CN115300437B - Moisturizing and anti-aging skin care composition and preparation method and application thereof - Google Patents

Moisturizing and anti-aging skin care composition and preparation method and application thereof Download PDF

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CN115300437B
CN115300437B CN202210815615.4A CN202210815615A CN115300437B CN 115300437 B CN115300437 B CN 115300437B CN 202210815615 A CN202210815615 A CN 202210815615A CN 115300437 B CN115300437 B CN 115300437B
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moisturizing
skin care
care composition
mixture
parts
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CN115300437A (en
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黄斌斌
谢明宏
唐妍娟
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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]
    • A61K8/9794Liliopsida [monocotyledons]
    • 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
    • A61K2800/59Mixtures
    • A61K2800/592Mixtures of compounds complementing their respective functions
    • A61K2800/5922At least two compounds being classified in the same subclass of A61K8/18
    • 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
    • A61K2800/805Corresponding aspects not provided for by any of codes A61K2800/81 - A61K2800/95
    • 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
    • A61K2800/82Preparation or application process involves sonication or ultrasonication

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  • Life Sciences & Earth Sciences (AREA)
  • Veterinary Medicine (AREA)
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  • Cosmetics (AREA)

Abstract

The application discloses a moisturizing and anti-aging skin care composition, and a preparation method and application thereof, wherein the skin care composition comprises the following components in parts by weight: 20-50 parts of hops, 20-40 parts of longan fruits, 10-30 parts of buddleia officinalis, 10-20 parts of radix peucedani, and 5-20 parts of vetiver roots; the application has remarkable capability of inhibiting hyaluronidase, and can relieve skin inflammation injury to a certain extent when acting on skin; the skin color is lightened while moisturizing, and the dark yellow skin is improved; the components have good synergistic effect, can better lock the moisture of skin and reduce the water diversion, thereby achieving the effect of moisturizing.

Description

Moisturizing and anti-aging skin care composition and preparation method and application thereof
Technical Field
The application relates to the technical field of skin care compositions, in particular to a moisturizing and anti-aging skin care composition, and a preparation method and application thereof.
Background
Skin is the largest organ of the human body, has barrier, absorption, secretion, excretion, metabolism, immunity, thermoregulation and sensory functions, and care of skin is an indispensable problem in daily life. The most prominent problem of skin is that it causes a series of skin problems such as dryness, roughness, itching, allergy, spots, wrinkles and the like of the skin with age and season changes, and skin moisturizing is of great importance;
the prior Chinese patent with publication number of CN112641671A discloses a moisturizing composition and a preparation process thereof, wherein the moisturizing composition comprises the following components in parts by weight: 25-30 parts of water, 10-40 parts of glycerol and polyether-26 parts of glycerol: 10-25 parts of panthenol, 1-10 parts of panthenol, 0.5-3 parts of PCA sodium, 0.01-1 part of thickening agent, 0.01-1 part of neutralizer, 0-0.5 part of essence and 0.1-1 part of preservative. The preparation process is simple, the prepared moisturizing composition is low in cost and high in operability, has excellent effects in improving wrinkled skin lines, improving skin hydration degree, improving skin roughness, improving skin uniformity and the like, and can improve the whitening and moisturizing functions of skin after long-term use, so that the skin has luster and elasticity; wherein, the added panthenol and PCA sodium can effectively improve the defects of dark complexion, roughness and matt skin; the added glycerol polyether-26 can enhance the effects of moisturizing, whitening, brightening and removing wrinkles and resisting aging of the product;
the prior Chinese patent publication No. CN114010524A discloses a moisturizing composition for cosmetics, which comprises the following raw materials in percentage by mass: 5.5 to 7.5 percent of glyceroglycosides, 0.8 to 2 percent of ectoin, 3.0 to 5.5 percent of citrulline and the balance of water. The application has the characteristics of good air permeability, short-term improvement of skin moisture content and instant wrinkle reduction;
at present, the moisturizing products including the cosmetics are difficult to realize the sustainable moisturizing effect, and the moisturizing effect can be realized only by continuous use, so that the moisturizing products rebound quickly after stopping; therefore, the development of the cosmetic with continuous and effective moisturizing effect has practical significance and broad market prospect.
Disclosure of Invention
The application aims to provide a moisturizing and anti-aging skin care composition, and a preparation method and application thereof, so as to solve the problems that the existing moisturizing product is difficult to realize a continuous moisturizing effect, the moisturizing effect can be realized only by continuous use, and the moisturizing effect rebounds soon after stopping.
In order to achieve the above purpose, the present application provides the following technical solutions: the moisturizing and anti-aging skin care composition comprises the following components in parts by weight: 20 to 50 parts of hops, 20 to 40 parts of longan fruits, 10 to 30 parts of buddleia officinalis, 10 to 20 parts of root of peucedanum praeruptorum, and 5 to 20 parts of vetch root.
Wherein the hop extraction part is petals, the dried leaves of the hop are removed She Maohou, and the place of production is Shandong; the longan fruit extraction part is fruit, and the production place is Guangdong; the extraction part of the buddleja officinalis is leaves, and the production place is Hubei; the root of the peucedanum praeruptorum dunn is the root, and the producing area is Sichuan; the root of vetiver is the root, and the origin is Fujian.
A method for preparing a moisturizing and anti-aging skin care composition, comprising the steps of:
step 1, raw material pretreatment, namely respectively crushing hops, longan fruits, buddleja officinalis, white flower peucedanum root and vetiver root, uniformly mixing the crushed hops, longan fruits, buddleja officinalis and Hu Genhe vetiver root before white flowers to obtain a raw material mixture for later use;
step 2, adding the raw material mixture obtained in the step 1 into 85% ethanol, carrying out reflux extraction for 35-55 minutes at 55-75 ℃, cooling to 42-52 ℃, and carrying out vacuum suction filtration by using a-0.05-0.1 mpa circulating water type multipurpose vacuum pump and a glass crucible to obtain a clear mixture;
step 3, repeating the operation of the step 2;
step 4, injecting the clarified mixture obtained after the suction filtration in the step 2 and the step 3 into a rotary steaming bottle, and rotary steaming all ethanol at the temperature of 85-100 ℃ to obtain a mixture solid;
step 5, adding the mixture solid obtained in the step 4 into an ultrasonic extractor, weighing a solvent, adding the solvent into the ultrasonic extractor, stirring at a speed of 30-45 r/min, soaking for 20-40 min, then starting heating to 70-95 ℃, setting the ultrasonic frequency to 350-450W, setting the working frequency to 6-10 KHz, and setting the ultrasonic extraction time to 60-100 min;
step 6, after ultrasonic extraction is finished, cooling to 45-65 ℃, and filtering with 200-300 mesh filter cloth to a storage tank to obtain a mixed solution I for later use;
step 7, collecting and mixing filter residues obtained in the step 3, adding deionized water, adding 0.1-0.5% of special enzyme for plant extraction, setting the pH to be 4.0-5.0, setting the temperature to be 45-52 ℃, carrying out enzymolysis for 240-360 minutes, inactivating the enzyme at the temperature of 90-100 ℃ for 20-30 minutes after the enzymolysis is finished, and filtering by using 200-300 meshes of filter cloth to obtain an enzyme treatment mixture II for later use;
step 8, mixing the filter residue obtained by enzymolysis with a solvent according to the mass ratio of 1:10-30, placing the mixture into a water bath at 75-95 ℃ for extraction for 150-210 minutes to obtain a filter residue extracting solution, cooling the filter residue extracting solution to 42-52 ℃, and filtering the filter residue extracting solution with a 200-300-mesh filter cloth to obtain a mixture III for later use;
step 9, repeating the operation of the step 8, and repeating the water bath extraction once to obtain a mixture IV for standby;
step 10, combining and mixing the mixture II, III, IV, and then diluting with deionized water, wherein the dilution ratio is as follows: 1:3-1:10 to obtain a mixture V;
step 11, mixing the mixture I, V together, and concentrating by using a rotary evaporator to obtain a concentrated mixture, namely the moisturizing and anti-aging skin care composition.
Wherein, in the step 1, crushed hops, longan fruits, buddleja officinalis flowers and Hu Genhe rock orchid roots before white flowers are filtered through a 80-250 mesh sieve.
In the step 2, the mass fraction ratio of the raw material mixture to the ethanol is 1:10-1:20.
Wherein in step 5, the mass ratio of the mixture solid and the solvent is 1:30.
In the step 5, the solvent is one or more of butanediol, propylene glycol, glycerol and 1, 2-hexanediol, deionized water is added into the solvent, and the mass ratio of the solvent to the deionized water is 1:1-1:10.
In the step 7, the mass ratio of the filter residue to the deionized water is 1:10-1:50.
Wherein in the step 7, the plant extraction special enzyme consists of 1 ten thousand U/g cellulase, 1 ten thousand U/g hemicellulase, 3 ten thousand U/g glucanase, 1 ten thousand U/g pectinase and 1 ten thousand U/g papain.
Wherein in step 8, the solvent is one or more of butanediol, glycerol and 2, 3-butanediol.
The application of the moisturizing and anti-aging skin care composition is that the moisturizing and anti-aging skin care composition is mixed with one of common toning lotion, essence, face cream, eye cream and emulsion to obtain the skin care product with moisturizing and anti-aging effects, wherein the addition amount of the moisturizing and anti-aging skin care composition is 1-10% of the weight of the skin care product.
Among them, solvent butanediol producing area Japanese Kagaku Kogyo Co., ltd. (DAICEL CORPORATION); 2, 3-butanediol producing area Shandong Qingzhixing Biotechnology Co., ltd; glycerol production area: sco brown chemical (Zhangjihong Kong) Co., ltd; propylene glycol production site SKC PICGLOBAL co., ltd; deionized water: EDI ultrapure water is self-produced; special enzyme for plant extraction (Nanning east Henghua channel Biotechnology Co., ltd.).
Wherein, the preparation equipment is as follows: ultrasonic extractor (model: SCIENTZ-5T, purchase Ningbo new Zhi Biotech Co., ltd.), circulating water type multipurpose vacuum pump (model: SHB-111, zhengzhou great wall department trade Co., ltd.), glass crucible (aperture 16-30 um, about 30 mL), CF-44 sealing swing pulverizer (fineness of finished product: 80-250 mm), rotational speed 25000r/min, zhejiang Jieqiao Jielian Innovative medical materials and instruments factory, rotary evaporator (model: RE-52A, zhengzhou reach instrument and technology Co., ltd.).
Compared with the prior art, the application has the beneficial effects that:
the moisturizing and anti-aging skin care composition prepared by the application has remarkable capability of inhibiting hyaluronidase, and can relieve skin inflammation and injury to a certain extent when acting on skin; the skin color is lightened while moisturizing, and the dark yellow skin is improved;
the moisturizing and anti-aging skin care composition prepared by the application can be applied to a facial mask, so that the moisture content of the skin can be effectively improved, wherein the components have good synergistic effect, the moisture of the skin can be better locked, and the moisture flow can be reduced, so that the moisturizing effect can be achieved;
the moisturizing and anti-aging skin care composition prepared by the application can reduce wrinkles, improve the skin roughness and the lubrication degree, and inhibit the collagenase activity and the elastase activity when applied to the cream.
Drawings
FIG. 1 shows the rate of change of skin moisture content at various time points after the application of the product of application example 1 of the present application, relative to the rate before the application.
Detailed Description
The technical scheme of the application is further described in detail below with reference to the specific embodiments, but the technical scheme is not limited in any way, and any limited modifications made by anyone within the protection scope of the application are still within the protection scope of the application. The raw materials adopted in the technical scheme provided by the application are purchased from the market through conventional means except special descriptions.
Example 1
The moisturizing and anti-aging skin care composition comprises the following components in parts by weight: 30 parts of hops, 24 parts of longan fruits, 18 parts of butterflybush flower, 13 parts of white flower peucedanum root and 15 parts of vetiver root.
Example 2
The moisturizing and anti-aging skin care composition comprises the following components in parts by weight: 50 parts of hops, 20 parts of longan fruits, 12 parts of buddleia officinalis, 12 parts of white flower peucedanum root and 6 parts of vetiver root.
Example 3
The moisturizing and anti-aging skin care composition comprises the following components in parts by weight: 20 parts of hops, 40 parts of longan fruits, 25 parts of butterflybush flower, 10 parts of white flower peucedanum root and 5 parts of vetiver root.
Example 4
The moisturizing and anti-aging skin care composition comprises the following components in parts by weight: 25 parts of hops, 25 parts of longan fruits, 30 parts of butterflybush flowers, 13 parts of white flower peucedanum roots and 7 parts of vetiver roots.
Example 5
The moisturizing and anti-aging skin care composition comprises the following components in parts by weight: 40 parts of hops, 28 parts of longan fruits, 15 parts of butterflybush flower, 11 parts of white flower peucedanum root and 6 parts of vetiver root.
Examples 1-5 were prepared using the following preparation examples, the components in each example being different in parts by weight, the specific preparation method being as follows:
a method for preparing a moisturizing and anti-aging skin care composition, comprising the steps of:
step 1, raw material pretreatment, namely respectively crushing hops, longan fruits, buddleja officinalis, white flower peucedanum root and vetiver root, uniformly mixing the crushed hops, longan fruits, buddleja officinalis and Hu Genhe vetiver root before white flowers to obtain a raw material mixture for later use;
step 2, adding the raw material mixture obtained in the step 1 into 85% ethanol, carrying out reflux extraction for 40 minutes at 60 ℃, cooling to 48 ℃, and carrying out vacuum suction filtration by using a-0.01 mpa circulating water type multipurpose vacuum pump and a glass crucible to obtain a clear mixture;
step 3, repeating the operation of the step 2;
step 4, injecting the clarified mixture obtained after suction filtration in the step 2 and the step 3 into a rotary steaming bottle, and rotary steaming all ethanol at 90 ℃ to obtain a mixture solid;
step 5, adding the mixture solid obtained in the step 4 into an ultrasonic extractor, weighing a solvent, adding the solvent into the ultrasonic extractor, stirring at a speed of 40 revolutions per minute, soaking for 30 minutes, then starting heating to 85 ℃, setting the ultrasonic frequency to 400W, setting the working frequency to 8KHz, and performing ultrasonic extraction for 90 minutes;
step 6, after ultrasonic extraction is finished, cooling to 55 ℃, and filtering with 250-mesh filter cloth to a storage tank to obtain a mixed solution I for later use;
step 7, collecting and mixing filter residues obtained in the suction filtration of the step 3, adding deionized water, adding 0.3% of special enzyme for plant extraction, setting the pH value to be 4.0, carrying out enzymolysis for 300 minutes at 48 ℃, inactivating the enzyme at 95 ℃ for 25 minutes after the enzymolysis is finished, and filtering with a 250-mesh filter cloth to obtain an enzyme treatment mixture II for later use;
step 8, mixing the filter residue obtained by enzymolysis with a solvent according to the mass ratio of 1:15, extracting in a water bath at 85 ℃ for 200 minutes to obtain a filter residue extracting solution, cooling the filter residue extracting solution to 48 ℃, and filtering with a 250-mesh filter cloth to obtain a mixture III for later use;
step 9, repeating the operation of the step 8, and repeating the water bath extraction once to obtain a mixture IV for standby;
step 10, combining and mixing the mixture II, III, IV, and then diluting with deionized water, wherein the dilution ratio is as follows: 1:6 to obtain a mixture V;
step 11, mixing the mixture I, V together, and concentrating by a rotary evaporator to obtain a concentrated mixture, namely the moisturizing and anti-aging skin care composition.
Comparative example 1
Compared with example 1, the hop is replaced by deionized water, and the content and the process of other components are unchanged.
Comparative example 2
Compared with example 1, the longan fruit is replaced by hops, and the content and the process of other components are unchanged.
Comparative example 3
Compared with the example 1, the buddleja officinalis, the white flower front Hu Genyong longan fruits and the hops are replaced, and the content and the process of other components are unchanged.
Comparative example 4
Compared with example 1, the preparation method does not contain buddleja officinalis, and is replaced by longan fruits, and the content and the process of other components are unchanged.
Comparative example 5
Compared with the example 1, the buddleja officinalis and vetiver root are replaced by longan fruits and white flower peucedanum root, and the content and the process of other components are unchanged.
Experimental example
In order to demonstrate the technical gist of the technical scheme provided by the present application, experimental data of examples 1 to 5 and comparative examples 1 to 5 provided by the present application are given below;
1. in vitro test-test for inhibition of hyaluronidase Activity
1.1, test principle:
hyaluronidase (HAase) can hydrolyze sodium hyaluronate indiscriminately to obtain the product beta-N-acetylglucosamine, which can be condensed with borate under alkaline condition to generate chromogen, and chromogen and p-dimethylaminobenzaldehyde are chromogenic under acidic condition. In this test, the enzyme reaction is limited by inhibiting the activity of hyaluronidase by adding an analyte. In view of the conjugation effect of the generation system, the absorption wavelength at the maximum absorbance is used as the optimal selection wavelength, and the inhibition efficiency of the test substance on the hyaluronidase is reflected by examining the change of absorbance.
1.2 Experimental procedure
(1) Reagent set-up
Acetic acid buffer (pH 3.5), 0.5% sodium hyaluronate, 100U/ml hyaluronidase, 0.1% sodium hydroxide, 0.1% sodium borate, 1% centella asiatica extract, 0.1mol/L p-dimethylaminobenzaldehyde
(2) A, receiving a sample: the test examples 1 to 5 and comparative examples 1 to 5 were diluted with acetic acid buffer to 1% concentration samples, respectively; adding 0.5ml of hyaluronidase, 0.5ml of sample, 0.5ml of sodium hyaluronate, 0.1ml of sodium hydroxide and 0.5ml of sodium borate into a test tube respectively, shaking uniformly, and dripping 1ml of 0.1mol/L of p-dimethylaminobenzaldehyde; the samples were transferred to 96-well plates in a water bath at 37℃for 30min, and absorbance at 582nm was measured.
(3) A subject blank control: to the test tube, 0.5ml of acetic buffer, 0.5% sodium hyaluronate, 100U/ml hyaluronidase, 0.1% sodium hydroxide and 0.1% sodium borate were added, respectively, and the mixture was shaken well, 1ml of p-dimethylaminobenzaldehyde (0.1 mol/L) was added dropwise thereto, and the mixture was prevented from being transferred to a 96-well plate at 30℃for 30 minutes, and the absorbance at 582nm was measured.
(4) B negative control: 0.5ml of centella asiatica extract, 0.5ml of hyaluronidase, 0.5ml of sample, 0.5ml of sodium hyaluronate, 0.1ml of sodium hydroxide and 0.5ml of sodium borate are added into a test tube respectively, and are sufficiently shaken, 1ml of 0.1mol/L of p-dimethylaminobenzaldehyde is added dropwise, the mixture is prevented from being transferred to a 96-well plate at 30 ℃ for 30min, and the absorbance at 582nm is measured.
(5) B negative blank control: to the test tube, 0.5ml of acetic buffer, 0.5% sodium hyaluronate, 100U/ml hyaluronidase, 0.1% sodium hydroxide and 0.1% sodium borate were added, respectively, and the mixture was shaken well, 1ml of p-dimethylaminobenzaldehyde (0.1 mol/L) was added dropwise thereto, and the mixture was prevented from being transferred to a 96-well plate at 30℃for 30 minutes, and the absorbance at 582nm was measured.
1.3, the calculation formula of the hyaluronidase activity inhibition rate (1) is as follows:
1.4, results of the test data are shown in Table 1, which shows the inhibition rate of hyaluronidase activity
TABLE 1 inhibition of hyaluronidase Activity
1.5 conclusion
From the results shown in Table 1, the inhibition rate of hyaluronidase for examples 1-5 was about 52.9% or more, and the inhibition rate of hyaluronidase for comparative examples 1-5 was about 21.5% or less, and the inhibition rate of hyaluronidase for examples 1-5 was about 2 times that for the blank control, as compared with the negative control; the higher the inhibition rate is obtained through experimental data analysis, the better the anti-allergic and anti-inflammatory effects are. From Table 1, the moisturizing and skin-care composition provided by the application has remarkable hyaluronidase inhibition capability, which shows that the moisturizing and skin-care composition has good anti-allergic and anti-inflammatory activities, and can relieve inflammatory injuries of skin to a certain extent when acting on the skin.
2. In vitro test-free radical scavenging test
Examples 1-5 and comparative examples 1-5 were validated against Shanghai household chemical industry Association group Standard T/SHRH 006-2018 cosmetic-free radical (DPPH) scavenging Experimental methods.
2.1, test principle:
1, 1-diphenyl-2-trinitrophenylhydrazine (DPPH for short) is a stable long-life free radical, and the ethanol solution is dark purple and has strong absorption near 517 nm. When a free radical scavenger exists, the light absorption of the DPPH ethanol solution is weakened due to the single electron pairing with the free radical scavenger. The degree of discoloration of the DPPH ethanol solution is in a linear relation with the number of electrons received by the DPPH ethanol solution, so that the test sample can be evaluated for the capability of scavenging free radicals, namely, the higher the scavenging rate is, the stronger the capability of scavenging free radicals for resisting oxidation is.
2.2 Experimental procedure
(1) Reagent preparation
Ethanol solution of DPPH: 40mg of DPPH is weighed, added with absolute ethyl alcohol for dissolution and fixed volume in a 1000mL volumetric flask, and the concentration of DPPH is prepared to be 40mg/L. The low-temperature refrigerator is preserved in dark, and the effective period is 5 days.
Liquid to be measured: the moisturizing skin-care compositions of examples 1-5 and comparative examples 1-5 were diluted to a concentration of 1.0% with phosphate buffer.
Positive control: the vitamin C was diluted to a concentration of 1.5X10-4 g/l with distilled water.
(2) Experimental method
A1 test sample group: adding 1.0mL of DPPH test solution with the mass concentration of 40mg/L and 1.0mL of sample to be tested into a test tube, supplementing the total volume to 3mL by absolute ethyl alcohol, shaking uniformly, carrying out light-shielding reaction for 30min, transferring 1.0mL into a 96-well plate, and measuring absorbance at 517nm wavelength;
a2 blank sample group: adding 2mL of absolute ethyl alcohol and 1.0mL of a sample to be detected into a test tube, shaking uniformly, carrying out light-shielding reaction for 30min, transferring 1.0mL into a 96-well plate, and measuring absorbance at 517nm wavelength;
a3 negative control group: adding 1.0mL of DPPH test solution with the mass concentration of 40mg/L and 2mL of absolute ethyl alcohol into a test tube, shaking uniformly, carrying out light-shielding reaction for 30min, taking 1mL, transferring into a 96-well plate, and measuring absorbance at 517nm wavelength;
positive control group: 1.0mL of DPPH test solution with the mass concentration of 40mg/L and 1.0mL of positive control sample are added into a test tube, the total volume is supplemented to 3mL by absolute ethyl alcohol, the test tube is uniformly shaken, the test tube reacts for 30min in a dark place, and 1.0mL of the test tube is transferred into a 96-well plate to measure absorbance at the wavelength of 517 nm.
2.3, detection results
(1) The calculation formula of the DPPH free radical clearance (2) of the sample is as follows:
(2) The test data results are shown in Table 2.
Table 2 data results
2.4 conclusion
As is clear from the test results, examples 1 to 5 have an outstanding DPPH radical scavenging ability, and the scavenging rate is about 80% or more. Compared with the examples 1 to 5, the comparative examples 1 to 5 have poorer effects, and the clearance rate reaches less than 45 percent; the protocol of examples 1-5 was about equivalent to the 1.5X10-4 g/l concentration clearance of the positive control, but about twice that of comparative examples 1,2, 3, 5; the moisturizing skin care composition disclosed by the application can be used for moisturizing, brightening skin and improving dark yellow skin.
Application example 1
The moisture-preserving skin-care composition materials of the example 1 (A) and the comparative example 1 (B) and the mask matrix are not added in the essence mask liquid formula with the moisture-preserving effect, and the test is carried out; the test formulation table 3 is as follows:
table 3A essence facial mask with moisturizing effect
Production process
(1) Weighing the raw materials of the group A, adding the raw materials into an emulsifying pot, stirring at a speed of 35-45 r/min, homogenizing at a speed of 3000r/min for 2-3 minutes to obtain semitransparent viscous liquid, heating to 83-85 ℃ under stirring, and keeping the temperature for 15-20 minutes to obtain transparent liquid;
(2) Cooling, stirring at a speed of 30-40 r/min, and vacuumizing to-0.03 mpa;
(3) Cooling to below 45 ℃, weighing the raw materials of the group B, adding the raw materials into an emulsifying pot, and stirring at the speed of 30-40 r/min for 5-8 minutes to obtain yellowish transparent viscous liquid;
(4) Weighing the raw materials of the group C, uniformly mixing in a container, preheating, dissolving and transparency in a water bath kettle at 75-78 ℃, adding into an emulsifying kettle, stirring at a speed of 30-40 r/min for 8-15 min, homogenizing at a low speed of 1000r/min for 1-3 min to obtain yellowish transparent viscous liquid;
(5) Weighing the raw materials of the group D, adding the raw materials into an emulsifying pot, and stirring at the speed of 30-40 r/min for 5-8 minutes to obtain yellowish transparent viscous liquid;
(6) Qualified physical and chemical indexes are detected, filtered by filter cloth with 200-400 meshes, and then placed in a storage tank for 24H for microorganism detection.
The internal control standard of the essence mask liquid with the moisturizing effect is as follows:
appearance: a yellowish transparent viscous liquid;
smell: rose water fragrance;
pH:5.5~6.8
viscosity: 25 ℃, the rotating speed of No. 2 is more than or equal to 800mpa;
stability: cold-resistant: the temperature is maintained for 24 hours at minus 8+/-2 ℃ and has no obvious difference from the temperature before the test after the temperature is restored to the room temperature.
Heat resistance: the temperature is kept for 24 hours at 40+/-1 ℃, and no obvious difference exists between the temperature after the temperature is restored to the room temperature and the temperature before the test.
Microorganism: colony count: less than or equal to 10FCU/g;
total number of mold and yeast: less than or equal to 10CFU/g;
heat-resistant coliform group: cannot be detected;
staphylococcus aureus: cannot be detected;
pseudomonas aeruginosa: cannot be detected;
heavy metal: mercury is less than or equal to 1mg/kg; lead is less than or equal to 10mg/kg; arsenic is less than or equal to 2mg/kg; cadmium is less than or equal to 5mg/kg.
The matching degree of the facial mask liquid and plant cotton fibers such as Xinjiang cotton fibers, mugwort leaf fibers, banana fiber cotton and the like, which are tested for 90 days, reaches 99 percent.
The essence mask liquid with the moisturizing effect is subjected to a moisturizing performance test:
the essence mask liquids of the example 1, the comparative example 1 and the mask substrate are evaluated by a 4-hour human body moisturizing test, and the skin moisture content is tested before use and after use for 1h, 2h, 3h and 4h, so that the higher the skin moisture content value is, the higher the skin moisture content is.
Volunteer requirements:
volunteer population: 24, 6 per group, female;
no cosmetic allergy history, no cosmetic is used for 3 days before use, no skin disease patient, no pregnant or lactation woman, and health;
age: 25-35 years old;
test area: forearm flexor side;
test period: 4H;
test instrument:
skin moisture content tester Corneometer (CM 825,Courage and Khazaka, germany).
Positive control:
0.05% sodium hyaluronate (molecular weight: 1.3-1.35X 105, shandong An Hua biological medicine Co., ltd.).
The testing process comprises the following steps:
(1) Controlling the indoor temperature to be 20-22 ℃; relative humidity 50+ -5% RH
(2) 24 persons were divided into 4 groups of 6 persons each, example 1 was group a, comparative example 1 was group B, the mask base was a substance not containing any moisturizing skin care composition, and sodium hyaluronate was a positive control group.
(3) The test skin area was tested prior to use, recorded as 0h data and marked.
(4) Cutting the test sample into 4cm x 4cm size, attaching the test sample in a test area before marking the test sample for use, removing the mask after 20min of attachment, massaging until absorption, and performing a return visit.
(4) Applying for 20min, removing the mask, massaging to 1h, 2h, 3h, and 4h after absorption, and retesting. The test was performed with the area of the mask to which the sample was not applied as a blank.
The test result calculation formula:
initial value: refers to the base value (data before use, 0 h) without any product.
Mean value ofWhere x = individual parameter measurement, n = number of valid data
Difference from initial value xT after use-xT before use
Test results:
the skin moisture content test results before and after the products are used for 1h, 2h, 3h and 4h are shown in Table 4 and FIG. 1.
Table 4 average values of skin moisture content before product use, after product use for 1h, 2h, 3h, 4h and statistical results (n=24);
TABLE 4 Table 4
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Conclusion:
as can be seen from the data in table 4 and fig. 1, the technical scheme provided by the application is that the moisturizing and skin-protecting composition example 1 has good moisturizing effect when applied to an essence mask liquid with moisturizing effect; after the moisturizing skin care composition is used for 1h, the moisture content of the skin reaches a peak value, and the moisture content of the moisturizing skin care composition is obviously higher than that of a blank group without a mask and is also higher than that of a comparison example 1 and a positive comparison sample, so that the moisture content of the skin can be effectively improved when the moisturizing skin care composition is applied to the mask, wherein the components have good synergistic effect, and the moisture retention effect of the mask can be influenced due to the lack of any component, so that the moisturizing skin care composition can better lock the moisture of the skin and reduce the moisture flowing water, thereby achieving the moisturizing effect.
Application 2
A moisturizing cream with 5% of the moisturizing cream material of the example 5 (A) and the moisturizing cream material of the comparative example 5 (B) and the cream base, respectively, and without the moisturizing cream material of the example and the comparative example, is tested; test formulation table 5 is as follows:
table 5A cream with moisturizing and moisturizing effects
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The production process comprises the following steps:
1) Weighing the raw materials of the group A, adding the raw materials into an oil pan, stirring and heating the raw materials to 78-83 ℃ at the speed of 35r/min, and dissolving and transparentizing the raw materials for later use;
2) Weighing the raw materials of the group B, adding the raw materials into an emulsifying pot, stirring and heating the raw materials to 83-85 ℃ at the speed of 35r/min, and dissolving and transparentizing the raw materials;
3) Weighing the raw materials of the group C, uniformly mixing in a container until the viscous liquid is added into an emulsifying pot, and stirring for 15 minutes at 65-70 r/min until the liquid is semitransparent;
4) Pumping the dissolved group A raw materials into an emulsifying pot by using a vacuum pump of-0.05 mpa, stirring at a speed of 45-55 r/min, and homogenizing at a high speed of 30000r/min for 15 minutes to obtain milky liquid;
5) Weighing the raw materials of the group D, adding the raw materials into an emulsifying pot, stirring at a speed of 35-45 r/min, and homogenizing at a speed of 5000r/min for 1 min to obtain viscous emulsion;
6) Cooling, vacuumizing to-0.03 mpa, and stirring at a speed of 35-38 r/min;
7) Cooling to below 45 ℃, weighing the raw materials of the group E, adding the raw materials into an emulsifying pot, and stirring at the speed of 35-38 r/min for 15 minutes to obtain white emulsion;
8) Respectively weighing the raw materials of the group F, adding the raw materials into an emulsifying pot, and stirring at the speed of 35-38 r/min for 10 minutes to obtain white emulsion;
9) Weighing the raw materials G, adding the raw materials G into an emulsifying pot, and stirring at the speed of 35-38 r/min for 10 minutes to obtain white emulsion;
10 And (3) discharging after the physical and chemical indexes are checked to be qualified.
Wherein, the physical and chemical indexes are as follows:
appearance: white bright emulsion
pH:5.5~6.8
Smell: fragrance of the flower water;
stability cold-resistant: keeping at minus 8+/-2 ℃ for 24 hours, and recovering the room temperature without layering;
stability and heat resistance: keeping the temperature of (40+/-1) ℃ for 24 hours, and recovering the room temperature without layering;
and (3) centrifugal examination: 2000r/min,20min, no layering;
microorganism: colony count: less than or equal to 10FCU/g;
total number of mold and yeast: less than or equal to 10CFU/g;
heat-resistant coliform group: cannot be detected;
staphylococcus aureus: cannot be detected;
pseudomonas aeruginosa: cannot be detected;
heavy metal: mercury is less than or equal to 1mg/kg; lead is less than or equal to 10mg/kg; arsenic is less than or equal to 2mg/kg; cadmium is less than or equal to 5mg/kg.
Wherein, the teriparation nano-liquid consists of 0.3 to 1.0 percent of polyglycerol-10 heptastearate, 10.0 to 15.0 percent of glycerol, 15.0 to 25.0 percent of butanediol, 18.0 to 22.0 percent of isododecane, 42.0 to 48.0 percent of caprylic/capric triglyceride and 3.0 to 5.0 percent of deionized water, and is obtained by a low-temperature or normal-temperature dispersion and emulsification technology, and the purpose of use is enhanced.
The experiment of reducing wrinkles is carried out on the cream with moisturizing and moisturizing functions:
the efficacy of the cream A, B and the matrix for reducing wrinkles and improving skin roughness and lubricity is evaluated by 4-week human body test.
(1) And (3) pretreatment of test: 15 volunteers were selected, aged 38-48 years with wrinkles and healthy skin without damage, and the cream A, B and matrix were tested separately for 5 persons each. The support smears the test sample on the face twice a day. During the experiment, the subject was unable to apply any other cosmetics at the experimental site. The subjects were tested after 0, 1,2, 3, 4 weeks of continuous use of the test samples.
(2) The testing method comprises the following steps: skin conditions were measured on the face at weeks 0, 1,2, 3, and 4 using a skin wrinkle tester VISIOMETER SV 600. The test parameter is skin roughness Rt, which is the difference from the highest peak to the lowest valley of the skin texture, and is called Rl in the software of the instrument; average roughness RZ the average roughness is the arithmetic average of 5 consecutive segments of the same length, the larger the values called R3, R1 and R3 in the software of the instrument, the more severe the wrinkles, the worse the skin roughness, the lubricity.
(3) And (3) calculating a formula:
skin roughness R1 change value=r1 Fourth periphery -R1 Initial value
Skin roughness change rate R1 change rate = [ (R1) Fourth periphery -R1 Initial value )/R1 Initial value ]X 100%; skin average roughness R3 change value=r3 Fourth periphery -R3 Initial value
Rate of change of skin roughness R3 rate of change = [ (R3) Fourth periphery -R3 Initial value )/R3 Initial value ]X 100%; initial value: refers to the base value without any product (data before use, 0 weeks);
the test results of specific R1 are shown in table 6, and the test results of R3 are shown in table 7:
TABLE 6 variation of skin roughness R1 (in mm) after application of cream A, B and base product
TABLE 7 variation of average roughness R3 of skin (in mm) after application of cream A, B and base product
Conclusion:
table 6 shows the change of the roughness R1 of the skin around the substrate product using the cream A, B, and the experimental results of Table 6 show that the product using the cream A can significantly reduce the difference from the highest peak to the lowest valley of the skin, i.e. the roughness of the skin can be significantly reduced, and the roughness of the skin can be reduced by more than 21.42% after the product using the cream A is used around. Table 7 shows the change of average roughness R3 of the skin around the use of the cream A, B and the matrix product, and the experimental results in Table 7 show that the average roughness of the skin can be reduced by more than 54.79% after the use of the cream A for four weeks. From the results shown in tables 6 and 7, it can be seen that the moisturizing skin care composition of the present application can reduce wrinkles, improve skin roughness and lubricity, and inhibit collagenase activity and elastase activity by adding the cream of the present application.
All other embodiments, which can be made by those skilled in the art based on the embodiments of the application without making any inventive effort, are intended to be within the scope of the application.

Claims (9)

1. A moisturizing, anti-aging and skin care composition characterized by: the composition comprises the following components in parts by weight: 20-50 parts of hops, 20-40 parts of longan fruits, 10-30 parts of buddleia officinalis, 10-20 parts of radix peucedani, and 5-20 parts of vetiver roots;
the preparation method of the moisturizing and anti-aging skin care composition comprises the following steps of:
step 1, raw material pretreatment, namely respectively crushing hops, longan fruits, buddleja officinalis, white flower peucedanum root and vetiver root, uniformly mixing the crushed hops, longan fruits, buddleja officinalis and Hu Genhe vetiver root before white flowers to obtain a raw material mixture for later use;
step 2, adding the raw material mixture obtained in the step 1 into 85% ethanol, carrying out reflux extraction for 35-55 minutes at 55-75 ℃, cooling to 42-52 ℃, and carrying out vacuum suction filtration by using a-0.05-0.1 mpa circulating water type multipurpose vacuum pump and a glass crucible to obtain a clear mixture;
step 3, repeating the operation of the step 2;
step 4, injecting the clarified mixture obtained after the suction filtration in the step 2 and the step 3 into a rotary steaming bottle, and rotary steaming all ethanol at the temperature of 85-100 ℃ to obtain a mixture solid;
step 5, adding the mixture solid obtained in the step 4 into an ultrasonic extractor, weighing a solvent, adding the solvent into the ultrasonic extractor, stirring at a speed of 30-45 r/min, soaking for 20-40 min, then starting heating to 70-95 ℃, setting the ultrasonic frequency to 350-450W, setting the working frequency to 6-10 KHz, and setting the ultrasonic extraction time to 60-100 min;
step 6, after ultrasonic extraction is finished, cooling to 45-65 ℃, and filtering with 200-300 mesh filter cloth to a storage tank to obtain a mixed solution I for later use;
step 7, collecting and mixing filter residues obtained in the step 3, adding deionized water, adding 0.1-0.5% of special enzyme for plant extraction, setting the pH to be 4.0-5.0, setting the temperature to be 45-52 ℃, carrying out enzymolysis for 240-360 minutes, inactivating the enzyme at the temperature of 90-100 ℃ for 20-30 minutes after the enzymolysis is finished, and filtering by using 200-300 meshes of filter cloth to obtain an enzyme treatment mixture II for later use;
step 8, mixing the filter residue obtained by enzymolysis with a solvent according to the mass ratio of 1:10-30, placing the mixture into a water bath at 75-95 ℃ for extraction for 150-210 minutes to obtain a filter residue extracting solution, cooling the filter residue extracting solution to 42-52 ℃, and filtering the filter residue extracting solution with a 200-300-mesh filter cloth to obtain a mixture III for later use;
step 9, repeating the operation of the step 8, and repeating the water bath extraction once to obtain a mixture IV for standby;
step 10, combining and mixing the mixture II, III, IV, and then diluting with deionized water, wherein the dilution ratio is as follows: 1:3-1:10 to obtain a mixture V;
step 11, mixing the mixture I, V together, and concentrating by using a rotary evaporator to obtain a concentrated mixture, namely the moisturizing and anti-aging skin care composition.
2. The moisturizing and anti-aging skin care composition according to claim 1, wherein in the step 1, the crushed hops, longan fruits, butterflybush flowers and front Hu Genhe rock orchid roots are filtered through a 80-250 mesh sieve.
3. A moisturizing and anti-aging skin care composition according to claim 1, wherein in step 2, the mass fraction ratio of the raw material mixture to ethanol is 1:10-1:20.
4. A moisturizing and anti-aging skin care composition according to claim 1, wherein in step 5, the mass ratio of the mixture solids to the solvent is 1:30.
5. A moisturizing and anti-aging skin care composition according to claim 1, wherein in step 5, the solvent is one or more of butanediol, propylene glycol, glycerol and 1, 2-hexanediol, deionized water is added into the solvent, and the mass ratio of the solvent to the deionized water is 1:1-1:10.
6. The moisturizing and anti-aging skin care composition according to claim 1, wherein in the step 7, the mass ratio of the filter residue to the deionized water is 1:10-1:50.
7. A moisturizing and anti-aging skin care composition according to claim 1, wherein in step 7, the plant extract specific enzyme consists of 1 ten thousand U/g cellulase, 1 ten thousand U/g hemicellulase, 3 ten thousand U/g glucanase, 1 ten thousand U/g pectinase and 1 ten thousand U/g papain.
8. A moisturizing and anti-aging skin care composition according to claim 1, wherein in step 8, the solvent is one or more of butylene glycol, glycerin, and 2, 3-butylene glycol.
9. The use of a moisturizing and anti-aging skin care composition according to claim 1 or a product obtained from a moisturizing and anti-aging skin care composition according to any one of claims 2 to 8 for preparing a moisturizing and anti-aging skin care cosmetic, wherein the moisturizing and anti-aging skin care composition is mixed with one of a conventional cosmetic lotion, essence, cream, eye cream and emulsion to obtain a skin care product with moisturizing and anti-aging effects, and the moisturizing and anti-aging skin care composition is added in an amount of 1 to 10% by weight of the skin care product.
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