CN115487113B - Emulsion containing clove fruit extract and preparation method and application thereof - Google Patents

Emulsion containing clove fruit extract and preparation method and application thereof Download PDF

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CN115487113B
CN115487113B CN202211178490.5A CN202211178490A CN115487113B CN 115487113 B CN115487113 B CN 115487113B CN 202211178490 A CN202211178490 A CN 202211178490A CN 115487113 B CN115487113 B CN 115487113B
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ethyl acetate
clove
fruits
extract
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CN115487113A (en
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刘平怀
左遨勋
高玉梅
范艺灜
岑祥妮
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Hainan University
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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
    • A61K8/97Cosmetics 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
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    • A61K8/9789Magnoliopsida [dicotyledons]
    • 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
    • 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
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/40Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing nitrogen
    • A61K8/44Aminocarboxylic acids or derivatives thereof, e.g. aminocarboxylic acids containing sulfur; Salts; Esters or N-acylated derivatives thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
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    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P17/00Drugs for dermatological disorders
    • A61P17/18Antioxidants, e.g. antiradicals
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q1/00Make-up preparations; Body powders; Preparations for removing make-up
    • A61Q1/02Preparations containing skin colorants, e.g. pigments
    • 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
    • A61Q17/04Topical preparations for affording protection against sunlight or other radiation; Topical sun tanning 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
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • A61Q19/02Preparations for care of the skin for chemically bleaching or whitening the skin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • A61Q19/10Washing or bathing preparations
    • 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
    • A61K2800/522Antioxidants; Radical scavengers
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    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
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    • Y02A40/00Adaptation technologies in agriculture, forestry, livestock or agroalimentary production
    • Y02A40/90Adaptation technologies in agriculture, forestry, livestock or agroalimentary production in food processing or handling, e.g. food conservation
    • 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 provides an emulsion containing clove fruit extract, which comprises clove fruit extract, glucamate SSE-20, glucate SS, eumulgin SG and a cosmetic matrix. The emulsion containing the clove fruit extract provided by the invention has better moisturizing effect, provides lasting moisturizing effect for skin, and has certain whitening and antioxidation effects.

Description

Emulsion containing clove fruit extract and preparation method and application thereof
Technical Field
The invention belongs to the technical field of daily chemical products, and particularly relates to an emulsion containing clove fruit extract, a preparation method and application thereof.
Background
Emulsion additives refer to small or trace amounts of substances added during the production, processing and use of the emulsion, and are used in the emulsion in small amounts but have a remarkable effect. The emulsion additive is a raw material frequently used in the modern emulsion industry, and has obvious effects in enhancing the efficacy value of basic emulsion and the like.
The myrtaceae plant clove (Eugenia caryophyllata thunder.) is a perfume native to indonesia, has been introduced into tropical areas around the world, and is one of the traditional importation "south medicine" in china. The clove is used as a traditional imported Chinese medicinal material, the application value of the clove is widely developed, and the traditional Chinese medicinal material has the formula preparations such as stomach medicine, tendon relaxing paste, nose paste, sleep aiding powder and the like; there are also life applications involving hunting, such as persistent essence, mosquito repellent, antibacterial hand sanitizer, traditional Chinese medicine distiller's yeast, etc. According to the laws of plant resource chemistry, different parts of the same plant may contain the same or similar components, and clove is used as a medicinal plant, the main medicinal value of which is in flower buds, but the development of active components of other parts such as fruits, leaves and rhizomes is also necessary. The clove is firstly carried in Tripterygium wilfordii parviflorum, the fruits of which are used as medicines in the first place in Liang Daitao Hongyi parviflorum, and the subsequent southern grass and wood shape are recorded, the national traditional Chinese medicine administration has recorded the clove fruits as one of 39 Chinese medicinal material varieties which are mainly developed in China, the pharmacological activity of the clove is covered in a plurality of aspects, such as clove oil contained in the mother clove, the clove has stronger antifungal and mildew-proof activity, and can be used as a natural antifungal agent for fruit storage in winter; the clove decoction has obvious inhibition effect on pathogenic bacteria such as tubercle bacillus, typhoid bacillus, shigella dysenteriae and the like, and can treat related diseases caused by the pathogenic bacteria; the ethyl acetate extract contained in the clove fruit has stronger acaricidal activity and the like.
Therefore, how to use the extract containing the clove fruits in the emulsion ensures that the emulsion has better moisturizing effect, provides lasting moisturizing effect for skin, and has certain whitening and antioxidation effects at the same time, thus the problem to be solved is solved.
Disclosure of Invention
In view of the above, the technical problem to be solved by the invention is to provide the emulsion containing the clove fruit extract, and the preparation method and the application thereof.
The invention provides an emulsion containing clove fruit extract, which comprises clove fruit extract, glucamate SSE-20, glucate SS, eumulgin SG and a cosmetic matrix.
Preferably, the clove fruit extract is ethyl acetate extract of clove fruit.
Preferably, the material is prepared from the following raw materials in parts by mass:
1 to 3 parts of Glucamate SSE-20, 0.5 to 1.5 parts of Glucate SS, 0.2 to 0.4 part of Eumulgin SG, 3 to 5 parts of ethyl acetate extract of clove fruits and 81.5 to 106.16 parts of cosmetic matrix.
Preferably, the material is prepared from the following raw materials in parts by mass:
1 to 3 parts of Glucamate SSE-20, 0.5 to 1.5 parts of Glucate SS, 1 to 3 parts of stearic acid, 2 to 4 parts of ethylhexyl methoxycinnamate, 6 to 8 parts of octyl dodecanol, 0.2 to 0.4 part of Eumulgin SG, 0.04 to 0.06 part of EDTA disodium, 3 to 5 parts of glycerin, 0.05 to 0.15 part of xanthan gum, 0.3 to 0.5 part of hydroxyethyl acrylate, 0.05 to 0.15 part of citric acid, 0.05 to 0.15 part of methyl paraben, 3 to 5 parts of ethyl acetate extract of clove fruits, 3 to 5 parts of 1, 3-butanediol, 3 to 5 parts of beta-glucan, 0.05 to 0.15 part of pentaerythritol tetra (bis-tert-butyl hydroxy hydrocinnamate) ester and 60 to 70 parts of water.
Preferably, the material is prepared from the following raw materials in parts by mass:
0.5 to 2.5 parts of Glucamate SSE-20, 0.3 to 1.2 parts of Glucate SS, 0.5 to 2.5 parts of stearic acid, 1.5 to 3.5 parts of ethylhexyl methoxycinnamate, 5.5 to 7.5 parts of octyl dodecanol, 0.15 to 0.35 part of Eumulgin SG, 0.03 to 0.05 part of EDTA disodium, 2 to 4 parts of glycerin, 0.02 to 0.12 part of xanthan gum, 0.2 to 0.4 part of hydroxyethyl acrylate, 0.03 to 0.12 part of citric acid, 0.03 to 0.12 part of methylparaben, 2 to 4 parts of clove fruit ethyl acetate extract, 2 to 4 parts of 1, 3-butanediol, 2 to 4 parts of beta-glucan, 0.03 to 0.13 part of pentaerythritol tetrakis (bis-tert-butyl hydroxy hydrocinnamate) and 60 to 70 parts of water.
Preferably, the material is prepared from the following raw materials in parts by mass:
glucamate SSE-20 parts, glucate SS 1 part, stearic acid 2 parts, ethylhexyl methoxycinnamate 3 parts, octyldodecanol 7 parts, eumulgin SG 0.3 parts, disodium EDTA 0.05 parts, glycerin 4 parts, xanthan gum 0.1 parts, hydroxyethyl acrylate 0.4 parts, citric acid 0.1 parts, methylparaben 0.1 parts, clove fruit ethyl acetate extract 4 parts, 1, 3-butanediol 4 parts, beta-glucan 4 parts, pentaerythritol tetrakis (bis-t-butylhydroxyhydrocinnamate) 0.1 parts, water 67.85 parts.
The invention also provides a preparation method of the emulsion, which comprises the following steps:
a) Mixing Glucamate SSE-20 with Glucate SS, stearic acid, ethylhexyl methoxycinnamate, octyl dodecanol and pentaerythritol tetra (di-tert-butyl hydroxy hydrocinnamate), and mechanically stirring until the solids are completely dissolved to obtain an oil phase;
b) Dissolving water, hydroxyethyl acrylate, eumulgin SG, 1, 3-butanediol, beta-glucan, glycerol, methyl benzoate and xanthan gum under stirring to obtain a water phase;
c) Mixing and emulsifying the oil phase and the water phase to obtain emulsion;
d) Adding flos Caryophylli fruit extract and EDTA disodium into the emulsion, mixing, and adjusting pH to obtain emulsion containing flos Caryophylli fruit extract.
Preferably, the pH is adjusted to 4.0 to 5.0.
The invention also provides application of the emulsion in preparation of cosmetics with moisturizing and antioxidative properties.
Preferably, the cosmetic is selected from skin-cleaning products, lotions, creams, essences, barrier, sun protection, foundations or concealers.
Compared with the prior art, the invention provides an emulsion containing the clove fruit extract, which comprises the clove fruit extract, glucamate SSE-20, glucate SS, eumulgin SG and a cosmetic matrix. The two emulsifying agents used in the invention are Glucamate SSE-20, glucate SS and Eumulgin SG, wherein the oil phase emulsifying agents Glucamate SSE-20 and Glucate SS are nonionic emulsifying agents with unique performance, are one of glucoside derivatives from natural corn starch, the Glucamate SS has water-in-oil emulsifying activity, and the Glucamate SSE-20 is an oil-in-water emulsifying agent, and the two emulsifying agents are combined to generate high-quality emulsifying effect; moreover, the viscosities produced by Glucamate SSE-20 and Glucate SS are resistant to the damaging effects of mechanical work or shear stress applied after emulsion formation, provided that the viscosity is reduced by pumping and filling during the production operation, the viscosity generally reverts within days. In addition, the aqueous phase emulsifier Eumulgin SG is a liquid crystal amino acid emulsifier, has very good compatibility with electrolyte, and is very suitable for various formulations rich in additives and formulations of skin care products containing water-soluble sunscreens; the excellent emulsifying capacity of the skin-care cream can achieve the aim of improving skin feel by adjusting the dosages of grease, wax and polymer, has excellent compatibility with various electrolytes, water-soluble UV-sunscreens and inorganic and organic sunscreens, promotes the formation of lamellar liquid crystal phases and has excellent moisturizing capacity; it is also an emulsifier with very high safety and is therefore also suitable for use in a variety of different types of skin care product formulations.
In addition, the clove fruit ethyl acetate extract is added into the clove fruit emulsion, wherein the ethyl acetate extract is obtained by sectional extraction through an ethanol solvent extraction method, has rich special fragrance, contains flavonoid, polyphenol, polysaccharide and other compounds as main components, has strong effects of moisturizing, sun-screening, bacteriostasis, antioxidation and the like, can improve the skin care effect of the emulsion, and better improves the moisturizing and antioxidation performances of the emulsion.
Detailed Description
The invention provides an emulsion containing clove fruit extract, which is characterized by comprising clove fruit extract, glucamate SSE-20, glucate SS, eumulgin SG and a cosmetic matrix.
In some embodiments of the invention, the clove fruit extract is ethyl acetate extract of clove fruit.
The ethyl acetate extract of the clove fruits is obtained by sectional extraction after an ethanol solvent extraction method, has intense special fragrance, contains flavonoid, polyphenol, polysaccharide and other compounds as main components, has strong effects of preserving moisture, preventing sun, inhibiting bacteria, resisting oxidation and the like, can improve the skin care effect of the emulsion, and better promotes the moisturizing and resisting oxidation performances of the emulsion.
Specifically, the ethyl acetate extract of the clove fruits provided by the invention is prepared according to the following method:
extracting ethyl acetate extract of the clove fruits by adopting a solvent extraction method:
grinding and pulverizing natural air-dried flos Caryophylli fruit with high-speed pulverizer, repeatedly stirring and leaching with high-concentration ethanol, concentrating to obtain flos Caryophylli fruit solid extract,
then dispersing the solid extract of the clove fruits into ultrapure water, adding petroleum ether for extraction, standing for layering, removing a petroleum ether layer, adding dichloromethane for extraction, standing for layering, removing a dichloromethane layer, and finally adding ethyl acetate for extraction to obtain an ethyl acetate layer;
and (3) evaporating, concentrating and volatilizing the ethyl acetate layer by rotary evaporation, and collecting the obtained ethyl acetate extract of the clove fruits.
Wherein, the volume concentration of the high-concentration ethanol is 85-95%;
the mass-volume ratio of the natural air-dried clove fruits to the high-concentration ethanol is 6kg:15L
The mass volume ratio of the solid extract of the clove fruits to the ultrapure water is 2kg:5L; the volume ratio of the ultrapure water to the petroleum ether to the dichloromethane to the ethyl acetate is 5:3.5:6:6.
in some embodiments of the invention, the emulsion containing the clove fruit extract is prepared from the following raw materials in parts by mass:
1 to 3 parts of Glucamate SSE-20, 0.5 to 1.5 parts of Glucate SS, 0.2 to 0.4 part of Eumulgin SG, 3 to 5 parts of ethyl acetate extract of clove fruits and 81.5 to 106.16 parts of cosmetic matrix.
The cosmetic matrix is not particularly limited, and can be used as a raw material matrix and an auxiliary material matrix for preparing emulsion.
In some specific embodiments of the invention, the emulsion containing the clove fruit extract is prepared from the following raw materials in parts by mass:
1 to 3 parts of Glucamate SSE-20, 0.5 to 1.5 parts of Glucate SS, 1 to 3 parts of stearic acid, 2 to 4 parts of ethylhexyl methoxycinnamate, 6 to 8 parts of octyl dodecanol, 0.2 to 0.4 part of Eumulgin SG, 0.04 to 0.06 part of EDTA disodium, 3 to 5 parts of glycerin, 0.05 to 0.15 part of xanthan gum, 0.3 to 0.5 part of hydroxyethyl acrylate, 0.05 to 0.15 part of citric acid, 0.05 to 0.15 part of methyl paraben, 3 to 5 parts of ethyl acetate extract of clove fruits, 3 to 5 parts of 1, 3-butanediol, 3 to 5 parts of beta-glucan, 0.05 to 0.15 part of pentaerythritol tetra (bis-tert-butyl hydroxy hydrocinnamate) ester and 60 to 70 parts of water.
In some preferred embodiments, the emulsion containing the clove fruit extract is prepared from the following raw materials in parts by mass:
0.5 to 2.5 parts of Glucamate SSE-20, 0.3 to 1.2 parts of Glucate SS, 0.5 to 2.5 parts of stearic acid, 1.5 to 3.5 parts of ethylhexyl methoxycinnamate, 5.5 to 7.5 parts of octyl dodecanol, 0.15 to 0.35 part of Eumulgin SG, 0.03 to 0.05 part of EDTA disodium, 2 to 4 parts of glycerin, 0.02 to 0.12 part of xanthan gum, 0.2 to 0.4 part of hydroxyethyl acrylate, 0.03 to 0.12 part of citric acid, 0.03 to 0.12 part of methylparaben, 2 to 4 parts of clove fruit ethyl acetate extract, 2 to 4 parts of 1, 3-butanediol, 2 to 4 parts of beta-glucan, 0.03 to 0.13 part of pentaerythritol tetrakis (bis-tert-butyl hydroxy hydrocinnamate) and 60 to 70 parts of water.
In some more preferred embodiments of the present invention, the emulsion containing the clove fruit extract is prepared from the following raw materials in parts by mass:
glucamate SSE-20 parts, glucate SS 1 part, stearic acid 2 parts, ethylhexyl methoxycinnamate 3 parts, octyldodecanol 7 parts, eumulgin SG 0.3 parts, disodium EDTA 0.05 parts, glycerin 4 parts, xanthan gum 0.1 parts, hydroxyethyl acrylate 0.4 parts, citric acid 0.1 parts, methylparaben 0.1 parts, clove fruit ethyl acetate extract 4 parts, 1, 3-butanediol 4 parts, beta-glucan 4 parts, pentaerythritol tetrakis (bis-t-butylhydroxyhydrocinnamate) 0.1 parts, water 67.85 parts.
The invention also provides a preparation method of the emulsion containing the clove fruit extract, which comprises the following steps:
a) Mixing Glucamate SSE-20 with Glucate SS, stearic acid, ethylhexyl methoxycinnamate, octyl dodecanol and pentaerythritol tetra (di-tert-butyl hydroxy hydrocinnamate), and mechanically stirring until the solids are completely dissolved to obtain an oil phase;
b) Dissolving water, hydroxyethyl acrylate, eumulgin SG, 1, 3-butanediol, beta-glucan, glycerol, methyl benzoate and xanthan gum under stirring to obtain a water phase;
c) Mixing and emulsifying the oil phase and the water phase to obtain emulsion;
d) Adding flos Caryophylli fruit extract and EDTA disodium into the emulsion, mixing, and regulating pH with citric acid to obtain emulsion containing flos Caryophylli fruit extract.
Specifically, heating an oil phase pot which is prepared to be cleaned and dried, adding an oil phase emulsifier, stearic acid, ethylhexyl methoxycinnamate, octyl dodecanol and pentaerythritol tetra (di-tert-butyl hydroxy hydrocinnamate), and mechanically stirring uniformly until the solid is completely dissolved to obtain an oil phase; the heating temperature is 80-90 ℃.
Adding deionized water into a water phase pot, adding hydroxyethyl acrylate, a water phase emulsifier, 1, 3-butanediol, glycerol, methyl paraben and xanthan gum, wherein the xanthan gum needs to be added with glycerol in advance, stirring to dissolve the xanthan gum, increasing the water bath temperature to 80-90 ℃, and mechanically stirring uniformly to completely dissolve the xanthan gum to obtain a water phase;
adding the uniformly dispersed oil phase components into the water phase, adjusting the water bath temperature to 80-90 ℃, and setting the homogenizing speed to 3000-3500 r.min -1 Homogenizing for 5-8 min, stopping heating after the emulsification process is finished, and continuing stirring until cooling to room temperature.
And finally adding the ethyl acetate extract of the clove fruits and EDTA disodium, continuously stirring for 5-8 min, and regulating the pH value to obtain the final finished emulsion. The pH adjustment requires complete cooling to room temperature. Wherein the pH is 4.0-5.0.
The preparation method of the emulsion containing the clove fruit extract provided by the invention has the advantages of simple process and convenient operation.
The invention also provides application of the emulsion containing the clove fruit extract in preparation of cosmetics with moisturizing and oxidation resistance.
Wherein the cosmetic is selected from skin care products, lotions, creams, essences, barrier, sunscreens, foundations or concealers.
According to the invention, the addition of the clove fruit extract is combined with a specific kind of emulsifier, so that the emulsion has a better moisturizing effect, a lasting moisturizing effect is provided for skin, and a certain whitening and antioxidation effect is provided.
In order to further understand the present invention, the emulsion containing the clove fruit extract provided by the present invention, the preparation method and application thereof are described below with reference to examples, and the scope of the present invention is not limited by the following examples.
In the following examples, ethyl acetate extracts of clove fruits were prepared as follows:
extracting ethyl acetate extract of the clove fruits by adopting a solvent extraction method:
taking 6kg of natural air-dried clove fruits, grinding and crushing by a high-speed grinder, repeatedly stirring and leaching for 72h by using 15L of ethanol with the volume concentration of 95% for 7 times, combining leaching liquor, and concentrating to obtain the solid extract of the clove fruits.
Then dispersing 2kg of the solid extract of the clove fruits into 5L of ultrapure water, adding 3.5L of petroleum ether for extraction, standing for layering, removing a petroleum ether layer, adding 6L of dichloromethane for extraction, standing for layering, removing a dichloromethane layer, and finally adding 6L of ethyl acetate for extraction to obtain an ethyl acetate layer;
and (3) evaporating the ethyl acetate layer by rotary evaporation, concentrating and volatilizing, and collecting 124g of the obtained ethyl acetate extract of the clove fruits.
Example 1
Glucamate SSE-20 parts, glucate SS 1 part, stearic acid 2 parts, ethylhexyl methoxycinnamate 3 parts, octyldodecanol 7 parts, eumulgin SG 0.3 parts, disodium EDTA 0.05 parts, glycerin 4 parts, xanthan gum 0.1 parts, hydroxyethyl acrylate 0.4 parts, citric acid 0.1 parts, methylparaben 0.1 parts, clove fruit ethyl acetate extract 4 parts, 1, 3-butanediol 4 parts, beta-glucan 4 parts, pentaerythritol tetrakis (bis-t-butylhydroxyhydrocinnamate) 0.1 parts, water 67.85 parts.
The preparation method of the emulsion containing the clove fruit extract comprises the following steps:
heating the cleaned and dried oil phase pot to 85 ℃, adding an oil phase emulsifier, stearic acid, ethylhexyl methoxycinnamate, octyl dodecanol and pentaerythritol tetra (di-tert-butyl hydroxy hydrocinnamate), and mechanically stirring uniformly until the solid is completely dissolved; adding deionized water into a water phase pot, adding hydroxyethyl acrylate, a water phase emulsifier, 1, 3-butanediol, glycerol, methyl paraben and xanthan gum, wherein the xanthan gum needs to be added with glycerol in advance, stirring to dissolve the xanthan gum, increasing the water bath temperature to 85 ℃, and mechanically stirring uniformly until the xanthan gum is completely dissolved; adding the uniformly dispersed oil phase components into the water phase, adjusting the water bath temperature to 85 ℃, and setting the homogenization speed to 3000 r.min -1 Homogenizing for 5min, stopping heating after the emulsification process is finished, continuing stirring until cooling to room temperature, adding flos Caryophylli fruit ethyl acetate extract and EDTA disodium, continuing stirring for 6min, and regulating pH to obtain final emulsion.
Example 2
Glucamate SSE-20 parts, glucate SS 0.5 parts, stearic acid 1 part, ethylhexyl methoxycinnamate 2 parts, octyldodecanol 6 parts, eumulgin SG 0.2 parts, disodium EDTA 0.04 parts, glycerol 3 parts, xanthan gum 0.05 parts, hydroxyethyl acrylate 0.3 parts, citric acid 0.05 parts, methylparaben 0.05 parts, clove fruit ethyl acetate extract 3 parts, 1, 3-butanediol 3 parts, beta-glucan 3 parts, pentaerythritol tetrakis (bis-t-butylhydroxyhydrocinnamate) 0.05 parts, water 76.76 parts.
The preparation method of the emulsion containing the clove fruit extract comprises the following steps:
heating the cleaned and dried oil phase pot to 85 ℃, adding an oil phase emulsifier, stearic acid, ethylhexyl methoxycinnamate, octyl dodecanol and pentaerythritol tetra (di-tert-butyl hydroxy hydrocinnamate), and mechanically stirring uniformly until the solid is completely dissolved; adding deionized water into water phase pot, adding hydroxyethyl acrylate, water phase emulsifier, 1, 3-butanediol, glycerol, methyl hydroxybenzoate and xanthan gum, wherein the xanthan gum needs to be added with glycerol in advance, stirring to make itDissolving, raising the temperature of the water bath to 85 ℃, and mechanically stirring uniformly until the water bath is completely dissolved; adding the uniformly dispersed oil phase components into the water phase, adjusting the water bath temperature to 85 ℃, and setting the homogenization speed to 3000 r.min -1 Homogenizing for 5min, stopping heating after the emulsification process is finished, continuing stirring until cooling to room temperature, adding flos Caryophylli fruit ethyl acetate extract and EDTA disodium, continuing stirring for 6min, and regulating pH to obtain final emulsion.
Example 3
Glucamate SSE-20.5 parts, glucate SS 1 part, stearic acid 1.5 parts, ethylhexyl methoxycinnamate 3.5 parts, octyldodecanol 7.5 parts, eumulgin SG 0.3 parts, disodium EDTA 0.05 parts, glycerin 4 parts, xanthan gum 0.1 parts, hydroxyethyl acrylate 0.4 parts, citric acid 0.1 parts, methylparaben 0.1 parts, ethyl acetate extract of clove fruit 4 parts, 1, 3-butanediol 4 parts, beta-glucan 4 parts, pentaerythritol tetrakis (bis-t-butylhydroxyhydrocinnamate) 0.1 parts, water 67.85 parts.
The preparation method of the emulsion containing the clove fruit extract comprises the following steps:
heating the cleaned and dried oil phase pot to 85 ℃, adding an oil phase emulsifier, stearic acid, ethylhexyl methoxycinnamate, octyl dodecanol and pentaerythritol tetra (di-tert-butyl hydroxy hydrocinnamate), and mechanically stirring uniformly until the solid is completely dissolved; adding deionized water into a water phase pot, adding hydroxyethyl acrylate, a water phase emulsifier, 1, 3-butanediol, glycerol, methyl paraben and xanthan gum, wherein the xanthan gum needs to be added with glycerol in advance, stirring to dissolve the xanthan gum, increasing the water bath temperature to 85 ℃, and mechanically stirring uniformly until the xanthan gum is completely dissolved; adding the uniformly dispersed oil phase components into the water phase, adjusting the water bath temperature to 85 ℃, and setting the homogenization speed to 3000 r.min -1 Homogenizing for 5min, stopping heating after the emulsification process is finished, continuing stirring until cooling to room temperature, adding flos Caryophylli fruit ethyl acetate extract and EDTA disodium, continuing stirring for 6min, and regulating pH to obtain final emulsion.
The ethyl acetate extract of the clove fruits prepared by the invention is subjected to effective chemical component measurement:
(1) Material
Gallic acid, fu Lin Fen, sodium carbonate, absolute ethyl alcohol, anthrone and glucose.
(2) Test design
The test was performed with reference to T/AHFIA005-2018 determination of total polyphenol content in plant extracts and products thereof and GB/T15672-2009 determination of total sugar content in edible fungi.
(3) Test results
The linear formula of the measurement results is shown below:
total polyphenols: y=0.0091 x+0.0105, r 2 =0.9996;
Total polysaccharide: y=0.0070 x+0.0673, r 2 =0.9991;
TABLE 1 determination of effective chemical components
The content measurement results of the effective chemical components of the ethyl acetate extract of the clove fruits are shown in table 1. As shown in Table 1, the total polyphenol and total polysaccharide content of the extract was high, and the ratio was 69.62%. The material has strong effects of moisture preservation, sun protection, bacteriostasis, antioxidation and the like, can improve the skin care effect of the emulsion, and better promotes the moisture preservation and antioxidation performance of the emulsion.
In vitro moisturizing efficacy assay for different moisturizing combinations:
(1) Material
Glycerol; 1, 3-butanediol; beta-glucan; water; ethyl acetate extract of lilac fruit.
(2) Test design
Accurately weighing the samples according to the following three combinations, placing the samples in a dry culture dish, transferring the dry culture dish into a biochemical incubator with constant temperature of 27 ℃, weighing the samples every 1 hour, recording the quality change, and finally calculating the moisture retention rate by using a moisture retention rate formula.
Combination A:4.8g of ethyl acetate extract of Syringa oblonga fruits +4.8g of water
Combination B:1.2g of glycerol+1.2 g of 1, 3-butanediol+1.2 g of beta-glucan+1.2 g of ethyl acetate extract of Syringa fruits+4.8 g of water
Combination C:1.6g of glycerol+1.6 g of 1, 3-butanediol+1.6 g of beta-glucan+4.8 g of water
Wherein: m is M 0 Initial sample to be measured+mass of drying dish (g), M 1 The mass (g) of the sample to be measured and the drying dish after n hours.
(3) Test results
Table 2 three combination in vitro moisturizing efficacy assays
The results of the moisture test of the clove fruit emulsion are shown in Table 2, and the moisture retention capacity of the combination of 4.8g of ethyl acetate extract of clove fruit, 4.8g of water, 1.2g of glycerin, 1.2g of 1, 3-butanediol, 1.2g of beta-glucan, 1.2g of ethyl acetate extract of clove fruit, 4.8g of water, 1.6g of glycerin, 1.6g of 1, 3-butanediol, 1.6g of beta-glucan and 4.8g of water is measured at the constant temperature of 27 ℃, the measurement is carried out once every 1 hour, and the measurement is carried out continuously for 10 hours and recorded. It can be seen that the moisture retention rate of the combination C is slightly higher than that of the combination A and the combination B within 0-4h, and the moisture retention capacity of the combination C is rapidly reduced after 5h and is lower than that of the combination A and the combination B; the moisturizing performance of the combination A and the moisturizing performance of the combination B tend to be consistent after 9 hours, but the moisturizing capability of the combination B before the combination A is larger than that of the combination A, so that the result shows that the moisturizing combination added with the ethyl acetate extract of the clove fruits has a lasting moisturizing effect, and the moisturizing combination has better mixed use effect with moisturizing agents such as glycerin, 1, 3-butanediol, beta-glucan and the like and has a certain synergistic effect.
Moisture retention effect test:
(1) Material
Mice used for the test were supplied by the Haikou Yu Biotech company; emulsion to be measured: example 1 is a test group, with matrix emulsion without added clove fruit extract as positive control, without emulsion as blank control; environmental conditions: ambient temperature 20-27 ℃, relative humidity: 50% -70% of guinea pig cage: a nontoxic plastic cage; padding: sterilizing the log litter.
(2) Test design
9 male white guinea pigs (about 250 g) were prepared, hair on the back of the guinea pigs was cut off with an epilator, the hair was deeply dehaired before the formal test, the dehaired area was about 2x 6cm, and the dehaired parts were gently rubbed with aqueous cotton yarn, after 30min, 1g of clove fruit emulsion, 1g of emulsion matrix and blank control were applied in this order from left to right, the dehaired area water content of 9 guinea pigs was measured separately with a moisture meter, and thereafter the measurement was performed every 1h and the data were recorded.
(3) Test results
Table 3 determination of moisture retention properties of emulsions
The results of the moisture test of the clove fruit emulsion are shown in Table 3. The water content of the skin of the test group and the matrix group guinea pigs is obviously improved after the administration, the water content of the skin of the test group reaches the highest value in 1h of the administration, and the water content is 33.56+/-0.62%, which indicates that the clove fruit emulsion has better skin moisturizing effect; after 1h, the water content of the skin water of the guinea pigs in the test group and the matrix group is reduced, but the skin water content of the guinea pigs in the test group is slightly higher than that in the matrix group in comparison with the blank control group; the water content of the three groups of skin water is almost equal after 5 hours of administration, the water content is approximately restored to the original level, and the clove fruit formula emulsion has the effects of moisturizing and preserving moisture to a certain extent.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.

Claims (7)

1. An emulsion containing ethyl acetate extract of clove (Eugenia caryophyllata) fruits with moisturizing and oxidation resistance is characterized by being prepared from the following raw materials in parts by mass:
1-3 parts of Glucamate SSE-20, 0.5-1.5 parts of Glucate SS, 1-3 parts of stearic acid, 2-4 parts of ethylhexyl methoxycinnamate, 6-8 parts of octyl dodecanol, 0.2-0.4 part of Eumulgin SG, 0.04-0.06 part of disodium EDTA, 3-5 parts of glycerol, 0.05-0.15 part of xanthan gum, 0.3-0.5 part of hydroxyethyl acrylate, 0.05-0.15 part of citric acid, 0.05-0.15 part of methylparaben, 3-5 parts of ethyl acetate extract of clove fruits, 3-5 parts of 1, 3-butanediol, 3-5 parts of beta-glucan, 0.05-0.15 part of pentaerythritol tetra (bis-tert-butylhydroxyhydrocinnamate) and 60-70 parts of water;
the ethyl acetate extract of the clove fruits is prepared according to the following method:
grinding and crushing natural air-dried clove fruits by a high-speed grinder, repeatedly stirring and leaching by using high-concentration ethanol with the volume concentration of 85-95%, concentrating to obtain a solid extract of the clove fruits,
then dispersing the solid extract of the clove fruits into ultrapure water, adding petroleum ether for extraction, standing for layering, removing a petroleum ether layer, adding dichloromethane for extraction, standing for layering, removing a dichloromethane layer, and finally adding ethyl acetate for extraction to obtain an ethyl acetate layer;
and (3) evaporating, concentrating and volatilizing the ethyl acetate layer by rotary evaporation, and collecting the obtained ethyl acetate extract of the clove fruits.
2. An emulsion containing ethyl acetate extract of clove (Eugenia caryophyllata) fruits with moisturizing and oxidation resistance is characterized by being prepared from the following raw materials in parts by mass:
0.5 to 2.5 parts of Glucamate SSE-20, 0.3 to 1.2 parts of Glucate SS, 0.5 to 2.5 parts of stearic acid, 1.5 to 3.5 parts of ethylhexyl methoxycinnamate, 5.5 to 7.5 parts of octyl dodecanol, 0.15 to 0.35 part of Eumulgin SG, 0.03 to 0.05 part of EDTA disodium, 2 to 4 parts of glycerin, 0.02 to 0.12 part of xanthan gum, 0.2 to 0.4 part of hydroxyethyl acrylate, 0.03 to 0.12 part of citric acid, 0.03 to 0.12 part of methylparaben, 2 to 4 parts of clove fruit ethyl acetate extract, 2 to 4 parts of 1, 3-butanediol, 2 to 4 parts of beta-glucan, 0.03 to 0.13 part of pentaerythritol tetrakis (bis-tert-butylhydroxyhydrocinnamate), and 60 to 70 parts of water;
the ethyl acetate extract of the clove fruits is prepared according to the following method:
grinding and crushing natural air-dried clove fruits by a high-speed grinder, repeatedly stirring and leaching by using high-concentration ethanol with the volume concentration of 85-95%, concentrating to obtain a solid extract of the clove fruits,
then dispersing the solid extract of the clove fruits into ultrapure water, adding petroleum ether for extraction, standing for layering, removing a petroleum ether layer, adding dichloromethane for extraction, standing for layering, removing a dichloromethane layer, and finally adding ethyl acetate for extraction to obtain an ethyl acetate layer;
and (3) evaporating, concentrating and volatilizing the ethyl acetate layer by rotary evaporation, and collecting the obtained ethyl acetate extract of the clove fruits.
3. Emulsion according to claim 1 or 2, characterized in that it is prepared from the following raw materials in parts by mass:
2 parts of Glucamate SSE-20, 1 part of Glucate SS, 2 parts of stearic acid, 3 parts of ethylhexyl methoxycinnamate, 7 parts of octyldodecanol, 0.3 part of Eumulgin SG, 0.05 part of disodium EDTA, 4 parts of glycerin, 0.1 part of xanthan gum, 0.4 part of hydroxyethyl acrylate, 0.1 part of citric acid, 0.1 part of methylparaben, 4 parts of ethyl acetate extract of clove fruits, 4 parts of 1, 3-butanediol, 4 parts of beta-glucan, 0.1 part of pentaerythritol tetrakis (bis-tert-butylhydroxyhydrocinnamate) ester and 67.85 parts of water.
4. A method for preparing the emulsion according to any one of claims 1 to 3, comprising the steps of:
a) Mixing Glucamate SSE-20 with Glucate SS, stearic acid, ethylhexyl methoxycinnamate, octyl dodecanol and pentaerythritol tetra (di-tert-butyl hydroxy hydrocinnamate), and mechanically stirring until the solids are completely dissolved to obtain an oil phase;
b) Dissolving water, hydroxyethyl acrylate, eumulgin SG, 1, 3-butanediol, beta-glucan, glycerol, methyl benzoate and xanthan gum under stirring to obtain a water phase;
c) Mixing and emulsifying the oil phase and the water phase to obtain emulsion;
d) Adding ethyl acetate extract of Syringa oblonga fruits and EDTA disodium into the emulsion, mixing, and adjusting pH to obtain emulsion containing ethyl acetate extract of Syringa oblonga fruits.
5. The method according to claim 4, wherein the pH is adjusted to 4.0 to 5.0.
6. Use of the emulsion according to any one of claims 1 to 3 for preparing a cosmetic having moisturizing and antioxidative properties.
7. The use according to claim 6, characterized in that said cosmetic is selected from skin-cleaning products, lotions, creams, essences, barrier cosmetics, sun-protection cosmetics, foundations or concealers.
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