Synthetic method of antibacterial and bacteriostatic gel

Abstract

The invention belongs to the technical field of disinfection product application, and particularly relates to a synthesis method of antibacterial and bacteriostatic gel. According to the method, polyphenol compounds, flavonoid compounds and alkaloid compounds in Chinese chestnut waste are obtained through extraction of the Chinese chestnut waste and dissolved in glycerin by adding glycerin, meanwhile, the bonding capacity of the gel is improved through cooperation with arrangement of polyethyleneimine and acrylic acid and through the reaction of polyethyleneimine and acrylic acid, and therefore the gel is not prone to cracking. And in cooperation with water absorption of glycerol and acrylic acid, long-acting moisturizing and long-acting degerming are ensured.

Description

Technical Field

[0001] The present invention belongs to the technical field of the application of disinfection products, and particularly relates to a synthesis method of an antibacterial and bacteriostatic gel. Background Art

[0002] During the industrial production process of chestnuts, a large number of by-products are usually generated, such as flowers, chestnut burs, leaves, skins, branches and shells. Developing these wastes and converting them into valuable biological resources can not only obtain economic, ecological and social benefits, but also promote the healthy development of the chestnut industry. Among them, the leaves, skins and branches of chestnuts contain a large amount of polyphenolic compounds, flavonoid compounds and alkaloid compounds, and these compounds themselves have antioxidant, antibacterial, whitening and immune-enhancing abilities, and have potential research value.

[0003] At the same time, hand sanitizer is an extremely common item in daily life. Hand sanitizer is mainly used to clean the hands and maintain the cleanliness of the hands. Hand sanitizer is also set in some public places. Due to the large number of people in public places, there may be more bacteria. Once you touch an object with your hands, there is a possibility of residual bacteria on the hands. Using hand sanitizer to clean the hands reduces the probability of bacterial infection to a certain extent.

[0004] In order to achieve the purpose of green environmental protection, existing gels mostly use natural ingredients as bactericides, such as aloe vera, tea polyphenols, etc. Although these natural ingredients can achieve the purpose of sterilization, they are not waste products themselves, and a large amount of cultivation is required or it will affect the use of other products (such as cosmetics). Therefore, how to use the wastes in the industrial production process of chestnuts to prepare handwashing gels to achieve the purpose of sterilization and cost reduction. Summary of the Invention

[0005] In view of the technical problems existing in the existing natural ingredient hand sanitizer, the present invention proposes a synthesis method of an antibacterial and bacteriostatic gel that is simple in method, convenient in operation and can effectively utilize the wastes of chestnut leaves, skins and branches to achieve the purpose of antibacterial and bacteriostatic.

[0006] To achieve the above purpose, the technical solution adopted by the present invention is: the present invention provides a synthesis method of an antibacterial and bacteriostatic gel, which includes the following components: 5-10 parts of water-soluble chitosan; 5-8 parts of surfactin; 10-15 parts of gel polymer excipient; 0.01 part - 0.02 part of polyethyleneimine; 0.01 part - 0.02 part of acrylic acid; 4-8 parts of glycerol; 5-10 parts of chestnut waste extract; 0.01 part - 0.02 part of photoinitiator, and its synthesis method includes the following steps:

[0007] a. First, put the weighed polyethyleneimine, acrylic acid and photoinitiator into deionized water and continuously stir until they are completely dispersed to obtain solution A;

[0008] b. Add surfactin to deionized water and ultrasonicate for 10 - 15 min until it is completely dissolved. Then add chestnut waste extract and glycerol to it and continuously stir for 10 - 15 min to obtain Solution B.

[0009] c. Add the gel polymer excipient to deionized water, stir magnetically for 2 - 3 h, and then let it stand at room temperature for 8 - 12 h to fully hydrate and obtain Solution C.

[0010] d. Slowly add Solution A and Solution B to Solution C. At the same time, add water-soluble chitosan and continuously stir and mix until the gel is initially formed. Then let it stand at room temperature for 12 h to naturally swell, and the antibacterial and bacteriostatic gel is obtained.

[0011] Preferably, the surfactin is a secondary metabolite secreted extracellularly by Bacillus.

[0012] Preferably, the gel polymer excipient is at least one of carbomer 934 and hydroxypropyl methylcellulose.

[0013] Preferably, the photoinitiator is 2 - hydroxy - 2 - methyl - 1 - [4 - (2 - hydroxyethoxy)phenyl] - 1 - propanone.

[0014] Preferably, the chestnut waste extract is chestnut leaves, chestnut bark, and chestnut branches discarded during the production of chestnuts.

[0015] Preferably, the extraction method of the chestnut waste extract includes the following steps:

[0016] A. First, wash, air-dry, and then bake the chestnut leaves, chestnut bark, and chestnut branches discarded during the production of chestnuts in an oven at 60 °C until constant weight, pulverize, and sieve the powder through a 60 - mesh sieve for later use.

[0017] B. Weigh the chestnut waste powder, place the chestnut waste powder in a 50% ethanol solution according to a solid - liquid ratio of 1:20, ultrasonically extract for 20 min, repeat the extraction twice, centrifuge the extract at 8000 r·min-1 for 5 min, filter by suction, concentrate under reduced pressure, and vacuum freeze - dry for 12 h to obtain the chestnut waste extract.

[0018] Compared with the prior art, the advantages and positive effects of the present invention are as follows:

[0019] The present invention provides a method for synthesizing an antibacterial and bacteriostatic gel. By extracting chestnut waste, polyphenolic compounds, flavonoid compounds, and alkaloid compounds therein are obtained and dissolved in glycerol by adding glycerol. Meanwhile, with the setting of polyethyleneimine and acrylic acid, the reaction of polyethyleneimine and acrylic acid is utilized to improve the bonding ability of the gel. Then, combined with the water absorption of glycerol and acrylic acid, long-term moisture retention and long-term sterilization are ensured. Detailed implementation mode

[0020] In order to more clearly understand the above-mentioned objects, features, and advantages of the present invention, the present invention will be further described below in conjunction with embodiments. It should be noted that, without conflict, the embodiments of the present application and the features in the embodiments can be combined with each other.

[0021] Many specific details are set forth in the following description in order to fully understand the present invention. However, the present invention can also be implemented in other ways different from those described herein. Therefore, the present invention is not limited by the specific embodiments disclosed in the following specification.

[0022] According to the analysis of the extracts of chestnut leaves, bark, and branches waste, it can be determined that gallic acid, protocatechuic acid, ferulic acid, ellagic acid, protocatechuic aldehyde, vanillic acid, syringic acid, coniferyl acid, bamboo acid, coumarin, scopoletin, and myricetin, quercitol, kaempferol, quercetin, etc. are contained in the chestnut leaves, bark, and branches waste. These extracts have the effects of antioxidation, antibacterial, and anti-inflammatory, but they have the problem of being insoluble or poorly soluble in water. Therefore, in the formula of the present invention, glycerol is added. Glycerol has two functions in the gel provided by the present invention. One is to dissolve these extracts, and the second function is that glycerol has water absorption, and its water absorption effect can maintain moisture for a long time.

[0023] Polyethyleneimine has a high cation density and activity and can undergo chemical reactions with a variety of substances. In the antibacterial field, polyethyleneimine exhibits certain antibacterial activity, especially has a certain inhibitory effect on Gram-negative bacteria such as Escherichia coli. At the same time, it also has a certain water absorption.

[0024] The addition of acrylic acid has two purposes. One is that the two polyelectrolytes with opposite charges have a large number of anionic -COO - and cationic -NH3 + groups, which can form a strong cohesive and adhesive electrostatic effect, making the gel have lasting stability. The other is that the toxicity of polyethyleneimine comes from the cation. By using the reaction of the two, its toxicity can be reduced, and only the stability after the combination of the two is retained.

[0025] Example 1, this example provides an antibacterial and bacteriostatic gel

[0026] First, weigh 5 parts by weight of water-soluble chitosan; 5 parts of surfactin; 10 parts of gel polymer excipient; 0.01 part of polyethyleneimine; 0.01 part of acrylic acid; 4 parts of glycerol; 5 parts of chestnut waste extract; 0.01 part of photoinitiator, and set aside.

[0027] Then, put the weighed polyethyleneimine, acrylic acid and photoinitiator into deionized water and continuously stir until they are completely dispersed to obtain Solution A. Here, the photoinitiator is 2-hydroxy-2-methyl-1-[4-(2-hydroxyethoxy)phenyl]-1-propanone, that is, photoinitiator I2959. Its purpose is to promote the photopolymerization reaction of polyethyleneimine and acrylic acid to form a hydrogel.

[0028] Then, add surfactin (secondary metabolite secreted extracellularly by Bacillus) into deionized water and ultrasonicate for 10 - 15 min until it is completely dissolved. The secondary metabolite of Bacillus has an inhibitory effect on a broad spectrum of viruses, such as influenza virus, coronavirus, rhinovirus, etc., showing good antiviral activity. Add the chestnut waste extract and glycerol into it and continuously stir for 10 - 15 min to obtain Solution B. The main purpose of Solution B is to antibacterial and bacteriostatic.

[0029] Next, add Carbomer 934 into deionized water, stir magnetically for 2 - 3 h and then stand at room temperature for 8 - 12 h to make it fully hydrated to obtain Solution C. Here, Carbomer 934 is mainly used as a thickener.

[0030] Slowly add Solution A and Solution B into Solution C. At the same time, add water-soluble chitosan. The purpose of water-soluble chitosan here is also antibacterial and bacteriostatic. Continuously stir and mix until the gel is initially formed, and then stand at room temperature for 12 h to allow it to swell naturally, thus obtaining the antibacterial and bacteriostatic gel.

[0031] Example 2, this example provides an antibacterial and bacteriostatic gel

[0032] First, weigh 10 parts by weight of water-soluble chitosan; 8 parts of surfactin; 15 parts of gel polymer excipient; 0.02 part of polyethyleneimine; 0.02 part of acrylic acid; 8 parts of glycerol; 10 parts of chestnut waste extract; 0.02 part of photoinitiator, and set aside.

[0033] Then, put the weighed polyethyleneimine, acrylic acid and photoinitiator into deionized water and continuously stir until they are completely dispersed to obtain Solution A. Here, the photoinitiator is 2-hydroxy-2-methyl-1-[4-(2-hydroxyethoxy)phenyl]-1-propanone, that is, photoinitiator I2959. Its purpose is to promote the photopolymerization reaction of polyethyleneimine and acrylic acid to form a hydrogel.

[0034] Then, add surfactin (an extracellular secondary metabolite produced by Bacillus) into deionized water, and ultrasonicate for 10 - 15 min until it is completely dissolved. The secondary metabolite of Bacillus has an inhibitory effect on a broad spectrum of viruses, such as influenza virus, coronavirus, rhinovirus, etc., showing good antiviral activity. Add chestnut waste extract and glycerol into it, and continuously stir for 10 - 15 min to obtain Solution B. The main purpose of Solution B is to antibacterial and bacteriostatic.

[0035] Next, add hydroxypropyl methylcellulose into deionized water, stir magnetically for 2 - 3 h, and then let it stand at room temperature for 8 - 12 h to fully hydrate to obtain Solution C. Here, the role of hydroxypropyl methylcellulose in the gel is mainly as a water-soluble polymer compound to form a thermoreversible gel.

[0036] Slowly add Solution A and Solution B into Solution C. At the same time, add water-soluble chitosan. The purpose of the water-soluble chitosan here is also for antibacterial and bacteriostatic. Continuously stir and mix until the gel is initially formed, and then let it stand at room temperature for 12 h to allow it to swell naturally, thus obtaining the antibacterial and bacteriostatic gel.

[0037] Example 3, this example provides an antibacterial and bacteriostatic gel

[0038] First, weigh 8 parts of water-soluble chitosan; 7 parts of surfactin; 6 parts of hydroxypropyl methylcellulose and 6 parts of carbomer 934; 0.015 parts of polyethyleneimine; 0.015 parts of acrylic acid; 6 parts of glycerol; 8 parts of chestnut waste extract; 0.015 parts of photoinitiator, and set aside.

[0039] Then, add the weighed polyethyleneimine, acrylic acid and photoinitiator into deionized water and continuously stir until they are completely dispersed to obtain Solution A. Here, the photoinitiator is 2-hydroxy-2-methyl-1-[4-(2-hydroxyethoxy)phenyl]-1-propanone, that is, photoinitiator I2959. Its purpose is to promote the photopolymerization reaction of polyethyleneimine and acrylic acid to form a hydrogel.

[0040] Then, add surfactin (an extracellular secondary metabolite produced by Bacillus) into deionized water, and ultrasonicate for 10 - 15 min until it is completely dissolved. The secondary metabolite of Bacillus has an inhibitory effect on a broad spectrum of viruses, such as influenza virus, coronavirus, rhinovirus, etc., showing good antiviral activity. Add chestnut waste extract and glycerol into it, and continuously stir for 10 - 15 min to obtain Solution B. The main purpose of Solution B is to antibacterial and bacteriostatic.

[0041] Next, add hydroxypropyl methylcellulose and carbomer 934 together into deionized water, stir magnetically for 2 - 3 h, and then let it stand at room temperature for 8 - 12 h to fully hydrate to obtain Solution C.

[0042] Slowly add Solution A and Solution B into Solution C. Meanwhile, add water-soluble chitosan. The purpose of the water-soluble chitosan here is also for antibacterial and bacteriostatic purposes. Continuously stir and mix until the gel is initially formed, and then let it stand at room temperature for 12 h to allow natural swelling, thus obtaining the antibacterial and bacteriostatic gel.

[0043] Test: Test the antibacterial and bacteriostatic gels prepared in the above three examples. The test reference standards are: "Disinfection Technical Specification" (2002 Edition) 2.2.1.4, 2.2.3.2.1, "Technical Specifications for Cosmetics Safety" (2015 Edition), "Hygienic Standards for Disposable Sanitary Products" GB 15979-2002, and "Procedures and Methods for Toxicological Evaluation of the Safety of Disinfectants" GB / T 38496-2020 issued by the National Health Commission.

[0044] The evaluation basis is: "Disinfection Technical Specification" (2002 Edition), "Hygienic Standards for Disposable Sanitary Products" GB 15979-2002, "Technical Specifications for Cosmetics Safety" (2015 Edition), "Technical Requirements for Hygienic and Safety Evaluation of Disinfection Products" WS628-2018, and Enterprise Standard Q / MJ 003-2022.

[0045] Test conclusion:

[0046] 1. Stability test: For the tested bacteriostatic gel sample (batch number: 20241218), after sealing the sample and placing it in a constant temperature oven at 54 °C for 14 days, the degradation rate of the active ingredient is 7.2%. According to the provisions of "Disinfection Technical Specification" (2002 Edition) 2.2.3.2.1 issued by the National Health Commission, the validity period of this product can be set as 12 months.

[0047] 2. pH value: The pH value of the tested bacteriostatic gel sample (batch number: 20241218) is 4.2 (25 °C).

[0048] 3. Lead, arsenic, and mercury: The lead content of the tested bacteriostatic gel sample (batch number: 20241218) is 0.08 mg / kg, the arsenic content is 0.006 mg / kg, and the mercury content is 0.012 mg / kg, which meets the limit values in Table 2 of Chapter 1 of "Technical Specifications for Cosmetics Safety" (2015 Edition).

[0049] 4. Bacteriostatic test: For the tested bacteriostatic gel sample (batch number: 20241218), after acting for 2.0 minutes, the bacteriostatic rates against Escherichia coli, Staphylococcus aureus, and Candida albicans can all reach over 90%, showing strong bacteriostatic effects and meeting the relevant requirements of "Hygienic Standards for Disposable Sanitary Products" GB 15979-2002.

[0050] 5. Microbiological index detection: The detection results of the microbiological indexes of the tested bacteriostatic gel sample (batch number: 20241218) meet the relevant requirements of the "Hygienic Standard for Disposable Sanitary Products GB15979-2002".

[0051] 6. Mucous membrane irritation test: According to the mucous membrane irritation intensity grading standard in the "Disinfection Technical Specification" (2002 edition) of the National Health Commission, the result of the mucous membrane irritation test of the submitted original gel sample on New Zealand rabbits is non-irritating, meeting the safety requirements of 2.3.13.1 in the "Disinfection Technical Specification" (2002 edition) of the National Health Commission.

[0052] The above are only the preferred embodiments of the present invention, and are not intended to limit the present invention in other forms. Any person skilled in the art may use the disclosed technical content to make changes or modifications into equivalent embodiments with equivalent changes and apply them to other fields. However, any simple modification, equivalent change and modification made to the above embodiments based on the technical essence of the present invention without departing from the technical solution content of the present invention still fall within the protection scope of the technical solution of the present invention.

Claims

1. A method for synthesizing an antibacterial and antibacterial gel, characterized in that: The invention comprises the following ingredients: 5-10 parts of water-soluble chitosan; 5-8 parts of surfactant; 10-15 parts of gel polymer excipient; 0.01-0.02 parts of polyethyleneimine; 0.01-0.02 parts of acrylic acid; 4-8 parts of glycerol; 5-10 parts of chestnut waste extract; and 0.01-0.02 parts of photoinitiator. The synthesis method comprises the following steps: a. First, weigh polyethyleneimine, acrylic acid and photoinitiator and place them in deionized water and stir them continuously until they are completely dispersed to obtain solution A; b. Add surfactant to deionized water, sonicate for 10-15 minutes to completely dissolve it, then add chestnut waste extract and glycerol, and stir continuously for 10-15 minutes to obtain solution B; c. Add the gel polymer excipient to deionized water, stir magnetically for 2-3 hours, and then stand at room temperature for 8-12 hours to fully hydrate it to obtain solution C; d. Slowly add solution A and solution B into solution C. At the same time, add water-soluble chitosan and keep stirring until the gel is initially formed. Then let it stand at room temperature for 12 hours to allow it to swell naturally to obtain the antibacterial and antimicrobial gel.

2. The method for synthesizing an antibacterial and antibacterial gel according to claim 1, characterized in that: The surfactin is a secondary metabolite produced by Bacillus and secreted outside the cell.

3. The method for synthesizing an antibacterial and antibacterial gel according to claim 1, characterized in that: The gel polymer excipient is at least one of carbomer 934 and hydroxypropyl methylcellulose.

4. The method for synthesizing an antibacterial and antibacterial gel according to claim 1, characterized in that: The photoinitiator is 2-hydroxy-2-methyl-1-[4-(2-hydroxyethoxy)phenyl]-1-propanone.

5. The method for synthesizing an antibacterial and antibacterial gel according to claim 1, characterized in that: The chestnut waste extract is chestnut leaves, chestnut bark and chestnut branches discarded in the chestnut production process.

6. The method for synthesizing an antibacterial and antibacterial gel according to claim 1, characterized in that: The method for extracting the chestnut waste extract comprises the following steps: A. First, wash and air-dry the discarded chestnut leaves, chestnut bark and chestnut branches in the chestnut production process, dry them in a 60°C oven to constant weight, crush them, and pass the powder through a 60-mesh sieve for later use; B. Weigh the chestnut waste powder, put it into 50% ethanol solution at a solid-liquid ratio of 1:20, and ultrasonically extract it for 20 minutes. Repeat the extraction twice. The extract was heated at 8000 r / min. -1 The extract was centrifuged for 5 min, filtered, concentrated under reduced pressure, and freeze-dried in vacuum for 12 h to obtain the chestnut waste extract.