A bacteriostatic composition, bacteriostatic liquid, applications and methods of preparation

Abstract

The present application relates to the technical field of skin bacteriostasis, and particularly relates to a bacteriostatic composition, application of the bacteriostatic composition, bacteriostatic liquid prepared from the bacteriostatic composition and a preparation method of the bacteriostatic liquid. The bacteriostatic composition comprises the following components in parts by weight: forsythia suspensa extract 0.1-0.8 parts, honeysuckle extract 0.1-0.8 parts, citrus extract 0.1-0.8 parts, o-cymen-5-ol 0.05-0.15 parts and benzalkonium chloride 0.01-0.08 parts. The bacteriostatic composition has excellent bacteriostatic effect, and is mild and non-irritating to skin and mucosa, and can be used to prepare bacteriostatic leave-on products for disinfecting children's skin.

Description

TECHNICAL FIELD

[0001] The present application relates to the field of skin bacteriostatic technology, and in particular to a bacteriostatic composition, application thereof and a bacteriostatic liquid prepared from the bacteriostatic composition and a preparation method thereof. BACKGROUND

[0002] Children's toys and daily clothes are easy to contact with children's sweat and saliva, and are prone to breed bacteria. Even if the supplies look clean to the naked eye, the surface and interior thereof can have a very high bacterial density. Children's hands contact toys, daily clothes and other articles every day, which are the most contacted parts of the body with bacteria throughout the day. At the same time, children also eat snacks or apply skin supplies with their hands, and the bacteria in the hands and the nail gap can enter the body through the hand-mouth route, causing physical discomfort or diseases. Therefore, it is necessary to carry out daily protection of children's hand hygiene, especially in outdoor or public places. However, it is obviously difficult to wash hands at any time and anywhere, and therefore a free-washing bacteriostatic product for children is more convenient for daily bacteriostasis.

[0003] At present, the bacteriostatic components of the free-washing product commonly used for hand bacteriostasis mainly include medical alcohol, hypochlorous acid, benzalkonium chloride and polyhexamethylene guanidine hydrochloride. Among them, alcohol is a medium-efficiency disinfectant, and hypochlorous acid is a high-efficiency disinfectant, both of which have strong disinfection effects. Benzalkonium chloride and polyhexamethylene guanidine hydrochloride are low-efficiency disinfectants, and have relatively poor disinfection effects. However, alcohol has disinfection effect only when the concentration is above 70%, and the alcohol with such a concentration has certain irritation to the skin and mucous membrane, and can cause strong discomfort or damage to the eyes if it is accidentally contacted. In addition, the alcohol with such a concentration is flammable, and has safety hazards during storage. Hypochlorous acid is unstable, and can be decomposed and lose effectiveness if not properly stored. In addition, the smell of hypochlorous acid is not good, and therefore a large amount of additives are often used in the hand bacteriostatic free-washing product containing hypochlorous acid to maintain the stability and cover the bad smell. However, the use of additives also increases the insecurity of the product. SUMMARY

[0004] In view of the problems of skin and mucous membrane irritation and instability of the current free-washing product for hand bacteriostasis, the present application provides a bacteriostatic composition, a bacteriostatic liquid, application and a preparation method.

[0005] To achieve the above-mentioned application purposes, the embodiments of the present application adopt the following technical solutions:

[0006] In one aspect, the present application provides a bacteriostatic composition, which comprises the following components in the following weight proportions: 0.1-0.8 parts of forsythia suspensa extract, 0.1-0.8 parts of honeysuckle extract, 0.1-0.8 parts of citrus extract, 0.05-0.15 parts of o-cymen-5-ol and 0.01-0.08 parts of benzalkonium chloride.

[0007] In the bacteriostatic composition, both benzalkonium chloride and o-cymen-5-ol have broad bactericidal properties, strong bactericidal effect, and can kill and inhibit various bacteria, fungi, viruses and the like, and have little irritation to skin and mucous membrane. Meanwhile, o-cymen-5-ol also has ultraviolet absorption and antioxidant properties, can absorb ultraviolet rays of specific wavelengths, thereby enhancing the stability of other components in the composition to ultraviolet light, and inhibiting oxidation of other components in the composition.

[0008] The forsythia extract has different degrees of inhibitory effect on Staphylococcus aureus, Shigella dysenteriae, Salmonella typhi, Vibrio cholerae, Escherichia coli, Pseudomonas aeruginosa, Bordetella pertussis, Mycobacterium tuberculosis, Streptococcus pneumoniae, Streptococcus haemolyticus, and influenza virus, and also has antifungal effect. The honeysuckle extract has certain inhibitory and killing effect on various pathogenic bacteria such as Staphylococcus aureus, Streptococcus haemolyticus, Escherichia coli, Shigella dysenteriae, Vibrio cholerae, Salmonella typhi, Salmonella paratyphi, Streptococcus pneumoniae, Streptococcus meningitidis, Pseudomonas aeruginosa, Mycobacterium tuberculosis, Shigella dysenteriae, Streptococcus mutans, and can inhibit influenza virus, orphan virus, herpes virus, and leptospira. The citrus extract contains rich polyphenols and flavonoids, has good antioxidant and bacteriostatic effect, and has significant comprehensive resistance to Penicillium, green mold and anthrax fungus.

[0009] The present application finds in the research that, compared with benzalkonium chloride and o-cymen-5-ol alone, the combination of the forsythia extract, the honeysuckle extract and the citrus extract with benzalkonium chloride and o-cymen-5-ol not only still has excellent bacteriostatic effect, but also can enhance skin elasticity, promote mucous membrane repair, significantly reduce the irritation of benzalkonium chloride and o-cymen-5-ol to skin and mucous membrane, so that the bacteriostatic composition is non-irritating, mild and safe to skin and mucous membrane, and can be used to prepare skin bacteriostatic leave-on products suitable for children. Meanwhile, the bacteriostatic composition has no bleaching or other damaging effect on textiles, and even if the clothes are stained during use, the clothes will not be damaged, so the bacteriostatic composition can also be used for disinfection of children's clothes.

[0010] Preferably, the bacteriostatic composition comprises the following ingredients in the following weight proportions: 0.1-0.5 parts of forsythia extract, 0.1-0.5 parts of honeysuckle extract, 0.1-0.5 parts of citrus extract, 0.05-0.1 parts of o-cymen-5-ol and 0.02-0.07 parts of benzalkonium chloride.

[0011] Preferably, the bacteriostatic composition comprises the following ingredients in the following weight proportions: 0.1-0.2 parts of forsythia extract, 0.1-0.2 parts of honeysuckle extract, 0.1-0.2 parts of citrus extract, 0.06-0.08 parts of o-cymen-5-ol and 0.03-0.05 parts of benzalkonium chloride.

[0012] Preferably, the bacteriostatic composition comprises the following ingredients in parts by weight: 0.1 parts of forsythia suspensa extract, 0.1 parts of honeysuckle extract, 0.2 parts of citrus extract, 0.08 parts of o-cymen-5-ol and 0.05 parts of benzalkonium chloride. The bacteriostatic composition obtained from the above ingredients has more excellent bacteriostatic effect and is more mild and non-irritating to the skin and mucous membrane.

[0013] Alternatively, the forsythia suspensa extract is prepared by ultrasonic extraction of forsythia suspensa with 15-25% v / v ethanol aqueous solution at 25-35℃, first at a frequency of 25-35 kHz for 20-30 min and then at a frequency of 50-70 kHz for 15-25 min; after extraction, the obtained filtrate is concentrated to 1.2-1.3 g / ml to obtain the forsythia suspensa extract; wherein the mass of the 15-25% v / v ethanol aqueous solution is 5-8 times the mass of the forsythia suspensa.

[0014] The forsythia suspensa extract obtained by the above preparation method can further improve the bacteriostatic effect of the bacteriostatic composition and make the irritability of the bacteriostatic composition more significantly reduced when combined with the honeysuckle extract and the citrus extract.

[0015] Alternatively, the honeysuckle extract is prepared by ultrasonic extraction of honeysuckle with 45-65% v / v ethanol aqueous solution at 45-60℃, first at a frequency of 20-35 kHz for 20-30 min and then at a frequency of 55-70 kHz for 15-20 min; after extraction, the obtained filtrate is concentrated to 1.2-1.3 g / ml to obtain the honeysuckle extract; wherein the mass of the 45-65% v / v ethanol aqueous solution is 7-10 times the mass of the honeysuckle.

[0016] The honeysuckle extract obtained by the above preparation method has better bacteriostatic effect and can reduce the irritability of the bacteriostatic composition.

[0017] Optionally, the preparation method of the citrus extract is as follows: crushing the citrus peels, boiling with water for 20-40 min, filtering, discarding the filtrate, and obtaining filter residue a; adding water equivalent to 5-8 times the mass of the citrus peels to the filter residue a, adding cellulase and pectinase, mixing uniformly, enzymolysis at 40-50℃ for 2-3 h, then increasing the temperature to 90-95℃ for 5-10 min to inactivate the enzymes, filtering, and obtaining filtrate b and filter residue b; adding 45-55% v / v ethanol aqueous solution to the filter residue b, ultrasonic extraction at a frequency of 40-55 kHz for 30-45 min, filtering, and obtaining filtrate c; mixing the filtrate b and the filtrate c, and concentrating to 1.2-1.3 g / ml, and obtaining the citrus extract; wherein the mass of the 45-55% v / v ethanol aqueous solution is 5-8 times the mass of the citrus peels, the mass of the cellulase is 1-1.5% of the mass of the citrus peels, and the mass of the pectinase is 3-4% of the mass of the citrus peels.

[0018] The citrus extract prepared by the above preparation method has excellent effects of improving the bacteriostatic effect and reducing the irritation to the skin and mucous membrane in the composition, and can further improve the bacteriostatic effect of the composition and reduce the irritation.

[0019] In the second aspect, the embodiments of the present application also provide applications of the above bacteriostatic composition in preparing a skin bacteriostatic leave-on product for children or a bacteriostatic product for the surface of clothes.

[0020] The above bacteriostatic composition has excellent bacteriostatic effect, is mild and safe to the skin and mucous membrane, and does not damage clothes, and can be prepared into a skin bacteriostatic leave-on product for children or a bacteriostatic product for the surface of clothes, such as a bacteriostatic gel or a bacteriostatic liquid.

[0021] In the third aspect, the embodiments of the present application also provide a bacteriostatic liquid comprising the above bacteriostatic composition. The bacteriostatic liquid can be directly applied to the skin of hands or other parts, or can be filled into a spray device as a spray to be sprayed on the skin or the surface of clothes.

[0022] The bacteriostatic liquid comprises the following ingredients in parts by weight:

[0023]

[0024]

[0025] The humectant is at least one selected from propylene glycol, butylene glycol and glycerol;

[0026] The solubilizing agent is PEG-40 hydrogenated castor oil;

[0027] The antioxidant is ethylenediaminetetraacetic acid disodium salt (EDTA disodium salt);

[0028] The preservative is phenoxyethanol.

[0029] The above preferred raw materials are all common components of daily-use products suitable for children's skin, high in safety, non-irritating to the skin and mucous membrane, and will not cause obvious discomfort of the skin and mucous membrane of children within the above dosage range. Among them, allantoin has the effects of light-proof, sterilization, preservation, oxidation resistance and analgesia, which helps to improve the stability of the bacteriostatic liquid, prolong the shelf life, and help to maintain skin moisture and promote skin and mucous membrane tissue repair.

[0030] In a fourth aspect, the present application also provides a preparation method of the above bacteriostatic liquid, comprising the following steps:

[0031] The humectant is added to the water, and stirred until dissolved;

[0032] The o-cymen-5-ol and benzalkonium chloride are added, and stirred to disperse uniformly;

[0033] The solubilizer, forsythia extract, honeysuckle extract, citrus extract, essence, antioxidant, preservative and allantoin are added, and mixed uniformly to obtain the bacteriostatic liquid.

[0034] The temperature for adding the humectant is preferably 75-85℃, which can accelerate the dissolution of the humectant and improve the production efficiency.

[0035] The solution temperature when the o-cymen-5-ol and benzalkonium chloride are added is preferably 48-52℃, which can accelerate the dissolution of the o-cymen-5-ol and benzalkonium chloride components, and at the same time avoid decomposition or reaction between them to generate impurities at high temperature.

[0036] The solution temperature when the remaining components are added is preferably 43-47℃, which can promote the forsythia extract, honeysuckle extract and citrus extract to mix uniformly with other components with the assistance of the solubilizer, and at the same time avoid decomposition of the above components at higher temperature. DETAILED DESCRIPTION

[0037] In order to make the purpose, technical scheme and advantages of the present application more clear, the present application will be further described in detail below in combination with specific examples. It should be understood that the specific examples described herein are only used to explain the present application, and are not used to limit the present application.

[0038] The experimental methods used in the following examples are all conventional methods in the art unless otherwise specified.

[0039] The forsythia and honeysuckle used in the following examples all meet the relevant provisions of each medicinal material in the text of the Chinese Pharmacopoeia (2015 edition) Part I.

[0040] The raw materials, reagents and the like used in the following examples were obtained from commercial sources unless otherwise specified.

[0041] Examples 1-11

[0042] Preparation of the bacteriostatic composition of the present application: the components in each example include the following ingredients in the proportions by weight as shown in Table 1:

[0043] Table 1 Bacteriostatic composition of Examples 1-11

[0044]

[0045] In Example 1, the preparation method of the forsythia extract is ultrasonic extraction with 20% v / v ethanol aqueous solution at 30°C: first ultrasonic extraction at 30 kHz for 25 min, then ultrasonic extraction at 60 kHz for 20 min; after extraction, filtration is performed, and the obtained filtrate is reduced to 1.25 g / ml under reduced pressure, and then obtained; wherein the mass of the 20% v / v ethanol aqueous solution is 6 times the mass of the forsythia;

[0046] The preparation method of the honeysuckle extract is ultrasonic extraction with 55% v / v ethanol aqueous solution at 50°C: first ultrasonic extraction at 30 kHz for 25 min, then ultrasonic extraction at 60 kHz for 18 min; after extraction, filtration is performed, and the obtained filtrate is reduced to 1.25 g / ml under reduced pressure, and then obtained; wherein the mass of the 55% v / v ethanol aqueous solution is 8 times the mass of the honeysuckle;

[0047] The preparation method of the citrus extract is as follows: the citrus peel is crushed, boiled with water for 30 min, filtered, and the filtrate is discarded to obtain filter residue a; 7 times the mass of the citrus peel in water is added to the filter residue a, and cellulase and pectinase are added, mixed uniformly, and enzymolysis is performed at 45°C for 2.5 h, then the temperature is increased to 93°C for 7 min to inactivate the enzyme, and then filtration is performed to obtain filtrate b and filter residue b; 50% v / v ethanol aqueous solution is added to the filter residue b, ultrasonic extraction is performed at 50 kHz for 40 min, and then filtration is performed to obtain filtrate c; the filtrate b and the filtrate c are mixed, and then reduced to 1.2 g / ml under reduced pressure, and then obtained; wherein the mass of the 55% v / v ethanol aqueous solution is 7 times the mass of the citrus peel, the mass of the cellulase is 1.25% of the mass of the citrus peel, and the mass of the pectinase is 3.5% of the mass of the citrus peel.

[0048] In Example 2, the preparation method of the forsythia extract is ultrasonic extraction with 15% v / v ethanol aqueous solution at 25°C: first ultrasonic extraction at 25 kHz for 30 min, then ultrasonic extraction at 50 kHz for 25 min; after extraction, filtration is performed, and the obtained filtrate is reduced to 1.2 g / ml under reduced pressure, and then obtained; wherein the mass of the 15% v / v ethanol aqueous solution is 5 times the mass of the forsythia;

[0049] The preparation method of the honeysuckle extract is ultrasonic extraction with 45% v / v ethanol aqueous solution at 45°C: first ultrasonic extraction at 20 kHz for 30 min, and then ultrasonic extraction at a frequency of 55 kHz for 20 min; after the extraction is completed, filtration is performed, and the obtained filtrate is concentrated under reduced pressure to 1.2 g / ml, and then the honeysuckle extract is obtained; wherein the mass of the 45% v / v ethanol aqueous solution is 7 times the mass of the honeysuckle;

[0050] The preparation method of the citrus extract is as follows: the citrus peel is crushed, water is added for decoction for 20 min, and then filtration is performed, and the filtrate is discarded, and filter residue a is obtained; water equivalent to 5 times the mass of the citrus peel is added to the filter residue a, and cellulase and pectinase are further added, and then mixed uniformly, and then enzymolysis is performed at 40°C for 3 h, and then the temperature is increased to 90°C for 10 min for enzyme inactivation, and then filtration is performed, and filter residue b and filtrate b are obtained; 45% v / v ethanol aqueous solution is added to the filter residue b, and ultrasonic extraction is performed at a frequency of 40 kHz for 45 min, and then filtration is performed, and filtrate c is obtained; the filtrate b and the filtrate c are mixed, and then concentrated under reduced pressure to 1.2 g / ml, and then the citrus extract is obtained; wherein the mass of the 55% v / v ethanol aqueous solution is 5 times the mass of the citrus peel, the mass of the cellulase is 1% of the mass of the citrus peel, and the mass of the pectinase is 3% of the mass of the citrus peel.

[0051] In Example 3, the preparation method of the forsythia extract is ultrasonic extraction with 25% v / v ethanol aqueous solution at 35°C: first ultrasonic extraction at 35 kHz for 20 min, and then ultrasonic extraction at a frequency of 70 kHz for 15 min; after the extraction is completed, filtration is performed, and the obtained filtrate is concentrated under reduced pressure to 1.3 g / ml, and then the forsythia extract is obtained; wherein the mass of the 25% v / v ethanol aqueous solution is 8 times the mass of the forsythia;

[0052] The preparation method of the honeysuckle extract is ultrasonic extraction with 65% v / v ethanol aqueous solution at 60°C: first ultrasonic extraction at 35 kHz for 20 min, and then ultrasonic extraction at a frequency of 70 kHz for 15 min; after the extraction is completed, filtration is performed, and the obtained filtrate is concentrated under reduced pressure to 1.3 g / ml, and then the honeysuckle extract is obtained; wherein the mass of the 65% v / v ethanol aqueous solution is 10 times the mass of the honeysuckle;

[0053] The preparation method of the citrus extract is as follows: the citrus peel is crushed, water is added for decoction for 40 min, and then filtration is performed, and the filtrate is discarded, and filter residue a is obtained; water equivalent to 8 times the mass of the citrus peel is added to the filter residue a, and cellulase and pectinase are further added, and then mixed uniformly, and then enzymolysis is performed at 50°C for 2 h, and then the temperature is increased to 95°C for 5 min for enzyme inactivation, and then filtration is performed, and filter residue b and filtrate b are obtained; 55% v / v ethanol aqueous solution is added to the filter residue b, and ultrasonic extraction is performed at a frequency of 55 kHz for 30 min, and then filtration is performed, and filtrate c is obtained; the filtrate b and the filtrate c are mixed, and then concentrated under reduced pressure to 1.3 g / ml, and then the citrus extract is obtained; wherein the mass of the 55% v / v ethanol aqueous solution is 8 times the mass of the citrus peel, the mass of the cellulase is 1.5% of the mass of the citrus peel, and the mass of the pectinase is 4% of the mass of the citrus peel.

[0054] In Examples 4-11, the preparation methods of the forsythia extract, honeysuckle extract and citrus extract are the same as those in Example 1.

[0055] Examples 12-22

[0056] The present application provides a leave-on bacteriostatic liquid for children's skin and a preparation method thereof. In each example, the components are included in the following proportions by weight as shown in Table 2:

[0057] Table 2 Leave-on bacteriostatic liquid of Examples 12-22

[0058]

[0059]

[0060] The preparation methods of the forsythia extract, honeysuckle extract and citrus extract are the same as those in Example 1.

[0061] The preparation method of the bacteriostatic liquid is as follows:

[0062] Add the humectants (propylene glycol, butylene glycol and glycerol) in the corresponding formula to water, heat to 80°C and stir until completely dissolved;

[0063] Cool to 50°C, add o-cymen-5-ol and benzalkonium chloride, and stir to disperse evenly;

[0064] Cool to 45°C, add PEG-40 hydrogenated castor oil, honeysuckle extract, citrus extract, fragrance, disodium EDTA, phenoxyethanol and allantoin, and mix evenly;

[0065] Cool to 40°C to obtain the bacteriostatic liquid.

[0066] Comparative Example 1

[0067] This comparative example provides a bacteriostatic composition, the components of which are the same as those in Example 1.

[0068] The preparation method of the citrus extract is as follows: Citrus peel is decocted with 10 times water for 2 times, 30 min each time; filter, combine the filtrates, and concentrate the filtrate under reduced pressure to 1.25 g / ml to obtain the extract;

[0069] The preparation methods of the forsythia extract and honeysuckle extract are the same as those in Example 1.

[0070] Comparative Example 2

[0071] This comparative example provides a bacteriostatic composition, the components of which are the same as those in Example 1.

[0072] The preparation method of the citrus extract is as follows: the citrus peel is extracted with 7 times of 55% v / v ethanol aqueous solution by heating and refluxing for 2 times, each for 30 min; the filtrate is combined and concentrated under reduced pressure to 1.25 g / ml, to obtain the citrus extract.

[0073] The preparation methods of the forsythia extract and the honeysuckle extract are the same as those in Example 1.

[0074] Comparative Example 3

[0075] This comparative example provides a bacteriostatic composition, which has the same components as those in Example 1.

[0076] The preparation method of the forsythia extract is as follows: the forsythia is extracted with 7 times of 20% v / v ethanol aqueous solution by ultrasonic extraction for 45 min, the ultrasonic frequency being 45 Hz; the filtrate is filtered and concentrated under reduced pressure to 1.25 g / ml, to obtain the forsythia extract.

[0077] The preparation methods of the honeysuckle extract and the citrus extract are the same as those in Example 1.

[0078] Comparative Example 4

[0079] This comparative example provides a bacteriostatic composition, which has the same components as those in Example 1.

[0080] The preparation method of the forsythia extract is as follows: the forsythia is extracted with 10 times of water by decocting for 2 times, each for 30 min; the filtrate is combined and concentrated under reduced pressure to 1.25 g / ml, to obtain the forsythia extract.

[0081] The preparation methods of the honeysuckle extract and the citrus extract are the same as those in Example 1.

[0082] Comparative Example 5

[0083] This comparative example provides a bacteriostatic composition, which has the same components as those in Example 1.

[0084] The preparation method of the forsythia extract is as follows: the forsythia is extracted with 7 times of 55% v / v ethanol aqueous solution by heating and refluxing for 2 times, each for 30 min; the filtrate is combined and concentrated under reduced pressure to 1.25 g / ml, to obtain the forsythia extract.

[0085] The preparation methods of the honeysuckle extract and the citrus extract are the same as those in Example 1.

[0086] Comparative Example 6

[0087] This comparative example provides a bacteriostatic composition, which has the same components as those in Example 1.

[0088] The preparation method of the forsythia extract is as follows: the forsythia is extracted with 7 times of 20% v / v ethanol aqueous solution by ultrasonic extraction for 45 min, the ultrasonic frequency being 45 Hz; the filtrate is filtered and concentrated under reduced pressure to 1.25 g / ml, to obtain the forsythia extract.

[0089] The preparation methods of honeysuckle extract and citrus extract are the same as those in Example 1.

[0090] Comparative Example 7

[0091] This comparative example provides an antibacterial composition, the ingredients of which are the same as those in Example 1.

[0092] The preparation method of the honeysuckle extract is as follows: decoct the honeysuckle with 10 times the amount of water for 2 times, each time for 30 minutes; filter, combine the filtrates, and concentrate the filtrates under reduced pressure to 1.25g / ml to obtain the extract;

[0093] The preparation methods of Forsythia suspensa extract and Citrus aurantium extract are the same as those in Example 1;

[0094] Comparative Example 8

[0095] This comparative example provides an antibacterial composition, the ingredients of which are the same as those in Example 1.

[0096] The preparation method of the honeysuckle extract is as follows: extracting the honeysuckle with 7 times 57% v / v ethanol aqueous solution by heating and refluxing for 2 times, each time for 30 minutes; filtering, and concentrating the filtrate under reduced pressure to 1.25g / ml to obtain the extract;

[0097] The preparation methods of the forsythia extract and the citrus extract are the same as those in Example 1.

[0098] Comparative Example 9

[0099] This comparative example provides an antibacterial composition, the ingredients of which are the same as those in Example 1.

[0100] The preparation method of the honeysuckle extract is as follows: extracting the honeysuckle with 8 times 55% v / v ethanol aqueous solution by ultrasonic extraction for 45 minutes at an ultrasonic frequency of 45 Hz; filtering, and concentrating the filtrate under reduced pressure to 1.25 g / ml to obtain the extract;

[0101] The preparation methods of the forsythia extract and the citrus extract are the same as those in Example 1.

[0102] Comparative Example 10

[0103] This comparative example provides an antibacterial composition, comprising the following components in parts by weight:

[0104] 0.08 parts of o-cymene-5-ol and 0.05 parts of benzalkonium chloride.

[0105] Comparative Example 11

[0106] This comparative example provides an antibacterial liquid and a preparation method thereof. The component ratio and preparation method of the antibacterial liquid are the same as those in Example 12, wherein the preparation methods of the Forsythia suspensa extract and the honeysuckle extract are the same as those in Example 1, and the preparation method of the citrus extract is the same as that in Comparative Example 1.

[0107] Comparative Example 12

[0108] This comparative example provides a bacteriostatic solution and a preparation method thereof, the component ratio and the preparation method of which are the same as those of Example 12, wherein the preparation methods of the forsythia extract solution and the honeysuckle extract solution are the same as those of Example 1, and the preparation method of the citrus extract solution is the same as that of Comparative Example 2.

[0109] Comparative Example 13

[0110] This comparative example provides a bacteriostatic solution and a preparation method thereof, the component ratio and the preparation method of which are the same as those of Example 12, wherein the preparation methods of the forsythia extract solution and the honeysuckle extract solution are the same as those of Example 1, and the preparation method of the citrus extract solution is the same as that of Comparative Example 3.

[0111] Comparative Example 14

[0112] This comparative example provides a bacteriostatic solution and a preparation method thereof, the component ratio and the preparation method of which are the same as those of Example 12, wherein the preparation methods of the forsythia extract solution and the honeysuckle extract solution are the same as those of Example 1, and the preparation method of the citrus extract solution is the same as that of Comparative Example 4.

[0113] Comparative Example 15

[0114] This comparative example provides a bacteriostatic solution and a preparation method thereof, the component ratio and the preparation method of which are the same as those of Example 12, wherein the preparation methods of the forsythia extract solution and the honeysuckle extract solution are the same as those of Example 1, and the preparation method of the citrus extract solution is the same as that of Comparative Example 5.

[0115] Comparative Example 16

[0116] This comparative example provides a bacteriostatic solution and a preparation method thereof, the component ratio and the preparation method of which are the same as those of Example 12, wherein the preparation methods of the forsythia extract solution and the honeysuckle extract solution are the same as those of Example 1, and the preparation method of the citrus extract solution is the same as that of Comparative Example 6.

[0117] Comparative Example 17

[0118] This comparative example provides a bacteriostatic solution and a preparation method thereof, the component ratio and the preparation method of which are the same as those of Example 12, wherein the preparation methods of the forsythia extract solution and the honeysuckle extract solution are the same as those of Example 1, and the preparation method of the citrus extract solution is the same as that of Comparative Example 7.

[0119] Comparative Example 18

[0120] This comparative example provides a bacteriostatic solution and a preparation method thereof, the component ratio and the preparation method of which are the same as those of Example 12, wherein the preparation methods of the forsythia extract solution and the honeysuckle extract solution are the same as those of Example 1, and the preparation method of the citrus extract solution is the same as that of Comparative Example 8.

[0121] Comparative Example 19

[0122] The present comparative example provides a bacteriostatic solution and a preparation method thereof, the component ratio and the preparation method of which are the same as those of Example 12, wherein the preparation methods of the forsythia suspensa extract and the citrus extract are the same as those of Example 1, and the preparation method of the honeysuckle extract is the same as that of Comparative Example 9.

[0123] Comparative Example 20

[0124] The present comparative example provides a bacteriostatic solution and a preparation method thereof, the component ratio of which is based on that of Example 12, and the forsythia suspensa extract, the honeysuckle extract and the citrus extract are removed, and the preparation method is the same as that of Example 12.

[0125] Test Example 1

[0126] The bacteriostatic effects of the bacteriostatic compositions prepared in Examples 1 to 11 and Comparative Examples 1 to 10 above are investigated in the present test example.

[0127] The component ratio of the nutrient agar medium used in the following experiments is as follows: 10 g of proteose peptone, 3 g of beef extract, 5 g of sodium chloride, 17 g of agar, and 1000 mL of distilled water.

[0128] The components of the Sabouraud medium are as follows: 10 g of proteose peptone, 20 g of agar, and 40 g of glucose, and 1 L of distilled water.

[0129] Test strains: Staphylococcus aureus (ATCC 6538), Escherichia coli (8099), and Candida albicans (ATCC 10231).

[0130] 1. Experimental method

[0131] The nutrient agar medium slant culture (24 h) of the test bacteria of the 5th generation was washed with 5 mL of 0.03 mol / L phosphate buffer (hereinafter referred to as PBS) to remove the bacterial mat, and was diluted with the above PBS to prepare a bacterial suspension with a concentration of 5 x 10 4 cfu / mL.

[0132] The bacteriostatic composition samples prepared in Examples 1 to 11 and Comparative Examples 1 to 10 were used as the test sample solution, and 4 tubes of the test sample solution (5 mL) and the control sample solution (having the same components as the test sample solution, but not containing the forsythia suspensa extract, the honeysuckle extract, the citrus extract, o-cymen-5-ol and benzalkonium chloride, and being sterilized) were taken.

[0133] Respectively, in each of the test sample and control sample, 100 μL of the above bacterial suspension was added, mixed uniformly, and the timing was started. After 2 min, 5 min, 10 min, and 20 min, 0.5 mL of the mixed sample was respectively put into a test tube containing 5 mL of PBS, mixed thoroughly, and 0.5 mL was respectively taken and placed on two plates. Nutrient agar medium (bacteria) or Sabouraud agar medium (yeast) at 40-50°C was used for pouring, the plates were rotated to make the agar solidify, and after the agar solidified, the plates were turned over and incubated at 35°C±2°C for 48 h (bacteria) or 72 h (yeast). The viable bacterial colonies were counted.

[0134] The test was repeated 3 times, and the bacteriostatic rate was calculated according to the following formula:

[0135] X=(A-B) / A*100%;

[0136] In the formula, X is the bacteriostatic rate, A is the average number of bacterial colonies of the control sample, and B is the average number of bacterial colonies of the test sample.

[0137] 2. Experimental results

[0138] The average bacteriostatic rate of each bacteriostatic composition at different action times was recorded, and the results are shown in Tables 3-5.

[0139] Table 3: Bacteriostatic data against Staphylococcus aureus

[0140]

[0141]

[0142] Table 4: Bacteriostatic data against Escherichia coli

[0143]

[0144] Table 5: Bacteriostatic data against Candida albicans

[0145]

[0146]

[0147] As can be seen from the test results in Tables 3-5, the bacteriostatic compositions obtained in Examples 1-3 and 7 have a bacteriostatic rate of >99.9% against Staphylococcus aureus, Escherichia coli, and Candida albicans at 5-20 min. The bacteriostatic compositions obtained in other examples also have good bacteriostatic effects against Staphylococcus aureus, Escherichia coli, and Candida albicans, and the bacteriostatic rate of the bacteriostatic compositions obtained in Examples 1-11 is better than that of the bacteriostatic compositions obtained in the comparative examples.

[0148] Test Example 2

[0149] The test example investigates the skin irritation of the bacteriostatic solution prepared in the above Examples 12-22 and Comparative Examples 11-20.

[0150] 1. Experimental method

[0151] Sixty-three New Zealand rabbits with intact skin, female, weighing 2.0-2.5 kg, were fed with ordinary grade rabbit maintenance feed, at a temperature of 20-26°C and a relative humidity of 40%-70%.

[0152] According to the Disinfection Technical Standard (2002 edition) 2.3.3.3.1, the bacteriostatic solution prepared in Examples 12-22 and Comparative Examples 11-20 was subjected to a complete skin irritation test (3 rabbits were used for each sample): about 24 hours before the experiment, the fur on both sides of the rabbit's back was removed without damaging the skin, and the fur was removed in an area of about 3 cm x 3 cm on both the left and right sides. 0.5 ml of the test solution was applied to the skin, then covered with two layers of gauze and one layer of glass paper, and fixed with adhesive tape. The other side of the skin was applied with 0.5 ml of distilled water as a blank control. The application time was 4 hours, and the test material was removed by washing with warm water for 1 min. The skin reaction was observed at 1 hour, 24 hours and 48 hours after the test material was removed, and the skin irritation reaction score was evaluated according to Table 6. The results are shown in Tables 7 and 8.

[0153] Table 6 Skin irritation reaction score criteria

[0154]

[0155] Table 7 Test results of the bacteriostatic solution prepared in Examples 11-22

[0156]

[0157]

[0158] Table 8 Test results of the bacteriostatic solution prepared in Comparative Examples 11-20

[0159]

[0160]

[0161] As can be seen from the results in Tables 7 and 8, the bacteriostatic solution prepared in Examples 12-22 had no skin irritation to the rabbit, while the bacteriostatic solution prepared in Comparative Examples 11-20 had skin irritation to the rabbit.

[0162] Test Example 3

[0163] The test example investigates the eye irritation of the bacteriostatic solution prepared in the above Examples 12-22 and Comparative Examples 11-20.

[0164] 1. Experimental method

[0165] 63 New Zealand rabbits of eye health, female, weighing 2.0-2.5 kg, were fed with ordinary grade rabbit feed, temperature 20-26℃, relative humidity 40%-70%.

[0166] According to the "Disinfection Technical Specification" (2002 edition) 2.3.4.3, the prepared bacteriostatic solution of Examples 12-22 and Comparative Examples 11-20 was subjected to acute eye irritation test (3 rabbits were tested for each sample): about 24 h before the experiment, the eyes of the rabbits were examined, and the selected animals were all free of eye irritation symptoms, corneal defects and conjunctival damage. During the test, 0.1 ml of the tested sample was taken and dropped into the conjunctival sac of one eye of the rabbit. The other eye was used as a normal control with normal saline. After dropping the tested sample, the eye was passively closed for 4 s, and then washed with normal saline after 30 s. The irritation intensity of each animal to the eye was calculated at 1 h, 24 h, 48 h and 72 h after dropping the eye, and the acute eye irritation reaction score was evaluated according to Table 9. The results are shown in Tables 10 and 11 (the values in the table are the average scores of 3 rabbits corresponding to each sample).

[0167] Table 9 Acute irritation reaction score standard

[0168]

[0169] Table 10 Test results of bacteriostatic solution obtained in Examples 11-22

[0170]

[0171]

[0172]

[0173] Table 11 Test results of bacteriostatic solution obtained in Comparative Examples 11-20

[0174]

[0175]

[0176] From the results of Tables 10 and 11, it can be seen that the bacteriostatic solution obtained in Examples 12-17, 19-22 has no irritation to the eyes of white rabbits, Example 18 has slight irritation to the eyes of white rabbits, and the bacteriostatic solution obtained in Comparative Examples 11-20 has irritation to the eyes of white rabbits.

[0177] From the results of Test Examples 1, 2 and 3, it can be seen that the bacteriostatic composition provided by the examples of the present application has excellent bacteriostatic effect, and compared with the comparative examples, the bacteriostatic composition provided by the examples of the present application has almost no irritation to the skin and eyes.

[0178] The above merely provides the preferred embodiment of the present application, and is not used to limit the present application, and any modification, equivalent replacement or improvement made in the spirit and principle of the present application should be included in the protection scope of the present application.

Claims

1. An antibacterial composition, characterized in that The raw materials are composed by weight of: 0.1-0.8 parts of forsythia extract, 0.1-0.8 parts of honeysuckle extract, 0.1-0.8 parts of citrus extract, 0.05-0.15 parts of o-cymene-5-ol and 0.01-0.08 parts of benzalkonium chloride; The preparation method of the Forsythia suspensa extract comprises: subjecting the Forsythia suspensa to ultrasonic extraction at 25-35° C. using a 15-25% v / v ethanol aqueous solution, first extracting at a frequency of 25-35 kHz for 20-30 minutes, and then extracting at a frequency of 50-70 kHz for 15-25 minutes; filtering after the extraction, and concentrating the resulting filtrate to 1.2-1.3 g / ml to obtain the Forsythia suspensa extract; wherein the mass of the 15-25% v / v ethanol aqueous solution is 5-8 times the mass of the Forsythia suspensa; The preparation method of the honeysuckle extract comprises: subjecting the honeysuckle to ultrasonic extraction with a 45-65% v / v ethanol aqueous solution at 45-60° C., first extracting at a frequency of 20-35 kHz for 20-30 minutes, and then extracting at a frequency of 55-70 kHz for 15-20 minutes; after the extraction is completed, filtering and concentrating the obtained filtrate to 1.2-1.3 g / ml to obtain the honeysuckle extract; wherein the mass of the 45-65% v / v ethanol aqueous solution is 7-10 times the mass of the honeysuckle; The preparation method of the citrus extract comprises the following steps: crushing the citrus peel, adding water to boil for 20 to 40 minutes, filtering, and discarding the filtrate to obtain a filter residue a; adding water equivalent to 5 to 8 times the mass of the citrus peel to the filter residue a, then adding cellulase and pectinase, mixing them evenly, performing enzymatic hydrolysis at 40 to 50° C. for 2 to 3 hours, then heating to 90 to 95° C. and maintaining for 5 to 10 minutes to inactivate the enzymes, and filtering to obtain a filtrate b and a filter residue b; adding 45 to 55% v / v ethanol water to the filter residue b. solution, ultrasonically extracting at a frequency of 40-55 kHz for 30-45 min, filtering to obtain filtrate c; mixing the filtrate b and the filtrate c and concentrating to 1.2-1.3 g / ml to obtain the citrus extract; wherein the mass of the 45-55% v / v ethanol aqueous solution is 5-8 times the mass of the citrus peel, the mass of the cellulase is 1-1.5% of the mass of the citrus peel, and the mass of the pectinase is 3-4% of the mass of the citrus peel.

2. The antibacterial composition according to claim 1, characterized in that The raw materials are composed of 0.1-0.5 parts of forsythia extract, 0.1-0.5 parts of honeysuckle extract, 0.1-0.5 parts of citrus extract, 0.05-0.1 parts of o-cymene-5-ol and 0.02-0.07 parts of benzalkonium chloride by weight.

3. The antibacterial composition according to claim 2, characterized in that The raw materials are composed by weight of: 0.1-0.2 parts of forsythia extract, 0.1-0.2 parts of honeysuckle extract, 0.1-0.2 parts of citrus extract, 0.06-0.08 parts of o-cymene-5-ol and 0.03-0.05 parts of benzalkonium chloride.

4. The antibacterial composition according to claim 3, characterized in that The raw materials are composed of: 0.1 part of forsythia extract, 0.1 part of honeysuckle extract, 0.2 part of citrus extract, 0.08 part of o-cymene-5-ol and 0.05 part of benzalkonium chloride by weight.

5. Use of the antibacterial composition according to any one of claims 1 to 4 in the preparation of a disposable antibacterial product for children's skin or an antibacterial product for clothing surfaces.

6. An antibacterial solution, characterized in that The invention comprises the antibacterial composition according to claim 1.

7. The antibacterial liquid according to claim 6, characterized in that The raw materials are composed of parts by weight: 80-95 parts water; 5~11 parts of moisturizer; 0.5~2 parts of solubilizer; Allantoin 0.05~0.2 parts; 0.1~0.3 parts of antioxidant; 0.3~0.8 parts of preservatives; 0.05~0.3 parts of flavor; 0.1-0.8 parts of Forsythia suspensa extract; 0.1-0.8 parts of honeysuckle extract; 0.1-0.8 parts of citrus extract; 0.05-0.15 parts of o-cymene-5-ol; 0.01~0.08 parts of benzalkonium chloride.

8. The antibacterial liquid according to claim 7, characterized in that The moisturizing agent is selected from at least one of propylene glycol, glycerin and butylene glycol; and / or The solubilizing agent is PEG-40 hydrogenated castor oil; and / or The antioxidant is disodium ethylenediaminetetraacetic acid; and / or The preservative is phenoxyethanol.

9. The method for preparing the antibacterial solution according to claim 7 or 8, characterized in that: The following steps are involved: adding the moisturizing agent to the water and stirring until dissolved; Add the o-cymene-5-ol and benzalkonium chloride, and stir to disperse evenly; The solubilizer, forsythia extract, honeysuckle extract, citrus extract, essence, antioxidant, preservative and allantoin are added and mixed evenly to obtain the antibacterial solution.

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