CN113520902A - Whitening emulsion and preparation method thereof - Google Patents

Whitening emulsion and preparation method thereof Download PDF

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Publication number
CN113520902A
CN113520902A CN202010287733.3A CN202010287733A CN113520902A CN 113520902 A CN113520902 A CN 113520902A CN 202010287733 A CN202010287733 A CN 202010287733A CN 113520902 A CN113520902 A CN 113520902A
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whitening
parts
extract
emulsion
whitening composition
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郑立波
赵迪
王霞
罗鑫宇
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Beijing Liyansiyan Biotechnology Co ltd
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Beijing Youyue Baishi Technology Development 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
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/67Vitamins
    • A61K8/673Vitamin B group
    • A61K8/675Vitamin B3 or vitamin B3 active, e.g. nicotinamide, nicotinic acid, nicotinyl aldehyde
    • 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
    • A61K8/92Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof
    • A61K8/922Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof of vegetable origin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/96Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/97Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
    • A61K8/9783Angiosperms [Magnoliophyta]
    • A61K8/9789Magnoliopsida [dicotyledons]
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • 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
    • A61Q19/08Anti-ageing 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
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/59Mixtures
    • A61K2800/592Mixtures of compounds complementing their respective functions
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/59Mixtures
    • A61K2800/592Mixtures of compounds complementing their respective functions
    • A61K2800/5922At least two compounds being classified in the same subclass of A61K8/18

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Abstract

The invention discloses a whitening emulsion and a preparation method thereof. The whitening emulsion includes carbomer, glycerin, cetostearyl alcohol/cocoyl glucoside, glyceryl tri (ethyl hexanoate), pentaerythritol distearate, cyclopentadimethylsiloxane, disodium EDTA, sodium hydroxide, and a whitening composition including niacinamide, a giant knotweed extract, and a pepper extract. Experiments prove that the whitening emulsion has good effects of removing free radicals, improving skin color, controlling grease secretion and improving red blood streak by adding the whitening composition, can achieve the integral whitening effect, and has wide application prospect in the field of skin care products.

Description

Whitening emulsion and preparation method thereof
Technical Field
The invention belongs to the field of daily chemicals, and particularly relates to a whitening emulsion and a preparation method thereof.
Background
The safety and efficacy of cosmetics are issues of intense interest to consumers and skin care product developers. At present, a plurality of whitening methods exist, and if the skin problems are rapidly and effectively improved in a short time and the face appearance is improved, scientific beautifying and skin care products are needed.
Most of the whitening products on the market take nicotinamide and VC as main whitening agents. Niacinamide is a water-soluble vitamin and is a member of the vitamin B group. Nicotinamide can inhibit the transfer of melanin, and make skin slowly whiten and more bright. The high-content nicotinamide product has a certain sensitization rate. Meanwhile, melanin produced by the skin has a protective effect on the skin, and excessive inhibition of the production or formation of melanin may have an adverse effect on the skin. For example, the "chalking event by creosol" in Japan is the chalking phenomenon caused by severe destruction of skin melanin after the skin care agent is used. In addition, the other main whitening component VC is easy to discolor and unstable.
The realization of low whitening efficiency through a single approach is one of the problems of the conventional whitening products. Therefore, the development of safe and efficient skin whitening compositions and skin care preparations is a problem to be solved in the art.
Disclosure of Invention
The composition with the whitening effect is formed by compounding plant components such as giant knotweed rhizome extract, pepper extract and the like and nicotinamide, and is formed into skin care emulsion by compounding cosmetic auxiliary materials. The skin care product not only solves the problem of sensitization risk caused by large usage amount of whitening nicotinamide, improves the product safety, but also has the synergistic effect of all the components, and has multiple skin care effects of removing free radicals, improving red blood streak, balancing skin color, balancing grease and the like. The problems of single whitening way and unobvious effect are solved.
According to the invention, the emulsion comprises the following raw materials in parts by weight: carbomer, glycerin, cetostearyl alcohol/cocoyl glucoside, glyceryl tri (ethyl hexanoate), pentaerythritol distearate, cyclopentadimethylsiloxane, disodium EDTA, sodium hydroxide, and a whitening composition.
According to the present invention, the whitening composition includes niacinamide, giant knotweed rhizome extract and pepper extract.
According to some embodiments of the invention, the ingredients are used in an amount of: 0.1-0.5wt% of carbomer, 1.0-10.0 wt% of glycerol, 0.5-5.0 wt% of cetearyl alcohol/coco glucoside, 1.0-5.0 wt% of glycerol tri (ethyl hexanoate), 0.1-2.0 wt% of pentaerythritol distearate, 1.0-5.0 wt% of cyclopenta dimethyl silicone, 0.01-0.1 wt% of disodium EDTA, 0.02-0.1 wt% of sodium hydroxide and 0.5-20.0 wt% of the whitening composition.
According to some preferred embodiments of the present invention, the ingredients are used in an amount of: 0.2-0.4wt% carbomer, 3.0-7.0 wt% glycerin, 2.0-4.0wt% cetearyl alcohol/coco glucoside, 1.0-3.5 wt% glyceryl tri (ethyl hexanoate), 0.5-2.0 wt% pentaerythritol distearate, 1.0-3.0 wt% cyclopenta dimethyl siloxane, 0.02-0.05wt% disodium EDTA, 0.04-0.08 wt% sodium hydroxide, and 5.0-15 wt% of the whitening composition.
According to some embodiments of the invention, the whitening composition further comprises 1, 3-propanediol.
According to some embodiments of the invention, the whitening composition further comprises PEG-40 hydrogenated castor oil.
According to some further embodiments of the present invention, the whitening composition comprises the following raw materials in parts by weight: 1-10 parts of nicotinamide, 0.01-5 parts of giant knotweed extract, 0.01-0.2 part of pepper extract, 0.01-5 parts of 1, 3-propylene glycol and 0.02-0.5 part of PEG-40 hydrogenated castor oil.
According to the invention, the nicotinamide is used in an amount of 1 to 10 parts by weight, and may be, for example, 1, 1.1, 1.5, 2, 2.2, 2.3, 2.4, 2.5, 2.8, 3, 3.1, 3.2, 3.5, 3.8, 4, 4.5, 5, 5.5, 5.8, 6, 6.4, 6.5, 7, 7.4, 7.6, 7.8, 8, 8.8, 9, 9.5, 10 parts by weight, and also values between the aforementioned values.
According to the invention, the polygonum cuspidatum extract is used in an amount of 0.01-5 parts by weight, such as 0.01, 0.02, 0.03, 0.05, 0.1, 0.2, 0.3, 0.6, 0.8, 0.9, 1, 1.1, 1.5, 2, 2.2, 2.3, 2.4, 2.5, 2.8, 3, 3.1, 3.2, 3.5, 3.8, 4, 4.5, 5 parts by weight, and values in between.
According to the invention, the pepper extract is used in an amount of 0.01-0.2 parts by weight, which may be, for example, 0.01, 0.02, 0.03, 0.04, 0.05, 0.06, 0.08, 0.09, 0.1, 0.15, 0.2 parts by weight, and values in between.
According to the invention, the 1, 3-propanediol is used in an amount of 0.01 to 5 parts by weight, and may be, for example, 0.01, 0.05, 0.1, 0.2, 0.3, 0.5, 0.6, 0.8, 0.9, 1, 1.1, 1.5, 1.8, 2, 2.2, 2.3, 2.4, 2.5, 2.8, 3, 3.1, 3.2, 3.5, 3.8, 4, 4.5, 5 parts by weight, and also values in between the above-mentioned values.
According to the invention, the PEG-40 hydrogenated castor oil is used in an amount of 0.02 to 0.5 parts by weight, and may be, for example, 0.02, 0.03, 0.05, 0.06, 0.1, 0.15, 0.2, 0.25, 0.3, 0.33, 0.35, 0.4, 0.45, 0.47, 0.48, 0.5 parts by weight, and points between the above values.
According to some preferred embodiments of the present invention, the whitening composition comprises the following raw materials in parts by weight: 2-6 parts of nicotinamide, 0.1-4 parts of giant knotweed rhizome extract, 0.1-0.2 part of pepper extract, 0.25-5 parts of 1, 3-propylene glycol and 0.2-0.4 part of PEG-40 hydrogenated castor oil.
According to some embodiments of the present invention, the whitening composition may be prepared by:
(1) mixing the pepper extract with 1, 3-propylene glycol and PEG-40 hydrogenated castor oil, and dissolving to obtain mixed solution;
(2) adding nicotinamide and giant knotweed rhizome extract into the mixed solution obtained in the step (1), and uniformly stirring.
According to the present invention, the whitening emulsion further comprises a preservative.
According to the invention, the preservative may be, for example, phenoxyethanol/caprylyl glycol/decyl glycol.
According to the invention, the whitening emulsion is prepared by a method comprising the following steps:
(1) adding water, carbomer, glycerol and EDTA disodium into an emulsification tank, heating to 80-85 ℃, and uniformly stirring;
(2) adding cetearyl alcohol/coco glucoside, glycerol tri (ethyl hexanoate), pentaerythritol distearate, and cyclopenta dimethyl silicone into an oil phase tank, heating to 80-85 deg.C, and stirring;
(3) pumping the oil phase in the oil phase tank into an emulsification tank, starting homogenization at the rotation speed of 2500-.
(4) Cooling to 45-60 ℃, and adding sodium hydroxide;
(5) adding the whitening composition, and stirring uniformly.
According to the present invention, the whitening composition and the preservative are added in the step (5).
According to the invention, the preservative may be phenoxyethanol/caprylyl glycol/decanediol.
According to the invention, the skin care composition is formed by compounding the nicotinamide with the plant source polygonum cuspidatum extract and the plant source pepper extract, and the skin care emulsion is formed by compounding the auxiliary materials of cosmetics, so that the problems of poor whitening effect and possible safety caused by the independent use of the nicotinamide are solved, the effects of removing free radicals, removing red blood streaks and controlling oil can be achieved while whitening through the compounding and synergy of various components, and the skin care composition has a wide application prospect in skin care products.
Description of the drawings:
FIG. 1 is a graph showing the radical scavenging effect of example 4 and comparative examples 1 to 5;
FIG. 2 is a chart showing the results of the VISIA test on the skin color of a sample from example 8;
FIG. 3 is a chart showing the results of the VISIA test on the red blood streak status of a sample from example 8;
FIG. 4 is a chart of the results of the VISIA test on the skin color of the comparative example 6 sample from the subjects;
FIG. 5 is a chart showing the results of the VISIA test conducted on the red blood cells of the comparative example 6;
FIG. 6 is a chart showing the results of VISIA test on the oil secretion of the sample of example 8;
FIG. 7 is a VISIA test result chart of the oil secretion of the sample of comparative example 6 tested by the subject.
The specific implementation mode is as follows:
the present invention will be described in detail with reference to the following embodiments, which will become more apparent by describing the embodiments and processes of the present invention. It should be understood by those skilled in the art that the detailed description is only a part of the examples, but not all examples, and is intended to illustrate the invention and not to limit the scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention. The examples were carried out under the conventional conditions, unless otherwise specified. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
Table main raw material and source
Name (R) Standard Chinese name Suppliers of goods
Nicotinamide Nicotinamide DSM
Polygonum cuspidatum extract Water, butanediol, and rhizoma Polygoni Cuspidati (POLYGONUM CUSPIDATUM) extract Shanghai Jia Ye
Pepper extract Fructus Piperis (Piper NIGRUM) extract Beijing Xinnuo Jiucangheng
1, 3-propanediol 1, 3-propanediol (DuPont)
PEG-40 hydrogenated Castor oil PEG-40 hydrogenated Castor oil BASF
Carbomer 940 Carbomer Lubrizol
Glycerol Glycerol Green treasure
MONTANOV 68 Cetearyl alcohol/coco glucoside SEPPIC
Crodamol™ GTEH Glycerol tri (ethylhexanoate) ester CRODA
Cutina PES Pentaerythritol distearate Kening medicine
KF-995 Cyclopenta dimethyl siloxane Huizhike
EDTA disodium salt EDTA disodium salt AkzoNobel
Sodium hydroxide Sodium hydroxide BEIJING CHEMICAL PLANT
Microcare®PHDG Phenoxyethanol/caprylyl glycol/decyl glycol THOR
Notoginseng radix extract Water, butanediol, and Notoginseng radix (PANAX NONONOGONSENG) root extract Shanghai Jia Ye
VC Ethyl Ether 3-O-Ethylascorbic acid Beijing Xinnuo Jiucangheng
Example 1
Weighing the following raw materials in parts by weight:
1 part by weight of nicotinamide, 5 parts by weight of giant knotweed extract, 0.01 part by weight of pepper extract, 0.01 part by weight of 1, 3-propylene glycol and 0.02 part by weight of PEG-40 hydrogenated castor oil;
mixing the above fructus Piperis extract with 1, 3-propylene glycol and PEG-40 hydrogenated castor oil, and dissolving to obtain mixed solution;
adding nicotinamide and giant knotweed rhizome extract into the mixed solution, and uniformly stirring to obtain the whitening composition A.
Example 2
Weighing the following raw materials in parts by weight:
10 parts of nicotinamide, 0.01 part of giant knotweed rhizome extract, 0.2 part of pepper extract, 5 parts of 1, 3-propylene glycol and 0.4 part of PEG-40 hydrogenated castor oil.
Mixing the above fructus Piperis extract with 1, 3-propylene glycol and PEG-40 hydrogenated castor oil, and dissolving to obtain mixed solution;
And adding the nicotinamide and the polygonum cuspidatum extract into the obtained mixed solution, and uniformly stirring to obtain the whitening composition B.
Example 3
Weighing the following raw materials in parts by weight:
3 parts of nicotinamide, 3 parts of giant knotweed rhizome extract, 0.1 part of pepper extract, 2.5 parts of 1, 3-propylene glycol and 0.2 part of PEG-40 hydrogenated castor oil,
mixing the above fructus Piperis extract with 1, 3-propylene glycol and PEG-40 hydrogenated castor oil, and dissolving to obtain mixed solution;
adding nicotinamide and giant knotweed rhizome extract into the mixed solution, and uniformly stirring to obtain the whitening composition C.
Example 4
Weighing the following raw materials in parts by weight:
6 parts of nicotinamide, 5 parts of giant knotweed rhizome extract, 0.2 part of pepper extract, 5 parts of 1, 3-propylene glycol, 0.4 part of PEG-40 hydrogenated castor oil,
mixing the above fructus Piperis extract with 1, 3-propylene glycol and PEG-40 hydrogenated castor oil, and dissolving to obtain mixed solution;
and adding the nicotinamide and the polygonum cuspidatum extract into the obtained mixed solution, and uniformly stirring to obtain the whitening composition D.
Comparative example 1
Weighing the following raw materials in parts by weight:
2 parts of nicotinamide, 9 parts of giant knotweed rhizome extract, 0.2 part of pepper extract, 5 parts of 1, 3-propylene glycol, 0.4 part of PEG-40 hydrogenated castor oil,
Mixing the above fructus Piperis extract with 1, 3-propylene glycol and PEG-40 hydrogenated castor oil, and dissolving to obtain mixed solution;
adding nicotinamide and rhizoma Polygoni Cuspidati extract into the mixed solution, and stirring to obtain skin care composition.
Comparative example 2
Weighing the following raw materials in parts by weight:
3 parts of nicotinamide, 8 parts of giant knotweed rhizome extract, 0.2 part of pepper extract, 5 parts of 1, 3-propylene glycol, 0.4 part of PEG-40 hydrogenated castor oil,
mixing the above fructus Piperis extract with 1, 3-propylene glycol and PEG-40 hydrogenated castor oil, and dissolving to obtain mixed solution;
adding nicotinamide and rhizoma Polygoni Cuspidati extract into the mixed solution, and stirring to obtain skin care composition.
Comparative example 3
Weighing the following raw materials in parts by weight:
6 parts of nicotinamide, 5 parts of pseudo-ginseng extract, 0.2 part of pepper extract, 5 parts of 1, 3-propylene glycol, 0.4 part of PEG-40 hydrogenated castor oil,
mixing the above fructus Piperis extract with 1, 3-propylene glycol and PEG-40 hydrogenated castor oil, and dissolving to obtain mixed solution;
adding nicotinamide and Notoginseng radix extract into the mixed solution, and stirring to obtain skin care composition.
Comparative example 4
Weighing the following raw materials in parts by weight:
6.0 parts of nicotinamide, 5.2 parts of giant knotweed extract, 5 parts of 1, 3-propylene glycol, 0.4 part of PEG-40 hydrogenated castor oil,
mixing the above fructus Piperis extract with 1, 3-propylene glycol and PEG-40 hydrogenated castor oil, and dissolving to obtain mixed solution;
adding nicotinamide and rhizoma Polygoni Cuspidati extract into the mixed solution, and stirring to obtain skin care composition.
Comparative example 5
Weighing the following raw materials in parts by weight:
VC ethyl ether 0.2 weight parts, giant knotweed rhizome extract 8.2 weight parts, pepper extract 0.3 weight parts, 1, 3-propylene glycol 7.5 weight parts, PEG-40 hydrogenated castor oil 0.6 weight parts,
mixing the above fructus Piperis extract with 1, 3-propylene glycol and PEG-40 hydrogenated castor oil, and dissolving to obtain mixed solution;
adding VC ethyl ether and rhizoma Polygoni Cuspidati extract into the mixed solution, and stirring to obtain skin care composition.
Efficacy evaluation test
Experiment for eliminating free radicals in vitro
1. Experimental methods
(1) DPPH free radical (DPPH) scavenging experiments
DPPH is a very stable nitrogen-centered radical, is very stable in organic solvents, is purple in color, has a characteristic absorption peak at 517nm, and when it encounters a radical scavenger, the lone electron of DPPH is paired, resulting in a lighter color and a lower absorbance at the maximum absorption wavelength. Therefore, the effect of removing DPPH can be evaluated by measuring the change in absorbance.
20mg of DPPH (Sigma Co.) was weighed out accurately, and the volume was adjusted to a 250ml volumetric flask using absolute ethanol to obtain a 20mmol/L DPPH solution, and the compositions prepared in example 4 and comparative example were diluted with distilled water to obtain test solutions having different concentrations, respectively. Respectively taking 2ml of test solution with different concentrations and 2ml of 20mmol/L DPPH, uniformly mixing, reacting for 30min, measuring the change of absorbance at the wavelength of 517nm, replacing a contrast solvent with absolute ethyl alcohol, and calculating the inhibition rate according to the following formula.
Inhibition (%) = [1- (Ai-Aj)/Ac ] × 100.
In the formula, Ai is the absorbance of a mixed solution consisting of 2ml of DPPH solution and 2ml of test solutions with different concentrations; aj is the absorbance of a mixed solution consisting of 2ml of test solutions with different concentrations and 2ml of absolute ethyl alcohol; ac was the absorbance of a mixture of 2ml of DPPH solution and 2ml of absolute ethanol.
(2) Hydroxy radical (. OH) scavenging experiments
The hydroxyl free radical is the most active free radical in active oxygen, can almost react with any biomacromolecule in living cells, has extremely high reaction speed, and is the free radical which has the greatest harm to organisms. The clearance rate of the hydroxyl radical is determined by measuring the product obtained by salicylic acid capturing the hydroxyl radical, and if a substance with the function of clearing the hydroxyl radical is added into the reaction system, the absorbance value of the reaction liquid can be reduced. The amount of hydroxyl radicals and the ability of the substance to be determined to scavenge hydroxyl radicals can therefore be described spectrophotometrically. The specific experimental process is as follows:
The compositions prepared in the above examples and comparative examples were diluted 50-fold. Hydroxyl radicals are generated by the Fenton reaction, OH oxidizes salicylic acid to generate 2, 3-dihydroxybenzoic acid with characteristic absorption at 510nm, and the OH clearance is determined by measuring the product obtained by capturing OH with salicylic acid. 3ml of 2mmol/L FeSO4 and 3ml of 1mmol/L H2O2 were added to a 25ml colorimetric cylinder, shaken, then 3ml of 6mmol/L salicylic acid was added, shaken, heated in a water bath at 37 ℃ for 15min, taken out, and the absorbance A0 was measured. Then adding the above composition with concentration of 2% 0.2ml, 0.4ml, 0.6ml, 0.8ml and 1.0ml respectively, then adding distilled water 0.8ml, 0.6ml, 0.4ml, 0.2ml and 0ml respectively, shaking, heating in water bath for 15min, taking out and measuring absorbance Ax. In order to eliminate the decrease of absorbance value of the system caused by adding 1.0ml of the composition and distilled water, the same method is adopted, the absorbance value A00 is measured after keeping the temperature for 15min, then 1ml of distilled water is added, the absorbance Axx is measured after shaking up, and the decrease of A is A00-Axx.
The composition has the following clearance rate to OH: OH clearance (%) =100(a 0-Ax-a decrease)/a 0.
(3) Superoxide anion radical scavenging experiment
Taking 4.5ml of 0.05mol/L Tris-HCl buffer solution with pH 8.2, placing the solution in a water bath at 25 ℃ for preheating for 20min, respectively adding 1ml of the compositions prepared in the above examples and comparative examples and 0.4ml of 25mmol/L pyrogallol solution, uniformly mixing, reacting in the water bath at 25 ℃ for 5min, adding 1.0ml of 8mol/L HCl to terminate the reaction, taking the Tris-HCl buffer solution as a reference, measuring absorbance at 299nm, and calculating the clearance rate. Blank controls replaced the sample with 1ml of deionized water and three replicates for each treatment.
Formula for calculating clearance: superoxide anion radical clearance (%) =100(a1-a2)/a1, wherein a1 is the average absorbance of the blank and a2 is the average absorbance of the whitening composition.
2. The results of the experiment are shown in FIG. 1.
The results shown in the figure demonstrate that the examples of the present invention have a certain scavenging capacity for DPPH, hydroxyl radicals and superoxide anion radicals. The inventors repeated the above experiments with other examples to arrive at the same conclusion.
Example 5 preparation of whitening emulsion
Raw materials and dosage
Name (R) Standard Chinese name Amount (wt%)
Example 1 preparation of whitening composition —— 0.5
Carbomer 940 Carbomer 0.5
Glycerol Glycerol 1.0
MONTANOV 68 Cetearyl alcohol/coco glucoside 0.5
Crodamol™ GTEH Glycerol tri (ethylhexanoate) ester 1.0
Cutina PES Pentaerythritol distearate 0.1
KF-995 Cyclopenta dimethyl siloxane 1.0
EDTA disodium salt EDTA disodium salt 0.01
Sodium hydroxide Sodium hydroxide 0.1
Microcare®PHDG Phenoxyethanol/caprylyl glycol/decyl glycol 0.4
Water (W) Water (W) 94.89
The preparation method comprises the following steps:
(1) adding water, carbomer, glycerol and EDTA disodium into an emulsification tank, heating to 80-85 ℃, and uniformly stirring;
(2) adding cetearyl alcohol/coco glucoside, glycerol tri (ethyl hexanoate), pentaerythritol distearate, and cyclopenta dimethyl silicone into an oil phase tank, heating to 80-85 deg.C, and stirring;
(3) pumping the oil phase in the oil phase tank into an emulsification tank, starting homogenization at 2500rpm for 3 min.
(4) Cooling to 45 ℃, and adding sodium hydroxide;
(5) the whitening composition prepared in example 1 and phenoxyethanol/caprylyl glycol/decanediol were added and stirred well.
Example 6 preparation of whitening emulsion
Raw materials and dosage
Name (R) Standard Chinese name Amount (wt%)
Example 2 preparation of whitening composition —— 10
Carbomer 940 Carbomer 0.25
Glycerol Glycerol 5.0
MONTANOV 68 Cetearyl alcohol/coco glucoside 3.0
Crodamol™ GTEH Glycerol tri (ethylhexanoate) ester 3.5
Cutina PES Pentaerythritol distearate 0.5
KF-995 Cyclopenta dimethyl siloxane 1.0
EDTA disodium salt EDTA disodium salt 0.1
Sodium hydroxide Sodium hydroxide 0.04
Microcare®PHDG Phenoxyethanol/caprylyl glycol/decyl glycol 0.8
Water (W) Water (W) 75.81
The preparation method comprises the following steps:
(1) adding water, carbomer, glycerol and EDTA disodium into an emulsification tank, heating to 80-85 ℃, and uniformly stirring;
(2) adding cetearyl alcohol/coco glucoside, glycerol tri (ethyl hexanoate), pentaerythritol distearate, and cyclopenta dimethyl silicone into an oil phase tank, heating to 80-85 deg.C, and stirring;
(3) pumping the oil phase in the oil phase tank into an emulsification tank, starting homogenization at 3500rpm for 5 min.
(4) Cooling to 55 deg.C, and adding sodium hydroxide;
(5) the whitening composition prepared in example 2 and phenoxyethanol/caprylyl glycol/decanediol were added and stirred well.
Example 7 whitening emulsion preparation
Raw materials and dosage:
name (R) Standard Chinese name Amount (wt%)
Example 3 preparation of whitening composition —— 20
Carbomer 940 Carbomer 0.1
Glycerol Glycerol 10
MONTANOV 68 Cetearyl alcohol/coco glucoside 5
Crodamol™ GTEH Glycerol tri (ethylhexanoate) ester 5
Cutina PES Pentaerythritol distearate 2
KF-995 Cyclopenta dimethyl siloxane 5
EDTA disodium salt EDTA disodium salt 0.1
Sodium hydroxide Sodium hydroxide 0.02
Microcare®PHDG Phenoxyethanol/caprylyl glycol/decyl glycol 1.0
Water (W) Water (W) 51.78
The preparation method comprises the following steps:
(1) adding water, carbomer, glycerol and EDTA disodium into an emulsification tank, heating to 80-85 ℃, and uniformly stirring;
(2) Adding cetearyl alcohol/coco glucoside, glycerol tri (ethyl hexanoate), pentaerythritol distearate, and cyclopenta dimethyl silicone into an oil phase tank, heating to 80-85 deg.C, and stirring;
(3) pumping the oil phase in the oil phase tank into an emulsification tank, starting homogenization at 6000rpm for 10 min.
(4) Cooling to 60 deg.C, and adding sodium hydroxide;
(5) the whitening composition prepared in example 3 and phenoxyethanol/caprylyl glycol/decanediol were added and stirred well.
Example 8 preparation of whitening emulsion
Raw materials and dosage:
name (R) Standard Chinese name Amount (wt%)
Example 4 preparation of whitening composition —— 12
Carbomer 940 Carbomer 0.2
Glycerol Glycerol 6
MONTANOV 68 Cetearyl alcohol/coco glucoside 2
Crodamol™ GTEH Glycerol tri (ethylhexanoate) ester 2
Cutina PES Pentaerythritol distearate 0.5
KF-995 Cyclopenta dimethyl siloxane 2
EDTA disodium salt EDTA disodium salt 0.03
Sodium hydroxide Sodium hydroxide 0.04
Microcare®PHDG Phenoxyethanol/caprylyl glycol/decyl glycol 0.5
Water (W) Water (W) 74.73
The preparation method comprises the following steps:
(1) adding water, carbomer, glycerol and EDTA disodium into an emulsification tank, heating to 80-85 ℃, and uniformly stirring;
(2) adding cetearyl alcohol/coco glucoside, glycerol tri (ethyl hexanoate), pentaerythritol distearate, and cyclopenta dimethyl silicone into an oil phase tank, heating to 80-85 deg.C, and stirring;
(3) Pumping the oil phase in the oil phase tank into an emulsification tank, starting homogenization at 5000rpm, and homogenizing for 5 min.
(4) Cooling to 50 deg.C, and adding sodium hydroxide;
(5) the whitening composition prepared in example 4 and phenoxyethanol/caprylyl glycol/decanediol were added and stirred well.
Comparative example 6
The procedure was as in example 8 except that the whitening composition was not added.
Efficacy testing
First, red melanin, skin tone and red blood streak test
The test is carried out by adopting a single-center, random, double-blind and self-face left-right contrast method, and 38 testees with dark yellow skin color are screened for test. The tested lotion is used by the tested subject on the left face and the right face respectively within 6 weeks in the morning and evening, and the dosage is based on the actual dosage required for applying the tested lotion on the face. VISIA-CR was taken as a facial image and MX18 instrumental measurement 3 times before and at weeks 2 and 6 after the start of the test. Before each test, a subject needs to clean the face with clear water and then sits in a room with constant temperature and humidity for 30min, the face cannot be wiped with paper, and the test is carried out after the face is naturally dried; analyzing the improvement condition of the facial erythema and melanin of the subjects through the measurement result of the MX18 instrument; the results of the VISIA-CR skin test were used to analyze the skin color and red blood streak improvement before and after the subjects used the lotion.
1. Melanin content MI value
The experimental method comprises the following steps: the melanin content MI values were measured 3 times in the cheek regions of the subjects at weeks 0, 2 and 6, respectively, and averaged.
The apparatus used was: mexameter MX18
And (3) testing period: 6 weeks
The results of the experiment are as follows:
average value of melanin content Example 5 Example 6 Example 7 Example 8 Comparative example 6
Week 0 125 134 139 137 143
Week 2 121 132 132 129 140
Week 6 110 126 108 102 135
Rate of change of melanin content Example 5 Example 6 Example 7 Example 8 Comparative example 6
Week 2 -3.20% -1.49% -5.04% -5.84% -2.10%
Week 6 -12.00% -5.97% -22.30% -25.55% -5.59%
2. EI value of red pigment content
The experimental method comprises the following steps: at weeks 0, 2 and 6, 3 measurements of the EI value of the red pigment content were made in the cheek regions of the subjects, and averaged.
The apparatus used was: mexameter MX18
The results of the experiment are as follows:
red pigment contentMean value of Example 5 Example 6 Example 7 Example 8 Comparative example 6
Week 0 236 240 239 228 225
Week 2 239 241 236 224 227
Week 6 224 233 217 203 222
Rate of change of red pigment content Example 5 Example 6 Example 7 Example 8 Comparative example 6
Week 2 1.27% 0.42% -1.26% -1.75% 0.89%
Week 6 -5.08% -2.92% -9.21% -10.96% -1.33%
The results show that the embodiment of the invention obviously improves the contents of skin melanin and red pigment.
3. Skin tone and redness testing
The experimental method comprises the following steps: VISIA-CR was used to observe the skin color and red blood streak improvement in subjects at 0 week 2 week 6 week.
The apparatus used was: VISIA-CR skin tester
Introduction of corresponding light sources:
integral skin color evenness: standard Natural light 2
Red blood streak: red Areas Red region
And (3) testing period: 6 weeks
And (3) testing a sample: example 8, comparative example 6 emulsions
The results of the experiments are shown in FIGS. 2-5.
The VISIA picture results show that the skin-care lotion has a certain effect of improving the skin color condition and the red blood streak of a subject in the example 8, and the skin-care lotion prepared by the inventor in other examples achieves the same effect.
Second, oil secretion test
In addition, the inventor also finds that the whitening emulsion has a certain inhibiting effect on skin oil secretion, so that 30 subjects with relatively strong skin oil secretion are screened out and divided into 2 groups, and each group contains 15 persons; the test samples were used face-wide using a single-center, randomized, double-blind, placebo-controlled approach. One group used the sample of example 8 and the other group used the sample of comparative example 6, each once a day, in the morning and evening, based on the amount actually required for applying to the face. VISIA-CR was taken 3 times before the start of the test and at weeks 2 and 6 after the start of the test. Before each test, a subject needs to clean the face with clear water, sits still in a room with constant temperature and humidity for 30min, cannot wipe the face with paper, and shoots the face with a VISIA-CR skin tester after naturally drying; the results of the VISIA-CR skin test were used to analyze the oil secretion before and after the application of the emulsion to the subjects.
The apparatus used was: VISIA-CR skin tester
Introduction of corresponding light sources:
oil secretion: porphyrin light
And (3) testing period: 6 weeks
Results of the experiment
As can be seen from the results of VISIA images, example 8 exhibited a certain improvement effect on the secretion of fats of the subjects, whereas comparative example 6 exhibited a poor improvement effect on the secretion of fats.
The skin care emulsion disclosed by the invention realizes the integral whitening effect by adding the whitening composition, is safe and non-irritant, and has a wide application prospect in the field of skin care products.

Claims (10)

1. The whitening emulsion comprises the following raw materials in parts by weight: carbomer, glycerin, cetostearyl alcohol/cocoyl glucoside, glycerol tri (ethyl hexanoate), pentaerythritol distearate, cyclopentadimethylsiloxane, disodium EDTA, sodium hydroxide, and a whitening composition comprising niacinamide, polygonum cuspidatum extract, and pepper extract.
2. The whitening emulsion of claim 1, wherein the ingredients are present in an amount, based on the total weight of the emulsion, of: 0.1-0.5wt% of carbomer, 1.0-10.0 wt% of glycerol, 0.5-5.0 wt% of cetearyl alcohol/coco glucoside, 1.0-5.0 wt% of glycerol tri (ethyl hexanoate), 0.1-2.0 wt% of pentaerythritol distearate, 1.0-5.0 wt% of cyclopenta dimethyl silicone, 0.01-0.1 wt% of disodium EDTA, 0.02-0.1 wt% of sodium hydroxide and 0.5-20.0 wt% of the whitening composition.
3. The whitening emulsion of claim 2, wherein the ingredients are present in an amount, based on the total weight of the emulsion, of: 0.2-0.4wt% carbomer, 3.0-7.0 wt% glycerin, 2.0-4.0wt% cetearyl alcohol/coco glucoside, 1.0-3.5 wt% glyceryl tri (ethyl hexanoate), 0.5-2.0 wt% pentaerythritol distearate, 1.0-3.0 wt% cyclopenta dimethyl siloxane, 0.02-0.05wt% disodium EDTA, 0.04-0.08 wt% sodium hydroxide, and 5.0-15 wt% of the whitening composition.
4. The whitening emulsion according to claim 2 or 3, wherein the whitening emulsion comprises the following raw materials in parts by weight based on the total weight of the whitening composition: 1-10 parts of nicotinamide, 0.01-5 parts of giant knotweed extract and 0.01-0.2 part of pepper extract.
5. The whitening emulsion of claim 4, wherein the whitening composition comprises the following raw materials in parts by weight: 2-6 parts of nicotinamide, 0.1-4 parts of giant knotweed extract and 0.1-0.2 part of pepper extract.
6. The whitening emulsion of claim 5, wherein the whitening composition further comprises 1, 3-propanediol and/or PEG-40 hydrogenated castor oil.
7. The whitening emulsion of claim 6, wherein the whitening composition comprises the following raw materials in parts by weight based on the total weight of the whitening composition: 1-10 parts of nicotinamide, 0.01-5 parts of giant knotweed extract, 0.01-0.2 part of pepper extract, 0.01-5 parts of 1, 3-propylene glycol and 0.02-0.5 part of PEG-40 hydrogenated castor oil.
8. The whitening emulsion of claim 7, wherein the whitening composition comprises the following raw materials in parts by weight: 2-6 parts of nicotinamide, 0.1-4 parts of giant knotweed rhizome extract, 0.1-0.2 part of pepper extract, 0.25-5 parts of 1, 3-propylene glycol and 0.2-0.4 part of PEG-40 hydrogenated castor oil.
9. The whitening emulsion of any one of claims 6-8, wherein the whitening composition is prepared by a method comprising:
(1) mixing the pepper extract with 1, 3-propylene glycol and PEG-40 hydrogenated castor oil, and dissolving to obtain mixed solution;
(2) adding nicotinamide and giant knotweed rhizome extract into the mixed solution obtained in the step (1), and uniformly stirring.
10. A method of preparing the whitening emulsion of any one of claims 1-9, comprising the steps of:
(1) adding water, carbomer, glycerol and EDTA disodium into an emulsification tank, heating to 80-85 ℃, and uniformly stirring;
(2) adding cetearyl alcohol/coco glucoside, glycerol tri (ethyl hexanoate), pentaerythritol distearate, and cyclopenta dimethyl silicone into an oil phase tank, heating to 80-85 deg.C, and stirring;
(3) pumping the oil phase in the oil phase tank into an emulsification tank, homogenizing at 2500-;
(4) Cooling to 45-60 ℃, and adding sodium hydroxide;
(5) adding the whitening composition, and stirring uniformly.
CN202010287733.3A 2020-04-13 2020-04-13 Whitening emulsion and preparation method thereof Pending CN113520902A (en)

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