherichia coli and candida albicans are effectively killed, and the skin-care components are added to care hands.
Currently, the commonly used thickeners on the market are polyvinyl alcohol, polyvinylpyrrolidone, xanthan gum, sodium alginate, carboxymethyl cellulose, hydroxypropyl methyl cellulose, hydroxybutyl methyl cellulose, ethyl methyl cellulose, carboxymethyl methyl cellulose, hydroxymethyl ethyl cellulose, hydroxypropyl cellulose, hydroxyethyl cellulose, and the like. Most thickeners contain hydroxyl groups, which are electronegative; the electronegative hydroxyl can neutralize the charge of the cationic bactericide, so that the psi potential is reduced, the zeta potential is reduced, and finally aggregation and precipitation occur.
The invention can also adopt the following technical scheme:
in the above-mentioned hand-washing-free disinfecting gel, the cationic bactericide is one or more of chlorhexidine gluconate, chlorhexidine acetate, polyhexamethylene biguanide hydrochloride, polyhexamethylene guanidine hydrochloride, benzalkonium bromide, benzalkonium chloride, benzethonium chloride, double-chain quaternary ammonium salt and polymer quaternary ammonium salt.
In the above hand-washing-free disinfecting gel, further, the skin-care moisturizer is a polyhydric alcohol skin-care moisturizer, and includes: one or more of butylene glycol, glycerol, propylene glycol, sorbitol, polyethylene glycol, polypropylene glycol, and hexylene glycol.
In the above-mentioned hand-washing-free disinfecting gel, further, the thickener is a synthetic polymer thickener, comprising: one or more of polyvinyl alcohol, polyvinylpyrrolidone, xanthan gum, modified starch, carboxymethyl cellulose, hydroxypropyl methyl cellulose, hydroxybutyl methyl cellulose, ethyl methyl cellulose, carboxymethyl methyl cellulose, hydroxymethyl ethyl cellulose, hydroxypropyl cellulose and hydroxyethyl cellulose.
In the above hand-washing-free disinfecting gel, further, the hand-washing-free disinfecting gel comprises the following components in parts by mass: 0.05 to 2 percent of cationic bactericide, 2 to 10 percent of skin-care humectant, 0.1 to 1.5 percent of thickening agent and the balance of purified water.
A preparation method of a no-clean hand disinfection gel comprises the following steps:
the method comprises the following steps: uniformly dispersing the thickening agent in a skin-care humectant, standing and swelling to prepare a solution A;
step two: uniformly dispersing the cationic bactericide in purified water, and uniformly stirring to prepare a solution B;
step three: adding the solution A into the solution B, stirring uniformly, standing to remove bubbles, condensing, filling and sealing to obtain a finished product.
The invention uses skin-care ingredients to pretreat the thickening agent by a compounding technology. The skin care component and the thickening agent compound system have a synergistic effect under certain conditions, so that the dissolving speed of the thickening agent is increased. After the skin care component and the thickening agent are compounded, the dissolving speed of the thickening agent can be effectively increased after the skin care component of cellulose substances and the thickening agent are compounded.
The thickener generally needs to be stirred for 1-2 hours to be dissolved completely until the thickener is clear, and the skin care ingredients can be dissolved and cleared in a short time when being added. The skin care ingredients herein act as organic solvents and increase the dissolution rate of the thickener. Therefore, after the skin care ingredients and the thickening agent are compounded, the dissolving speed of the thickening agent can be effectively increased.
In conclusion, the invention has the following advantages and positive effects:
1. the invention adopts the compounding technology to pretreat the thickening agent, so that the compounded thickening agent and the cationic bactericide are well compounded, and the system is clear and transparent and has no precipitate.
2. After the skin care component and the thickening agent are compounded, the dissolving speed of the thickening agent can be effectively increased.
3. The hand-washing-free disinfection gel provided by the invention does not contain ethanol, and the problems of skin dryness, chapping, irritation and the like caused by ethanol are avoided. Meanwhile, the hand-washing-free disinfection gel provided by the invention can achieve the same disinfection effect as the hand-washing-free disinfection gel added with ethanol under the condition that the ethanol is not added.
4. The non-washing hand disinfection gel provided by the invention can rapidly kill common pathogenic bacteria by using the cationic bactericide, and ensures the sterilization effect.
5. The hand-washing-free gel provided by the invention is added with skin-care moisturizing components, moisturizes and moisturizes hands, effectively takes care of hands, and simultaneously has a weakly acidic formula, the pH value of the weakly acidic formula is close to that of the skin, so that the hands are protected.
6. The hand-washing-free disinfection gel provided by the invention has the advantages of simple preparation process, no need of heating, cost saving and suitability for industrial scale-up production.
Drawings
FIG. 1 shows the killing effect of the example three at different times;
FIG. 2 is a photograph comparing the results of the experiment in example III;
FIG. 3 is a photograph comparing the results of the experiment in example two.
Detailed Description
Example one
The dissolution rate of the comparative thickener was formulated as follows:
the formula I is as follows: 0.6g of hydroxypropyl methylcellulose and 99.4mL of purified water.
And a second formula: 0.6g of hydroxypropyl methyl cellulose, 2mL of glycerol and 97.4mL of purified water.
The configuration method comprises the following steps:
the formula I is as follows:
the method comprises the following steps: accurately weighing hydroxypropyl methylcellulose (accurate to 0.001g) and placing in a glass container;
step two: accurately measuring purified water, adding the purified water into a glass container filled with hydroxypropyl methyl cellulose, and stirring at room temperature until the purified water is clear;
and a second formula:
the method comprises the following steps: accurately weighing hydroxypropyl methylcellulose (accurate to 0.001g) and placing in a glass container;
step two: accurately measuring glycerol, adding into a glass container weighed with hydroxypropyl methyl cellulose, and fully stirring to fully disperse the hydroxypropyl methyl cellulose in the glycerol;
step three: accurately measuring purified water, adding the purified water into a glass container filled with hydroxypropyl methyl cellulose glycerol dispersion, and stirring at room temperature until the mixture is clear.
The technical method of the formula I needs to be stirred for 1-2 hours at room temperature to dissolve until the solution is clear; and the second formula is prepared by stirring at room temperature for 10-30 min to clarify.
Example two
The hand-washing-free disinfecting gel is prepared from the following formula:
the formula I is as follows: 2g of polyhexamethylene biguanide hydrochloride, 10mL of glycerol, 1.5g of hydroxypropyl methyl cellulose and 100mL of purified water.
And a second formula: 2g of polyhexamethylene biguanide hydrochloride, 1.5g of hydroxypropyl methylcellulose and 100mL of purified water.
The configuration method comprises the following steps:
the formula I is as follows:
the method comprises the following steps: accurately weighing hydroxypropyl methylcellulose (accurate to 0.001g) and placing in a glass container;
step two: accurately measuring purified water, adding the purified water into a glass container filled with hydroxypropyl methyl cellulose, and stirring at room temperature until the purified water is clear;
step three: polyhexamethylene biguanide hydrochloride was accurately weighed, added to the hydroxypropylmethylcellulose solution, and stirred at room temperature.
And a second formula:
the method comprises the following steps: accurately weighing hydroxypropyl methylcellulose (accurate to 0.001g) and placing in a glass container;
step two: accurately measuring glycerol, adding into a glass container weighed with hydroxypropyl methyl cellulose, and fully stirring to fully disperse the hydroxypropyl methyl cellulose in the glycerol;
step three: accurately measuring purified water, adding the purified water into a glass container filled with hydroxypropyl methyl cellulose glycerol dispersion, and stirring at room temperature until the mixture is clear.
Step four: polyhexamethylene biguanide hydrochloride was accurately weighed, added to the step trimethylolpropane methylcellulose solution, and stirred at room temperature.
As shown in figure A in attached figure 3 of the specification, the hand-washing-free disinfection gel prepared according to the technical scheme of the formula I generates obvious precipitation; as shown in figure B, the no-clean hand disinfection gel prepared according to the technical scheme of the formula II does not generate precipitates.
EXAMPLE III
The hand-washing-free disinfecting gel consists of the following formula: 2g of polyhexamethylene biguanide hydrochloride, 2mL of glycerol, 1.5g of hydroxypropyl methyl cellulose and 100mL of purified water.
The preparation method of the hand-washing-free disinfection gel comprises the following steps:
the method comprises the following steps: dispersing 1.5g of hydroxypropyl methyl cellulose in 2mL of glycerol, standing and swelling to prepare a solution A;
step two: uniformly dispersing polyhexamethylene biguanide hydrochloride in purified water, and uniformly stirring to prepare a solution B;
step three: and adding the solution A into the solution B, uniformly stirring, standing to remove bubbles, forming a condensation shape, filling and sealing to obtain a finished product 1.
And (3) microorganism killing experiment:
according to the requirement of microorganism killing indexes 4.2.3 GB 27950-2011 hand disinfectant sanitary requirement, the invention adopts escherichia coli 8099, staphylococcus aureus ATCC6538 and candida albicans ATCC10231 to verify the microorganism killing performance of the finished product 1. The invention adopts a quantitative suspension killing experiment method in the disinfection technical Specification (2002 edition) of the Ministry of health to carry out a microorganism killing experiment on a finished product 1. The method comprises the following specific steps:
firstly, equipment:
test strains: staphylococcus aureus ATCC6538, Escherichia coli 8099, Candida albicans ATCC 10231. The generation number of the above strains is 4 th generation, and PBS is used for preparing bacterial suspension.
Experimental samples: finished product 1, finished product 2 and finished product 3
Neutralizing agent: 3.9% D/E neutralized Broth
Secondly, the method comprises the following steps:
1. preparation of bacterial suspension: selecting bacteria with a content of 1 × 108CFU/mL～5×108CFU/mL bacterial suspension was subjected to neutralizer identification test.
2. And (3) identification test of a neutralizer: the test bacterium is Escherichia coli. The test groups are: (1) disinfectant + bacterial suspension, (2) (disinfectant + bacterial suspension) + neutralizer, (3) neutralizer + bacterial suspension, (4) (disinfectant + neutralizer) + bacterial suspension, (5) diluent + bacterial suspension, and (6) diluent + neutralizer + culture medium. Diluting the sample stock solution by 10 times in the same ratio as the neutralizer, and acting for 1.5 min. The experiment was repeated 3 times.
3. And (3) testing the killing performance: according to the quantitative sterilization test of the suspension, the finished product is 1, the action time is 1min, and the test is repeated for 3 times. The test environment temperature is 21-22 ℃.
4. The culture temperature is as follows: 35 ℃ plus or minus 2 DEG C
As a result:
1. neutralizer identification test
3 times of repeated experiments prove that the composition,the average number of growing colonies in group 1 was aseptically grown, and the average number of growing colonies in group 2 was 1.6X 103CFU/mL, similar average number of growing colonies in groups 3, 4, and 5, with an error rate of 4.76% between groups, and sterile growth in group 6 (Table 1).
TABLE 1 identification of product 1 neutralizer
Note: negative control sterile growth
2. Killing effect on Staphylococcus aureus, Escherichia coli and Candida albicans for 1min and 5min
As shown in the attached figure 1 of the specification, the killing logarithm of the finished product 1 to Candida albicans is more than 4.00 in 1min and 5 min; log kill was >5.00 for both E.coli and S.aureus at 1min and 5 min.
The A picture in the attached figure 2 of the specification is a candida albicans positive control without adding a finished product 1; and B is a candida albicans sample after the finished product 1 acts. As shown in the attached figure 2 of the specification, the finished product 1 has a strong killing effect on Candida albicans.
Example four
The hand-washing-free disinfecting gel consists of the following formula: 10g of chlorhexidine acetate, 100mL of polyethylene glycol-400100, 1g of xanthan gum and 1000mL of purified water.
The preparation method of the hand-washing-free disinfection gel comprises the following steps:
the method comprises the following steps: dispersing 1g of xanthan gum in 40mL of polyethylene glycol-400, standing and swelling to prepare a solution A;
step two: uniformly dispersing chlorhexidine acetate in purified water, and uniformly stirring to prepare a solution B;
step three: and adding the solution A into the solution B, uniformly stirring, standing to remove bubbles, forming a condensation shape, filling and sealing to obtain a finished product 2.
EXAMPLE five
The hand-washing-free disinfecting gel consists of the following formula: 0.5g of benzalkonium bromide, 40mL of propylene glycol, 15g of methyl cellulose and 1000mL of purified water.
The preparation method of the hand-washing-free disinfection gel comprises the following steps:
the method comprises the following steps: dispersing 15g of methyl cellulose in 40mL of propylene glycol, standing and swelling to prepare a solution A;
step two: uniformly dispersing benzalkonium bromide in purified water, and uniformly stirring to prepare a solution B;
step three: and adding the solution A into the solution B, uniformly stirring, standing to remove bubbles, forming a condensation shape, filling and sealing to obtain a finished product 3.
The microorganism killing experiment of the hand-washing-free disinfection gel comprises the following steps:
according to the requirement of microorganism killing indexes 4.2.3 of GB 27950 + 2011 hand disinfectant sanitary requirement, the invention adopts escherichia coli 8099, staphylococcus aureus ATCC6538 and candida albicans ATCC10231 to verify the microorganism killing performance of the finished products 1, 2 and 3. The invention adopts a quantitative suspension killing experiment method in the disinfection technical Specification (2002 edition) of the Ministry of health to respectively carry out a microorganism killing experiment on a finished product 1, a finished product 2 and a finished product 3. The method comprises the following specific steps:
killing experiment of staphylococcus aureus and escherichia coli:
firstly, equipment:
test strains: staphylococcus aureus ATCC6538, escherichia coli 8099. The generation number of the above strains is 4 th generation, and PBS is used for preparing bacterial suspension.
Experimental samples: finished product 1, finished product 2 and finished product 3
Neutralizing agent: 3.9% D/E neutralized Broth
Secondly, the method comprises the following steps:
5. preparation of bacterial suspension: selecting bacteria with a content of 1 × 108CFU/mL～5×108CFU/mL bacterial suspension was subjected to neutralizer identification test.
6. And (3) identification test of a neutralizer: the test bacterium is Escherichia coli. The test groups are: (1) disinfectant + bacterial suspension, (2) (disinfectant + bacterial suspension) + neutralizer, (3) neutralizer + bacterial suspension, (4) (disinfectant + neutralizer) + bacterial suspension, (5) diluent + bacterial suspension, and (6) diluent + neutralizer + culture medium. Diluting the sample stock solution by 10 times in the same ratio as the neutralizer, and acting for 1.5 min. The experiment was repeated 3 times.
7. And (3) testing the killing performance: according to the quantitative sterilization test of the suspension, the finished product is 1, the action time is 1min, and the test is repeated for 3 times. The test environment temperature is 21-22 ℃.
8. The culture temperature is as follows: 35 ℃ plus or minus 2 DEG C
As a result:
1. Neutralizer identification test
3 repeated experiments prove that the average number of growing colonies in the group 1 is aseptic growth, and the average number of growing colonies in the group 2 is 1.4 x 103CFU/mL, similar average number of growing colonies in groups 3, 4, and 5, with an error rate of 4.76% between groups, and sterile growth in group 6 (Table 1).
TABLE 1 identification of product 1 neutralizer
Note: negative control sterile growth
2. Killing effect on staphylococcus aureus and escherichia coli
Repeated experiments for 3 times prove that the finished product 1 acts for 0.5min, the killing logarithm value of the finished product to staphylococcus aureus is more than 5.00, and the killing logarithm value of the finished product to escherichia coli is more than 5.00 (Table 2).
TABLE 2 results of killing Staphylococcus aureus and Escherichia coli in product 1
Taking 3.9% D/E neutralizing broth as neutralizer, acting for 1min, and killing the staphylococcus aureus with log value of more than 5.00 and Escherichia coli with log value of more than 5.00.
1. Neutralizer identification test
3 replicates demonstratedThe average number of growing colonies in group 1 was aseptically grown, and the average number of growing colonies in group 2 was 1.7X 103CFU/mL, similar average number of growing colonies in groups 3, 4, and 5, with an error rate of 2.27% between groups, and sterile growth in group 6 (Table 3).
TABLE 3 identification of product 2 neutralizer
Note: negative control sterile growth
2. Killing effect on staphylococcus aureus and escherichia coli
Repeated experiments for 3 times prove that the finished product 2 acts for 0.5min, the killing logarithm value of the finished product to staphylococcus aureus is more than 5.00, and the killing logarithm value of the finished product to escherichia coli is more than 5.00 (Table 4).
TABLE 4 results of killing Staphylococcus aureus and Escherichia coli in product 2
Taking 3.9% D/E neutralizing broth as neutralizer, and acting for 0.5min to obtain final product 2 with killing log value of greater than 5.00 for Staphylococcus aureus and killing log value of greater than 5.00 for Escherichia coli.
1. Neutralizer identification test
3 repeated experiments prove that the average number of growing colonies in the group 1 is aseptic growth, and the average number of growing colonies in the group 2 is 1.6 x 103CFU/mL, similar average number of growing colonies in groups 3, 4, and 5, with an error rate of 13.33% between groups, and sterile growth in group 6 (Table 5).
TABLE 5 identification of product 3 neutralizer
Note: negative control sterile growth
2. Killing effect on staphylococcus aureus and escherichia coli
Repeated experiments for 3 times prove that the finished product 3 acts for 0.5min, the killing logarithm value of the product to staphylococcus aureus is more than 5.00, and the killing logarithm value of the product to escherichia coli is more than 5.00 (Table 6).
TABLE 6 results of killing Staphylococcus aureus and Escherichia coli in product 3
3.9 percent of D/E neutralizing broth is taken as a neutralizer, the finished product acts for 0.5min, the killing log value of the product to staphylococcus aureus is more than 5.00, and the killing log value of the product to escherichia coli is more than 5.00.
Killing experiment of candida albicans:
firstly, equipment:
test strains: candida albicans ATCC 10231. The generation number of the above strains is 4 th generation, and PBS is used for preparing bacterial suspension.
Experimental samples: finished product 1, finished product 2 and finished product 3
Neutralizing agent: 3.9% D/E neutralized Broth
Secondly, the method comprises the following steps:
1. preparation of bacterial suspension: selecting bacteria with a content of 1 × 108CFU/mL～5×108CFU/mL bacterial suspension was subjected to neutralizer identification test.
2. And (3) identification test of a neutralizer: the test bacteria are Candida albicans. The test groups are: (1) disinfectant + bacterial suspension, (2) (disinfectant + bacterial suspension) + neutralizer, (3) neutralizer + bacterial suspension, (4) (disinfectant + neutralizer) + bacterial suspension, (5) diluent + bacterial suspension, and (6) diluent + neutralizer + culture medium. Diluting the sample stock solution by 10 times in the same ratio as the neutralizer, and acting for 1.5 min. The experiment was repeated 3 times.
3. And (3) testing the killing performance: according to the quantitative sterilization test of the suspension, the sample stock solution acts for 1min, and the test is repeated for 3 times. The test environment temperature is 21-22 ℃.
4. The culture temperature is as follows: 35 ℃ plus or minus 2 DEG C
As a result:
1. Neutralizer identification test
3 repeated experiments prove that the average number of growing colonies in the group 1 is aseptic growth, and the average number of growing colonies in the group 2 is 1.6 x 103CFU/mL, similar average number of growing colonies in groups 3, 4, and 5, with an error rate of 6.25% between groups, and sterile growth in group 6 (Table 7).
TABLE 7 identification of product 1 neutralizer
Note: negative control sterile growth
2. Killing effect on candida albicans
3 times of repeated tests prove that the finished product 1 acts for 1min, and the killing log value of the candida albicans is more than 4.00 (Table 8).
TABLE 8 results of killing Candida albicans by product 1
3.9 percent of D/E neutralizing broth is taken as a neutralizer, the finished product is acted for 1min, and the killing logarithm value of Candida albicans is more than 4.00.
1. Neutralizer identification test
3 repeated experiments prove that the average number of growing colonies in the group 1 is aseptic growth, and the average number of growing colonies in the group 2 is 1.6 x 103CFU/mL, similar average number of growing colonies in groups 3, 4, and 5, with an error rate of 9.89% between groups, and sterile growth in group 6 (Table 9).
TABLE 9 identification of product 2 neutralizer
Note: negative control sterile growth
2. Killing effect on candida albicans
3 times of repeated experiments prove that the finished product 2 acts for 1min, and the killing log value of the candida albicans is more than 4.00 (Table 10).
TABLE 10 results of Candida albicans killing for product 2
3.9 percent of D/E neutralizing broth is taken as a neutralizer, and the finished product 2 acts for 1min, and the killing logarithm value of Candida albicans is more than 4.00.
1. Neutralizer identification test
3 repeated experiments prove that the average number of growing colonies in the group 1 is aseptic growth, and the average number of growing colonies in the group 2 is 1.6 x 103CFU/mL, similar average number of growing colonies in groups 3, 4, and 5, with an error rate of 9.89% between groups, and sterile growth in group 6 (Table 11).
TABLE 11 identification of product 3 neutralizer
Note: negative control sterile growth
2. Killing effect on candida albicans
3 times of repeated experiments prove that the finished product 3 acts for 1min, and the killing log value of the candida albicans is more than 4.00 (Table 12).
TABLE 12 results of killing Candida albicans by product 3
3.9 percent of D/E neutralizing broth is taken as a neutralizer, the finished product is acted for 1min, and the killing logarithm value of Candida albicans is more than 4.00.
In conclusion, the invention can provide the no-wash hand disinfection gel which takes the cationic bactericide as the main bactericidal component, is compounded by the nonionic cellulose ether and the cationic bactericide, has stable performance, can quickly sterilize and long-acting bacteriostasis, has fresh and cool hand feeling without stickiness after use, is added with the effective skin care component, and can mildly care the hand, and the preparation method thereof.
The present invention has been described in detail with reference to the above examples, but the description is only for the preferred examples of the present invention and should not be construed as limiting the scope of the present invention. All equivalent changes and modifications made within the scope of the present invention shall fall within the scope of the present invention.
Claims (6)
1. A hand-washing-free disinfection gel is characterized in that: the hand-washing-free disinfection gel comprises the following components in parts by mass: 0.05 to 5 percent of cationic bactericide, 0.1 to 20 percent of skin-care humectant, 0.1 to 5 percent of thickening agent and the balance of purified water.
2. The no-wash hand sanitizer gel according to claim 1, wherein: the cationic bactericide is one or more of chlorhexidine gluconate, chlorhexidine acetate, polyhexamethylene biguanide hydrochloride, polyhexamethylene guanidine hydrochloride, benzalkonium bromide, benzalkonium chloride, benzethonium chloride, double-chain quaternary ammonium salt and polymer quaternary ammonium salt.
3. The no-wash hand sanitizer gel according to claim 1, wherein: the skin caring humectant is one or more of butanediol, glycerol, propylene glycol, sorbitol, polyethylene glycol, Aloe extract and herba Menthae extract.
4. The no-wash hand sanitizer gel according to claim 1, wherein: the thickener is one or more of polyvinyl alcohol, polyvinylpyrrolidone, xanthan gum, sodium alginate, carboxymethyl cellulose, hydroxypropyl methyl cellulose, hydroxybutyl methyl cellulose, ethyl methyl cellulose, carboxymethyl methyl cellulose, hydroxymethyl ethyl cellulose, hydroxypropyl cellulose and hydroxyethyl cellulose.
5. The no-wash hand sanitizer gel according to claim 1, wherein: the hand-washing-free disinfection gel comprises the following components in parts by mass: 0.05 to 2 percent of cationic bactericide, 2 to 10 percent of skin-care humectant, 0.1 to 1.5 percent of thickening agent and the balance of purified water.
6. A preparation method of a hand-washing-free disinfection gel is characterized by comprising the following steps: the preparation method of the hand-washing-free disinfection gel comprises the following steps:
the method comprises the following steps: uniformly dispersing the thickening agent in a skin-care humectant, standing and swelling to prepare a solution A;
step two: uniformly dispersing the cationic bactericide in purified water, and uniformly stirring to prepare a solution B;
step three: adding the solution A into the solution B, stirring uniformly, standing to remove bubbles, condensing, filling and sealing to obtain a finished product.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111838171A (en) * | 2020-08-14 | 2020-10-30 | 上海黛龙生物工程科技有限公司 | Compound disinfectant and preparation method thereof |
| CN113288860A (en) * | 2021-03-11 | 2021-08-24 | 江西车仆实业有限公司 | Convenient and easy-to-produce hand-washing-free disinfection gel and preparation method thereof |
| CN113349201A (en) * | 2021-07-05 | 2021-09-07 | 无锡宏霸医疗科技有限公司 | Ethanol-gel-free no-wash disinfectant and preparation method thereof |
| CN113952246A (en) * | 2021-12-06 | 2022-01-21 | 安福超威日化有限公司 | Cationic bacteriostatic hand-washing-free gel and preparation method thereof |
| CN114432209A (en) * | 2020-10-30 | 2022-05-06 | 安徽德莱康生物医疗科技有限公司 | Hand-protecting type washing-free disinfection gel and preparation method thereof |
| CN116898742A (en) * | 2023-09-13 | 2023-10-20 | 山东安捷高科消毒科技有限公司 | Hand disinfection gel capable of killing multiple drug-resistant bacteria and inactivating viruses and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102614113A (en) * | 2012-04-24 | 2012-08-01 | 杨定乾 | Compound washing-free disinfection gel |
| CN103768007A (en) * | 2012-10-26 | 2014-05-07 | 杭州元祺生物科技有限公司 | Medical disinfecting gel |
| CN105362103A (en) * | 2015-12-19 | 2016-03-02 | 南京巨鲨显示科技有限公司 | Quick-drying hand disinfection emulsion |
| CN109771315A (en) * | 2019-04-02 | 2019-05-21 | 凯斯芙生物科技(北京)有限公司 | A kind of disposable hand-wrist bones gel of environment-friendly type and preparation method thereof |
-
2020
- 2020-01-17 CN CN202010052407.4A patent/CN111135302A/en not_active Withdrawn
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102614113A (en) * | 2012-04-24 | 2012-08-01 | 杨定乾 | Compound washing-free disinfection gel |
| CN103768007A (en) * | 2012-10-26 | 2014-05-07 | 杭州元祺生物科技有限公司 | Medical disinfecting gel |
| CN105362103A (en) * | 2015-12-19 | 2016-03-02 | 南京巨鲨显示科技有限公司 | Quick-drying hand disinfection emulsion |
| CN109771315A (en) * | 2019-04-02 | 2019-05-21 | 凯斯芙生物科技(北京)有限公司 | A kind of disposable hand-wrist bones gel of environment-friendly type and preparation method thereof |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111838171A (en) * | 2020-08-14 | 2020-10-30 | 上海黛龙生物工程科技有限公司 | Compound disinfectant and preparation method thereof |
| CN114432209A (en) * | 2020-10-30 | 2022-05-06 | 安徽德莱康生物医疗科技有限公司 | Hand-protecting type washing-free disinfection gel and preparation method thereof |
| CN113288860A (en) * | 2021-03-11 | 2021-08-24 | 江西车仆实业有限公司 | Convenient and easy-to-produce hand-washing-free disinfection gel and preparation method thereof |
| CN113349201A (en) * | 2021-07-05 | 2021-09-07 | 无锡宏霸医疗科技有限公司 | Ethanol-gel-free no-wash disinfectant and preparation method thereof |
| CN113952246A (en) * | 2021-12-06 | 2022-01-21 | 安福超威日化有限公司 | Cationic bacteriostatic hand-washing-free gel and preparation method thereof |
| CN113952246B (en) * | 2021-12-06 | 2023-09-22 | 安福超威日化有限公司 | Cationic antibacterial hand-washing-free gel and preparation method thereof |
| CN116898742A (en) * | 2023-09-13 | 2023-10-20 | 山东安捷高科消毒科技有限公司 | Hand disinfection gel capable of killing multiple drug-resistant bacteria and inactivating viruses and preparation method thereof |
| CN116898742B (en) * | 2023-09-13 | 2023-12-22 | 山东安捷高科消毒科技有限公司 | Hand disinfection gel capable of killing multiple drug-resistant bacteria and inactivating viruses and preparation method thereof |
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