CN114522133B - Antibacterial microemulsion, preparation method and application thereof, moisturizing water, moisturizing emulsion, moisturizing cream and preparation method thereof - Google Patents

Antibacterial microemulsion, preparation method and application thereof, moisturizing water, moisturizing emulsion, moisturizing cream and preparation method thereof Download PDF

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CN114522133B
CN114522133B CN202210181092.2A CN202210181092A CN114522133B CN 114522133 B CN114522133 B CN 114522133B CN 202210181092 A CN202210181092 A CN 202210181092A CN 114522133 B CN114522133 B CN 114522133B
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microemulsion
moisturizing
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extract
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CN114522133A (en
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王伟
魏泽丰
刘慧敏
彭佳倩
蒋晶晶
陈银锋
刘清雷
王百荟
徐雯颖
何绮潼
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Shanghai Institute of Technology
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/96Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/98Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution of animal origin
    • A61K8/987Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution of animal origin of species other than mammals or birds
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/02Cosmetics or similar toiletry preparations characterised by special physical form
    • A61K8/04Dispersions; Emulsions
    • A61K8/06Emulsions
    • A61K8/068Microemulsions
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/96Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/97Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
    • A61K8/9783Angiosperms [Magnoliophyta]
    • A61K8/9789Magnoliopsida [dicotyledons]
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q17/00Barrier preparations; Preparations brought into direct contact with the skin for affording protection against external influences, e.g. sunlight, X-rays or other harmful rays, corrosive materials, bacteria or insect stings
    • A61Q17/005Antimicrobial preparations
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/52Stabilizers
    • A61K2800/524Preservatives
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/59Mixtures
    • A61K2800/592Mixtures of compounds complementing their respective functions
    • A61K2800/5922At least two compounds being classified in the same subclass of A61K8/18
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02ATECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A50/00TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
    • Y02A50/30Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change

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Abstract

The invention belongs to the technical field of daily chemical products, and particularly relates to a bacteriostatic microemulsion, a preparation method and application thereof, moisturizing water, moisturizing emulsion, moisturizing cream and a preparation method thereof. The invention provides a bacteriostatic microemulsion, which comprises the following components in percentage by mass: 1 to 15 percent of cinnamon extract, 0.5 to 2 percent of gallnut extract, 0.5 to 4 percent of tea extract, 20 to 80 percent of emulsifying agent, 2 to 20 percent of auxiliary emulsifying agent and 4 to 75 percent of water. The antibacterial microemulsion provided by the invention can effectively inhibit the growth of gram-positive bacteria, gram-negative bacteria, saccharomycetes and mould, and can realize the synergistic effect among antibacterial active substances by proportioning different antibacterial active substances according to a certain proportion, so as to achieve the effect of broad-spectrum antibacterial. The antibacterial component in the antibacterial microemulsion provided by the invention is natural plant extract, so that the irritation to human skin is small, and the use safety of cosmetics can be improved.

Description

Antibacterial microemulsion, preparation method and application thereof, moisturizing water, moisturizing emulsion, moisturizing cream and preparation method thereof
Technical Field
The invention belongs to the technical field of daily chemical products, and particularly relates to a bacteriostatic microemulsion, a preparation method and application thereof, moisturizing water, moisturizing emulsion, moisturizing cream and a preparation method thereof.
Background
With the continuous development of social economy, the quality of life of people is continuously improved, which means that the quality pursuit of consumers on cosmetics is also continuously improved. Cosmetics are generally applied to the human body, which also requires absolute safety of the cosmetics to ensure the health of the user. In order to inhibit the growth and reproduction of microorganisms in cosmetics, it is generally required to ensure the stability of the quality of the cosmetics by adding preservatives, relatively prolong the shelf life of the cosmetics, and not to cause deterioration due to external pollution after the cosmetics are used with their covers opened. These microorganisms deteriorate cosmetics, and are liable to cause damage to the skin of the user, and further cause symptoms such as allergy and ulcer, and impair physical health.
The preservative is a substance added to cosmetics in order to inhibit the growth of microorganisms in the cosmetics. As one of the components added to cosmetics, a preservative for cosmetics has the following characteristics: (1) security; (2) broad spectrum; (3) stability; (4) compatibility; (5) chemically inert; (6) cost performance. However, most of the cosmetic preservatives currently used on the market are chemically synthesized preservatives mainly including parabens, phenoxyethanol, benzyl alcohol, formaldehyde, imidazolidinyl urea, and chemically synthesized-source preservatives have a certain safety risk and skin irritation, and although they are generally used in cosmetics at low concentrations, they are still considered as one of the main factors causing allergy to users.
Therefore, the natural antibacterial component accords with the pursuit of people on health and nature, and the natural antibacterial extract mainly comprises substances with antibacterial effect, such as polyphenol, flavonoid, saponin, alkaloid, organic acid and the like in plants. However, the natural antibacterial extracts widely used at present, such as magnolia officinalis, moutan bark, mugwort, dandelion and the like, have the defects of poor antibacterial effect and narrow antibacterial spectrum.
Disclosure of Invention
In view of the above, the invention provides a bacteriostatic microemulsion, a preparation method and application thereof, moisturizing water, moisturizing emulsion, moisturizing cream and a preparation method thereof.
In order to solve the technical problems, the invention provides the following technical scheme:
the invention provides a bacteriostatic microemulsion, which comprises the following components in percentage by mass:
Figure BDA0003522303180000021
preferably, the composition comprises the following components in percentage by mass:
Figure BDA0003522303180000022
the invention provides a preparation method of the antibacterial microemulsion, which comprises the following steps:
dissolving the tea leaf extract in water to obtain water phase;
dissolving Galla chinensis extract in auxiliary emulsifier to obtain Galla chinensis extract solution;
Mixing the gallnut extract solution, the emulsifying agent and the cinnamon extract for the first time to obtain an oil phase;
and carrying out second mixing on the water phase and the oil phase to obtain the antibacterial microemulsion.
The invention provides application of the bacteriostatic microemulsion prepared by the preparation method in daily chemical products as a preservative.
The invention provides moisturizing water which comprises the following components in percentage by mass:
Figure BDA0003522303180000023
Figure BDA0003522303180000031
the antibacterial microemulsion is the antibacterial microemulsion.
The invention provides a preparation method of the moisturizing water, which comprises the following steps:
mixing a humectant, a skin conditioning agent, a rheology modifier, a chelating agent, a solubilizer and water to obtain primary moisturizing water;
and mixing the primary moisturizing water with the antibacterial microemulsion to obtain the moisturizing water.
The invention provides an emulsion, which comprises the following components in percentage by mass:
Figure BDA0003522303180000032
the antibacterial microemulsion is the antibacterial microemulsion.
The invention provides a preparation method of the moisturizing emulsion, which comprises the following steps:
mixing a humectant, a skin conditioning agent, a rheology modifier, a chelating agent and water to obtain a water phase;
mixing grease, an emulsifying agent, an antioxidant and a pH value regulator to obtain an emulsion;
And mixing the water phase, the emulsion and the antibacterial microemulsion to obtain the moisturizing emulsion.
The invention provides a moisturizing cream which comprises the following components in percentage by mass:
Figure BDA0003522303180000033
Figure BDA0003522303180000041
the antibacterial microemulsion is the antibacterial microemulsion.
The invention provides a preparation method of the moisturizing cream, which comprises the following steps:
mixing a humectant, a skin conditioning agent, a rheology modifier, a chelating agent and water to obtain a water phase;
mixing grease and an emulsifying agent to obtain an emulsion;
and mixing the water phase, the emulsion and the antibacterial microemulsion to obtain the moisturizing cream.
The invention provides a bacteriostatic microemulsion, which comprises the following components in percentage by mass: 1 to 15 percent of cinnamon extract,0.5about 2 percent of Chinese gall extract,0.24% of tea extract, 20% to 80% of emulsifying agent, 2% to 20% of auxiliary emulsifying agent and 4% to 75% of water. The antibacterial microemulsion provided by the invention can effectively inhibit the growth of gram-positive bacteria, gram-negative bacteria, saccharomycetes and mould, and can realize the synergistic effect among antibacterial active substances by proportioning different natural antibacterial extracts according to a certain proportion, so as to achieve the effect of broad-spectrum antibacterial. According to the antibacterial microemulsion provided by the invention, components with poor water solubility such as cinnamon extract and the like are embedded into a microemulsion system, so that the water solubility of antibacterial components is improved, and the concentration of the antibacterial components in cosmetics is increased, and therefore, the antibacterial components with poor water solubility are applied to the cosmetics. The antibacterial component in the antibacterial microemulsion provided by the invention is natural plant extract, so that the irritation to human skin is small, and the use safety of cosmetics can be improved.
Detailed Description
The invention provides a bacteriostatic microemulsion, which comprises the following components in percentage by mass:
Figure BDA0003522303180000042
the invention has no special requirement on the components and adopts the conventional commercial products in the field.
The antibacterial microemulsion provided by the invention comprises 1-15% of cinnamon extract, preferably 6-15%, more preferably 6-15%, and even more preferably 10-13.5% by mass. The invention preferably adopts a steam distillation method to extract dry bark and dry leaves of cinnamon to obtain cinnamon extract; the distillation time of the steam distillation is preferably 20 to 40min, more preferably 25 to 30min; the feed liquid ratio of the steam distillation method is preferably 40-60: 1, more preferably 50 to 55:1. In the present invention, the cinnamon extract is a yellow liquid. In the invention, the main component of the cinnamon extract is cinnamaldehyde which has extremely strong antibacterial activity to microorganisms, however, the cinnamon extract has the characteristics of low water solubility, easy volatilization, sensitivity to environmental conditions and the like, and is difficult to apply to cosmetics as water phase anticorrosion; and with the extension of time, cinnamaldehyde is easy to oxidize in the air in the application process, so that the content of active ingredients in the essential oil is reduced, and the overall antibacterial activity is reduced. According to the invention, the cinnamon extract is embedded into a microemulsion system, so that the water solubility of the cinnamon extract is improved, and the concentration of the cinnamon extract in cosmetics is increased.
The antibacterial microemulsion provided by the invention comprises 0.5-2% of gallnut extract, preferably 1-1.5%, and more preferably 0.8-1.08% by mass percent. The invention preferably utilizes a reflux extraction method to extract the gallnut to obtain the gallnut extract. In the present invention, the extraction solvent for reflux extraction is preferably an aqueous ethanol solution, and the volume concentration of ethanol in the aqueous ethanol solution is preferably 60 to 80%, more preferably 65 to 70%; the feed liquid ratio of the reflux extraction method is preferably 10-20:1, more preferably 15-18:1; the extraction time of the reflux extraction method is preferably 60-90 min, more preferably 70-80 min; the extraction temperature of the reflux extraction method is preferably 80 to 90 ℃, more preferably 85 to 88 ℃. In the present invention, the repeated extraction of gallnut is preferably performed, and the number of repetition times of the repeated extraction is preferably 2 to 4 times, more preferably 3 times.
In the present invention, it is preferable that the method further comprises:
filtering the extracted product, and taking filtrate;
concentrating the filtrate, and drying to obtain Galla chinensis extract.
The invention has no special requirement on the filtration, and can be realized by adopting a conventional mode in the field.
In the present invention, the concentration is preferably reduced pressure distillation, and the temperature of the reduced pressure distillation is preferably 35 to 45 ℃, more preferably 40 to 42 ℃; the time is preferably 30 to 45 minutes, more preferably 35 to 40 minutes. In the present invention, the drying is preferably freeze-drying, and the temperature of the freeze-drying is preferably-48 to-52 ℃, more preferably-50 ℃; the time for the freeze-drying is preferably 12 to 72 hours, more preferably 24 to 48 hours.
In the invention, the active ingredient of the gallnut extract is preferably gallic acid, the gallic acid has good antioxidation and antibacterial activity, and the gallic acid has good inhibition effect on staphylococcus aureus, escherichia coli, salmonella enteritidis and salmonella typhimurium.
The antibacterial microemulsion provided by the invention comprises 0.2-4% of tea extract, preferably 1-3%, and more preferably 1.15-2% by mass. The invention preferably utilizes a water extraction method to extract the tea to obtain the tea extract. The ratio of the water to the water by the water leaching method is preferably 20-30: 1, more preferably 23 to 25:1. In the present invention, the extraction time of the water extraction method is preferably 40 to 50 minutes, more preferably 43 to 45 minutes; the extraction temperature of the solvent extraction method is preferably 60 to 70 ℃, more preferably 65 to 68 ℃. In the present invention, the tea leaves are preferably repeatedly extracted, and the number of repetition times of the repeated extraction is preferably 3 to 5 times, more preferably 4 times.
In the present invention, the water extraction preferably further comprises:
filtering the extracted product, and taking filtrate;
concentrating the filtrate, and drying to obtain tea extract.
The invention has no special requirement on the filtration, and can be realized by adopting a conventional mode in the field.
In the present invention, the concentration is preferably reduced pressure distillation, and the temperature of the reduced pressure distillation is preferably 50 to 65 ℃, more preferably 55 to 60 ℃; the time is preferably 35 to 50 minutes, more preferably 40 to 50 minutes. In the present invention, the drying is preferably freeze-drying, and the temperature of the freeze-drying is preferably-48 to-52 ℃, more preferably-50 ℃; the time for the freeze-drying is preferably 12 to 72 hours, more preferably 24 to 48 hours.
In the invention, the active ingredient of the tea extract is tea polyphenol; the tea polyphenol has obvious inhibition effect on gram positive bacteria and gram negative bacteria, has good antibacterial selectivity, and can promote the growth of beneficial bacteria.
The antibacterial microemulsion provided by the invention has broad-spectrum antibacterial effect under the combined action of cinnamon extract, chinese gall extract and tea extract, and can have good inhibition effect on bacteria and fungi.
The antibacterial microemulsion provided by the invention comprises 20-80% of emulsifying agent, preferably 25-70%, more preferably 30-50% by mass. In the present invention, the emulsifier preferably includes one or more of tween-80, tween-60 and tween-20, more preferably tween-80.
The antibacterial microemulsion provided by the invention comprises 2-20% of auxiliary emulsifier, preferably 6-15%, more preferably 10-13.5% by mass. In the present invention, the co-emulsifier preferably includes one or more of glycerin, ethylene glycol, 1, 3-butylene glycol and propylene glycol, more preferably glycerin.
The antibacterial microemulsion provided by the invention also comprises 4-75% of water, preferably 4-60% of water, and more preferably 23-40% of water. In the present invention, the water is preferably deionized water.
In the invention, the antibacterial microemulsion has good antibacterial activity, is stable in shape, is not easy to delaminate, is mild and has no irritation, and can be applied to cosmetics.
The invention also provides a preparation method of the antibacterial microemulsion according to the technical scheme, which comprises the following steps:
dissolving the tea leaf extract in water to obtain water phase;
dissolving Galla chinensis extract in auxiliary emulsifier to obtain Galla chinensis extract solution;
mixing the gallnut extract solution, the emulsifying agent and the cinnamon extract for the first time to obtain an oil phase;
and carrying out second mixing on the water phase and the oil phase to obtain the antibacterial microemulsion.
The invention provides cinnamon extract, chinese gall extract and tea extract. The sources of the cinnamon extract, the gallnut extract and the tea extract are not particularly limited, and the cinnamon extract, the gallnut extract and the tea extract can be prepared by adopting conventional commercial products or extracting; when the cinnamon extract, the gallnut extract and the tea extract are prepared by adopting an extraction method, the extraction method is preferably performed according to the extraction method described in the technical scheme, and the detailed description is not repeated here.
The invention dissolves the tea extract in water to obtain water phase. In the present invention, the water is preferably deionized water. In the present invention, the mass ratio of the tea extract to water is preferably 1:18 to 22, more preferably 1:20. In the present invention, the temperature of the dissolution is preferably 30 to 70 ℃, more preferably 40 to 60 ℃. In the present invention, the dissolution is preferably performed under stirring at a rotation speed of preferably 100 to 1500r/min, more preferably 400 to 1000r/min. The invention has no special requirement on the dissolution time, so long as the dissolution is complete.
The invention dissolves the gallnut extract in the auxiliary emulsifier to obtain the gallnut extract solution. In the invention, the mass ratio of the gallnut extract to the auxiliary emulsifier is preferably 12-14: 1, more preferably 12.5 to 13.5:1. In the present invention, the temperature of the dissolution is preferably 30 to 70 ℃, more preferably 50 to 60 ℃. In the present invention, the dissolution is preferably performed under ultrasonic conditions, the power of the ultrasonic is preferably 200 to 400W, more preferably 250 to 300W, and the time of the ultrasonic is preferably 5 to 20min, more preferably 10 to 15min.
And (3) carrying out first mixing on the gallnut extract solution, the emulsifying agent and the cinnamon extract to obtain an oil phase. In the present invention, the mass ratio of the emulsifier to the cinnamon extract is preferably 1:3.6 to 6.3, more preferably 1:4 to 5. In the invention, the mass ratio of the gallnut extract to the cinnamon extract is preferably 1:4.3-14, more preferably 1:6-10. In the present invention, the first mixing is preferably performed under stirring, and the stirring speed is preferably 100 to 1500r/min, more preferably 500 to 1000r/min. The invention has no special requirement on the stirring time, and can be uniformly mixed.
After obtaining the water phase and the oil phase, the invention carries out secondary mixing on the water phase and the oil phase to obtain the antibacterial microemulsion. In the present invention, the mass ratio of the aqueous phase to the oil phase is preferably 1 to 2 to 4, more preferably 1:2.3 to 3.3. In the present invention, the second mixing is preferably performed under stirring, and the stirring speed is preferably 100 to 1500r/min, more preferably 650 to 1000r/min. The stirring time is not particularly limited as long as the stirring time can be uniformly mixed.
In the invention, the formation of the microemulsion is a spontaneous process, and the bacteriostatic microemulsion can be obtained by controlling the proportion of the oil phase, the water phase, the emulsifier and the auxiliary emulsifier.
The invention also provides an application of the antibacterial microemulsion prepared by the technical scheme or the preparation method of the technical scheme in daily chemical products as a preservative. In the present invention, the daily chemical product includes moisturizing water, moisturizing lotion, moisturizing cream, shampoo or body wash, more preferably moisturizing water, moisturizing lotion or moisturizing cream. In the invention, the mass percentage of the antibacterial microemulsion in the daily chemical product is preferably 0.3-1%, more preferably 0.5-0.6%.
The invention also provides moisturizing water which comprises the following components in percentage by mass:
Figure BDA0003522303180000081
the moisturizing water provided by the invention comprises 9.05-18.1% of moisturizing agent, preferably 10-15% of moisturizing agent by mass percent. In the present invention, the humectant preferably includes one or more of sodium hyaluronate, butylene glycol, and glycerin. When the humectant includes two or more of the above specific substances, the proportion of the specific substances is not particularly limited as long as the amount of the humectant can be satisfied. In an embodiment of the invention, the humectant is sodium hyaluronate, butylene glycol and glycerin in a mass ratio of 0.1:4:5.9.
The moisturizing water provided by the invention comprises 0.6-1.3% of skin conditioning agent, preferably 0.8-1.2% by mass. In the present invention, the skin conditioning agent preferably includes allantoin and/or DL-panthenol, more preferably allantoin and DL-panthenol. The mass ratio of the allantoin to the DL-panthenol is not particularly limited, and in the embodiment of the invention, the mass ratio of the allantoin to the DL-panthenol is 1:4.
The moisturizing water provided by the invention comprises 0.1-0.6% of antibacterial microemulsion, preferably 0.2-0.5%, and more preferably 0.3-0.4% by mass percent.
The moisturizing water provided by the invention comprises 0.1-0.15% of rheological modifier, preferably 0.12-0.13% by mass. In the present invention, the rheology modifier is preferably xanthan gum.
The moisturizing water provided by the invention comprises 0.01-0.05% of chelating agent, preferably 0.02-0.03% by mass. In the present invention, the chelating agent is preferably disodium ethylenediamine tetraacetate.
The moisturizing water provided by the invention comprises 0.48-0.52% of solubilizer, preferably 0.5% by mass. In the present invention, the solubilizing agent is preferably PEG-60 hydrogenated castor oil.
The moisturizing water provided by the invention comprises the balance of water, and the water is preferably deionized water.
The invention also provides a preparation method of the moisturizing water, which comprises the following steps:
mixing a humectant, a skin conditioning agent, a rheology modifier, a chelating agent, a solubilizer and water to obtain primary moisturizing water;
and mixing the primary moisturizing water with the antibacterial microemulsion to obtain the moisturizing water.
According to the invention, the moisturizing agent, the skin conditioning agent, the rheology modifier, the chelating agent, the solubilizer and the water are mixed to obtain the primary moisturizing water. In the present invention, the temperature of the mixing is preferably 80 to 90 ℃, more preferably 85 to 88 ℃; the mixing is preferably performed under stirring, and the stirring speed is preferably 8000-12000 r/min, more preferably 10000-11000 r/min; the stirring time is preferably 4.8 to 5.2 minutes, more preferably 5 minutes.
After primary moisturizing water is obtained, the primary moisturizing water and the antibacterial microemulsion are mixed to obtain the moisturizing water. The present invention is not particularly limited as long as the mixing can be uniformly performed. In an embodiment of the invention, the mixing is preferably performed under stirring.
The invention also provides an emulsion, which comprises the following components in percentage by mass:
Figure BDA0003522303180000091
Figure BDA0003522303180000101
the moisturizing emulsion provided by the invention comprises 4.5-13.0% of grease, preferably 8-10% of grease by mass percent. In the present invention, the grease preferably includes one or more of caprylic/capric triglyceride, cetyl ethyl hexanoate and hydrogenated polyisobutene, more preferably caprylic/capric triglyceride, cetyl ethyl hexanoate and hydrogenated polyisobutene. When the grease comprises more than two specific substances, the mass ratio of the specific substances is not particularly limited, and any ratio is adopted. In an embodiment of the invention, the grease is caprylic/capric triglyceride, cetyl ethyl hexanoate and hydrogenated polyisobutene in a mass ratio of 5:2:1.
The moisturizing emulsion provided by the invention comprises 4.12-9.1% of moisturizing agent, preferably 6-8% of moisturizing agent by mass percent. In the present invention, the humectant preferably includes one or more of sodium hyaluronate, butylene glycol, and trehalose. When the humectant includes two or more of the above specific substances, the proportion of the specific substances is not particularly limited as long as the amount of the humectant can be satisfied. In an embodiment of the invention, the humectant is sodium hyaluronate, butylene glycol and trehalose in a mass ratio of 0.08:6:0.5.
The moisturizing emulsion provided by the invention comprises 0.6-1.3% of skin conditioning agent, preferably 0.9-1.1% by mass. In the present invention, the skin conditioning agent preferably includes allantoin and/or DL-panthenol, more preferably allantoin and DL-panthenol. The mass ratio of the allantoin to the DL-panthenol is not particularly limited, and in the embodiment of the invention, the mass ratio of the allantoin to the DL-panthenol is 2:7.
The moisturizing emulsion provided by the invention comprises 0.1-0.6% of antibacterial microemulsion, preferably 0.2-0.5%, and more preferably 0.3-0.4% by mass percent.
The moisturizing emulsion provided by the invention comprises 0.2-0.5% of rheological modifier, preferably 0.3-0.4% by mass. In the present invention, the rheology modifier is preferably an aqueous carbomer solution, and the mass concentration of the aqueous carbomer solution is preferably 0.8 to 1.2%, more preferably 1%.
The moisturizing emulsion provided by the invention comprises 0.01-0.1% of chelating agent, preferably 0.06-0.08% by mass. In the present invention, the chelating agent is preferably disodium ethylenediamine tetraacetate.
The moisturizing emulsion provided by the invention comprises 1.2-2.8% of emulsifying agent, preferably 1.8-2% by mass. In the present invention, the emulsifier preferably comprises one or more of alkyl alcohol, alkyl glycoside, cetostearyl alcohol and cetostearyl glucoside. In the present invention, the alkyl alcohol is preferably a C14-20 alkyl alcohol, more preferably a C16-18 alkyl alcohol; the alkyl glycoside is preferably a C12-20 alkyl glycoside, more preferably a C15-18 alkyl glycoside. When the emulsifier comprises more than two specific substances, the mass ratio of the specific substances is not particularly limited, and any ratio is adopted. In an embodiment of the invention, the emulsifier is a C16 alkyl alcohol, a C15 alkyl glycoside, cetostearyl alcohol, and cetostearyl glucoside; the mass ratio of the C16 alkyl alcohol to the C15 alkyl glycoside to the cetostearyl alcohol to the cetostearyl glucoside is 8:3:5:2.
The moisture-preserving emulsion provided by the invention comprises 0.02-0.06% of pH value regulator, preferably 0.03-0.05% by mass percent. In the present invention, the pH of the moisturizing emulsion is preferably 5 to 7, more preferably 5.5 to 6.5. In the present invention, the pH adjustor is preferably aminomethylpropanol.
The moisturizing emulsion provided by the invention comprises 0.05-0.1% of antioxidant, preferably 0.07-0.09% of antioxidant by mass percent. In the present invention, the antioxidant is preferably tocopherol acetate.
The moisturizing emulsion provided by the invention comprises the balance of water, preferably deionized water, in percentage by mass.
The invention also provides a preparation method of the moisturizing emulsion, which comprises the following steps:
mixing a humectant, a skin conditioning agent, a rheology modifier, a chelating agent and water to obtain a water phase;
mixing grease, an emulsifying agent, an antioxidant and a pH value regulator to obtain an emulsion;
and mixing the water phase, the emulsion and the antibacterial microemulsion to obtain the moisturizing emulsion.
According to the invention, the humectant, the skin conditioning agent, the rheology modifier, the chelating agent and water are mixed to obtain a water phase. In the present invention, the temperature of the mixing is preferably 78 to 82 ℃, more preferably 79 to 80 ℃; the mixing is preferably performed under stirring, and the mode of the mixing is not particularly limited in the present invention as long as the mixing can be uniformly performed.
The invention mixes grease, emulsifying agent, antioxidant and pH value regulator to obtain emulsion. In the present invention, the temperature of the mixing is preferably 78 to 82 ℃, more preferably 79 to 80 ℃; the mixing is preferably performed under stirring, and the mode of the mixing is not particularly limited in the present invention as long as the mixing can be uniformly performed.
After obtaining the water phase and the emulsion, the invention mixes the water phase, the emulsion and the antibacterial microemulsion to obtain the moisturizing emulsion. In the present invention, the mixing preferably includes the steps of:
transferring the emulsion into a water phase to obtain a primary moisturizing emulsion;
and mixing the primary moisturizing emulsion with the antibacterial microemulsion to obtain the moisturizing emulsion.
The emulsion is transferred into a water phase to obtain the primary moisturizing emulsion. In the present invention, the transfer is preferably accompanied by stirring at a rotation speed of 9000 to 11000r/min, more preferably 9500 to 10000r/min; the stirring time is preferably 4.8 to 5.2 minutes, more preferably 5 minutes.
After the primary moisturizing emulsion is obtained, the primary moisturizing emulsion and the antibacterial microemulsion are mixed to obtain the moisturizing emulsion. The present invention preferably further comprises, prior to mixing: and cooling the primary moisturizing emulsion. In the present invention, the temperature after the temperature reduction is preferably 53 to 57 ℃, more preferably 55 to 56 ℃. The cooling mode is not particularly limited, as long as the required temperature can be reached. The present invention is not particularly limited as long as the mixing can be uniformly performed.
The invention also provides a moisturizing cream which comprises the following components in percentage by mass:
Figure BDA0003522303180000121
the moisturizing cream provided by the invention comprises 12.0-22.0% of grease, preferably 17-20% of grease by mass percent. In the present invention, the grease preferably includes one or more of caprylic/capric triglyceride, olive oil, cyclomethicone and cyclopentadimethicone, more preferably caprylic/capric triglyceride, olive oil, cyclomethicone and cyclopentadimethicone. When the grease comprises more than two specific substances, the mass ratio of the specific substances is not particularly limited, and any ratio is adopted. In the embodiment of the invention, the grease is caprylic/capric triglyceride, olive oil, cyclomethicone and cyclopentadimethicone with the mass ratio of 6:4:3:4.
The moisturizing cream provided by the invention comprises 9.05-15.1% of moisturizing agent, preferably 11-13% of moisturizing agent by mass percent. In the present invention, the humectant preferably includes one or more of sodium hyaluronate, butylene glycol, and glycerin. When the humectant includes two or more of the above specific substances, the proportion of the specific substances is not particularly limited as long as the amount of the humectant can be satisfied. In an embodiment of the invention, the humectant is sodium hyaluronate, butylene glycol and glycerin in a mass ratio of 0.08:5:6.
The moisturizing cream provided by the invention comprises 0.5-1.0% of skin conditioner, preferably 0.6-0.8% by mass. In the present invention, the skin conditioning agent is preferably DL-panthenol.
The moisturizing cream provided by the invention comprises 0.1-0.6% of antibacterial microemulsion, preferably 0.2-0.5%, and more preferably 0.3-0.4% by mass.
The moisturizing cream provided by the invention comprises 0.22-0.5% of a rheology modifier, preferably xanthan gum and/or aqueous carbomer solution, more preferably xanthan gum and aqueous carbomer solution. In the present invention, the mass concentration of the aqueous carbomer solution is preferably 0.8 to 1.2%, more preferably 1%. In the present invention, when the rheology is adjusted to be that of xanthan gum and carbomer aqueous solution, the mass ratio of the xanthan gum to the carbomer aqueous solution is preferably 0.02-0.1:0.2-0.4, more preferably 0.05-0.08:0.3.
The moisturizing cream provided by the invention comprises 0.01-0.15% of chelating agent, preferably 0.06-0.1% by mass. In the present invention, the chelating agent is preferably disodium ethylenediamine tetraacetate.
The moisturizing cream provided by the invention comprises 2.0-4.6% of emulsifying agent, preferably 3-4% of emulsifying agent, and more preferably 3.1-3.5% of emulsifying agent. In the present invention, the emulsifier preferably comprises one or more of arachidyl alcohol, behenyl alcohol, arachidyl alcohol glucoside, glyceryl stearate, PEG-100 stearate, cetyl stearyl alcohol and cetyl stearyl glucoside. When the emulsifier comprises more than two specific substances, the mass ratio of the specific substances is not particularly limited, and any ratio is adopted. In an embodiment of the present invention, the emulsifier is arachidyl alcohol, behenyl alcohol, arachidyl alcohol glucoside, glyceryl stearate, PEG-100 stearate, cetyl stearyl alcohol and cetyl stearyl glucoside, wherein the mass ratio of arachidyl alcohol, behenyl alcohol, arachidyl alcohol glucoside, glyceryl stearate, PEG-100 stearate, cetyl stearyl alcohol and cetyl stearyl glucoside is 0.5:0.4:0.2:0.6:0.7:0.5:0.2.
The moisturizing cream provided by the invention comprises the balance of water, and the water is preferably deionized water.
The invention also provides a preparation method of the moisturizing cream, which comprises the following steps:
mixing a humectant, a skin conditioning agent, a rheology modifier, a chelating agent and water to obtain a water phase;
mixing grease and an emulsifying agent to obtain an emulsion;
and mixing the water phase, the emulsion and the antibacterial microemulsion to obtain the moisturizing cream.
According to the invention, the humectant, the skin conditioning agent, the rheology modifier, the chelating agent and water are mixed to obtain a water phase. In the present invention, the temperature of the mixing is preferably 78 to 82 ℃, more preferably 79 to 80 ℃; the mixing is preferably performed under stirring, and the mode of the mixing is not particularly limited in the present invention as long as the mixing can be uniformly performed.
The invention mixes the grease and the emulsifying agent to obtain the emulsion. In the present invention, the temperature of the mixing is preferably 78 to 82 ℃, more preferably 79 to 80 ℃; the mixing is preferably performed under stirring, and the mode of the mixing is not particularly limited in the present invention as long as the mixing can be uniformly performed.
After obtaining the water phase and the emulsion, the invention mixes the water phase, the emulsion and the antibacterial microemulsion to obtain the moisturizing cream. In the present invention, the mixing preferably includes the steps of:
mixing the emulsion with the water phase to obtain primary moisturizing cream;
and mixing the primary moisturizing cream with the antibacterial microemulsion to obtain the moisturizing cream.
The emulsion and the water phase are mixed to obtain the primary moisturizing cream. In the present invention, the mixing is preferably accompanied by stirring at a rotation speed of 9000 to 11000r/min, more preferably 9500 to 10000r/min; the stirring time is preferably 4.8 to 5.2 minutes, more preferably 5 minutes.
After the primary moisturizing cream is obtained, the primary moisturizing cream and the antibacterial microemulsion are mixed to obtain the moisturizing cream. The present invention preferably further comprises, prior to mixing: and cooling the primary moisturizing cream. In the present invention, the temperature after the temperature reduction is preferably 53 to 57 ℃, more preferably 55 to 56 ℃. The cooling mode is not particularly limited, as long as the required temperature can be reached. The present invention is not particularly limited as long as the mixing can be uniformly performed.
The technical solutions provided by the present invention are described in detail below in conjunction with examples for further illustrating the present invention, but they should not be construed as limiting the scope of the present invention.
Example 1
Extracting leaves and bark of cortex Cinnamomi by steam distillation (feed-liquid ratio 50:1, extraction time 30 min) to obtain cortex Cinnamomi extract;
extracting Galla chinensis by reflux extraction (solvent is 65% ethanol water solution with mass concentration, feed-liquid ratio is 18:1, extraction temperature is 85deg.C, extraction time is 8min, and repeated extraction is 3 times); distilling the filtrate at 40deg.C under reduced pressure for 35min, and freeze drying at-50deg.C for 24 hr to obtain Galla chinensis extract;
extracting folium Camelliae sinensis by solvent extraction distillation (deionized water as solvent at a feed-liquid ratio of 25:1 and an extraction temperature of 65deg.C for 45min, repeating extraction for 4 times), and filtering the extracted product; distilling the filtrate at 50deg.C under reduced pressure for 40min, and freeze drying at-50deg.C for 24 hr to obtain tea extract;
dissolving 1.15g of tea extract (stirring at 40 ℃ C., 400 r/min) in 23g of deionized water to obtain water phase;
ultrasonic treating 1g Galla chinensis extract and 13.5g glycerol at 60deg.C under power of 200W for 10min to obtain Galla chinensis extract solution;
Uniformly stirring the gallnut extract solution, 13.5g of cinnamon extract and 50g of tween-80 at a rotating speed of 500r/min to obtain an oil phase;
and uniformly stirring the water phase and the oil phase at the speed of 650r/min to obtain the antibacterial microemulsion.
Examples 2 and 3 bacteriostatic microemulsions were prepared as in example 1, except that the amounts of the raw materials used were varied, and the amounts of the raw materials used in examples 2 and 3 were as shown in table 1.
TABLE 1 amounts of raw materials used in examples 1 to 3
Figure BDA0003522303180000151
The antibacterial microemulsion prepared in examples 1-3 is centrifuged for 10min at the rotation speed of 10000r/min and the temperature of 4 ℃ without layering, which indicates that the antibacterial microemulsion provided by the invention has good thermodynamic stability.
The irritation of example 1 was tested against chick embryo chorioallantoic membrane (chicken chorioallantoic membrane, CAM).
Test article: (1) Negative control, sodium chloride solution with the mass concentration of 0.9%; (2) positive control: 0.1mol/L sodium hydroxide; (3) solvent control: deionized water, isopropyl palmitate; (4) reference control: diluting with isopropyl palmitate, wherein the concentration of the propyl paraben is 0.05-0.3%; (5) sample: dilute with deionized water at a concentration of 0.1% to 0.6% of example 1.
According to SN/T2329-2009 standard, placing the chick embryo into an automatic incubator, setting the conditions to be 37.5+/-0.5 ℃ and the relative humidity to be 70%, and rotating the disc for 3-6 times/h.
9 days later, carrying out egg irradiation inspection, selecting fresh, clean and well-developed chick embryos, marking the positions of air chambers on the surfaces of eggshells, knocking a small hole in a marking range by using a needle head, and stripping eggshell parts with marks by using elbow forceps to expose white egg membranes. A proper amount of 0.9% sodium chloride solution is dripped into the egg membrane by a straw, and the sodium chloride solution is poured out after the egg membrane is wetted. And the inner membrane is removed by using forceps, so that the vascular membrane is not damaged. After observing and determining the structural integrity of the vascular system, 0.3mL of a test object is taken and directly dripped on the surface of the CAM, the CAM reaction condition is observed, and the occurrence time of each possible bleeding, coagulation and vascular dissolution toxic effect within 5min of action is recorded. 3 chick embryos were repeated for each group of subjects.
Observations were scored on the following criteria:
(1) Bleeding:
a) No bleeding (0 score);
b) Mild bleeding (1 min): bleeding from small blood vessels and small amount of bleeding (such as 0.5% TexaponASV, 5 min);
c) Moderate bleeding (2 minutes) bleeding from small and large vessels, and significant blood flow (e.g., 1.0% TexaponASV, 5 min);
d) Severe bleeding (3 minutes) almost all blood vessels bleed and a large amount of blood flows out (e.g. 5% texapon ASV, 5 min).
It should be noted that bleeding may be transient, and that the massive bleeding observed for the first 30 seconds may cover the bleeding response that occurs later.
(2) Coagulation
a) No clotting (0 min);
b) Light coagulation (1 minute) intravascular and/or extravascular light coagulation, and/or light turbidity of the CAM membrane (light coagulation such as 0.2% sodium hydroxide for 5min, light turbidity such as 0.3% acetic acid for 5 min);
c) Moderate coagulation (2 minutes) intravascular and/or extravascular moderate coagulation, and/or CAM membrane moderate turbidity
Figure BDA0003522303180000171
Turbidity (moderate coagulation such as 0.3% sodium hydroxide for 5min, moderate turbidity such as 3% acetic acid for 5 min);
d) Severe clotting (3 minutes) intravascular and/or extravascular Severe clotting, and/or Severe CAM membrane cloudiness (Severe clotting, e.g., 0.5% sodium hydroxide for 5min, severe cloudiness, e.g., 30% acetic acid for 5 min).
(3) Vascular thawing
a) Avascular thawing (0 minutes);
b) Mild vascular thawing (1 min) only small vessel thawing (e.g. 0.5% texaponasv, 5 min);
c) Moderate vascular thawing (2 minutes) tubule and macrovascular thawing (e.g. 1% TexaponASV, 5 min);
d) Severe vascular thawing (3 minutes) macrovascular and total vascular tree are thawed (e.g., 5% TexaponASV, 5 min).
Results were statistically analyzed using the stimulus score (IS) method, using the following calculation of the stimulus score (IS), with the results remaining two decimal places.
Wherein:
secH (bleeding time) - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - -string) is a time, in seconds(s) to be observed on the CAM membrane to initiate bleeding;
secL (vascular thawing time vessel lysis time) - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - -s) is the average time, in seconds(s) where onset of vascular thawing was observed on the CAM membrane;
secL (clotting time) - - - -the average time in seconds(s) at which clotting begins to occur is observed on the CAM membrane.
The eye irritation of the test subjects was classified according to the calculated IS values by table.
TABLE 2 evaluation of results of stimulation scoring
Figure BDA0003522303180000172
Figure BDA0003522303180000181
TABLE 3 chick embryo chorioallantoic membrane test record table
Figure BDA0003522303180000182
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Figure BDA0003522303180000191
The chick embryo chorioallantoic membrane test shows that the antibacterial microemulsion in the embodiment 1 has almost no irritation and is very mild, and compared with the chemical preservative propylparaben, the antibacterial microemulsion meets the requirements of modern people on health and green preservatives.
Comparative example 1
A microemulsion was prepared as in example 1, except that no tea extract was added.
Comparative example 2
A microemulsion was prepared as in example 1, except that the gallnut extract was not added.
Comparative example 3
A microemulsion was prepared as in example 1, except that tea extract and gallnut extract were not added.
Comparative example 4
A microemulsion was prepared as in example 1, except that no cinnamon extract was added.
Comparative example 5
A microemulsion was prepared as in example 1, except that cinnamon extract and nutgall extract were not added.
Comparative example 6
A microemulsion was prepared as in example 1, except that cinnamon extract and tea extract were not added.
The antibacterial activity of the microemulsions prepared in examples 1 to 3 and comparative examples 1 to 6 was measured as follows:
staphylococcus aureus ATCC6538, escherichia coli ATCC8739, pseudomonas aeruginosa ATCC9027, candida albicans ATCC10231 and aspergillus niger ATCC16404 are used as test strains.
Preparing a bacterial suspension:
preparing a liquid culture medium and a slant culture medium corresponding to strain growth, sterilizing, cooling to room temperature, picking a loop of strain (bacteria and microzyme) in the liquid culture medium by using an inoculating loop, picking spores by using an inoculating loop for aspergillus niger, streaking and inoculating on the slant culture medium, and subculturing for 2-3 generations to activate the strain.
Activated species (spores) were counted using a spread plate colony counting method. The plate colony counting method is to disperse the microbes in the sample completely into single cells after diluting the sample to be tested, and then to inoculate a certain amount of diluted sample solution onto the plate. After incubation at the appropriate temperature and time, each individual cell grows and propagates to form a visible colony, i.e., the individual colony should represent an individual cell in the original sample. Counting the number of colonies the number of bacteria in the sample can be calculated based on the dilution factor and the combined total amount of samples.
Accurately pressing the bacterial suspension to be tested to 10 -5 ~10 -8 A series of dilutions was made and 200. Mu.L of the dilution was inoculated into agar plates and spread evenly over the medium using a spreading bar. After bacteria or fungi are cultured for 2 days at the constant temperature of 37 ℃ or for 3 days at the constant temperature of 28 ℃, colonies formed by single cell propagation on a plate are recorded, a culture dish with the number of the colonies on the plate being 30-300 is reserved, and the number of bacteria in a sample is converted according to dilution times. According to the experimental requirement, the bacterial suspension is diluted to 1X 10 by a logarithmic dilution method 7 CFU/mL or 1X 10 8 CFU/mL。
Oxford cup method for measuring antibacterial effect of sample:
placing the sterilized culture medium into an ultra-clean workbench, cooling to 60 ℃, pouring into a flat plate, and horizontally placing until the culture medium is solidified for later use. 200. Mu.L of the bacterial suspension was removed by a pipette and applied to a plate and spread evenly with a spreading bar. A plurality of oxford cups with the inner diameter of 6mm after sterilization are prepared, the oxford cups are placed in a test plate by forceps, three oxford cups are placed in each dish, and 200 mu L of bacteriostatic microemulsion to be detected is injected into the oxford cups. Placing into a constant temperature incubator, culturing the bacteria plate at 37 ℃ for 24 hours, culturing the fungi plate at 28 ℃ for 48 hours, taking out, observing the growth condition of the bacterial colony, and measuring the size of the inhibition zone. The test results are shown in Table 4.
TABLE 4 bacteriostatic Activity of the bacteriostatic microemulsions prepared in examples 1 to 3 and comparative examples 1 to 6
Figure BDA0003522303180000201
Figure BDA0003522303180000211
Note that: + indicates that the diameter of the inhibition zone of the substance is larger than the experimental range, -indicates that the substance has no inhibition zone.
Determination criteria: the inhibition zone is more than or equal to 15mm and is highly sensitive, 10-15 mm is moderately sensitive, 7-9 mm is low sensitive, and no inhibition zone is insensitive.
From the results in Table 4, it can be seen that the natural active ingredient-containing antibacterial microemulsion prepared by the invention has excellent antibacterial activity on bacteria and fungi; the comparison results of the examples and the comparative examples show that under the combined action of the tea extract, the gallnut extract and the cinnamon extract, the antibacterial activity of the antibacterial microemulsion is obviously improved, and the antibacterial synergistic effect is achieved.
The bacteriostatic microemulsion, the bacteriostatic active components in the bacteriostatic microemulsion and the Minimum Inhibitory Concentration (MIC) of the propylparaben are detected according to the following method:
the product to be tested:
cinnamon extract, tea extract, gallnut extract, propylparaben and the bacteriostatic microemulsion prepared in example 1.
The test method comprises the following steps:
sterile 96 well cell culture plates were prepared, 200. Mu.L of sample solution was added to well 1, and 100. Mu.L of TSA or PDA liquid medium sterilized and cooled to room temperature was added to wells 2 to 10. Taking 100 μl of sample solution from No. 1 Kong Yi to No. 2, mixing thoroughly, and mixing The sample solution was removed to well 3, serially diluted to well 10 by repeating the procedure, and 100. Mu.L of the mixture in well 10 was discarded. Remove dilution to 1X 10 7 CFU/mL or 1X 10 5 The CFU/mL concentration bacterial suspension is placed in a hole No. 1-10, 100 mu L of a mixture of the bacterial suspension and the liquid culture medium is added in a hole No. 11, and 200 mu L of the liquid culture medium is added in a hole No. 12. The test results are shown in Table 5.
TABLE 5 minimum inhibitory concentration of each bacteriostatic active ingredient
Figure BDA0003522303180000221
Note that: -indicating that no minimum inhibitory concentration of the substance could be detected within the experimental concentration range.
As shown in Table 5, the tea extract and the gallnut extract have certain antibacterial activity on staphylococcus aureus, escherichia coli and pseudomonas aeruginosa, but have poor inhibition ability on saccharomycetes and aspergillus niger, and the antibacterial microemulsion containing natural active ingredients has high-efficiency and broad-spectrum antibacterial activity compared with single active substances. The cinnamon extract has excellent antibacterial capability, but the properties of hydrophobicity, strong irritation, spicy flavor and the like make the cinnamon extract difficult to be directly added into a cosmetic product as a raw material component, and the cinnamon extract is embedded into a microemulsion system by a microemulsion technology, so that the water solubility of antibacterial components is improved, the application limit of the cinnamon extract in cosmetics is reduced, and the bioavailability of the cinnamon extract is further improved.
Example 4
10% of humectant (0.1% of sodium hyaluronate, 4% of butanediol, 5.9% of glycerol), 1% of skin conditioning agent (0.2% of allantoin and 0.8% of DL-panthenol), 0.12% of rheology modifier (xanthan gum), 0.02% of chelating agent (disodium ethylenediamine tetraacetate), 0.5% of solubilizer (PEG-60 hydrogenated castor oil) and 88.26% of deionized water are stirred for 5min at a temperature of 85 ℃ and a rotating speed of 10000r/min, so that primary moisturizing water is obtained;
and uniformly stirring the primary moisturizing water and 0.1% of the antibacterial microemulsion prepared in the embodiment 1 to obtain the moisturizing water.
Example 5
Moisturizing water was prepared as in example 4 except that the mass percent of the bacteriostatic microemulsion was 0.2%.
Example 6
Moisturizing water was prepared as in example 4 except that the mass percent of the bacteriostatic microemulsion was 0.3%.
Example 7
Moisturizing water was prepared as in example 4 except that the mass percent of the bacteriostatic microemulsion was 0.4%.
Example 8
Moisturizing water was prepared as in example 4 except that the mass percent of the bacteriostatic microemulsion was 0.5%.
Example 9
Moisturizing water was prepared as in example 4 except that the mass percent of the bacteriostatic microemulsion was 0.6%.
Comparative example 7
Moisturizing water was prepared as in example 4, except that the mass percent of the bacteriostatic microemulsion was 0%.
Example 10
6.58% humectant (0.08% sodium hyaluronate, 6% butanediol, 0.5% trehalose), 0.9% skin conditioner (0.2% allantoin and 0.7% DL-panthenol), 0.3% rheology modifier (carbomer aqueous solution with mass concentration of 1%), 0.06% chelating agent (disodium ethylenediamine tetraacetate) and 82.24% deionized water are stirred at 80 ℃ to obtain a water phase;
8% of oil (5% caprylic/capric triglyceride, 2% cetyl ethyl hexanoate and 1% hydrogenated polyisobutene), 1.8% of emulsifier (0.8% C16 alkyl alcohol, 0.3% C15 alkyl glycoside, 0.5% cetyl alcohol and 0.2% cetostearyl glucoside), 0.07% of antioxidant (tocopheryl acetate) and 0.05% of pH regulator (aminomethylpropanol) were stirred at a temperature of 80℃to obtain an emulsion;
stirring the aqueous phase and the emulsion for 5min under the condition of 10000r/min to obtain primary moisturizing emulsion;
and (3) cooling the primary moisturizing emulsion to 55 ℃, and mixing with 0.1% of the antibacterial microemulsion prepared in the embodiment 1 to obtain the moisturizing emulsion.
Example 11
A moisturizing emulsion was prepared as in example 10, except that the mass percent of the bacteriostatic microemulsion was 0.2%.
Example 12
A moisturizing emulsion was prepared as in example 10, except that the mass percent of the bacteriostatic microemulsion was 0.3%.
Example 13
A moisturizing emulsion was prepared as in example 10, except that the mass percent of the bacteriostatic microemulsion was 0.4%.
Example 14
A moisturizing emulsion was prepared as in example 10, except that the mass percent of the bacteriostatic microemulsion was 0.5%.
Example 15
A moisturizing emulsion was prepared as in example 10, except that the mass percent of the bacteriostatic microemulsion was 0.6%.
Comparative example 8
A moisturizing emulsion was prepared as in example 10, except that the mass percent of the bacteriostatic microemulsion was 0%.
Example 16
11.08% humectant (0.08% sodium hyaluronate, 5% butylene glycol, 6% glycerin), 0.8% skin conditioning agent (DL-panthenol), 0.35% rheology modifier (0.3% carbomer aqueous solution with mass concentration of 1% and 0.05% xanthan gum), 0.06% chelating agent (disodium ethylenediamine tetraacetate) and 68.41% deionized water are stirred at 80 ℃ to obtain an aqueous phase;
17% oil (6% caprylic/capric triglyceride, 4% olive oil, 3% cyclomethicone and 4% cyclopentadimethicone), 3.1% emulsifier (0.5% arachidyl alcohol, 0.4% behenyl alcohol, 0.2% arachidyl alcohol glucoside, 0.6% glyceryl stearate, 0.7% PEG-100 stearate, 0.5% cetyl stearyl alcohol and 0.2% cetostearyl glucoside) were stirred at 80℃to obtain an emulsion;
stirring the aqueous phase and the emulsion for 5min under the condition of 10000r/min to obtain primary moisturizing cream;
and (3) after the primary moisturizing cream is cooled to 55 ℃, mixing the primary moisturizing cream with 0.1% of the antibacterial microemulsion prepared in the embodiment 1 to obtain the moisturizing cream.
Example 17
A moisturizing cream was prepared as in example 16, except that the mass percent of the bacteriostatic microemulsion was 0.2%.
Example 18
A moisturizing cream was prepared as in example 16, except that the mass percent of the bacteriostatic microemulsion was 0.3%.
Example 19
A moisturizing cream was prepared as in example 16, except that the mass percent of the bacteriostatic microemulsion was 0.4%.
Example 20
A moisturizing cream was prepared as in example 16, except that the mass percent of the bacteriostatic microemulsion was 0.5%.
Example 21
A moisturizing cream was prepared as in example 16, except that the mass percent of the bacteriostatic microemulsion was 0.6%.
Comparative example 9
A moisturizing cream was prepared as in example 16, except that the mass percent of the bacteriostatic microemulsion was 0%.
The moisturizing waters prepared in examples 4 to 9 and comparative example 7, the moisturizing emulsions prepared in examples 10 to 15 and comparative example 8, and the moisturizing creams prepared in examples 16 to 21 and comparative example 9 were examined for their anti-corrosive properties as follows.
5 parts of moisturizing water prepared in each of examples and comparative examples was taken30g of wet emulsion and moisturizing cream are placed in sterilized conical flasks, 3 parts are inoculated with 0.3mL of 1X 10 solution 8 Bacterial suspensions of CFU/mL staphylococcus aureus, escherichia coli, and pseudomonas aeruginosa; 2 portions of the mixture are inoculated with 0.3mL of 1X 10 7 CFU/mL candida albicans and aspergillus niger spore fungus suspension. Mixing uniformly by a vortex oscillator, standing at a dry and ventilated place, and preserving at room temperature (20-25 ℃). The colony count of each sample was tested once at 2 days, 7 days, 14 days, 28 days, respectively, within 28 days of inoculation. 1mL of the sample is removed, the sample is diluted to a proper concentration by sterile physiological saline logarithm, and the microbial content in the sample is calculated by adopting a plate counting method, and each group is tested in three times. The test results refer to the evaluation criteria of the European pharmacopoeia (EP 9.05.1.3) corrosion protection challenge test.
TABLE 6 evaluation criteria for anticorrosive effect (EP 9.05.1.3)
Figure BDA0003522303180000261
Note that: NI represents no microbial growth compared to the previous test time point
Standard a is the recommended preservative effect. In a reasonable case, for example, the risk of adverse reactions increases due to an increased preservative effect, allowing standard a to be unsatisfied, standard B must be met.
The test results are shown in tables 7 to 9.
Table 7 results of preservative challenge experiments on moisturizing waters
Figure BDA0003522303180000262
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Figure BDA0003522303180000271
Figure BDA0003522303180000281
/>
Table 8 results of anti-corrosion challenge experiments on moisturizing emulsions
Figure BDA0003522303180000282
/>
Figure BDA0003522303180000291
Table 9 results of antiseptic challenge experiments on moisturizing creams
Figure BDA0003522303180000292
/>
Figure BDA0003522303180000301
Figure BDA0003522303180000311
As can be seen from tables 7 to 9, the colony count of bacteria and fungi of the cosmetics in the blank group did not significantly decrease, and the cosmetics did not have preservative ability as compared with the cosmetics to which the natural active ingredient-containing bacteriostatic microemulsion of example 1 was added. In the three dosage forms, when the addition amount of the antibacterial microemulsion is 0.1-0.6%, the antibacterial microemulsion can pass through the anti-corrosion challenge test of bacteria and fungi in the evaluation standard of the anti-corrosion challenge test of European pharmacopoeia (EP 9.05.1.3), and the anti-corrosion effect is enhanced along with the increase of the addition amount of the antibacterial microemulsion. Considering the results of tables 5 to 7, the addition amount of the antibacterial microemulsion in the cosmetics should be 0.5 to 0.6 percent to achieve high-efficiency antiseptic capacity.
Although the foregoing embodiments have been described in some, but not all, embodiments of the invention, it should be understood that other embodiments may be devised in accordance with the present embodiments without departing from the spirit and scope of the invention.

Claims (10)

1. The antibacterial microemulsion comprises the following components in percentage by mass:
Figure FDA0004221580280000011
the emulsifier is Tween-80;
the auxiliary emulsifier is glycerol;
the extraction method of the cinnamon extract comprises the following steps: extracting leaves and bark of cinnamon by a steam distillation method to obtain cinnamon extract, wherein the feed-liquid ratio is 50:1, and the extraction time is 30min;
the extraction method of the gallnut extract comprises the following steps: extracting Galla chinensis by reflux extraction method with 65% ethanol water solution with mass concentration as solvent and feed-liquid ratio of 18:1, at 85deg.C for 8min, and repeating extraction for 3 times; distilling the filtrate at 40deg.C under reduced pressure for 35min, and freeze drying at-50deg.C for 24 hr to obtain Galla chinensis extract;
the extraction method of the tea extract comprises the following steps: extracting tea leaves by a solvent extraction distillation method, filtering the extracted product, wherein the solvent is deionized water, the feed-liquid ratio is 25:1, the extraction temperature is 65 ℃, the extraction time is 45min, and repeating the extraction for 4 times; distilling the filtrate at 50deg.C under reduced pressure for 40min, and freeze drying at-50deg.C for 24 hr to obtain tea extract;
The preparation method of the antibacterial microemulsion comprises the following steps:
dissolving the tea leaf extract in water to obtain water phase;
dissolving Galla chinensis extract in auxiliary emulsifier to obtain Galla chinensis extract solution;
mixing the gallnut extract solution, the emulsifying agent and the cinnamon extract for the first time to obtain an oil phase;
and carrying out second mixing on the water phase and the oil phase to obtain the antibacterial microemulsion.
2. The bacteriostatic microemulsion of claim 1, comprising the following components in percentage by mass:
Figure FDA0004221580280000012
Figure FDA0004221580280000021
3. a method of preparing the bacteriostatic microemulsion of claim 1 or 2, comprising the steps of:
dissolving the tea leaf extract in water to obtain water phase;
dissolving Galla chinensis extract in auxiliary emulsifier to obtain Galla chinensis extract solution;
mixing the gallnut extract solution, the emulsifying agent and the cinnamon extract for the first time to obtain an oil phase;
and carrying out second mixing on the water phase and the oil phase to obtain the antibacterial microemulsion.
4. Use of the bacteriostatic microemulsion according to claim 1 or 2 or the bacteriostatic microemulsion prepared by the preparation method according to claim 3 as a preservative in daily chemical products.
5. The moisturizing water comprises the following components in percentage by mass:
Figure FDA0004221580280000022
The bacteriostatic microemulsion is the bacteriostatic microemulsion of claim 1 or 2.
6. The method for preparing the moisturizing lotion according to claim 5, comprising the following steps:
mixing a humectant, a skin conditioning agent, a rheology modifier, a chelating agent, a solubilizer and water to obtain primary moisturizing water;
and mixing the primary moisturizing water with the antibacterial microemulsion to obtain the moisturizing water.
7. The moisturizing emulsion comprises the following components in percentage by mass:
Figure FDA0004221580280000023
Figure FDA0004221580280000031
the bacteriostatic microemulsion is the bacteriostatic microemulsion of claim 1 or 2.
8. The method for preparing the moisturizing emulsion as claimed in claim 7, comprising the following steps:
mixing a humectant, a skin conditioning agent, a rheology modifier, a chelating agent and water to obtain a water phase;
mixing grease, an emulsifying agent, an antioxidant and a pH value regulator to obtain an emulsion;
and mixing the water phase, the emulsion and the antibacterial microemulsion to obtain the moisturizing emulsion.
9. A moisturizing cream comprises the following components in percentage by mass:
Figure FDA0004221580280000032
the bacteriostatic microemulsion is the bacteriostatic microemulsion of claim 1 or 2.
10. The method for preparing the moisturizing cream as claimed in claim 9, comprising the following steps:
mixing a humectant, a skin conditioning agent, a rheology modifier, a chelating agent and water to obtain a water phase;
Mixing grease and an emulsifying agent to obtain an emulsion;
and mixing the water phase, the emulsion and the antibacterial microemulsion to obtain the moisturizing cream.
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