CN114948836B - Low alcohol disinfectant containing plant extracts and preparation method thereof - Google Patents

Low alcohol disinfectant containing plant extracts and preparation method thereof Download PDF

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CN114948836B
CN114948836B CN202210924188.3A CN202210924188A CN114948836B CN 114948836 B CN114948836 B CN 114948836B CN 202210924188 A CN202210924188 A CN 202210924188A CN 114948836 B CN114948836 B CN 114948836B
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parts
mass
plant extract
prepared
release agent
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CN114948836A (en
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周磊
周贵保
杜文虎
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Jiangxi Grass Coral Disinfection Products Co ltd
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Jiangxi Grass Coral Disinfection Products Co ltd
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Abstract

The invention relates to a production process of an alcohol disinfectant, in particular to a low-alcohol disinfectant containing plant extracts and a preparation method thereof. According to the invention, the nano-cellulose is used as an inner core, the silicon dioxide is used as an outer shell, and a unique core-shell structure is formed after carbonization, so that a novel slow-release agent is obtained, more plant extracts can be contained, and as the silicon dioxide grows by using the nano-cellulose as a carrier, most of formed pores are vertically directed to the central pores, so that an excellent slow-release effect is achieved, and the effective time of the plant extracts can be effectively prolonged. The low alcohol disinfectant containing the plant extracts is obtained by taking the two plant extracts of nerol and hydroxycitronellal as main disinfectants and utilizing the slow release agent for slow release, has good disinfection and bacteriostasis effects and long duration, and can also relieve fatigue and regulate emotion.

Description

Low alcohol disinfectant containing plant extracts and preparation method thereof
Technical Field
The invention relates to a production process of an alcohol disinfectant, in particular to a low-alcohol disinfectant containing plant extracts and a preparation method thereof.
Background
The 75% alcohol has excellent disinfection effect, but can have certain irritation effect on skin after being repeatedly used for many times, particularly, the skin damage condition of a first-line medical worker who uses the 75% alcohol disinfectant under the condition of long-term isolation clothes is serious, the skin of the first-line medical worker needs the alcohol disinfectant which can not damage the skin, the country has strict and definite regulations on disinfection product raw materials and the like, but the phenomenon that the skin of the medical worker is damaged due to long-term use of the alcohol disinfectant still exists. Furthermore, the bacteria have been found to be more and more resistant to cutaneous alcohol by a research survey conducted by Science relative Medicine, which found that enterococcus faecium has an increased resistance to high concentrations of alcohol, which increased resistance resulted in bacteria surviving for a longer period of time after exposure to alcohol; in addition, studies have shown that vancomycin-resistant enterococci also begin to adapt to alcohol, and the DNA of alcohol-resistant bacteria is mutated at specific genetic positions associated with cellular metabolism, and resistance to alcohol appears to have a complex genetic basis as well as resistance to antibiotics. Therefore, the method has potential risk by completely depending on the alcohol disinfectant with higher concentration, seeks for an external disinfection washing and care product with better antibacterial effect, higher safety and no stimulation, and has important application value for prevention and control of medical disinfection and daily disinfection.
In addition, since alcohol disinfectant has become popular, it is almost a necessary disinfectant product for every home. However, due to the high alcohol concentration, the inflammable characteristic of the alcohol has great potential safety hazard. The disinfecting alcohol is medical 75 degree ethanol, and can be used for disinfecting human body. Alcohol is flammable, and the vapor and air can form explosive mixtures, so that the alcohol can cause combustion and explosion when meeting open fire and high heat. Contact with the oxidant causes a chemical reaction or combustion. In a fire scene, the heated container is at risk of explosion. The steam is heavier than air and can be diffused to a far place at a lower position, and the steam can be ignited and reburnt when meeting open fire. Alcohol concentrations higher than 70% volatilize and increase the amount of flammable gases in the room air, which may cause deflagrations as long as there are small sparks in the air. In recent years, many alcohol disinfection solutions have been used improperly, which causes fire. This has an adverse effect on the storage and the widespread use of alcohol disinfectants. Therefore, low alcohol disinfection solution becomes a very valuable research direction.
Because low alcohol does not have excellent disinfection effect, new substances with disinfection and bacteriostasis effects need to be added to make up for the defect of insufficient disinfection and bacteriostasis performance of low alcohol. The plant source bacteriostatic agent is a medicament for preventing and treating plant diseases, which is processed by using certain parts of plants with bacteriostatic and bacteriostatic activities or extracting effective components of the parts and separated and purified monomer substances. Since the plant-derived bacteriostatic agent is derived from plants and is relatively safe, the plant-derived bacteriostatic agent is concerned by extensive researchers in recent years and becomes a hotspot of research on novel antibacterial agents. Natural plant extracts contain a large amount of substances having excellent antibacterial properties, such as flavones, polyols, aldehydes, etc. And the substance with antibacterial activity extracted from these natural plants has high solubility in alcohol, and is very suitable for the development of low alcohol. However, the defect is also obvious, compared with 75-degree alcohol disinfectant, the low-alcohol disinfectant containing plant extracts has higher production cost, and flavone, polyalcohol, aldehyde and other substances with bacteriostatic functions are as same as alcohol, are extremely volatile and cannot inhibit bacteria for a long time, so that workers still need to repeatedly coat and use for many times, which not only increases the use cost, but also increases the damage of the disinfectant to the skin.
CN 111972444A discloses a production process for preparing a low alcohol disinfectant containing plant components by adopting a wine brewing process, wherein alcohol, a cactus extract and a honeysuckle flower extract are mixed to obtain the low alcohol disinfectant containing the plant components. Although the plant extract has excellent disinfection and bacteriostasis effects, the plant extract has the defects of no long-acting disinfection and bacteriostasis, and the plant extract is directly adopted, is not purified, has poor solubility and is easy to generate impurities such as precipitate and the like.
Therefore, it is necessary to develop a low alcohol disinfectant solution capable of disinfecting for a long time.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a low alcohol disinfectant containing plant extracts and a preparation method thereof.
A low alcohol disinfectant containing plant extracts comprises the following raw materials in parts by mass: 0.4-0.5 part of polyhexamethylene biguanide hydrochloride, 0.1-0.2 part of didecyl dimethyl ammonium bromide, 0.5-1 part of plant extract, 1-2 parts of plant extract slow release agent, 3-4 parts of aloe freeze-dried powder, 0.1-1 part of hydroxyethyl cellulose, 16-18 parts of absolute ethyl alcohol and 73.3-78.9 parts of water.
The plant extract is at least one of nerol and hydroxycitronellal; preferably, the plant extract is prepared from nerol and hydroxycitronellal according to the mass ratio of (1-2): (1-2) mixing.
The preparation method of the plant extract sustained-release agent comprises the following steps:
s1, mixing 20-21 parts by mass of ethyl orthosilicate and 18-19 parts by mass of absolute ethyl alcohol, and stirring at the speed of 200-300r/min for 20-40min to obtain a solution A; then taking 18-19 parts of absolute ethyl alcohol, 9-10 parts of water and 0.5-0.6 part of hydrochloric acid to mix, then stirring at the speed of 200-300r/min for 20-40min to obtain a solution B, then adding the solution B into the solution A, and stirring at the rotating speed of 100-200r/min at the temperature of 30-40 ℃ for 20-40min to react to obtain a hydrolysate;
s2, adding 4-5 parts of nano cellulose into the hydrolysate prepared in the step S1 by mass, adjusting the pH value to 6.5-7.5 by using 0.03-0.05mol/L ammonia water, stirring at the rotating speed of 200-300r/min for reaction for 10-20min, and cooling to room temperature to obtain wet gel;
s3, adding 5-15 parts by mass of absolute ethyl alcohol into the wet gel prepared in the step S2, aging for 2-3 days, filtering to obtain gel, and drying at-20- (-40) DEG C for 24-48h to obtain aerogel;
s4, under the nitrogen atmosphere, carbonizing the aerogel prepared in the step S3 at 300-400 ℃ for 2-4h to obtain the nano silicon dioxide aerogel with the core-shell structure;
s5, crushing the nano silicon dioxide aerogel with the core-shell structure prepared in the step S4 to 5-10 microns, drying to obtain a slow release agent, mixing 10-15 parts by mass of the plant extract and 20-30 parts by mass of the slow release agent, stirring at a rotating speed of 100-200r/min for 3-5min, and drying to obtain the plant extract slow release agent.
A method for preparing low alcohol disinfectant containing plant extracts comprises the following steps:
(1) Mixing 0.1-1 part by mass of hydroxyethyl cellulose, 1-2 parts by mass of plant extract slow-release agent and 5-10 parts by mass of water, and stirring at the rotating speed of 200-300r/min for 20-40min to obtain emulsion A;
(2) Adding 3-4 parts of aloe freeze-dried powder, 0.4-0.5 part of polyhexamethylene biguanide hydrochloride, 0.1-0.2 part of didecyl dimethyl ammonium bromide, 0.5-1 part of plant extract and 16-18 parts of absolute ethyl alcohol into the emulsion A prepared in the step (1) according to the mass parts, mixing, stirring at the rotating speed of 200-300r/min for 10-20min, finally adding 63.3-73.9 parts of water, and continuously stirring for 10-20min to obtain the low alcohol disinfectant containing the plant extract.
The nerol is extracted from Citrus sinensis, fructus Citri Sarcodactylis of Rutaceae, or Lonicera japonica of Caprifoliaceae, is a natural plant extract, and has antibacterial effect. On the other hand, the rose-orange fragrance tea has pleasant rose and orange flower fragrance, the fragrance is relatively flat and mild, the citrus-like fruity fragrance is slight, the nerol is an isomer of geraniol, the fragrance is softer and more beautiful than the geraniol, the rose-orange fragrance tea is relatively cleaner, and the rose-orange fragrance tea has fresh fragrance and citrus fragrance, can effectively relieve fatigue, reduce depression and depression caused by high-intensity work, is very suitable for volunteers to use, can be used for sterilizing in a shelter or a household room, and can effectively relieve depression mood caused by isolation. The hydroxycitronellal also has the fragrance of linden, lily of the valley and fresh green grass, is widely applied to the preparation of spices, cannot cover the excellent antibacterial performance of the hydroxycitronellal, and has excellent antibacterial effect on common pathogenic bacteria such as staphylococcus aureus, staphylococcus epidermidis, escherichia coli, pseudomonas aeruginosa and the like. The nerol and the hydroxycitronellal mainly act on cell walls of bacteria, and both can damage cell membranes of the bacteria, so that the permeability of the bacteria is changed, and the bacteriostatic effect is achieved. The two are used together, so that the bacteriostatic effect is better.
Both nerol and hydroxycitronellal have good solubility in ethanol water solution, and can achieve good antibacterial effect only in a very small amount. However, the defects of the disinfectant are the same as those of most disinfectant, and the disinfectant is volatile and cannot inhibit bacteria for a long time.
Therefore, in order to solve the problem, the invention firstly takes the silicon dioxide aerogel as a slow release agent to adsorb nerol and hydroxycitronellal to prolong the action time of the disinfectant, and because the aerogel has low density, large surface area and dense pore channels, a large amount of plant extracts can be adsorbed and stored, and the smaller pore diameter is not beneficial to the violent movement of molecules, thereby playing the effect of delaying the volatilization of the plant extracts. However, according to the bacteriostatic test, the slow release effect of the silica aerogel is not ideal. It is considered that this is because when the aerogel is crushed into a particle size of 10 μm or less, the pore size length of the aerogel becomes short, and the performance of both the storage plant extract and the sustained-release plant extract thereof becomes poor. However, if the particle size is kept large, precipitation is likely to occur, and the appearance is impaired. Therefore, the nano-cellulose is added into the tetraethoxysilane hydrolysate, hydroxyl silicon generated by hydrolysis grows by taking the nano-cellulose as a carrier, the nano-cellulose wrapped by silicon dioxide is obtained, the nano-cellulose wrapped by the silicon dioxide is carbonized at high temperature, the volume is reduced, and a core-shell structure is formed, so that more plant extracts can be accommodated, and because the silicon dioxide grows by taking the nano-cellulose as the carrier, most of formed pores are vertically directed to the center, so that an excellent slow-release effect is achieved, and the effective time of the plant extracts can be effectively prolonged.
The invention has the beneficial effects
1. The novel sustained-release agent is prepared by taking the nano-cellulose as an inner core and the silicon dioxide as an outer shell, and forming a unique core-shell structure after carbonization, so that more plant extracts can be contained, and because the silicon dioxide grows by taking the nano-cellulose as a carrier, most of formed pores are vertically directed to the central pores, so that an excellent sustained-release effect is achieved, and the effective time of the plant extracts can be effectively prolonged.
2. The low alcohol disinfectant containing the plant extracts is obtained by taking the two plant extracts of nerol and hydroxycitronellal as main disinfectants and utilizing the slow release agent for slow release, has good disinfection and bacteriostasis effects and long duration, and can also relieve fatigue and regulate emotion.
Detailed Description
Aloe lyophilized powder is purchased from Xian Yiyu jade biotech GmbH.
Nanocellulose, brand: krama, purchased from shanghai ziming reagent factory (krama).
Polyhexamethylene biguanide hydrochloride, CAS No.: 32289-58-0.
Hydroxyethyl cellulose, CAS No.: 9004-62-0.
The hydrochloric acid concentration used in the examples was 28% by weight.
Example 1
A method for preparing low alcohol disinfectant containing plant extracts comprises the following steps:
(1) Mixing 0.6 part of hydroxyethyl cellulose and 8 parts of water by mass, and stirring at the rotating speed of 280r/min for 30min to obtain emulsion A;
(2) And (2) adding 3.6 parts of aloe freeze-dried powder, 0.491 part of polyhexamethylene biguanide hydrochloride, 0.198 part of didecyl dimethyl ammonium bromide, 0.8 part of plant extract and 16.2 parts of absolute ethyl alcohol into the emulsion A prepared in the step (1) according to the parts by mass, mixing at the rotating speed of 280r/min for 15min, finally adding 68.511 parts of water, and continuing to stir for 15min to obtain the low-alcohol disinfectant containing the plant extract.
The plant extract is prepared from nerol and hydroxycitronellal according to the mass ratio of 1:1 are mixed.
Example 2
A method for preparing low alcohol disinfectant containing plant extracts comprises the following steps:
(1) Mixing 0.6 part of hydroxyethyl cellulose, 1.6 parts of plant extract slow-release agent and 8 parts of water according to parts by mass, and stirring at the rotating speed of 280r/min for 30min to obtain emulsion A;
(2) And (2) adding 3.6 parts of aloe freeze-dried powder, 0.491 part of polyhexamethylene biguanide hydrochloride, 0.198 part of didecyl dimethyl ammonium bromide, 0.8 part of plant extract and 16.2 parts of absolute ethyl alcohol into the emulsion A prepared in the step (1) according to the mass parts, mixing at the rotating speed of 280r/min for 15min, finally adding 68.511 parts of water, and continuing to stir for 15min to obtain the low-alcohol disinfectant containing the plant extract.
The preparation method of the plant extract sustained-release agent comprises the following steps:
s1, mixing 20 parts of tetraethoxysilane and 18 parts of absolute ethyl alcohol by mass, and stirring for 30min at the speed of 280r/min to obtain a solution A; then taking 18 parts of absolute ethyl alcohol, 9 parts of water and 0.5 part of hydrochloric acid to mix, then stirring for 30min at the speed of 280r/min to obtain a solution B, then adding the solution B into the solution A, and stirring and reacting for 30min at the rotating speed of 180r/min at the temperature of 35 ℃ to obtain a hydrolysate;
s2, adjusting the pH value of the hydrolysate obtained in the step S1 to 7 by using 0.04mol/L ammonia water, stirring and reacting for 15min at the rotating speed of 280r/min, and cooling to room temperature to obtain wet gel;
s3, adding 10 parts by mass of absolute ethyl alcohol into the wet gel prepared in the step S2, ageing for 2 days, filtering to obtain gel, and drying at-30 ℃ for 48 hours to obtain aerogel;
s4, under the nitrogen atmosphere, carbonizing the aerogel prepared in the step S3 at 320 ℃ for 3 hours to obtain silicon dioxide aerogel;
and S5, crushing the silicon dioxide aerogel prepared in the step S4 to 5 microns, drying to obtain a slow release agent, mixing 15 parts of plant extract and 30 parts of slow release agent by mass, stirring at a rotating speed of 180r/min for 4min, and drying to obtain the plant extract slow release agent.
The plant extract is prepared from nerol and hydroxycitronellal according to the mass ratio of 1:1 are mixed.
Example 3
A preparation method of low alcohol disinfectant containing plant extracts comprises the following steps:
(1) Mixing 0.6 parts of hydroxyethyl cellulose, 1.6 parts of plant extract slow release agent and 8 parts of water by mass, and stirring at the rotating speed of 280r/min for 30min to obtain emulsion A;
(2) And (2) adding 3.6 parts of aloe freeze-dried powder, 0.491 part of polyhexamethylene biguanide hydrochloride, 0.198 part of didecyl dimethyl ammonium bromide, 0.8 part of plant extract and 16.2 parts of absolute ethyl alcohol into the emulsion A prepared in the step (1) according to the mass parts, mixing at the rotating speed of 280r/min for 15min, finally adding 68.511 parts of water, and continuing to stir for 15min to obtain the low-alcohol disinfectant containing the plant extract.
The preparation method of the plant extract sustained-release agent comprises the following steps:
s1, mixing 20 parts of tetraethoxysilane and 18 parts of absolute ethyl alcohol by mass, and stirring for 30min at the speed of 280r/min to obtain a solution A; then 18 parts of absolute ethyl alcohol, 9 parts of water and 0.5 part of hydrochloric acid are mixed, stirred for 30min at the speed of 280r/min to obtain a solution B, then the solution B is added into the solution A, and stirred and reacted for 30min at the temperature of 35 ℃ at the rotating speed of 180r/min to obtain a hydrolysate;
s2, adding 4 parts of nano cellulose into the hydrolysate prepared in the step S1 in parts by mass, adjusting the pH value to 7 by using 0.04mol/L ammonia water, stirring and reacting at the rotating speed of 280r/min for 15min, and cooling to room temperature to obtain wet gel;
s3, adding 10 parts by mass of absolute ethyl alcohol into the wet gel prepared in the step S2, ageing for 2 days, filtering to obtain gel, and drying at-30 ℃ for 48 hours to obtain aerogel;
s4, under the nitrogen atmosphere, carbonizing the aerogel prepared in the step S3 at 320 ℃ for 3h to obtain the nano silicon dioxide aerogel with the core-shell structure;
and S5, crushing the nano silicon dioxide aerogel with the core-shell structure prepared in the step S4 to 5 microns, drying to obtain a slow release agent, mixing 15 parts of plant extract and 30 parts of the slow release agent by mass, stirring at a rotating speed of 180r/min for 4min, and drying to obtain the plant extract slow release agent.
The plant extract is prepared from nerol and hydroxycitronellal according to the mass ratio of 1:1 by mixing.
Example 4
A method for preparing low alcohol disinfectant containing plant extracts comprises the following steps:
(1) Mixing 0.6 part of hydroxyethyl cellulose, 1.6 parts of plant extract slow-release agent and 8 parts of water according to parts by mass, and stirring at the rotating speed of 280r/min for 30min to obtain emulsion A;
(2) And (2) adding 3.6 parts of aloe freeze-dried powder, 0.491 part of polyhexamethylene biguanide hydrochloride, 0.198 part of didecyl dimethyl ammonium bromide, 0.8 part of plant extract and 16.2 parts of absolute ethyl alcohol into the emulsion A prepared in the step (1) according to the parts by mass, mixing at the rotating speed of 280r/min for 15min, finally adding 68.511 parts of water, and continuing to stir for 15min to obtain the low-alcohol disinfectant containing the plant extract.
The preparation method of the plant extract sustained-release agent comprises the following steps:
s1, mixing 20 parts of tetraethoxysilane and 18 parts of absolute ethyl alcohol by mass, and stirring at the speed of 280r/min for 30min to obtain a solution A; then 18 parts of absolute ethyl alcohol, 9 parts of water and 0.5 part of hydrochloric acid are mixed, stirred for 30min at the speed of 280r/min to obtain a solution B, then the solution B is added into the solution A, and stirred and reacted for 30min at the temperature of 35 ℃ at the rotating speed of 180r/min to obtain a hydrolysate;
s2, adding 4 parts of nano cellulose into the hydrolysate prepared in the step S1 in parts by mass, adjusting the pH value to 7 by using 0.04mol/L ammonia water, stirring and reacting at the rotating speed of 280r/min for 15min, and cooling to room temperature to obtain wet gel;
s3, adding 10 parts by mass of absolute ethyl alcohol into the wet gel prepared in the step S2, aging for 2 days, filtering to obtain gel, and drying at-30 ℃ for 48 hours to obtain aerogel;
s4, under the nitrogen atmosphere, carbonizing the aerogel prepared in the step S3 at 320 ℃ for 3 hours to obtain nano silicon dioxide aerogel with a core-shell structure;
and S5, crushing the nano silicon dioxide aerogel with the core-shell structure prepared in the step S4 to 5 microns, drying to obtain a slow release agent, mixing 15 parts of plant extract and 30 parts of the slow release agent by mass, stirring at a rotating speed of 180r/min for 4min, and drying to obtain the plant extract slow release agent.
The plant extract is nerol.
Example 5
A method for preparing low alcohol disinfectant containing plant extracts comprises the following steps:
(1) Mixing 0.6 part of hydroxyethyl cellulose, 1.6 parts of plant extract slow-release agent and 8 parts of water according to parts by mass, and stirring at the rotating speed of 280r/min for 30min to obtain emulsion A;
(2) And (2) adding 3.6 parts of aloe freeze-dried powder, 0.491 part of polyhexamethylene biguanide hydrochloride, 0.198 part of didecyl dimethyl ammonium bromide, 0.8 part of plant extract and 16.2 parts of absolute ethyl alcohol into the emulsion A prepared in the step (1) according to the mass parts, mixing at the rotating speed of 280r/min for 15min, finally adding 68.511 parts of water, and continuing to stir for 15min to obtain the low-alcohol disinfectant containing the plant extract.
The preparation method of the plant extract sustained-release agent comprises the following steps:
s1, mixing 20 parts of tetraethoxysilane and 18 parts of absolute ethyl alcohol by mass, and stirring for 30min at the speed of 280r/min to obtain a solution A; then 18 parts of absolute ethyl alcohol, 9 parts of water and 0.5 part of hydrochloric acid are mixed, stirred for 30min at the speed of 280r/min to obtain a solution B, then the solution B is added into the solution A, and stirred and reacted for 30min at the temperature of 35 ℃ at the rotating speed of 180r/min to obtain a hydrolysate;
s2, adding 4 parts of nano cellulose into the hydrolysate prepared in the step S1 in parts by mass, adjusting the pH value to 7 by using 0.04mol/L ammonia water, stirring and reacting at the rotating speed of 280r/min for 15min, and cooling to room temperature to obtain wet gel;
s3, adding 10 parts by mass of absolute ethyl alcohol into the wet gel prepared in the step S2, ageing for 2 days, filtering to obtain gel, and drying at-30 ℃ for 48 hours to obtain aerogel;
s4, under the nitrogen atmosphere, carbonizing the aerogel prepared in the step S3 at 320 ℃ for 3h to obtain the nano silicon dioxide aerogel with the core-shell structure;
and S5, crushing the nano silicon dioxide aerogel with the core-shell structure prepared in the step S4 to 5 microns, drying to obtain a slow release agent, mixing 15 parts of plant extract and 30 parts of the slow release agent by mass, stirring at a rotating speed of 180r/min for 4min, and drying to obtain the plant extract slow release agent.
The plant extract is hydroxycitronellal.
Comparative example 1
A low alcohol disinfectant containing plant components is prepared by referring to the scheme of example 1 in patent CN 111972444A. The specific scheme is as follows:
a production process for preparing low alcohol disinfectant containing plant components by adopting a wine brewing process comprises the following components in parts by mass: 40 parts of organic sorghum flour, 30 parts of glutinous rice flour, 50 parts of wheat starch, 4 parts of an additive, 100 parts of water, 10 parts of lotus leaf powder, 30 parts of a plant additive, 10 parts of a pH regulator, 5 parts of yeast, 0.5 part of polyhexamethylene biguanide hydrochloride and 0.5 part of didecyldimethyl ammonium bromide;
the pH adjuster is a phosphate buffer at pH = 6.0.
The preparation process comprises the following steps:
s1: preparing low-alcohol;
(1) Taking the wheat starch, the organic sorghum flour and the glutinous rice flour, and further feeding the wheat starch, the organic sorghum flour and the glutinous rice flour into a bulking machine for extrusion and bulking;
(2) Taking out the materials produced by extrusion and expansion in the expander, and putting the materials into a stirrer;
(3) Adding the additive into a stirrer, and stirring the materials for 5min by the stirrer to ensure full mixing;
(4) Taking out the materials in the stirrer, spreading and cooling to 20 ℃;
(5) Further putting the materials into a stirrer, adding yeast, and stirring the materials for 5min by the stirrer to ensure full mixing;
(6) Taking out clear liquid generated by material fermentation, and filtering the clear liquid generated by material fermentation by using a filtering membrane;
(7) Collecting and distilling the filtered clear liquid to obtain finished alcohol;
s2: adding water, polyhexamethylene biguanide hydrochloride solution, didecyldimethyl ammonium bromide solution and plant additive into the finished product alcohol, and further mixing and stirring for 15min;
s3: adding lotus leaf powder into the mixed solution in the step S2, and further mixing and stirring for 10min;
s4: adjusting the pH value; adding a pH regulator into the mixed solution stirred and mixed in the step S3 for regulating the pH value of the mixed solution to obtain a low alcohol disinfectant finished product containing plant components;
s5: bottling and storing the finished low alcohol disinfectant containing plant components.
The additive is 8wt% of amylase.
The plant additive is cactus extract, honeysuckle flower extract, folium artemisiae argyi extract, aloe extract, onion extract, citric acid extract, clove extract, fructus cnidii extract, sophora flower extract, spina date seed extract, waxberry extract, reed rhizome extract, chamomile extract, ash bark extract, mint extract, liquorice extract and walnut extract, and the weight ratio of the extracts is as follows: 1:2:1:2:3:2:1:2:2:3:1:2:1:2:3:1:1.
test example 1
Quantitative kill test for staphylococcus aureus suspension
1. Test samples: 20mL of the low alcohol disinfectant containing plant extracts obtained in examples 1 to 5 and the low alcohol disinfectant containing plant components obtained in comparative example 1 were placed in a test tube and placed in a sterile ventilated place for 24 hours, and then the test tube was washed with 16.2wt% alcohol and made to a volume of 20mL to obtain test samples.
2. Staphylococcus aureus ATCC 6538 (provided by rikah, guangdong, inc.): get the meridian 24 smallFresh slant culture (generation 5) is first washed with diluent (PBS) and then diluted with 3.0% bovine serum albumin diluent to reach 1 × 10 of recovered bacteria 7 cfu/mL~5×10 7 cfu/mL。
3. Neutralizing agent: 4 fold D/E neutralizes the broth.
4. Tryptic gland Soy agar Medium (TSA).
5. Local class 100 air cleaning laboratory.
6. An electric heating constant temperature water bath DZKW-D-2 (IE-0253).
LRH-250F Biochemical incubator (IE-0065).
The detection method comprises the following steps:
1. the inspection basis is as follows: sterilization Specification 2002 edition 2.1.1.7 and 2.1.1.5.
2. And (3) testing the environment: the temperature is 22.5-24.3 ℃, and the relative humidity is 52-57%.
3.1 neutralizer identification test
The test was carried out in an electric thermostat water bath at 20 ℃. The test sample and other liquid to be tested are put in an electric heating constant temperature water bath kettle for preheating for 5min at 20 ℃, and then 6 groups are divided for carrying out neutralization effect test determination. The test microorganism is Staphylococcus aureus, the neutralizing agent is 4 times D/E neutralizing broth, the killing time is 0.5min, and the neutralizing time is 10min. Samples were counted by pouring onto dishes of tryptic Chen Dadou agar medium (TSA). The experiment was repeated 3 times.
And (3) testing results: through detection: the neutralizing agent contains 4 times of D/E neutralizing broth, can neutralize residual test samples to kill staphylococcus aureus, and has no adverse effect on the growth and culture medium of tested bacteria.
3.2 quantitative kill test of suspensions
The test was carried out in an electric thermostat water bath at 20 ℃ and 1 ℃. Adding 4.0mL of test sample into a test tube, placing the test sample in an electric heating constant-temperature water bath kettle at 20 ℃ for preheating for 5min, adding 1.0mL of bacterial suspension, acting for 0.5min, adding 0.5mL of bacterial suspension into 4.5mL of neutralizing agent, neutralizing for 10min, sampling, and pouring a trypsin Chen Dadou agar culture medium (TSA) to check the number of residual viable bacteria. The test is simultaneously provided with positive and negative controls. The experiment was repeated 3 times.
The results are shown in Table 1.
Table 1: quantitative killing test result of staphylococcus aureus suspension
Figure 753872DEST_PATH_IMAGE002
As can be seen from Table 1, after 24 hours of air drying, the low alcohol disinfectant containing plant extracts prepared in example 1 almost completely volatilizes antibacterial substances, and the killing log value of the disinfectant on Staphylococcus aureus is only more than or equal to 1. This is because the plant extract slow-release agent is not added in example 1, and after 24 hours of volatilization, the plant extract with the bacteriostatic effect in the disinfectant is almost volatilized. After 24 hours of ventilation drying, the low alcohol disinfectant containing the plant extract prepared in the embodiment 2 only has the killing logarithm value of more than or equal to 3 to staphylococcus aureus, and does not meet the requirement of GB 27951-2011 'hygienic requirement for skin disinfectant' 4.3.3.1. Although the slow release agent made of silicon dioxide aerogel is added, the aerogel has low density, large surface area and dense pore channels, can adsorb and store a large amount of plant extracts, and has small pore diameter which is not beneficial to the violent movement of molecules, thereby playing the effect of delaying the volatilization of the plant extracts. However, according to the bacteriostatic test, the slow release effect of the silica aerogel is not ideal. It is considered that this is because when the aerogel is crushed into a particle size of 10 μm or less, the pore size length of the aerogel becomes short, and the performance of both the storage plant extract and the sustained-release plant extract thereof becomes poor. However, if the particle size is kept large, precipitation is likely to occur, and the appearance is impaired. After 24 hours of ventilation drying, the low alcohol disinfectant containing the plant extract prepared in the embodiment 3 has a killing log value of more than or equal to 5 for staphylococcus aureus, shows excellent bacteriostatic effect and meets the requirement of GB 27951-2011 'hygienic requirement for skin disinfectants' 4.3.3.1. This shows that the low alcohol disinfectant containing plant extracts prepared by the scheme of example 3 can be used for 24 hours for bacteriostasis without repeated disinfection, and the service life is greatly prolonged. The invention considers that the nano-cellulose is added into the tetraethoxysilane hydrolysate, so that hydroxyl silicon generated by hydrolysis grows by taking the nano-cellulose as a carrier to obtain the nano-cellulose wrapped by silicon dioxide, and the nano-cellulose wrapped by the silicon dioxide is carbonized at high temperature to reduce the volume and form a core-shell structure, so that more plant extracts can be accommodated. Examples 4 and 5 show that the single use of nerol or hydroxycitronellal can kill staphylococcus aureus with a killing log value of not less than 4 after 24 hours of ventilation drying, and the bacteriostatic effect is weakened compared with the synergistic effect of nerol and hydroxycitronellal used in example 3. The invention considers that the slow release effect of the slow release agent on a single substance is not weakened, but the single nerol or hydroxycitronellal has insufficient bacteriostatic effect on staphylococcus aureus, and the nerol or hydroxycitronellal are used synergistically to achieve better bacteriostatic effect. Comparative example 1 referring to the scheme of example 1 in patent CN 111972444A, a low alcohol disinfectant containing plant components was prepared as in example 1, and since no sustained release agent was added, after 24 hours of aeration drying, the bacteriostatic substances were almost completely volatilized, and thus the bacteriostatic effect was remarkably reduced.
Test example 2
Stability test
1. The test samples were: after the mild alcohol disinfectant containing plant extracts prepared in examples 1 to 5 and the mild alcohol disinfectant containing plant components prepared in comparative example 1 were packaged together, test samples were obtained.
2. An instrument device: HS-150 incubator (IE-0185), aiglent 7820A gas chromatograph (IE-0282).
3. All reagents used in the test are analytically pure.
4. The detection basis is as follows: second method of Sterilization Specification 2002 edition 2.2.3.2.1 and 2.2.1.2.11.
5. Storage conditions are as follows: sealing, and storing in a constant temperature and humidity box at 37 deg.C and 78% relative humidity for 90 days. 3. Detecting the environment: the temperature was 16.2 ℃ and the relative humidity was 54%.
Test protocol: the test sample was stored in a constant temperature and humidity chamber at 37 ℃ and a relative humidity of 78% for 90 days, and then color change, presence or absence of precipitation, and presence or absence of delamination of the sample were observed, and the change in the concentration of the plant extract was detected by a gas chromatograph. The results are shown in Table 2.
Table 2: results of stability test
Figure 139854DEST_PATH_IMAGE004
As can be seen from Table 2, the low alcohol disinfectant containing plant extracts according to examples 1 to 3 of the present invention showed no change in color, no precipitation, no delamination after standing for 90 days, and showed excellent stability as compared to comparative example 1. This is because the plant extract was directly used in comparative example 1 without purification, and the solubility was poor, and impurities such as precipitates were easily generated. From the concentration reduction rate of the plant extract, the reduction rate of the low alcohol disinfectant containing the plant extract prepared in example 3 is the lowest, because the slow release effect of the slow release agent adopted by the disinfectant is the best, and the plant extract volatilized from the disinfectant can be continuously supplemented, while the slow release effect of the slow release agent prepared by the silicon dioxide aerogel adopted in example 2 is poorer than that of the nano silicon dioxide aerogel with the core-shell structure prepared in example 3, and the concentration of the plant extract in the disinfectant is not fully supplemented, so the reduction rate is slightly higher. Example 1 no sustained release agent was added, so the rate of decrease was the greatest.

Claims (2)

1. A preparation method of a low alcohol disinfectant containing plant extracts is characterized by comprising the following steps:
(1) Mixing 0.1-1 parts of hydroxyethyl cellulose, 1-2 parts of plant extract slow release agent and 5-10 parts of water by mass, and stirring at the rotating speed of 200-300r/min for 20-40min to obtain emulsion A;
(2) Adding 3-4 parts of aloe freeze-dried powder, 0.4-0.5 part of polyhexamethylene biguanide hydrochloride, 0.1-0.2 part of didecyl dimethyl ammonium bromide, 0.5-1 part of plant extract and 16-18 parts of absolute ethyl alcohol into the emulsion A prepared in the step (1), mixing at the rotating speed of 200-300r/min for 10-20min, finally adding 63.3-73.9 parts of water, and continuing to stir for 10-20min to obtain the low alcohol disinfectant containing the plant extract;
the plant extract is prepared from nerol and hydroxycitronellal according to the mass ratio of 1:1, mixing;
the preparation method of the plant extract sustained-release agent comprises the following steps:
s1, mixing 20-21 parts by mass of ethyl orthosilicate and 18-19 parts by mass of absolute ethyl alcohol, and stirring at the speed of 200-300r/min for 20-40min to obtain a solution A; then taking 18-19 parts of absolute ethyl alcohol, 9-10 parts of water and 0.5-0.6 part of hydrochloric acid to mix, then stirring at the speed of 200-300r/min for 20-40min to obtain a solution B, then adding the solution B into the solution A, and stirring at the rotating speed of 100-200r/min at the temperature of 30-40 ℃ for 20-40min to react to obtain a hydrolysate;
s2, adding 4-5 parts of nano cellulose into the hydrolysate prepared in the step S1 by mass, adjusting the pH value to 6.5-7.5 by using 0.03-0.05mol/L ammonia water, stirring at the rotating speed of 200-300r/min for reaction for 10-20min, and cooling to room temperature to obtain wet gel;
s3, adding 5-15 parts by mass of absolute ethyl alcohol into the wet gel prepared in the step S2, aging for 2-3 days, filtering to obtain gel, and drying at-20 to-40 ℃ for 24-48 hours to obtain aerogel;
s4, under the nitrogen atmosphere, carbonizing the aerogel prepared in the step S3 at 300-400 ℃ for 2-4h to obtain the nano silicon dioxide aerogel with the core-shell structure;
s5, crushing the nano silicon dioxide aerogel with the core-shell structure prepared in the step S4 to 5-10 microns, drying to obtain a slow release agent, mixing 10-15 parts by mass of the plant extract and 20-30 parts by mass of the slow release agent, stirring at a rotating speed of 100-200r/min for 3-5min, and drying to obtain the plant extract slow release agent.
2. A low alcohol disinfectant containing plant extracts, which is characterized by being prepared by the preparation method of the low alcohol disinfectant containing plant extracts of claim 1.
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