CN111557880B - Whitening and firming plant essence care solution and preparation method thereof - Google Patents

Whitening and firming plant essence care solution and preparation method thereof Download PDF

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CN111557880B
CN111557880B CN202010607051.6A CN202010607051A CN111557880B CN 111557880 B CN111557880 B CN 111557880B CN 202010607051 A CN202010607051 A CN 202010607051A CN 111557880 B CN111557880 B CN 111557880B
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chinese violet
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powder
distilled water
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CN111557880A (en
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不公告发明人
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Guangdong Haitong Pharmaceutical Co.,Ltd.
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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
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/34Alcohols
    • A61K8/345Alcohols containing more than one hydroxy group
    • 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
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    • A61K8/58Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing atoms other than carbon, hydrogen, halogen, oxygen, nitrogen, sulfur or phosphorus
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    • 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
    • A61K8/60Sugars; 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
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    • 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
    • A61K8/9741Pteridophyta [ferns]
    • 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
    • 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
    • A61K2800/74Biological properties of particular ingredients
    • A61K2800/78Enzyme modulators, e.g. Enzyme agonists
    • A61K2800/782Enzyme inhibitors; Enzyme antagonists
    • 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
    • A61K2800/80Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
    • A61K2800/85Products or compounds obtained by fermentation, e.g. yoghurt, beer, wine

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Abstract

The invention discloses a whitening and firming plant essence care solution which comprises 0.01-20 wt% of a Chinese violet extract, or comprises 0.03-3 wt% of the Chinese violet extract, or comprises 0.05-1 wt% of the Chinese violet extract, or comprises 0.1-0.8 wt% of the Chinese violet extract, or comprises 0.2-0.6 wt% of the Chinese violet extract.

Description

Whitening and firming plant essence care solution and preparation method thereof
Technical Field
The invention relates to the field of cosmetics, and particularly relates to a whitening and firming plant essence care solution and a preparation method thereof.
Background
Herba Violae (Viola YEDOENSIS Makino) is whole herb of Viola YEDOENSIS Makino of Violaceae. Viola yedoensis Makino is a perennial herb and grows in fields, wastelands, hillside grasses, forest edges or bushes.
Viola YEDOENSIS Makino (Viola YEDOENSIS Makino) is bitter, pungent and cold in taste. It enters heart and liver meridians. Has the functions of clearing away heat and toxic material, cooling blood and detumescence, clearing away heat and promoting diuresis, is mainly used for treating furuncle, carbuncle swelling, scrofula, jaundice, dysentery, diarrhea, conjunctival congestion, pharyngitis and venomous snake bite, not only plays an important role in the aspect of traditional Chinese medicine, but also can be used in the aspects of animal husbandry, food and the like.
In daily chemical products, herba Violae (Viola YEDOENSIS Makino) extract is often added as plant antibacterial agent. In the prior art, the use of a VIOLA YEDOENSIS MAKINO extract as a whitening agent in cosmetics has not been reported.
Disclosure of Invention
In view of the defects of the prior art, the technical problems to be solved by the invention are as follows: the whitening and firming plant essence care solution is provided; and (II) providing a preparation method of the whitening and firming plant essence care solution.
The invention adopts the specific technical scheme that:
with the development of modernization of traditional Chinese medicines, a large number of active substances with whitening effect in traditional Chinese medicinal materials are found, such as phenols, flavonoids, flavonoid compounds, polysaccharides, volatile oil, organic acids, triterpenoid saponins and the like, and can inhibit melanin generation and promote melanin discharge from various ways. The main component of herba Violae is flavonoid, including apigenin, luteolin and glycoside compounds, and phenolic substances such as chicory glycoside and esculetin. Accordingly, the extract of Viola yedoensis Makino has a high possibility of being applied as a tyrosinase inhibitor and a melanin synthesis inhibitor in cosmetics as a whitening agent.
Preferably, the invention provides a method for extracting the extract of Chinese violet, which comprises the following steps:
the method comprises the following steps: adding the Chinese violet powder into distilled water, and uniformly mixing, wherein the mass ratio of the Chinese violet powder to the distilled water is (5-15) to (5-10); heating to 32-52 ℃, inoculating zymocyte, wherein the mass ratio of the zymocyte to the Chinese violet powder is (0.5-2.0): 100; fermenting at 32-52 deg.C for 12-72 hr to obtain pretreated herba Violae powder;
step two: adding pretreated Chinese violet powder into distilled water, wherein the mass ratio of the pretreated Chinese violet powder to the distilled water is (10-25): (100-120), heating to 95-125 ℃, boiling for 0.5-2.5h, and filtering to obtain filtrate A1 and filter residue B1; adding filter residue B1 into distilled water, wherein the mass ratio of the filter residue B1 to the distilled water is (5-15): (85-105), heating to 95-125 ℃, boiling for 0.5-1.5h, and filtering to obtain filtrate A2 and filter residue B2; mixing the filtrate A1 and filtrate A2, concentrating under reduced pressure, vacuum drying, and grinding to obtain herba Violae extract.
Preferably, the fermentation bacteria are at least one of lactobacillus bulgaricus, saccharomyces cerevisiae, bacillus subtilis, lactobacillus plantarum and aspergillus niger; further preferably, the zymocyte is a mixture of bacillus subtilis and aspergillus niger according to the mass ratio of 1 (1-5).
The inventor finds that if the Chinese violet powder is directly extracted, the Chinese violet extract has poor quality, less dissolved organic micromolecular active ingredients and poor whitening effect because the cell wall and cell membrane structures of the Chinese violet are difficult to penetrate; according to the invention, on the basis of directly extracting the Chinese violet powder in the prior art, a specific process of pretreating the Chinese violet powder by using zymophyte is added, and the cell wall and cell membrane structure of the Chinese violet is destroyed by using the zymophyte, so that organic micromolecule active ingredients in the Chinese violet cell are more easily dissolved out, the subsequent extraction process is facilitated, the quality of the Chinese violet extract is improved, and the whitening effect is improved.
Furthermore, the method adopts the bacillus subtilis and the aspergillus niger for mixed synergistic fermentation, so that the pretreatment is more thorough through the coordination interaction relationship among the strains, and the extraction of active ingredients in the Chinese violet is more facilitated; aspergillus niger can secrete a large amount of high-activity cellulase, pectinase, phytase, amylase and the like, effectively degrade pectin and fiber network structures in cell walls of the Chinese violet, and greatly destroy the cell wall structures of the Chinese violet; the bacillus subtilis can secrete a large amount of high-activity alkaline protease, lipase, glucoamylase and the like, further acts on cell membranes of the Chinese violet, destroys phospholipid bilayer structures of the cell membranes, and is coordinated and interacted with each other to synergize effects, so that the pretreated Chinese violet powder is easier to extract, the active ingredients in the obtained Chinese violet extract are higher in content, and the whitening effect is better.
Preferably, the invention provides a method for extracting the extract of Chinese violet, which comprises the following steps:
the method comprises the following steps: adding the Chinese violet powder into distilled water, and uniformly mixing, wherein the mass ratio of the Chinese violet powder to the distilled water is (5-15) to (5-10); heating to 32-52 ℃, inoculating zymocyte, wherein the mass ratio of the zymocyte to the Chinese violet powder is (0.5-2.0): 100; fermenting at 32-52 deg.C for 12-72 hr to obtain pretreated herba Violae powder;
step two: adding pretreated Chinese violet powder into distilled water, wherein the mass ratio of the pretreated Chinese violet powder to the distilled water is (10-25): (100-120), heating to 95-125 ℃, boiling for 0.5-2.5h, and filtering to obtain filtrate A1 and filter residue B1; adding filter residue B1 into distilled water, wherein the mass ratio of the filter residue B1 to the distilled water is (5-15): (85-105), heating to 95-125 ℃, boiling for 0.5-1.5h, and filtering to obtain filtrate A2 and filter residue B2; mixing the filtrate A1 with the filtrate A2, concentrating under reduced pressure, vacuum drying, and grinding to obtain powder X;
step three: placing the filter residue B2 into an extraction tank for supercritical extraction for 30-90min, wherein the extraction pressure is 35-50Mpa, and the extraction temperature is 45-70 deg.C; the main solvent is CO2Fluid, CO2The flow rate of the fluid is 10-18kg/h, and an entrainer is added, wherein the flow rate of the entrainer is 0.1-0.8g/min, so that an extract is obtained; centrifuging the extract, vacuum drying, and grindingObtaining powder Y; mixing powder X and powder Y to obtain herba Violae extract.
Preferably, the amount of the entrainer is 1.5-5.5 wt% of the filter residue B2.
Preferably, the entrainer is at least one of ethanol aqueous solution, methanol aqueous solution, acetone aqueous solution and ethyl acetate; further preferably, the entrainer is 50-95 wt% ethanol water and 50-95 wt% acetone water in a mass ratio (1-5): 1.
The invention is in CO2The entrainer is added in the supercritical extraction process, and the entrainer can enable active ingredients in the Chinese violet to be dissolved out more easily through generating Van der Waals force, hydrogen bond, weak complexation and other intermolecular forces between the entrainer and organic micromolecule active ingredients in the Chinese violet, so that the biological activity content of the Chinese violet extract is improved, and the whitening effect is better.
Preferably, the preparation method of the philippine violet herb powder comprises the following steps: cleaning newly picked herba Violae with root for 1-5 times, and drying to control water content at 1-5 wt%; and crushing the dried Chinese violet, and sieving the crushed Chinese violet with a 100-mesh and 300-mesh sieve to obtain the Chinese violet powder for later use.
The invention provides a whitening and firming plant essence care solution which comprises 0.01-20 wt% of a Chinese violet extract. The herba Violae extract contains flavonoids as main ingredients, and contains apigenin, luteolin, glycoside compounds, chicory glycoside, esculetin, etc. which can inhibit melanin generation and promote melanin discharge, thereby effectively whitening skin.
Preferably, the whitening and firming plant essence care solution comprises 0.03-3 wt% of the extract of the Chinese violet, or comprises 0.05-1 wt% of the extract of the Chinese violet, or comprises 0.1-0.8 wt% of the extract of the Chinese violet, or comprises 0.2-0.6 wt% of the extract of the Chinese violet.
Preferably, the whitening and firming plant essence care solution further comprises 0.02-2 wt% of an extract containing raw grass (ANASTATICA HIEROCHUNTICA), or comprises 0.1-1 wt% of an extract containing raw grass (ANASTATICA HIEROCHUNTICA), or comprises 0.12-0.52 wt% of an extract containing raw grass (ANASTATICA HIEROCHUNTICA).
The raw grass (ANASTATICA HIEROCHUNTICA) extract contained in the cosmetic mainly has the functions of a skin conditioner and an astringent, is used for moisturizing, moistening and astringing skin, and is safe; the extract containing the raw grass (ANASTATICA HIEROCHUNTICA) is rich in ketones, mainly comprises cycadin biflavone, amentoflavone, apigenin and the like, and has not been reported to be used as a whitening agent in cosmetics.
Preferably, the whitening and firming plant essence care solution comprises the following raw materials: 0.2-0.6 wt% of herba Violae (Viola YEDOENSIS Makino) extract, 0.1-0.5 wt% of cyclohexasiloxane, 1.0-5.0 wt% of glycerol, 3.0-6.0 wt% of 1, 3-butanediol, 0.05-0.5 wt% of palmityl alcohol, 0.1-0.5 wt% of trehalose, 0.01-0.5 wt% of alpha-arbutin, 0.01-0.10 wt% of butyl hydroxybenzoate, 0.01-0.10 wt% of sodium benzoate, and the balance of water.
Preferably, the whitening and firming plant essence care solution comprises the following raw materials: 0.2-0.6 wt% of herba Violae (Viola YEDOENSIS Makino) extract, 0.12-0.52 wt% of raw grass (ANASTATICA HIEROCHUNTICA) -containing extract, 0.1-0.5 wt% of cyclohexasiloxane, 1.0-5.0 wt% of glycerol, 3.0-6.0 wt% of 1, 3-butanediol, 0.05-0.5 wt% of palmityl alcohol, 0.1-0.5 wt% of trehalose, 0.01-0.5 wt% of alpha-arbutin, 0.01-0.10 wt% of oxybenzone butyl ester, 0.01-0.10 wt% of sodium benzoate and the balance of water.
Through a large number of experiments, the inventor discovers that the whitening agent prepared by compounding the Chinese violet extract and the raw grass-containing extract has synergistic effect and further improves the whitening effect; according to the invention, the Chinese violet extract with a specific content and the raw grass-containing extract are added, so that the Chinese violet extract and the raw grass-containing extract interact with each other in a coordinated manner to jointly nourish the skin; the Chinese violet extract and the green grass-containing extract are mutually complemented to further strengthen the inhibition on the catalytic activity of tyrosinase, and simultaneously, more whitening active ingredients act on tyrosinase and are combined with a catalytic center thereof through hydrogen bonds and hydrophobic acting force to occupy the central position required by the catalysis of L-tyrosine and other substrates by the tyrosinase in advance, so that the formation of melanin is effectively inhibited, and the skin whitening effect is better.
The preparation method of the whitening and firming plant essence care solution comprises the following steps: adding the cyclohexasiloxane, the glycerol and the 1, 3-butanediol into water according to a raw material formula, stirring for 10-20min, setting the temperature to be 75-85 ℃, and setting the rotating speed to be 300-600 rpm; sequentially adding the Chinese violet extract, the palmityl alcohol, the trehalose, the alpha-arbutin, the butyl hydroxybenzoate and the sodium benzoate, continuously stirring for 20-30min, setting the temperature to be 75-85 ℃, and setting the rotation speed to be 300-600 rpm; homogenizing and emulsifying for 5-10min, inspecting, and discharging to obtain the whitening and firming plant essence care solution.
The invention has the beneficial effects that: the prepared herba violae extract has a good whitening effect; on one hand, the active ingredients in the Chinese violet extract are used as reducing agents to antagonize the activation of oxygen on tyrosinase, so that the tyrosinase cannot be normally converted into a catalytic state from a deoxidation mode, and the tyrosinase is prevented from catalyzing to generate melanin; on the other hand, active ingredients in the Chinese violet extract can enter a hydrophobic pocket of a tyrosinase catalytic center and are combined with surrounding amino acid residues through hydrogen bonds and hydrophobic acting force, so that the positions of acting substrates of tyrosinase such as L-tyrosine and the like in the tyrosinase catalytic center are occupied, the formation of melanin is further inhibited, and the effect of whitening skin is achieved.
According to the invention, the herba violae powder is pretreated by zymophyte, so that the cell wall and cell membrane structure of the herba violae are destroyed, organic micromolecule active ingredients in the herba violae cells are easy to dissolve out, the subsequent extraction process is facilitated, and the quality of the herba violae extract is improved; furthermore, the method adopts the bacillus subtilis and the aspergillus niger for mixed synergistic fermentation, so that the pretreatment is more thorough through the coordination interaction relationship among the strains, and the extraction of active ingredients in the Chinese violet is more facilitated; aspergillus niger can secrete a large amount of high-activity cellulase, pectinase, phytase, amylase and the like, effectively degrade pectin and fiber network structures in cell walls of the Chinese violet, and greatly destroy the cell wall structures of the Chinese violet; the bacillus subtilis can secrete a large amount of high-activity alkaline protease, lipase, glucoamylase and the like, and further doesThe extract is used for cell membranes of the Chinese violet, destroys phospholipid bilayer structures of the cell membranes, and has synergistic interaction and synergistic effect, so that the pretreated Chinese violet powder is easier to extract, the obtained Chinese violet extract has higher active ingredient content, and the whitening effect is better. In addition, the present invention employs CO2The supercritical extraction is combined with water extraction, and a proper entrainer is added in the supercritical extraction process, so that the entrainer can generate Van der Waals force, hydrogen bonds, weak complexation and other intermolecular forces with organic micromolecule active ingredients in the Chinese violet, so that the active ingredients in the Chinese violet are dissolved out more easily, the biological activity content of the Chinese violet extract is improved, and the whitening effect is better.
Through a large number of experiments, the inventor discovers that the whitening agent prepared by compounding the Chinese violet extract and the raw grass-containing extract has synergistic effect and further improves the whitening effect; according to the invention, the Chinese violet extract with a specific content and the raw grass-containing extract are added, so that the Chinese violet extract and the raw grass-containing extract interact with each other in a coordinated manner to jointly nourish the skin; the Chinese violet extract and the green grass-containing extract are mutually complemented to further strengthen the inhibition on the catalytic activity of tyrosinase, and simultaneously, more whitening active ingredients act on tyrosinase and are combined with a catalytic center thereof through hydrogen bonds and hydrophobic acting force to occupy the central position required by the catalysis of L-tyrosine and other substrates by the tyrosinase in advance, so that the formation of melanin is effectively inhibited, and the skin whitening effect is better.
Detailed Description
The specific parameters of some materials in the examples and comparative examples of the present invention are as follows:
α -arbutin, CAS: 84380-01-8, the purity is more than or equal to 98%, and the product is purchased from Shanghai Hotan Biotechnology GmbH.
A method for preparing herba Violae (Viola YEDOENSIS Makino) powder comprises the following steps: cleaning newly picked herba Violae with root for 3 times with water, and drying to control water content at 3 wt%; and then crushing the dried Chinese violet, and sieving the crushed Chinese violet with a 200-mesh sieve to obtain the Chinese violet powder.
Comprises an extract of green grass (ANASTATICA HIEROCHUNTICA) prepared by the following method: taking dried grass containing water with the water content of 2.5 wt%, crushing and sieving with a 200-mesh sieve; adding the raw grass-containing powder into distilled water, wherein the mass ratio of the raw grass-containing powder to the distilled water is 20: 80, heating at 85 ℃ for 55 min; filtering, concentrating the filtrate under reduced pressure, vacuum drying, and grinding to obtain extract W1; adding the filter residue into 85 wt% ethanol water solution, wherein the mass ratio of the filter residue to the 85 wt% ethanol water solution is 10:70, extracting under reflux at 85 ℃ for 50min for 2 times, combining the 2 filtrates, concentrating the filtrate under reduced pressure, vacuum drying, grinding to obtain extract W2, and mixing the extract W2 and the extract W1 to obtain the crude grass-containing extract.
Unless otherwise specified, each of the raw materials used in the examples of the present invention and comparative examples was a commercially available unified raw material.
Comparative example 1
A whitening and firming plant essence care solution is composed of the following raw materials: 0.3 wt% of cyclohexasiloxane, 4.5 wt% of glycerol, 5.5 wt% of 1, 3-butanediol, 0.2 wt% of palmitol, 0.3 wt% of trehalose, 0.1 wt% of alpha-arbutin, 0.05 wt% of butyl hydroxybenzoate, 0.05 wt% of sodium benzoate and the balance of water.
The preparation method of the whitening and firming plant essence care solution comprises the following steps:
adding cyclohexasiloxane, glycerol and 1, 3-butanediol into water according to a raw material formula, stirring for 15min, setting the temperature to be 83 ℃ and the rotating speed to be 500 rpm; sequentially adding the palmityl alcohol, the trehalose, the alpha-arbutin, the butyl hydroxybenzoate and the sodium benzoate, continuously stirring for 25min, setting the temperature to be 83 ℃ and the rotation speed to be 500 rpm; homogenizing and emulsifying for 6min, inspecting, and discharging to obtain the whitening and firming plant essence care solution.
Example 1
A whitening and firming plant essence care solution is composed of the following raw materials: 0.5 wt% of an extract of Viola YEDOENSIS Makino, 0.3 wt% of cyclohexasiloxane, 4.5 wt% of glycerol, 5.5 wt% of 1, 3-butanediol, 0.2 wt% of palmityl alcohol, 0.3 wt% of trehalose, 0.1 wt% of alpha-arbutin, 0.05 wt% of hydroxybutyl benzoate, 0.05 wt% of sodium benzoate, and the balance of water.
The preparation method of the Chinese violet extract comprises the following steps:
adding the Chinese violet powder into distilled water, wherein the mass ratio of the Chinese violet powder to the distilled water is 13: 117, heating to 100 ℃, boiling for 1.5h, and filtering to obtain filtrate A1 and filter residue B1; adding filter residue B1 into distilled water, wherein the mass ratio of the filter residue B1 to the distilled water is 13: 91, heating to 100 ℃, boiling for 0.8h, and filtering to obtain filtrate A2 and filter residue B2; mixing the filtrate A1 and filtrate A2, concentrating under reduced pressure, vacuum drying, and grinding to obtain herba Violae extract.
The preparation method of the whitening and firming plant essence care solution comprises the following steps:
adding cyclohexasiloxane, glycerol and 1, 3-butanediol into water according to a raw material formula, stirring for 15min, setting the temperature to be 83 ℃ and the rotating speed to be 500 rpm; sequentially adding herba Violae extract, palmityl alcohol, trehalose, alpha-arbutin, butyl hydroxybenzoate and sodium benzoate, stirring for 25min at 83 deg.C and 500 rpm; homogenizing and emulsifying for 6min, inspecting, and discharging to obtain the whitening and firming plant essence care solution.
Example 2
A whitening and firming plant essence care solution is composed of the following raw materials: 0.5 wt% of an extract of Viola YEDOENSIS Makino, 0.3 wt% of cyclohexasiloxane, 4.5 wt% of glycerol, 5.5 wt% of 1, 3-butanediol, 0.2 wt% of palmityl alcohol, 0.3 wt% of trehalose, 0.1 wt% of alpha-arbutin, 0.05 wt% of hydroxybutyl benzoate, 0.05 wt% of sodium benzoate, and the balance of water.
The preparation method of the Chinese violet extract comprises the following steps:
the method comprises the following steps: adding the Chinese violet powder into distilled water, and uniformly mixing, wherein the mass ratio of the Chinese violet powder to the distilled water is 13: 7; heating to 39 ℃ and inoculating zymocyte, wherein the mass ratio of the zymocyte to the Chinese violet powder is 1.8: 100; fermenting at 39 deg.C for 60h to obtain pretreated herba Violae powder;
the fermentation bacteria are bacillus subtilis and aspergillus niger mixed according to the mass ratio of 1: 1;
step two: adding pretreated Chinese violet powder into distilled water, wherein the mass ratio of the pretreated Chinese violet powder to the distilled water is 20: 110 (the mass ratio of the Chinese violet powder to the distilled water is 13: 117), heating to 100 ℃, boiling for 1.5h, and filtering to obtain filtrate A1 and filter residue B1; adding filter residue B1 into distilled water, wherein the mass ratio of the filter residue B1 to the distilled water is 13: 91, heating to 100 ℃, boiling for 0.8h, and filtering to obtain filtrate A2 and filter residue B2; mixing the filtrate A1 and filtrate A2, concentrating under reduced pressure, vacuum drying, and grinding to obtain herba Violae extract;
wherein the effective viable count of the bacillus subtilis is more than or equal to 100 hundred million CFU/g, and the bacillus subtilis is food grade and purchased from Hubeixin Rundy chemical company, Inc.; the effective viable count of Aspergillus niger is more than or equal to 50 hundred million CFU/g, and the Aspergillus niger is food grade and purchased from Wuhan and is a far-developing science and technology company Limited.
The preparation method of the whitening and firming plant essence care solution comprises the following steps:
adding cyclohexasiloxane, glycerol and 1, 3-butanediol into water according to a raw material formula, stirring for 15min, setting the temperature to be 83 ℃ and the rotating speed to be 500 rpm; sequentially adding herba Violae extract, palmityl alcohol, trehalose, alpha-arbutin, butyl hydroxybenzoate and sodium benzoate, stirring for 25min at 83 deg.C and 500 rpm; homogenizing and emulsifying for 6min, inspecting, and discharging to obtain the whitening and firming plant essence care solution.
Comparative example 2
A whitening and firming plant essence care solution is composed of the following raw materials: 0.5 wt% of an extract of Viola YEDOENSIS Makino, 0.3 wt% of cyclohexasiloxane, 4.5 wt% of glycerol, 5.5 wt% of 1, 3-butanediol, 0.2 wt% of palmityl alcohol, 0.3 wt% of trehalose, 0.1 wt% of alpha-arbutin, 0.05 wt% of hydroxybutyl benzoate, 0.05 wt% of sodium benzoate, and the balance of water.
The preparation method of the Chinese violet extract comprises the following steps:
the method comprises the following steps: adding the Chinese violet powder into distilled water, and uniformly mixing, wherein the mass ratio of the Chinese violet powder to the distilled water is 13: 7; heating to 39 ℃ and inoculating zymocyte, wherein the mass ratio of the zymocyte to the Chinese violet powder is 1.8: 100; fermenting at 39 deg.C for 60h to obtain pretreated herba Violae powder;
the zymocyte is bacillus subtilis;
step two: adding pretreated Chinese violet powder into distilled water, wherein the mass ratio of the pretreated Chinese violet powder to the distilled water is 20: 110 (the mass ratio of the Chinese violet powder to the distilled water is 13: 117), heating to 100 ℃, boiling for 1.5h, and filtering to obtain filtrate A1 and filter residue B1; adding filter residue B1 into distilled water, wherein the mass ratio of the filter residue B1 to the distilled water is 13: 91, heating to 100 ℃, boiling for 0.8h, and filtering to obtain filtrate A2 and filter residue B2; mixing the filtrate A1 and filtrate A2, concentrating under reduced pressure, vacuum drying, and grinding to obtain herba Violae extract;
wherein the effective viable count of the bacillus subtilis is more than or equal to 100 hundred million CFU/g, and the bacillus subtilis is food grade and is purchased from Hubei Xin run German chemical industry Co.
The preparation method of the whitening and firming plant essence care solution comprises the following steps:
adding cyclohexasiloxane, glycerol and 1, 3-butanediol into water according to a raw material formula, stirring for 15min, setting the temperature to be 83 ℃ and the rotating speed to be 500 rpm; sequentially adding herba Violae extract, palmityl alcohol, trehalose, alpha-arbutin, butyl hydroxybenzoate and sodium benzoate, stirring for 25min at 83 deg.C and 500 rpm; homogenizing and emulsifying for 6min, inspecting, and discharging to obtain the whitening and firming plant essence care solution.
Comparative example 3
A whitening and firming plant essence care solution is composed of the following raw materials: 0.5 wt% of an extract of Viola YEDOENSIS Makino, 0.3 wt% of cyclohexasiloxane, 4.5 wt% of glycerol, 5.5 wt% of 1, 3-butanediol, 0.2 wt% of palmityl alcohol, 0.3 wt% of trehalose, 0.1 wt% of alpha-arbutin, 0.05 wt% of hydroxybutyl benzoate, 0.05 wt% of sodium benzoate, and the balance of water.
The preparation method of the Chinese violet extract comprises the following steps:
the method comprises the following steps: adding the Chinese violet powder into distilled water, and uniformly mixing, wherein the mass ratio of the Chinese violet powder to the distilled water is 13: 7; heating to 39 ℃ and inoculating zymocyte, wherein the mass ratio of the zymocyte to the Chinese violet powder is 1.8: 100; fermenting at 39 deg.C for 60h to obtain pretreated herba Violae powder;
the zymocyte is aspergillus niger;
step two: adding pretreated Chinese violet powder into distilled water, wherein the mass ratio of the pretreated Chinese violet powder to the distilled water is 20: 110 (the mass ratio of the Chinese violet powder to the distilled water is 13: 117), heating to 100 ℃, boiling for 1.5h, and filtering to obtain filtrate A1 and filter residue B1; adding filter residue B1 into distilled water, wherein the mass ratio of the filter residue B1 to the distilled water is 13: 91, heating to 100 ℃, boiling for 0.8h, and filtering to obtain filtrate A2 and filter residue B2; mixing the filtrate A1 and filtrate A2, concentrating under reduced pressure, vacuum drying, and grinding to obtain herba Violae extract;
wherein the effective viable count of Aspergillus niger is more than or equal to 50 hundred million CFU/g, and the Aspergillus niger is food grade and purchased from Wuhan and is a far-developing science and technology company Limited.
The preparation method of the whitening and firming plant essence care solution comprises the following steps:
adding cyclohexasiloxane, glycerol and 1, 3-butanediol into water according to a raw material formula, stirring for 15min, setting the temperature to be 83 ℃ and the rotating speed to be 500 rpm; sequentially adding herba Violae extract, palmityl alcohol, trehalose, alpha-arbutin, butyl hydroxybenzoate and sodium benzoate, stirring for 25min at 83 deg.C and 500 rpm; homogenizing and emulsifying for 6min, inspecting, and discharging to obtain the whitening and firming plant essence care solution.
Example 3
A whitening and firming plant essence care solution is composed of the following raw materials: 0.5 wt% of an extract of Viola YEDOENSIS Makino, 0.3 wt% of cyclohexasiloxane, 4.5 wt% of glycerol, 5.5 wt% of 1, 3-butanediol, 0.2 wt% of palmityl alcohol, 0.3 wt% of trehalose, 0.1 wt% of alpha-arbutin, 0.05 wt% of hydroxybutyl benzoate, 0.05 wt% of sodium benzoate, and the balance of water.
The preparation method of the Chinese violet extract comprises the following steps:
the method comprises the following steps: adding the Chinese violet powder into distilled water, and uniformly mixing, wherein the mass ratio of the Chinese violet powder to the distilled water is 13: 7; heating to 39 ℃ and inoculating zymocyte, wherein the mass ratio of the zymocyte to the Chinese violet powder is 1.8: 100; fermenting at 39 deg.C for 60h to obtain pretreated herba Violae powder;
the fermentation bacteria are bacillus subtilis and aspergillus niger mixed according to the mass ratio of 1: 1;
step two: adding pretreated Chinese violet powder into distilled water, wherein the mass ratio of the pretreated Chinese violet powder to the distilled water is 20: 110 (the mass ratio of the Chinese violet powder to the distilled water is 13: 117), heating to 100 ℃, boiling for 1.5h, and filtering to obtain filtrate A1 and filter residue B1; adding filter residue B1 into distilled water, wherein the mass ratio of the filter residue B1 to the distilled water is 13: 91, heating to 100 ℃, boiling for 0.8h, and filtering to obtain filtrate A2 and filter residue B2; mixing the filtrate A1 with the filtrate A2, concentrating under reduced pressure, vacuum drying, and grinding to obtain powder X;
step three: placing the filter residue B2 into an extraction tank for supercritical extraction for 65min, wherein the extraction pressure is 38Mpa and the extraction temperature is 51 ℃; the main solvent is CO2Fluid, CO2The flow rate of the fluid is 16kg/h, and an entrainer is added, wherein the flow rate of the entrainer is 0.3g/min, so that an extract is obtained; centrifuging and filtering the extract, drying in vacuum, and grinding to obtain powder Y; mixing the powder X and the powder Y to obtain a herba Violae extract;
the using amount of the entrainer is 3.6 wt% of the filter residue B2, and the entrainer is a mixture of 85 wt% ethanol aqueous solution and 85 wt% acetone aqueous solution according to the mass ratio of 5: 1;
wherein the effective viable count of the bacillus subtilis is more than or equal to 100 hundred million CFU/g, and the bacillus subtilis is food grade and purchased from Hubeixin Rundy chemical company, Inc.; the effective viable count of Aspergillus niger is more than or equal to 50 hundred million CFU/g, and the Aspergillus niger is food grade and purchased from Wuhan and is a far-developing science and technology company Limited.
The preparation method of the whitening and firming plant essence care solution comprises the following steps:
adding cyclohexasiloxane, glycerol and 1, 3-butanediol into water according to a raw material formula, stirring for 15min, setting the temperature to be 83 ℃ and the rotating speed to be 500 rpm; sequentially adding herba Violae extract, palmityl alcohol, trehalose, alpha-arbutin, butyl hydroxybenzoate and sodium benzoate, stirring for 25min at 83 deg.C and 500 rpm; homogenizing and emulsifying for 6min, inspecting, and discharging to obtain the whitening and firming plant essence care solution.
Comparative example 4
A whitening and firming plant essence care solution is composed of the following raw materials: 0.5 wt% of an extract of Viola YEDOENSIS Makino, 0.3 wt% of cyclohexasiloxane, 4.5 wt% of glycerol, 5.5 wt% of 1, 3-butanediol, 0.2 wt% of palmityl alcohol, 0.3 wt% of trehalose, 0.1 wt% of alpha-arbutin, 0.05 wt% of hydroxybutyl benzoate, 0.05 wt% of sodium benzoate, and the balance of water.
The preparation method of the Chinese violet extract comprises the following steps:
the method comprises the following steps: adding the Chinese violet powder into distilled water, and uniformly mixing, wherein the mass ratio of the Chinese violet powder to the distilled water is 13: 7; heating to 39 ℃ and inoculating zymocyte, wherein the mass ratio of the zymocyte to the Chinese violet powder is 1.8: 100; fermenting at 39 deg.C for 60h to obtain pretreated herba Violae powder;
the fermentation bacteria are bacillus subtilis and aspergillus niger mixed according to the mass ratio of 1: 1;
step two: adding pretreated Chinese violet powder into distilled water, wherein the mass ratio of the pretreated Chinese violet powder to the distilled water is 20: 110 (the mass ratio of the Chinese violet powder to the distilled water is 13: 117), heating to 100 ℃, boiling for 1.5h, and filtering to obtain filtrate A1 and filter residue B1; adding filter residue B1 into distilled water, wherein the mass ratio of the filter residue B1 to the distilled water is 13: 91, heating to 100 ℃, boiling for 0.8h, and filtering to obtain filtrate A2 and filter residue B2; mixing the filtrate A1 with the filtrate A2, concentrating under reduced pressure, vacuum drying, and grinding to obtain powder X;
step three: placing the filter residue B2 into an extraction tank for supercritical extraction for 65min, wherein the extraction pressure is 38Mpa and the extraction temperature is 51 ℃; CO 22The flow rate of the fluid solvent is 16 kg/h; obtaining an extract; centrifuging and filtering the extract, drying in vacuum, and grinding to obtain powder Y; mixing the powder X and the powder Y to obtain a herba Violae extract;
wherein the effective viable count of the bacillus subtilis is more than or equal to 100 hundred million CFU/g, and the bacillus subtilis is food grade and purchased from Hubeixin Rundy chemical company, Inc.; the effective viable count of Aspergillus niger is more than or equal to 50 hundred million CFU/g, and the Aspergillus niger is food grade and purchased from Wuhan and is a far-developing science and technology company Limited.
The preparation method of the whitening and firming plant essence care solution comprises the following steps:
adding cyclohexasiloxane, glycerol and 1, 3-butanediol into water according to a raw material formula, stirring for 15min, setting the temperature to be 83 ℃ and the rotating speed to be 500 rpm; sequentially adding herba Violae extract, palmityl alcohol, trehalose, alpha-arbutin, butyl hydroxybenzoate and sodium benzoate, stirring for 25min at 83 deg.C and 500 rpm; homogenizing and emulsifying for 6min, inspecting, and discharging to obtain the whitening and firming plant essence care solution.
Comparative example 5
A whitening and firming plant essence care solution is composed of the following raw materials: 0.5 wt% of an extract of Viola YEDOENSIS Makino, 0.3 wt% of cyclohexasiloxane, 4.5 wt% of glycerol, 5.5 wt% of 1, 3-butanediol, 0.2 wt% of palmityl alcohol, 0.3 wt% of trehalose, 0.1 wt% of alpha-arbutin, 0.05 wt% of hydroxybutyl benzoate, 0.05 wt% of sodium benzoate, and the balance of water.
The preparation method of the Chinese violet extract comprises the following steps:
the method comprises the following steps: adding the Chinese violet powder into distilled water, and uniformly mixing, wherein the mass ratio of the Chinese violet powder to the distilled water is 13: 7; heating to 39 ℃ and inoculating zymocyte, wherein the mass ratio of the zymocyte to the Chinese violet powder is 1.8: 100; fermenting at 39 deg.C for 60h to obtain pretreated herba Violae powder;
the fermentation bacteria are bacillus subtilis and aspergillus niger mixed according to the mass ratio of 1: 1;
step two: adding pretreated Chinese violet powder into distilled water, wherein the mass ratio of the pretreated Chinese violet powder to the distilled water is 20: 110 (the mass ratio of the Chinese violet powder to the distilled water is 13: 117), heating to 100 ℃, boiling for 1.5h, and filtering to obtain filtrate A1 and filter residue B1; adding filter residue B1 into distilled water, wherein the mass ratio of the filter residue B1 to the distilled water is 13: 91, heating to 100 ℃, boiling for 0.8h, and filtering to obtain filtrate A2 and filter residue B2; mixing the filtrate A1 with the filtrate A2, concentrating under reduced pressure, vacuum drying, and grinding to obtain powder X;
step three: placing the filter residue B2 into an extraction tank for supercritical extraction for 65min, wherein the extraction pressure is 38Mpa and the extraction temperature is 51 ℃; the main solvent is CO2Fluid, CO2The flow rate of the fluid is 16kg/h, and an entrainer is added, wherein the flow rate of the entrainer is 0.3g/min, so that an extract is obtained; centrifuging and filtering the extract, drying in vacuum, and grinding to obtain powder Y; mixing the powder X and the powder Y to obtain a herba Violae extract;
the using amount of the entrainer is 3.6 wt% of the filter residue B2, and the entrainer is 85 wt% of acetone aqueous solution;
wherein the effective viable count of the bacillus subtilis is more than or equal to 100 hundred million CFU/g, and the bacillus subtilis is food grade and purchased from Hubeixin Rundy chemical company, Inc.; the effective viable count of Aspergillus niger is more than or equal to 50 hundred million CFU/g, and the Aspergillus niger is food grade and purchased from Wuhan and is a far-developing science and technology company Limited.
The preparation method of the whitening and firming plant essence care solution comprises the following steps:
adding cyclohexasiloxane, glycerol and 1, 3-butanediol into water according to a raw material formula, stirring for 15min, setting the temperature to be 83 ℃ and the rotating speed to be 500 rpm; sequentially adding herba Violae extract, palmityl alcohol, trehalose, alpha-arbutin, butyl hydroxybenzoate and sodium benzoate, stirring for 25min at 83 deg.C and 500 rpm; homogenizing and emulsifying for 6min, inspecting, and discharging to obtain the whitening and firming plant essence care solution.
Comparative example 6
A whitening and firming plant essence care solution is composed of the following raw materials: 0.5 wt% of an extract of Viola YEDOENSIS Makino, 0.3 wt% of cyclohexasiloxane, 4.5 wt% of glycerol, 5.5 wt% of 1, 3-butanediol, 0.2 wt% of palmityl alcohol, 0.3 wt% of trehalose, 0.1 wt% of alpha-arbutin, 0.05 wt% of hydroxybutyl benzoate, 0.05 wt% of sodium benzoate, and the balance of water.
The preparation method of the Chinese violet extract comprises the following steps:
the method comprises the following steps: adding the Chinese violet powder into distilled water, and uniformly mixing, wherein the mass ratio of the Chinese violet powder to the distilled water is 13: 7; heating to 39 ℃ and inoculating zymocyte, wherein the mass ratio of the zymocyte to the Chinese violet powder is 1.8: 100; fermenting at 39 deg.C for 60h to obtain pretreated herba Violae powder;
the fermentation bacteria are bacillus subtilis and aspergillus niger mixed according to the mass ratio of 1: 1;
step two: adding pretreated Chinese violet powder into distilled water, wherein the mass ratio of the pretreated Chinese violet powder to the distilled water is 20: 110 (the mass ratio of the Chinese violet powder to the distilled water is 13: 117), heating to 100 ℃, boiling for 1.5h, and filtering to obtain filtrate A1 and filter residue B1; adding filter residue B1 into distilled water, wherein the mass ratio of the filter residue B1 to the distilled water is 13: 91, heating to 100 ℃, boiling for 0.8h, and filtering to obtain filtrate A2 and filter residue B2; mixing the filtrate A1 with the filtrate A2, concentrating under reduced pressure, vacuum drying, and grinding to obtain powder X;
step three: placing the filter residue B2 into an extraction tank for supercritical extraction for 65min, wherein the extraction pressure is 38Mpa and the extraction temperature is 51 ℃; the main solvent is CO2Fluid, CO2The flow rate of the fluid is 16kg/h, and an entrainer is added, wherein the flow rate of the entrainer is 0.3g/min, so that an extract is obtained; centrifuging and filtering the extract, drying in vacuum, and grinding to obtain powder Y; mixing the powder X and the powder Y to obtain a herba Violae extract;
the using amount of the entrainer is 3.6 wt% of the filter residue B2, and the entrainer is 85 wt% ethanol water solution;
wherein the effective viable count of the bacillus subtilis is more than or equal to 100 hundred million CFU/g, and the bacillus subtilis is food grade and purchased from Hubeixin Rundy chemical company, Inc.; the effective viable count of Aspergillus niger is more than or equal to 50 hundred million CFU/g, and the Aspergillus niger is food grade and purchased from Wuhan and is a far-developing science and technology company Limited.
The preparation method of the whitening and firming plant essence care solution comprises the following steps:
adding cyclohexasiloxane, glycerol and 1, 3-butanediol into water according to a raw material formula, stirring for 15min, setting the temperature to be 83 ℃ and the rotating speed to be 500 rpm; sequentially adding herba Violae extract, palmityl alcohol, trehalose, alpha-arbutin, butyl hydroxybenzoate and sodium benzoate, stirring for 25min at 83 deg.C and 500 rpm; homogenizing and emulsifying for 6min, inspecting, and discharging to obtain the whitening and firming plant essence care solution.
Example 4
A whitening and firming plant essence care solution is composed of the following raw materials: 0.35 wt% of an extract of Viola YEDOENSIS Makino, 0.15 wt% of an extract containing raw grass (ANASTATICA HIEROCHUNTICA), 0.3 wt% of cyclohexasiloxane, 4.5 wt% of glycerol, 5.5 wt% of 1, 3-butanediol, 0.2 wt% of palmitol, 0.3 wt% of trehalose, 0.1 wt% of alpha-arbutin, 0.05 wt% of oxybenzoic acid butyl ester, 0.05 wt% of sodium benzoate, and the balance of water.
The preparation method of the Chinese violet extract comprises the following steps:
the method comprises the following steps: adding the Chinese violet powder into distilled water, and uniformly mixing, wherein the mass ratio of the Chinese violet powder to the distilled water is 13: 7; heating to 39 ℃ and inoculating zymocyte, wherein the mass ratio of the zymocyte to the Chinese violet powder is 1.8: 100; fermenting at 39 deg.C for 60h to obtain pretreated herba Violae powder;
the fermentation bacteria are bacillus subtilis and aspergillus niger mixed according to the mass ratio of 1: 1;
step two: adding pretreated Chinese violet powder into distilled water, wherein the mass ratio of the pretreated Chinese violet powder to the distilled water is 20: 110 (the mass ratio of the Chinese violet powder to the distilled water is 13: 117), heating to 100 ℃, boiling for 1.5h, and filtering to obtain filtrate A1 and filter residue B1; adding filter residue B1 into distilled water, wherein the mass ratio of the filter residue B1 to the distilled water is 13: 91, heating to 100 ℃, boiling for 0.8h, and filtering to obtain filtrate A2 and filter residue B2; mixing the filtrate A1 with the filtrate A2, concentrating under reduced pressure, vacuum drying, and grinding to obtain powder X;
step three: placing the filter residue B2 into an extraction tank for supercritical extraction for 65min, wherein the extraction pressure is 38Mpa and the extraction temperature is 51 ℃; the main solvent is CO2Fluid, CO2The flow rate of the fluid is 16kg/h, and an entrainer is added, wherein the flow rate of the entrainer is 0.3g/min, so that an extract is obtained; the extract was subjected to centrifugal filtration to obtain an extract,vacuum drying, grinding to obtain powder Y; mixing the powder X and the powder Y to obtain a herba Violae extract;
the using amount of the entrainer is 3.6 wt% of the filter residue B2, and the entrainer is a mixture of 85 wt% ethanol aqueous solution and 85 wt% acetone aqueous solution according to the mass ratio of 5: 1;
wherein the effective viable count of the bacillus subtilis is more than or equal to 100 hundred million CFU/g, and the bacillus subtilis is food grade and purchased from Hubeixin Rundy chemical company, Inc.; the effective viable count of Aspergillus niger is more than or equal to 50 hundred million CFU/g, and the Aspergillus niger is food grade and purchased from Wuhan and is a far-developing science and technology company Limited.
The preparation method of the whitening and firming plant essence care solution comprises the following steps:
adding cyclohexasiloxane, glycerol and 1, 3-butanediol into water according to a raw material formula, stirring for 15min, setting the temperature to be 83 ℃ and the rotating speed to be 500 rpm; sequentially adding herba Violae extract, extract containing herba Hedyotis Auriculariae, palmityl alcohol, trehalose, alpha-arbutin, butyl hydroxybenzoate and sodium benzoate, stirring for 25min at 83 deg.C and 500 rpm; homogenizing and emulsifying for 6min, inspecting, and discharging to obtain the whitening and firming plant essence care solution.
Comparative example 7
A whitening and firming plant essence care solution is composed of the following raw materials: 0.5 wt% of an extract containing raw grass (ANASTATICA HIEROCHUNTICA), 0.3 wt% of cyclohexasiloxane, 4.5 wt% of glycerin, 5.5 wt% of 1, 3-butanediol, 0.2 wt% of palmitol, 0.3 wt% of trehalose, 0.1 wt% of alpha-arbutin, 0.05 wt% of oxybutyl ester, 0.05 wt% of sodium benzoate, and the balance of water.
The preparation method of the whitening and firming plant essence care solution comprises the following steps:
adding cyclohexasiloxane, glycerol and 1, 3-butanediol into water according to a raw material formula, stirring for 15min, setting the temperature to be 83 ℃ and the rotating speed to be 500 rpm; sequentially adding the extract containing the raw grass, the palmityl alcohol, the trehalose, the alpha-arbutin, the butyl hydroxybenzoate and the sodium benzoate, continuously stirring for 25min, setting the temperature to be 83 ℃, and setting the rotating speed to be 500 rpm; homogenizing and emulsifying for 6min, inspecting, and discharging to obtain the whitening and firming plant essence care solution.
Test example 1
Tyrosinase inhibition assay: dissolving tyrosinase in PBS buffer solution with the pH value of 6.8 to prepare 120U/mL tyrosinase solution; dissolving L-tyrosine in PBS buffer solution with the pH value of 6.8 to prepare 1.6 mol/L-tyrosine solution; dissolving a sample to be detected in PBS (phosphate buffer solution) with the pH value of 6.8 to prepare a sample solution to be detected of 0.5 mg/mL; 0.5mL of sample solution to be tested is taken, 0.5mL of tyrosinase solution and 1.5mL of PBS buffer solution with the pH value of 6.8 are added, the mixture is preheated at 37 ℃ for 12min, 0.5mL of L-tyrosine solution is added to react at 37 ℃ for 18min, the light absorption value is measured at 475nm, 5 groups are tested according to the same formula, and the average value is taken.
Tyrosinase inhibition (%) [1- (a1-a2)/(A3-a4) ] × 100
Wherein, A1: l-tyrosine, the light absorption value of the sample to be detected and the tyrosinase system; a2: the light absorption value of the sample to be detected, the tyrosinase and PBS buffer solution system; a3: the light absorption values of an L-tyrosine and tyrosinase system and a PBS buffer solution; a4: and (3) the light absorption value of a tyrosinase and PBS buffer solution system.
TABLE 1 tyrosinase inhibitory rate test table
Figure BDA0002559526100000151
Figure BDA0002559526100000161
The prepared herba violae extract has a good whitening effect; on one hand, the active ingredients in the Chinese violet extract are used as reducing agents to antagonize the activation of oxygen on tyrosinase, so that the tyrosinase cannot be normally converted into a catalytic state from a deoxidation mode, and the tyrosinase is prevented from catalyzing to generate melanin; on the other hand, active ingredients in the Chinese violet extract can enter a hydrophobic pocket of a tyrosinase catalytic center and are combined with surrounding amino acid residues through hydrogen bonds and hydrophobic acting force, so that the positions of acting substrates of tyrosinase such as L-tyrosine and the like in the tyrosinase catalytic center are preempted, the formation of melanin is further inhibited, and the skin whitening effect is achieved.
Comparing the embodiment 1 with the embodiment 2 and the comparative examples 2-3, it can be seen that the invention adopts zymophyte to pretreat the Chinese violet powder, which destroys the cell wall and cell membrane structure of the Chinese violet, so that the organic micromolecule active ingredients in the Chinese violet cell are easier to dissolve out, which facilitates the subsequent extraction process and improves the quality of the Chinese violet extract; furthermore, as can be seen from the comparison of the example 2 and the comparative examples 2-3, the invention adopts the mixing and synergistic fermentation of the bacillus subtilis and the aspergillus niger, so that the pretreatment is more thorough and the extraction of the active ingredients in the Chinese violet is more facilitated through the coordination and interaction relationship among the strains; aspergillus niger can secrete a large amount of high-activity cellulase, pectinase, phytase, amylase and the like, effectively degrade pectin and fiber network structures in cell walls of the Chinese violet, and greatly destroy the cell wall structures of the Chinese violet; the bacillus subtilis can secrete a large amount of high-activity alkaline protease, lipase, glucoamylase and the like, further acts on cell membranes of the Chinese violet, destroys phospholipid bilayer structures of the cell membranes, and is coordinated and interacted with each other to synergize effects, so that the pretreated Chinese violet powder is easier to extract, the active ingredients in the obtained Chinese violet extract are higher in content, and the whitening effect is better.
Test example 2
And (3) testing a whitening test: testing with MELAMIND skin pigment analyzer, selecting 250 healthy subjects of 20-55 years old, stopping using other whitening cosmetics during the testing process, respectively using the sample to be tested 1 time in the morning and evening, and continuously using for 7 days and 21 days, and determining each index by the same method; during testing, the environmental temperature is controlled to be 22 +/-1 ℃, the environmental humidity is controlled to be 50 +/-5%, the testing is repeated for 5 times, and the average value is taken; the blank group was tested without the use of test sample and other whitening cosmetics.
Melanin reduction rate (%) - (D1-D2)/D1X 100
Wherein D1 is the melanin content of the test sample which is not used at the beginning of the test; d2 is the melanin content after the test sample was used.
TABLE 2 Melanin reduction test Table
Figure BDA0002559526100000171
Compared with a blank group, the test results P of the samples to be tested of the examples 1 to 4, the comparative examples 1 to 4 and the comparative example 7 are less than 0.05, and have significant difference. The prepared herba violae extract has a good whitening effect; on one hand, the active ingredients in the Chinese violet extract are used as reducing agents to antagonize the activation of oxygen on tyrosinase, so that the tyrosinase cannot be normally converted into a catalytic state from a deoxidation mode, and the tyrosinase is prevented from catalyzing to generate melanin; on the other hand, active ingredients in the Chinese violet extract can enter a hydrophobic pocket of a tyrosinase catalytic center and are combined with surrounding amino acid residues through hydrogen bonds and hydrophobic acting force, so that the positions of acting substrates of tyrosinase such as L-tyrosine and the like in the tyrosinase catalytic center are preempted, the formation of melanin is further inhibited, and the skin whitening effect is achieved.
Comparing the embodiment 1 with the embodiment 2 and the comparative examples 2-3, it can be seen that the invention adopts zymophyte to pretreat the Chinese violet powder, which destroys the cell wall and cell membrane structure of the Chinese violet, so that the organic micromolecule active ingredients in the Chinese violet cell are easier to dissolve out, which facilitates the subsequent extraction process and improves the quality of the Chinese violet extract; furthermore, as can be seen from the comparison of the example 2 and the comparative examples 2-3, the invention adopts the mixing and synergistic fermentation of the bacillus subtilis and the aspergillus niger, so that the pretreatment is more thorough and the extraction of the active ingredients in the Chinese violet is more facilitated through the coordination and interaction relationship among the strains; aspergillus niger can secrete a large amount of high-activity cellulase, pectinase, phytase, amylase and the like, effectively degrade pectin and fiber network structures in cell walls of the Chinese violet, and greatly destroy the cell wall structures of the Chinese violet; the bacillus subtilis can secrete a large amount of high-activity alkaline protease, lipase, glucoamylase and the like, further acts on cell membranes of the Chinese violet, destroys phospholipid bilayer structures of the cell membranes, and is coordinated and interacted with each other to synergize effects, so that the pretreated Chinese violet powder is easier to extract, the active ingredients in the obtained Chinese violet extract are higher in content, and the whitening effect is better. This is achieved byIn addition, comparing example 3 with comparative examples 4 and 2, it can be seen that the present invention employs CO2The supercritical extraction is combined with water extraction, and a proper entrainer is added in the supercritical extraction process, so that the entrainer can generate Van der Waals force, hydrogen bond, weak complexation and other intermolecular forces with organic micromolecule active ingredients in the Chinese violet, so that the active ingredients in the Chinese violet are dissolved out more easily, the biological activity content of the Chinese violet extract is improved, and the whitening effect is better.
Comparing example 4 with example 3 and comparative example 7, it can be seen that the whitening agent prepared by compounding the viola yedoensis makino extract and the raw grass-containing extract has synergistic effect, and the whitening effect is further improved; according to the invention, the Chinese violet extract with a specific content and the raw grass-containing extract are added, so that the Chinese violet extract and the raw grass-containing extract interact with each other in a coordinated manner to jointly nourish the skin; the Chinese violet extract and the green grass-containing extract are mutually complemented to further strengthen the inhibition on the catalytic activity of tyrosinase, and simultaneously, more whitening active ingredients act on tyrosinase and are combined with a catalytic center thereof through hydrogen bonds and hydrophobic acting force to occupy the central position required by the catalysis of L-tyrosine and other substrates by the tyrosinase in advance, so that the formation of melanin is effectively inhibited, and the skin whitening effect is better.
The foregoing detailed description of the preferred embodiments of the invention has been presented. It should be understood that numerous modifications and variations could be devised by those skilled in the art in light of the present teachings without departing from the inventive concepts. Therefore, the technical solutions available to those skilled in the art through logic analysis, reasoning and limited experiments based on the prior art according to the concept of the present invention should be within the scope of protection defined by the claims.

Claims (2)

1. The whitening and firming plant essence care solution is characterized by comprising the following raw materials: 0.2-0.6 wt% of Chinese violet extract, 0.1-0.5 wt% of cyclohexasiloxane, 1.0-5.0 wt% of glycerol, 3.0-6.0 wt% of 1, 3-butanediol, 0.05-0.5 wt% of palmityl alcohol, 0.1-0.5 wt% of trehalose, 0.01-0.5 wt% of alpha-arbutin, 0.01-0.10 wt% of oxybenzoic acid butyl ester, 0.01-0.10 wt% of sodium benzoate and the balance of water;
the Chinese violet extract is prepared by the following method:
the method comprises the following steps: adding the Chinese violet powder into distilled water, and uniformly mixing, wherein the mass ratio of the Chinese violet powder to the distilled water is (5-15) to (5-10); heating to 32-52 ℃, inoculating zymocyte, wherein the mass ratio of the zymocyte to the Chinese violet powder is (0.5-2.0): 100; fermenting at 32-52 deg.C for 12-72 hr to obtain pretreated herba Violae powder;
step two: adding pretreated Chinese violet powder into distilled water, wherein the mass ratio of the pretreated Chinese violet powder to the distilled water is (10-25): (100-120), heating to 95-125 ℃, boiling for 0.5-2.5h, and filtering to obtain filtrate A1 and filter residue B1; adding filter residue B1 into distilled water, wherein the mass ratio of the filter residue B1 to the distilled water is (5-15): (85-105), heating to 95-125 ℃, boiling for 0.5-1.5h, and filtering to obtain filtrate A2 and filter residue B2; mixing the filtrate A1 with the filtrate A2, concentrating under reduced pressure, vacuum drying, and grinding to obtain powder X;
step three: placing the filter residue B2 into an extraction tank for supercritical extraction for 30-90min, wherein the extraction pressure is 35-50Mpa, and the extraction temperature is 45-70 deg.C; the main solvent is CO2Fluid, CO2The flow rate of the fluid is 10-18kg/h, and an entrainer is added, wherein the flow rate of the entrainer is 0.1-0.8g/min, so that an extract is obtained; centrifuging and filtering the extract, drying in vacuum, and grinding to obtain powder Y; mixing the powder X and the powder Y to obtain a herba Violae extract;
the entrainer is a mixture of 50-95 wt% ethanol aqueous solution and 50-95 wt% acetone aqueous solution according to the mass ratio of (1-5) to 1; the fermentation bacteria are the mixture of bacillus subtilis and aspergillus niger according to the mass ratio of 1 (1-5).
2. The preparation method of the whitening and tightening plant essence care solution according to claim 1, characterized by comprising the following steps: adding the cyclohexasiloxane, the glycerol and the 1, 3-butanediol into water according to a raw material formula, stirring for 10-20min, setting the temperature to be 75-85 ℃, and setting the rotating speed to be 300-600 rpm; sequentially adding the Chinese violet extract, the palmityl alcohol, the trehalose, the alpha-arbutin, the butyl hydroxybenzoate and the sodium benzoate, continuously stirring for 20-30min, setting the temperature to be 75-85 ℃, and setting the rotation speed to be 300-600 rpm; homogenizing and emulsifying for 5-10min, inspecting, and discharging to obtain the whitening and firming plant essence care solution.
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JP4464533B2 (en) * 2000-06-19 2010-05-19 株式会社ナリス化粧品 Cosmetics
CN106309221A (en) * 2016-08-31 2017-01-11 百朗德生物化学(海门)有限公司 Cosmetic composition capable of removing black eyes
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CN103932965A (en) * 2014-04-30 2014-07-23 王海云 Toxin-expelling young-keeping skin care product and preparation method
CN104055715A (en) * 2014-07-09 2014-09-24 广州丹奇日用化工厂有限公司 Oil-control cosmetic composition and preparation method thereof

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