CN115487113A - 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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Publication number
CN115487113A
CN115487113A CN202211178490.5A CN202211178490A CN115487113A CN 115487113 A CN115487113 A CN 115487113A CN 202211178490 A CN202211178490 A CN 202211178490A CN 115487113 A CN115487113 A CN 115487113A
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parts
portions
clove
emulsion
extract
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CN202211178490.5A
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CN115487113B (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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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
    • A61K8/9783Angiosperms [Magnoliophyta]
    • 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
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/60Sugars; Derivatives thereof
    • A61K8/602Glycosides, e.g. rutin
    • 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
    • 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
    • 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

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 a better moisturizing effect, provides a relatively long-lasting moisturizing effect for skin, and also has certain whitening and antioxidant 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 articles, and particularly relates to an emulsion containing a clove fruit extract, and a preparation method and application thereof.
Background
The emulsion additive refers to a small amount or trace substance added in the production process and the use process of the emulsion, and the dosage in the emulsion is small but the effect is obvious. The emulsion additive is a raw material frequently used in modern emulsion industry, and has obvious effects on enhancing the efficacy value of basic emulsion and the like.
Eugenia caryophyllata Thunb of Myrtaceae is a spice native to Indonesia, has been introduced to tropical regions around the world, and is one of the traditionally imported "south drugs" in China. Clove as a traditional imported Chinese medicinal material has been widely developed in application value, and has been formulated as stomach medicine, muscle relaxing ointment, nose patch, sleep-aiding powder and the like so far; in the aspect of life application, the plant growth regulator is also involved in hunting, such as lasting essence, mosquito repellent, bacteriostatic hand sanitizer, traditional Chinese medicine distiller's yeast and the like. According to the chemical law of plant resources, different parts of the same plant may contain the same or similar components, and clove as a medicinal plant has the main medicinal value in flower buds, but the development of active ingredients of other parts such as fruits, leaves and rhizomes is also necessary. The clove is originally filed in Lei Gong Pao Zhi Lun, the fruits of the clove are firstly seen in Liang Dai ceramic Hongjing named medical records by taking 'chicken tongue fragrance' as a medicine, the later southern herbal records also record the fruits, the national traditional Chinese medicine administration records the clove fruits as one of 39 Chinese medicinal material varieties which are mainly developed in China, the pharmacological activity of the clove fruits covers many aspects, for example, the clove oil contained in the clove bud has strong antifungal and antifungal activities, and can be used as a natural antifungal agent for storing fruits in winter; the clove decoction has obvious inhibition effect on pathogenic bacteria such as tubercle bacillus, typhoid bacillus, dysentery bacillus and the like, and can treat related diseases caused by the pathogenic bacteria; the ethyl acetate extract contained in the clove fruit has strong acaricidal activity and the like.
Therefore, how to use the clove fruit extract in the emulsion to enable the emulsion to have better moisturizing effect, provide relatively long-lasting moisturizing effect for skin and simultaneously have certain whitening and antioxidant effects is a problem to be solved.
Disclosure of Invention
In view of this, the technical problem to be solved by the present invention is to provide an emulsion containing a clove fruit extract, and a preparation method and an 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 an ethyl acetate extract of clove fruit.
Preferably, the feed additive is prepared from the following raw materials in parts by mass:
1 to 3 portions of Glucamate SSE-20, 0.5 to 1.5 portions of Glucate SS, 0.2 to 0.4 portion of Eumulgin SG, 3 to 5 portions of clove fruit ethyl acetate extract and 81.5 to 106.16 portions of cosmetic matrix.
Preferably, the feed is prepared from the following raw materials in parts by mass:
1 to 3 portions of Glucamate SSE-20, 0.5 to 1.5 portions of Glucate SS, 1 to 3 portions of stearic acid, 2 to 4 portions of ethylhexyl methoxycinnamate, 6 to 8 portions of octyldodecanol, 0.2 to 0.4 portion of Eumulgin SG, 0.04 to 0.06 portion of EDTA disodium, 3 to 5 portions of glycerin, 0.05 to 0.15 portion of xanthan gum, 0.3 to 0.5 portion of hydroxyethyl acrylate, 0.05 to 0.15 portion of citric acid, 0.05 to 0.15 portion of methyl paraben, 3 to 5 portions of clove fruit ethyl acetate extract, 3 to 5 portions of 1,3-butanediol, 3 to 5 portions of beta-glucan, 0.05 to 0.15 portion of pentaerythritol tetra (di-tert-butyl hydroxy hydrocinnamate) and 60 to 70 portions of water.
Preferably, the feed is prepared from the following raw materials in parts by mass:
0.5 to 2.5 portions of Glucamate SSE-20, 0.3 to 1.2 portions of Glucate SS, 0.5 to 2.5 portions of stearic acid, 1.5 to 3.5 portions of ethylhexyl methoxycinnamate, 5.5 to 7.5 portions of octyldodecanol, 0.15 to 0.35 portion of Eumulgin SG, 0.03 to 0.05 portion of EDTA disodium, 2 to 4 portions of glycerol, 0.02 to 0.12 portion of xanthan gum, 0.2 to 0.4 portion of hydroxyethyl acrylate, 0.03 to 0.12 portion of citric acid, 0.03 to 0.12 portion of methylparaben, 2 to 4 portions of clove fruit ethyl acetate extract, 1,3-2 to 4 portions of butanediol, 2 to 4 portions of beta-glucan, 0.03 to 0.13 portion of pentaerythritol tetra (di-tert-butyl hydroxy hydrocinnamate) and 60 to 70 portions of water.
Preferably, the feed additive 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, methyl paraben 0.1 parts, clove fruit ethyl acetate extract 4 parts, 1,3-butanediol 4 parts, beta-glucan 4 parts, pentaerythritol tetrakis (di-tert-butyl hydroxy hydrocinnamate) 0.1 parts, and water 67.85 parts.
The invention also provides a preparation method of the emulsion, which comprises the following steps:
a) Mechanically stirring Glucamate SSE-20, glucoate SS, stearic acid, ethylhexyl methoxycinnamate, octyldodecanol and pentaerythritol tetrakis (di-tert-butyl hydroxyhydrocinnamate) ester uniformly until the solid is completely dissolved to obtain an oil phase;
b) Stirring and dissolving water, hydroxyethyl acrylate, eumulgin SG, 1,3-butanediol, beta-glucan, glycerol, methyl paraben and xanthan gum to obtain a water phase;
c) Mixing and emulsifying the oil phase and the water phase to obtain an emulsion;
d) Adding the clove fruit extract and EDTA disodium into the emulsion, mixing, and adjusting the pH value to obtain the emulsion containing the clove fruit extract.
Preferably, the pH is adjusted to 4.0 to 5.0.
The invention also provides an application of the emulsion in preparing cosmetics with moisturizing and oxidation resisting properties.
Preferably, the cosmetic product is selected from a skin cleansing product, lotion, cream, serum, barrier, sunscreen, foundation or concealer.
Compared with the prior art, 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 two emulsifiers used in the invention are Glucamate SSE-20, glucate SS and Eumulgin SG, wherein the oil-phase emulsifiers Glucamate SSE-20 and Glucate SS are unique nonionic emulsifiers and are one of glucoside derivatives in natural corn starch, the Glucate SS has water-in-oil emulsifying activity, and the glucarate SSE-20 is an oil-in-water emulsifier which is combined to generate high-quality emulsification; moreover, the viscosity generated by Glucate SSE-20 and Glucate SS is resistant to the damaging effects of mechanical work or shear stress applied after emulsion formation, and can generally recover within days if the viscosity drops during production operations due to pumping and filling. In addition, the aqueous phase emulsifier Eumulgin SG is a liquid crystal form amino acid emulsifier, has good compatibility with electrolyte, and is very suitable for various formulas rich in additives and skin care product formulas containing water-soluble sun-screening agents; the skin-care product has excellent emulsifying capacity, achieves the purpose of improving skin feel by adjusting the dosage of grease, wax and polymer, has excellent compatibility with various electrolytes, water-soluble UV-sun-screening agents, inorganic sun-screening agents and organic sun-screening agents, promotes the formation of lamellar liquid crystal phase, and has excellent moisturizing capacity; it is also an emulsifier which is very safe and therefore suitable for use in a variety of different 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 after an ethanol solvent extraction method, the clove fruit emulsion has a strong special fragrance, the main components of the ethyl acetate extract comprise compounds such as flavonoids, polyphenols and polysaccharides, and the like, and the substances have strong effects of moisturizing, sun-blocking, bacteriostasis, antioxidation and the like, can improve the skin care effect of the emulsion, and better improve the moisturizing and antioxidation performance 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 clove fruit ethyl acetate extract.
The ethyl acetate extract of the clove fruit is obtained by performing sectional extraction after an ethanol solvent extraction method, has a strong special fragrance, contains compounds such as flavonoids, polyphenols and polysaccharides as main components, has strong effects of moisture retention, sun protection, bacteriostasis, oxidation resistance and the like, can improve the skin care effect of the emulsion, and can well improve the moisture retention and oxidation resistance of the emulsion.
Specifically, the ethyl acetate extract of the clove fruit provided by the invention is prepared according to the following method:
extracting the ethyl acetate extract of the clove fruit by adopting a solvent extraction method:
grinding and pulverizing naturally air dried clove fruit with high speed pulverizer, repeatedly stirring and extracting with high concentration ethanol, concentrating to obtain solid extract of clove fruit,
then dispersing the solid extract of the clove fruit 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) carrying out rotary evaporation, concentration and evaporation on the ethyl acetate layer, and collecting the obtained ethyl acetate extract of the clove fruit.
Wherein the volume concentration of the high-concentration ethanol is 85-95%;
the mass volume ratio of the naturally air-dried clove fruits to the high-concentration ethanol is 6kg
The mass volume ratio of the clove fruit solid extract 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 clove fruit extract-containing emulsion is prepared from the following raw materials in parts by mass:
1-3 parts of Glucamate SSE-20, 0.5-1.5 parts of glucoate SS, 0.2-0.4 part of Eumulgin SG, 3-5 parts of clove fruit ethyl acetate extract and 81.5-106.16 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 embodiments of the present invention, the clove fruit extract-containing emulsion is prepared from the following raw materials in parts by mass:
1 to 3 portions of Glucamate SSE-20, 0.5 to 1.5 portions of Glucate SS, 1 to 3 portions of stearic acid, 2 to 4 portions of ethylhexyl methoxycinnamate, 6 to 8 portions of octyldodecanol, 0.2 to 0.4 portion of Eumulgin SG, 0.04 to 0.06 portion of EDTA disodium, 3 to 5 portions of glycerin, 0.05 to 0.15 portion of xanthan gum, 0.3 to 0.5 portion of hydroxyethyl acrylate, 0.05 to 0.15 portion of citric acid, 0.05 to 0.15 portion of methyl paraben, 3 to 5 portions of clove fruit ethyl acetate extract, 3 to 5 portions of 1,3-butanediol, 3 to 5 portions of beta-glucan, 0.05 to 0.15 portion of pentaerythritol tetra (di-tert-butyl hydroxy hydrocinnamate) and 60 to 70 portions of water.
In some preferred embodiments, the clove fruit extract-containing emulsion is prepared from the following raw materials in parts by mass:
0.5-2.5 parts of Glucamate SSE-20, 0.3-1.2 parts of Glucate SS, 0.5-2.5 parts of stearic acid, 1.5-3.5 parts of ethylhexyl methoxycinnamate, 5.5-7.5 parts of octyldodecanol, 0.15-0.35 part of Eumulgin SG, 0.03-0.05 part of EDTA disodium, 2-4 parts of glycerol, 0.02-0.12 part of xanthan gum, 0.2-0.4 part of hydroxyethyl acrylate, 0.03-0.12 part of citric acid, 0.03-0.12 part of methylparaben, 2-4 parts of clove fruit ethyl acetate extract, 2-4 parts of 1,3-butanediol, 2-4 parts of beta-glucan, 0.03-0.13 part of pentaerythritol tetra (di-tert-butyl hydroxy hydrocinnamate) and 60-70 parts of water.
In some more preferred embodiments of the present invention, the clove fruit extract containing emulsion 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, methyl paraben 0.1 parts, clove fruit ethyl acetate extract 4 parts, 1,3-butanediol 4 parts, beta-glucan 4 parts, pentaerythritol tetrakis (di-tert-butyl hydroxy hydrocinnamate) 0.1 parts, and 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) Mechanically stirring Glucamate SSE-20, glucoate SS, stearic acid, ethylhexyl methoxycinnamate, octyldodecanol and pentaerythritol tetrakis (di-tert-butyl hydroxyhydrocinnamate) ester uniformly until the solid is completely dissolved to obtain an oil phase;
b) Stirring and dissolving water, hydroxyethyl acrylate, eumulgin SG, 1,3-butanediol, beta-glucan, glycerol, methyl paraben and xanthan gum to obtain a water phase;
c) Mixing and emulsifying the oil phase and the water phase to obtain an emulsion;
d) Adding the clove fruit extract and EDTA disodium into the emulsion, and adjusting the pH value with citric acid to obtain the emulsion containing the clove fruit extract.
Specifically, a cleaned and dried oil phase pot is prepared and heated, an oil phase emulsifier, stearic acid, ethylhexyl methoxycinnamate, octyldodecanol, pentaerythritol tetrakis (di-tert-butylhydroxyhydrocinnamate) ester are added, and the mixture is mechanically stirred 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 the glycerol in advance, stirring to dissolve the glycerol, raising the water bath temperature to 80-90 ℃, and mechanically stirring uniformly until the glycerol is completely dissolved to obtain a water phase;
adding the oil phase component which is uniformly dispersed into the water phase, adjusting the temperature of the water bath to 80-90 ℃, and setting the homogenizing speed to 3000-3500 r.min -1 And continuously homogenizing for 5-8 min, stopping heating after the emulsification process is finished, and continuously stirring until the temperature is cooled to the room temperature.
Finally, adding the ethyl acetate extract of the clove fruit and the EDTA disodium, and continuously stirring for 5-8 min to adjust the pH value to obtain the final emulsion product. Adjustment of the pH 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 is simple in process and convenient to operate.
The invention also provides application of the emulsion containing the clove fruit extract in preparing cosmetics with moisturizing and oxidation resisting properties.
Wherein the cosmetic is selected from the group consisting of a skin cleansing product, lotion, cream, essence, barrier, sunscreen, foundation, and concealer.
According to the invention, the clove fruit extract is added and the emulsifier of a specific type is combined, so that the emulsion has a better moisturizing effect, provides a relatively long-lasting moisturizing effect for skin, and has certain whitening and antioxidant effects.
In order to further understand the present invention, the following examples are provided to illustrate the emulsion containing clove fruit extract and the preparation method and application thereof, and the scope of the present invention is not limited by the following examples.
In the following examples, ethyl acetate extract of clove fruit was prepared as follows:
extracting the ethyl acetate extract of the clove fruit by adopting a solvent extraction method:
taking 6kg of naturally air-dried clove fruit, grinding and crushing by a high-speed crusher, repeatedly stirring and leaching for 7 times for 72 hours by using 15L of ethanol with the volume concentration of 95%, combining leaching liquor, and concentrating to obtain the solid extract of the clove fruit.
Dispersing 2kg of clove fruit solid extract 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) carrying out rotary evaporation, concentration and evaporation on the ethyl acetate layer, and collecting 124g of the obtained ethyl acetate extract of the clove fruit.
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, methyl paraben 0.1 parts, clove fruit ethyl acetate extract 4 parts, 1,3-butanediol 4 parts, beta-glucan 4 parts, pentaerythritol tetrakis (di-tert-butyl hydroxy hydrocinnamate) 0.1 parts, and water 67.85 parts.
The preparation method of the emulsion containing the clove fruit extract comprises the following steps:
heating a cleaned and dried oil phase pot to 85 ℃, adding an oil phase emulsifier, stearic acid, ethylhexyl methoxycinnamate, octyldodecanol 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 glycerol is required to be added in advance for the xanthan gum to be dissolved by stirring, raising the temperature of a water bath to 85 ℃, and mechanically stirring uniformly until the xanthan gum is completely dissolved; adding the uniformly dispersed oil phase into the water phase, adjusting the water bath temperature to 85 deg.C, and setting the homogenization speed at 3000r min -1 And continuously homogenizing for 5min, stopping heating after the emulsification process is finished, continuously stirring until the mixture is cooled to room temperature, and finally adding the ethyl acetate extract of the clove fruit and the EDTA disodium, continuously stirring for 6min, and adjusting the pH value to obtain the final emulsion product.
Example 2
Glucamate SSE-20 parts, glucate SS 0.5 part, stearic acid 1 part, ethylhexyl methoxycinnamate 2 parts, octyldodecanol 6 parts, eumulgin SG 0.2 part, disodium EDTA 0.04 part, glycerin 3 parts, xanthan gum 0.05 part, hydroxyethyl acrylate 0.3 part, citric acid 0.05 part, methyl paraben 0.05 part, clove fruit ethyl acetate extract 3 parts, 1,3-butanediol 3 parts, beta-glucan 3 parts, pentaerythritol tetrakis (di-tert-butyl hydroxy hydrocinnamate) 0.05 part, and water 76.76 parts.
The preparation method of the emulsion containing the clove fruit extract comprises the following steps:
heating a cleaned and dried oil phase pot to 85 ℃, adding an oil phase emulsifier, stearic acid, ethylhexyl methoxycinnamate, octyldodecanol and pentaerythritol tetra (di-tert-butyl hydroxy hydrocinnamate) ester, 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 glycerol is required to be added in advance for the xanthan gum to be dissolved by stirring, raising the temperature of a water bath to 85 ℃, and mechanically stirring uniformly until the xanthan gum is completely dissolved; adding the uniformly dispersed oil phase into the water phase, adjusting the water bath temperature to 85 deg.C, and setting the homogenization speed at 3000r min -1 And continuously homogenizing for 5min, stopping heating after the emulsification process is finished, continuously stirring until the mixture is cooled to room temperature, and finally adding the ethyl acetate extract of the clove fruit and the EDTA disodium, continuously stirring for 6min, and adjusting the pH value to obtain the final emulsion product.
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, glycerol 4 parts, xanthan gum 0.1 parts, hydroxyethyl acrylate 0.4 parts, citric acid 0.1 parts, methyl paraben 0.1 parts, clove fruit ethyl acetate extract 4 parts, 1,3-butanediol 4 parts, beta-glucan 4 parts, pentaerythritol tetrakis (di-tert-butyl hydroxyhydrocinnamate) 0.1 parts, and water 67.85 parts.
The preparation method of the emulsion containing the clove fruit extract comprises the following steps:
heating a cleaned and dried oil phase pot to 85 ℃, adding an oil phase emulsifier, stearic acid, ethylhexyl methoxycinnamate, octyldodecanol 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 glycerol is required to be added in advance for the xanthan gum to be dissolved by stirring, raising the temperature of a water bath to 85 ℃, and mechanically stirring uniformly until the xanthan gum is completely dissolved; will disperse evenlyAdding the oil phase into the water phase, adjusting the temperature of the water bath to 85 deg.C, and setting the homogenization speed at 3000r min -1 And continuously homogenizing for 5min, stopping heating after the emulsification process is finished, continuously stirring until the mixture is cooled to room temperature, and finally adding the ethyl acetate extract of the clove fruit and the EDTA disodium, continuously stirring for 6min, and adjusting the pH value to obtain the final emulsion product.
The ethyl acetate extract of the clove fruit prepared by the invention is subjected to effective chemical component determination:
(1) Material
Gallic acid, forlin phenol, sodium carbonate, absolute ethyl alcohol, anthrone and glucose.
(2) Design of experiments
The test is carried out by referring to T/AHFIA005-2018, namely determination of total polyphenol content in plant extracts and products thereof and GB/T15672-2009, namely determination of total sugar content in edible fungi.
(3) Test results
The linear formula of the measurement results is as follows:
total polyphenols: y =0.0091X +0.0105 2 =0.9996;
Total polysaccharide: y =0.007X +0.0673 2 =0.9991;
TABLE 1 measurement results of effective chemical components
Figure BDA0003864445280000091
The results of measuring the content of the effective chemical components of the ethyl acetate extract of the clove fruit are shown in table 1. As shown in Table 1, the total polyphenol and total polysaccharide content of the extract is high, and the ratio is 69.62%. The substances have strong effects of moisturizing, sun-screening, bacteriostasis, antioxidation and the like, can improve the skin care effect of the emulsion, and better improve the moisturizing and antioxidation performance of the emulsion.
In-vitro moisturizing efficacy determination of different moisturizing combinations:
(1) Material
Glycerol; 1,3-butanediol; beta-glucan; water; ethyl acetate extract of clove fruit.
(2) Design of experiments
Accurately weighing the samples according to the following three combinations, placing the samples in a dry culture dish, transferring the samples into a constant-temperature biochemical incubator at 27 ℃, weighing every 1 hour, recording the mass change, and finally calculating the moisture retention rate by using a moisture retention rate formula.
Combination A:4.8g ethyl acetate extract of Syzygium aromaticum fruit +4.8g water
And (B): 1.2g of glycerol +1.2g of 1, 3-butanediol +1.2g of beta-glucan +1.2g of ethyl acetate extract of clove fruit +4.8g of water
And (3) combination C:1.6g of glycerol +1.6g of 1, 3-butanediol +1.6g of beta-glucan +4.8g of water
Figure BDA0003864445280000092
Wherein: m is a group of 0 The mass (g) of the initial sample to be measured and the drying dish, M 1 The mass (g) of the sample to be tested + the drying dish after n hours.
(3) Test results
Table 2 three combination in vitro moisturizing efficacy assays
Figure BDA0003864445280000093
Figure BDA0003864445280000101
A moisturizing test result of an emulsion of clove fruit is shown in Table 2, and the moisturizing abilities of three combinations 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 segment extract of clove fruit +4.8g of water, 1.6g of glycerin +1.6g of 1, 3-butanediol +1.6g of beta-glucan +4.8g of water are measured under the condition of keeping a constant temperature of 27 ℃, and are measured once every 1h and continuously measured for 10h and recorded. It can be seen that within 0-4h, the moisturizing rate of the combination C is slightly higher than that of the combination A and the combination B, and after 5h, the moisturizing capability of the combination C is rapidly reduced and is lower than that of the combination A and the combination B; the moisturizing performances of the combination A and the combination B tend to be consistent after 9 hours, but the moisturizing capability of the combination B is higher than that of the combination A before, so the result shows that the moisturizing combination added with the clove fruit ethyl acetate extract has a lasting moisturizing effect, and the moisturizing combination has a better effect when being mixed 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
The mice used in the test were provided by Yu's Biotech, haikou; emulsion to be tested: example 1 is a test group with a matrix emulsion without added clove fruit extract as a positive control and without emulsion as a blank control; environmental conditions are as follows: ambient temperature 20-27 ℃, relative humidity: 50% -70%, guinea pig cage: a non-toxic plastic cage; padding: sterilizing the log bedding.
(2) Design of experiments
Preparing 9 male white guinea pigs (about 250 g), cutting hair on the backs of the guinea pigs by using a depilator, deeply depilating before the formal test, the depilating area is about 2x 6cm, lightly wiping the depilated part by using a water-containing cotton yarn, applying 1g of clove fruit emulsion, 1g of emulsion matrix and a blank control from left to right in sequence after 30min, respectively measuring the water content of the depilated area of the 9 guinea pigs by using a moisture tester, and measuring and recording the data once every 1 h.
(3) Test results
TABLE 3 determination of the moisturizing Properties of the emulsions
Figure BDA0003864445280000111
The moisturizing test results of a clove fruit emulsion are shown in table 3. The water content of the skin of the guinea pigs in the test group and the matrix group is remarkably improved after the skin is applied, the water content of the skin in the test group reaches the highest value within 1 hour after the skin is applied, and the water content is 33.56 +/-0.62%, so that the clove fruit emulsion has a good skin moisturizing effect; after 1h, the water content of the skin of the guinea pigs in the test group and the matrix group is reduced, but a certain water replenishing and moisturizing effect is still achieved compared with that of a blank control group, and the water content of the skin of the guinea pigs in the test group is slightly higher than that of the matrix group; after the lotion is applied for 5 hours, the water content of the skin water of the three groups is almost kept equal, and the water content is approximately recovered to the original level, so that the clove fruit formula lotion has certain water replenishing and moisturizing effects.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.

Claims (10)

1. An emulsion containing clove fruit extract, comprising clove fruit extract, glucamate SSE-20, glucate SS, eumulgin SG and a cosmetic base.
2. The emulsion of claim 1, wherein the clove fruit extract is clove fruit ethyl acetate extract.
3. The emulsion according to claim 1, which is prepared from the following raw materials in parts by mass:
1-3 parts of Glucamate SSE-20, 0.5-1.5 parts of glucoate SS, 0.2-0.4 part of Eumulgin SG, 3-5 parts of clove fruit ethyl acetate extract and 81.5-106.16 parts of cosmetic matrix.
4. The emulsion according to claim 1, which is prepared from the following raw materials in parts by mass:
1 to 3 portions of Glucamate SSE-20, 0.5 to 1.5 portions of Glucate SS, 1 to 3 portions of stearic acid, 2 to 4 portions of ethylhexyl methoxycinnamate, 6 to 8 portions of octyldodecanol, 0.2 to 0.4 portion of Eumulgin SG, 0.04 to 0.06 portion of EDTA disodium, 3 to 5 portions of glycerin, 0.05 to 0.15 portion of xanthan gum, 0.3 to 0.5 portion of hydroxyethyl acrylate, 0.05 to 0.15 portion of citric acid, 0.05 to 0.15 portion of methyl paraben, 3 to 5 portions of clove fruit ethyl acetate extract, 3 to 5 portions of 1,3-butanediol, 3 to 5 portions of beta-glucan, 0.05 to 0.15 portion of pentaerythritol tetra (di-tert-butyl hydroxy hydrocinnamate) and 60 to 70 portions of water.
5. The emulsion according to claim 1, which is prepared from the following raw materials in parts by mass:
0.5 to 2.5 portions of Glucamate SSE-20, 0.3 to 1.2 portions of Glucate SS, 0.5 to 2.5 portions of stearic acid, 1.5 to 3.5 portions of ethylhexyl methoxycinnamate, 5.5 to 7.5 portions of octyldodecanol, 0.15 to 0.35 portion of Eumulgin SG, 0.03 to 0.05 portion of EDTA disodium, 2 to 4 portions of glycerol, 0.02 to 0.12 portion of xanthan gum, 0.2 to 0.4 portion of hydroxyethyl acrylate, 0.03 to 0.12 portion of citric acid, 0.03 to 0.12 portion of methylparaben, 2 to 4 portions of clove fruit ethyl acetate extract, 1,3-2 to 4 portions of butanediol, 2 to 4 portions of beta-glucan, 0.03 to 0.13 portion of pentaerythritol tetra (di-tert-butyl hydroxy hydrocinnamate) and 60 to 70 portions of water.
6. The emulsion according to claim 1, which 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, methyl paraben 0.1 parts, clove fruit ethyl acetate extract 4 parts, 1,3-butanediol 4 parts, beta-glucan 4 parts, pentaerythritol tetrakis (di-tert-butyl hydroxy hydrocinnamate) 0.1 parts, and water 67.85 parts.
7. A process for the preparation of an emulsion according to any one of claims 1 to 6, characterized in that it comprises the following steps:
a) Mechanically stirring Glucamate SSE-20, glucoate SS, stearic acid, ethylhexyl methoxycinnamate, octyldodecanol and pentaerythritol tetrakis (di-tert-butyl hydroxyhydrocinnamate) ester uniformly until the solid is completely dissolved to obtain an oil phase;
b) Stirring and dissolving water, hydroxyethyl acrylate, eumulgin SG, 1,3-butanediol, beta-glucan, glycerol, methyl paraben and xanthan gum to obtain a water phase;
c) Mixing and emulsifying the oil phase and the water phase to obtain an emulsion;
d) Adding the clove fruit extract and EDTA disodium into the emulsion, mixing, and adjusting the pH value to obtain the emulsion containing the clove fruit extract.
8. The method according to claim 7, wherein the pH is adjusted to 4.0 to 5.0.
9. Use of an emulsion according to any one of claims 1 to 6 for the preparation of a cosmetic product having moisturising and antioxidant properties.
10. Use according to claim 9, characterized in that the cosmetic product is chosen from a skin cleansing product, a lotion, a cream, a serum, a barrier, a sun protection, a foundation or a concealer.
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