CN114099393A - Composition with tightening and anti-aging effects and preparation method and application thereof - Google Patents

Composition with tightening and anti-aging effects and preparation method and application thereof Download PDF

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CN114099393A
CN114099393A CN202111657141.7A CN202111657141A CN114099393A CN 114099393 A CN114099393 A CN 114099393A CN 202111657141 A CN202111657141 A CN 202111657141A CN 114099393 A CN114099393 A CN 114099393A
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parts
composition
resin
tightening
extract
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CN114099393B (en
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徐勇威
秦允荣
李威
阮桂梅
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Guangzhou Bio Tech Ltd Hong Zhong
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Guangzhou Bio Tech Ltd Hong Zhong
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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
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/64Proteins; Peptides; Derivatives or degradation products thereof
    • A61K8/645Proteins of vegetable origin; Derivatives or degradation products 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
    • A61K8/92Oils, 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
    • 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
    • A61Q19/08Anti-ageing preparations
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07KPEPTIDES
    • C07K1/00General methods for the preparation of peptides, i.e. processes for the organic chemical preparation of peptides or proteins of any length
    • C07K1/14Extraction; Separation; Purification
    • C07K1/145Extraction; Separation; Purification by extraction or solubilisation
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07KPEPTIDES
    • C07K1/00General methods for the preparation of peptides, i.e. processes for the organic chemical preparation of peptides or proteins of any length
    • C07K1/14Extraction; Separation; Purification
    • C07K1/34Extraction; Separation; Purification by filtration, ultrafiltration or reverse osmosis
    • CCHEMISTRY; METALLURGY
    • C12BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12PFERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P21/00Preparation of peptides or proteins
    • C12P21/06Preparation of peptides or proteins produced by the hydrolysis of a peptide bond, e.g. hydrolysate products
    • 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

Abstract

The invention provides a composition with tightening and anti-aging effects, which comprises the following components in parts by weight: 0.1-12 parts of hydrolyzed vegetable protein, 0.1-20 parts of resin extract, 1-50 parts of polyhydric alcohol and 30-90 parts of water. The invention belongs to the technical field of cosmetics, and the invention combines specific hydrolyzed vegetable protein and resin extract according to a proper mass proportion, can realize rapid skin smoothing and wrinkle reduction by a lower dosage, has obvious skin tightening effect which can be perceived by skin, and simultaneously has the effects of long-acting moisture retention, oxidation resistance, skin elasticity enhancement and aging resistance.

Description

Composition with tightening and anti-aging effects and preparation method and application thereof
Technical Field
The invention belongs to the technical field of cosmetics, and particularly relates to a composition with tightening and anti-aging effects, and a preparation method and application thereof.
Background
The skin is the largest organ covering the surface of the human body, not only has the functions of protecting, defending, regulating temperature and the like, but also is the important embodiment of the beauty of the human body. The skin is easily stimulated by external environments such as air pollution, ultraviolet rays, harmful chemicals and the like due to direct contact with the external environment, and simultaneously, the skin function is degraded due to the influence of internal factors such as age, diet, mental state, living habits and the like, so that the skin is loose and is easy to age.
In recent years, people are concerned about anti-aging of their organs with the increasing living standard and health awareness. Anti-aging cosmetics increasingly become one of the products which are urgently needed by the vast female consumers. At present, the number of natural-source firming and anti-aging products is small, part of raw materials are expensive, active ingredients are difficult to effectively extract and/or absorb, and most of the natural-source firming and anti-aging products are based on moisture retention and free radical removal and are relatively conventional nursing means. The tightening anti-aging products on the market use either synthetic polymer components to achieve tightening effects but cannot solve the aging problem of the skin, or small-molecule polypeptide active components to have certain anti-aging effects but have no tightening effects. Meanwhile, the existing compact anti-aging products often have the problems of slow effect, poor durability and high price.
Therefore, the compact anti-aging product which has the advantages of quick response, lasting efficacy and reasonable price has important significance.
Disclosure of Invention
In order to solve the problems in the prior art, the inventor deeply excavates and screens effective species with firming and anti-aging effects in cosmetic raw materials in the process of long-term production research, and unexpectedly discovers that the hydrolyzed vegetable protein and the resin extract extracted by a specific process are combined in a proper mass ratio, and the quick skin smoothing and wrinkle lightening can be realized by using a lower dosage, so that the composition has a remarkable skin tightening effect which can be perceived by skin, and meanwhile, the composition also has the effects of long-acting moisture retention, oxidation resistance, skin elasticity enhancement and aging resistance. The present invention has been completed based on the above findings.
The composition is mild and safe in components and has quick, effective and lasting tightening and anti-aging effects.
The main active components of the composition with the effects of tightening and resisting aging have the following effects:
the protein is involved in the metabolism of skin tissues, and the elasticity of skin is lost due to aging. The vegetable protein has good affinity to skin and scalp, and has good skin feeling, moisture keeping, nourishing, tightening, antiaging, soothing and repairing effects. For example, the hydrolyzed sesame protein of the present invention has the effects of preventing the skin from being damaged by the peroxide lipid, counteracting or neutralizing the accumulation of harmful substance radicals in cells, and treating dry and rough skin, and making the skin smooth and red.
The plant resin is mainly the secretion of colloid semi-transparent substances secreted by the bark of trees (such as pine trees and peach trees) for protecting the self growth due to mechanical damage (such as cutting, insect bite and the like) or pathogenicity, is composed of polysaccharide substances, is soluble in water or can swell when meeting water, and various resins are considered to have certain medicinal value and health care function. For example, the traditional Chinese medicine considers that peach gum has the effects of tonifying qi, regulating blood and promoting the production of body fluid, and the peach gum can also be used as an additive for producing Chinese patent medicines.
According to the invention, researches show that the peach resin extract contains galactose, rhamnose, alpha-glucuronic acid and other components and has the effects of moisturizing and resisting oxidation; the karaya resin extract contains D-galactose, D-xylose, L-arabinose and other components, and is a better skin conditioner; the two components supplement each other to exert the anti-aging effect synergistically, and polysaccharide in the peach resin extract mostly has a porous network structure and can be combined with protein to play a role in increasing the stability of the hydrolyzed vegetable protein.
The objects of the invention will be further illustrated by the following detailed description.
The invention provides a composition with tightening and anti-aging effects, which comprises the following components in parts by weight: 0.1-12 parts of hydrolyzed vegetable protein, 0.1-20 parts of resin extract, 1-50 parts of polyhydric alcohol and 30-90 parts of water.
Preferably, the composition with the effects of tightening and resisting aging comprises the following components in parts by weight: 3-10 parts of hydrolyzed vegetable protein, 8-15 parts of resin extract, 10-15 parts of polyhydric alcohol and 60-75 parts of water.
More preferably, the composition with tightening and anti-aging effects comprises the following components in parts by weight: 6-10 parts of hydrolyzed vegetable protein, 8-12 parts of resin extract, 11-13 parts of polyhydric alcohol and 66-72 parts of water.
Preferably, the composition with firming and anti-aging effects, the hydrolyzed vegetable protein comprises at least one of hydrolyzed sesame protein, hydrolyzed soybean protein, hydrolyzed lupin protein and hydrolyzed hazelnut protein.
Preferably, the resin extract is a mixture of peach resin extract and karaya extract in a mass ratio of 1 (0.5-2).
Preferably, the polyhydric alcohol comprises at least one of glycerol, dipropylene glycol, butylene glycol, propylene glycol, 1, 2-pentanediol, 1, 2-hexanediol, and ethylhexylglycerol. Butanediol, 1, 2-pentanediol and 1, 2-hexanediol are not only excellent polyhydric alcohol moisturizers, but also have the effects of further enhancing the stability of the system of the present invention and inhibiting the growth of microorganisms, and furthermore, ethylhexylglycerin is also a good preservative accelerator.
Correspondingly, the invention also provides a preparation method of the composition with the effects of tightening and resisting aging, which comprises the following steps: respectively preparing hydrolyzed vegetable protein and resin extract, dissolving in water, filtering with ceramic membrane, adding polyalcohol into the filtrate, stirring, and sterilizing to obtain composition with tightening and antiaging effects.
Preferably, the water is deionized water.
Preferably, the pore diameter of the ceramic membrane is 50-200 nm.
Preferably, the step of preparing the hydrolyzed vegetable protein comprises:
1) pre-treating plants: drying the plant components at 60-65 ℃, extracting for 2-3 times in a screw oil press for degreasing at the rotating speed of 20-60 r/min, and crushing the extracted plant cake to 10-200 meshes to obtain plant powder;
2) extracting crude plant protein: putting the plant powder into water according to the mass ratio of 1 (1-15) to liquid, adjusting the pH value to 8-11, carrying out ultrasonic extraction for 1-3 h for 1-3 times, wherein the ultrasonic power is 100-500W, filtering, and collecting a plant crude protein extracting solution;
3) preparing hydrolyzed vegetable protein: adjusting the pH value of the crude plant protein extract to 9-12, adjusting the temperature to 40-60 ℃, adding papain with the mass of 0.005-0.1% of that of the crude plant protein extract for enzymolysis for 1-4 h, adjusting the temperature to 70-80 ℃, and inactivating the enzyme for 10-30 min; adjusting the pH value to 3-5, centrifuging, collecting precipitate, and drying to obtain hydrolyzed vegetable protein;
the preparation method of the resin extract comprises the following steps:
1) pretreatment of resin: soaking the resin with water at 30-50 ℃ according to the mass ratio of the material to the liquid of 1 (1-5), removing bark and silt after full swelling, draining, drying, and crushing to 10-200 meshes to obtain resin powder;
2) extracting a crude resin extraction solution: putting the resin powder into water according to the mass ratio of material to liquid of 1 (1-15), adjusting the temperature to 70-80 ℃, performing ultrasonic extraction for 1-4 h with the ultrasonic power of 100-300W, filtering, and collecting the crude resin extraction liquid;
3) preparing a resin extract: adjusting the pH value of the resin crude extract to 3-6.5, adding mixed enzyme accounting for 0.001-0.02% of the mass of the resin crude extract for enzymolysis for 10-60 min, wherein the enzymolysis temperature is 45-60 ℃, then heating to 70-80 ℃, and inactivating the enzyme for 10-30 min; filtering, centrifuging the filtrate, collecting supernatant, and drying to obtain resin extract; the mixed enzyme is a mixture of pectinase and cellulase according to the mass ratio of 5: 2. Preferably, the centrifugation condition is 3000-6000 rpm for 5-30 min.
Correspondingly, the invention also provides application of the composition with the effects of tightening and resisting aging in preparation of cosmetics.
In addition, the invention also provides a cosmetic which comprises the composition with the effects of tightening and resisting aging and an auxiliary material. Preferably, the cosmetic is essence, and the auxiliary materials are conventional auxiliary materials in the field.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, the hydrolyzed plant protein extracted by a specific process and the resin extract are compounded for use, so that the tightening effect of the hydrolyzed plant protein and the moisturizing and antioxidant effects of the resin extract are fully exerted, the composition system has the effects of enhancing stability and synergia, the skin can be quickly smoothened and wrinkles can be reduced by using a lower dosage, and the composition has the remarkable skin tightening effect which can be perceived by the skin, and the long-acting effects of moisturizing, antioxidant, skin elasticity enhancement and aging resistance. By adding a certain amount of polyhydric alcohol into the composition of the system, the effects of further enhancing the stability of the system and inhibiting the growth of microorganisms are achieved. The preparation method of the composition provided by the invention does not need expensive equipment, is simple and efficient to operate, the extracted active ingredients are easy to absorb, and the prepared composition has stable quality.
Drawings
FIG. 1 is a schematic diagram of the immediate tightening effect of the essence of the composition of the present invention; wherein, 1-1 is the wrinkle condition of eyes before using the product, and 1-2 is the wrinkle condition of eyes after using the product for 5 min.
FIG. 2 is a schematic representation of the long-lasting tightening effect of a serum containing the composition of the present invention; wherein, 2-1 is the wrinkle condition of eyes before using the product, and 2-2 is the wrinkle condition of eyes after using the product for 1 month.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and examples.
The components, materials and apparatuses used in the examples of the present invention can be obtained from conventional commercial sources or can be obtained by known methods in the art, unless otherwise specified.
Example 1 composition having firming and anti-aging effects
A composition with tightening and anti-aging effects comprises the following components in parts by weight: 8 parts of hydrolyzed sesame protein, 5 parts of peach resin extract, 5 parts of karaya extract, 10 parts of butanediol, 2 parts of 1, 2-hexanediol, 0.05 part of ethylhexyl glycerol and 69.95 parts of water.
The preparation method of the composition with the effects of tightening and resisting aging comprises the following steps: respectively preparing hydrolyzed vegetable protein (hydrolyzed sesame protein) and resin extract (peach resin extract, karaya tree extract), dissolving in water, filtering with ceramic membrane with pore diameter of 100nm, adding polyalcohol (butanediol, 1, 2-hexanediol, and ethylhexylglycerin), stirring, and sterilizing to obtain composition with tightening and antiaging effects;
the preparation method of the hydrolyzed sesame protein comprises the following steps:
1) pretreatment of sesame: drying semen Sesami at 65 deg.C, squeezing in a screw oil press for 3 times to defat at 40r/min, and pulverizing the squeezed sesame cake to 50 mesh to obtain semen Sesami powder;
2) extracting crude sesame protein: adding the sesame powder into water according to the mass ratio of 1:12, adjusting the pH value to 10.2, performing ultrasonic extraction for 2 hours for 2 times, wherein the ultrasonic power is 200W, filtering, and collecting a sesame crude protein extracting solution;
3) preparing hydrolyzed sesame protein: adjusting the pH value of the crude sesame protein extract to 10.5, adjusting the temperature to 50 ℃, adding papain accounting for 0.03 percent of the mass of the crude sesame protein extract for enzymolysis for 2.5 hours, adjusting the temperature to 80 ℃, and inactivating the enzyme for 30 min; and adjusting the pH value to 4.5, centrifuging, collecting precipitate, and drying to obtain the hydrolyzed sesame protein.
The preparation method of the resin extract comprises the following steps:
1) pretreatment of resin: soaking peach gum and karaya gum in 50 deg.C water at a material-to-liquid ratio of 1:1, removing bark and silt after fully swelling, draining, oven drying, and pulverizing to 50 mesh to obtain resin powder;
2) extracting a crude resin extraction solution: putting the resin powder into water according to the mass ratio of 1:10, adjusting the temperature to 80 ℃, performing ultrasonic extraction for 4 hours with the ultrasonic power of 300W, filtering, and collecting the crude resin extraction liquid;
3) preparing a resin extract: adjusting the pH value of the resin crude extract to 5.5, adding mixed enzyme with the mass of 0.01% of the resin crude extract for enzymolysis for 60min, wherein the enzymolysis temperature is 60 ℃, then heating to 80 ℃, and inactivating the enzyme for 20 min; filtering, centrifuging the filtrate, collecting supernatant, and drying to obtain resin extract; the mixed enzyme is a mixture of pectinase and cellulase according to the mass ratio of 5: 2.
Example 2 composition having firming and anti-aging effects
A composition with tightening and anti-aging effects comprises the following components in parts by weight: 10 parts of hydrolyzed sesame protein, 4 parts of peach resin extract, 4 parts of karaya extract, 10 parts of butanediol, 2 parts of 1, 2-hexanediol, 0.05 part of ethylhexyl glycerol and 69.95 parts of water.
The preparation method is the same as that of example 1.
Example 3 composition having firming and anti-aging effects
A composition with tightening and anti-aging effects comprises the following components in parts by weight: 3 parts of hydrolyzed sesame protein, 7.5 parts of peach resin extract, 7.5 parts of karaya extract, 10 parts of butanediol, 2 parts of 1, 2-hexanediol, 0.05 part of ethylhexyl glycerol and 69.95 parts of water.
The preparation method is the same as that of example 1.
Example 4 composition with firming and anti-aging efficacy
The composition with the effects of tightening and resisting aging comprises the following components in parts by weight: 6 parts of hydrolyzed sesame protein, 6 parts of peach resin extract, 6 parts of karaya extract, 10 parts of butanediol, 2 parts of 1, 2-hexanediol, 0.05 part of ethylhexyl glycerol and 69.95 parts of water.
The preparation method is the same as that of example 1.
Comparative example 1
In comparison with example 1, in comparative example 1, the hydrolyzed sesame protein was replaced with water, and other conditions were the same as in example 1.
Comparative example 2
In comparison with example 1, in comparative example 2, the peach resin extract was replaced with water, and the other conditions were the same as in example 1.
Comparative example 3
In comparison with example 1, in comparative example 3, the karaya extract was replaced with water, and other conditions were the same as in example 1.
Comparative example 4
In comparison with example 1, in comparative example 4, the peach resin extract and the karaya extract were replaced with water, and the other conditions were the same as in example 1.
Comparative example 5
In comparison with example 1, in comparative example 5, hydrolyzed rice protein was obtained by the same treatment method except that sesame was replaced with rice, and the conditions were the same as in example 1.
Comparative example 6
In comparison with example 1, in comparative example 6, the peach resin extract and the karaya tree extract were replaced with the mastic resin extract and the bisabolo resin extract, respectively, and the other conditions were the same as in example 1.
Comparative example 7
Compared with the embodiment 1, the preparation process in the comparative example 7 is the conventional hot reflux extraction, namely, the plant components, the peach resin and the karaya gum are mixed according to the proportion of the invention, the mixture is put into water according to the material-liquid ratio of 1:10, the extraction temperature is 80 ℃, 4 hours, the slag is removed, the extracting solution is collected, the extracting solution passes through a ceramic membrane with the aperture of 100 nanometers, and the mass ratio of the filtering solution is 1: 0.2: 0.005 of a mixture of butylene glycol, 1, 2-hexanediol and ethylhexylglycerin, stirred well and sterilized to obtain the composition of comparative example 7.
Application example 1 essence containing the composition of example 1
An essence with a formula shown in table 1.
TABLE 1
Figure BDA0003446255730000081
The preparation method of the essence comprises the following steps:
(1) putting the component A into a water phase pot, stirring at 82 ℃ until the component A is completely dissolved, and cooling;
(2) dissolving the component B in advance at 6 ℃ until the component B is transparent, adding the component B into a water phase pot at a constant speed under the stirring condition when the component A is cooled to 60 ℃, and stirring until the component B is uniformly dispersed after the component B is added;
(3) cooling to below 40 deg.C, adding phase C, and stirring to disperse uniformly;
(4) after the inspection is qualified, filtering the mixture by 200 meshes and discharging the mixture.
Application examples 2 to 4
In application examples 2 to 4, the composition prepared in example 1 was replaced with the composition prepared in examples 2 to 4, respectively, as compared with application example 1, and the other conditions were the same as in application example 1.
Application of comparative examples 1 to 7
In comparison with application example 1, the compositions prepared in comparative examples 1 to 7 were replaced with the compositions prepared in comparative examples 1 to 7, respectively, and the other conditions were the same as in application example 1.
Comparative application example 8
In comparison with application example 1, the composition prepared in example 1 was replaced with water in application comparative example 8, and the other conditions were the same as in application example 1.
Test example 1 antioxidant Activity test
1.1 purpose of the experiment
The antioxidant effect of the compositions of the present invention was examined by comparing the commonly used antioxidant component VC in skin care products and testing the inhibitory effect of the compositions of different concentrations on DPPH, free radical, hydroxyl radical and superoxide radical.
1.2 sample preparation
Preparing VC solution with mass concentration of 0.001%, 0.05% and 1%.
The mass concentrations of the compositions prepared in examples 1 to 4 and comparative examples 1 to 7 were diluted in three gradients of 10%, 5% and 1%, respectively.
1.3 Experimental methods
1) DPPH & free radical scavenging ability measurement: respectively sucking 1mL of sample solution with different mass concentrations and 0.5mL of DPPH stock solution (mass concentration is 0.35mg/mL) into a test tube, reacting for 30min in a dark place at room temperature, and measuring an absorbance value A1 at 519 nm; sucking 0.5mL of DPPH stock solution and 1mL of pure water, and determining an absorbance value A0; 0.5mL of absolute ethanol and 1mL of the sample solution were aspirated, and the absorbance value A2 was measured. The clearance was calculated according to the following formula:
clearance ═ 1- (a1-a2)/a0 × 100%.
2) Determination of the hydroxyl radical scavenging capacity: respectively sucking 2mL of sample solutions with different mass concentrations and 2mL of 6mmol/L FeSO4Solution and 2mL of 6mmol/L H2O2Placing the solution in a test tube, standing for 10min, adding 2mL of 6mmol/L salicylic acid solution, standing for 30min, and measuring absorbance A1 at wavelength of 510 nm; replacing salicylic acid with pure water, and measuring the absorbance value A2 by the same method; the absorbance A0 was measured using pure water as a blank control. The clearance was calculated according to the following formula:
clearance ═ 1- (a1-a2)/a0 × 100%.
3) Determination of superoxide radical scavenging capacity: respectively sucking 2mL of sample solutions with different mass concentrations, 4.5mL of 50mmol/LTris-HCl (pH8.2) buffer solution and 0.4mL of 25mmol/L pyrogallol solution into a test tube, uniformly mixing, carrying out water bath at 25 ℃ for 5min, then adding 1mL of 8mmol/L HCl solution, uniformly mixing, and measuring an absorbance value A1 at the wavelength of 325 nm; in addition, pure water is used for replacing the sample solution to determine the absorbance value A0 by the same method; the absorbance value A2 was measured by the same method using pure water instead of pyrogallol solution.
The clearance was calculated according to the following formula: clearance ═ 1- (a1-a2)/a0 × 100%.
1.4 results of the experiment
1) The results of DPPH.radical scavenging ability are shown in Table 2.
TABLE 2
Figure BDA0003446255730000101
2) The results of the hydroxyl radical scavenging ability are shown in Table 3.
TABLE 3
Figure BDA0003446255730000111
3) The results of superoxide radical scavenging ability are shown in Table 4.
TABLE 4
Sample set Composition 1%
Example 1 77.6%
Example 2 74.4%
Example 3 70.1%
Example 4 73.8%
Comparative example 1 35.2%
Comparative example 2 38.4%
Comparative example 3 39.1%
Comparative example 4 30.3%
Comparative example 5 70.7%
Comparative example 6 76.7%
Comparative example 7 66.3%
VC solution 0.001% 58.4%
As can be seen from the data in tables 2, 3 and 4, examples 1 to 4 of the present invention all had antioxidant effects, and particularly, the inhibitory effect on superoxide radicals was more significant, as compared with the positive control group. As can be seen from comparative examples 1,2, 3 and 4, the hydrolyzed sesame protein had a stronger inhibitory effect on free radicals, and the inhibitory effects of the peach resin extract and the karaya extract were close. The effects of inhibiting free radical activity of examples 1-4 are significantly better than those of comparative examples 1-4 and 7, which show that the composition of the present invention, which is prepared by compounding hydrolyzed sesame protein, peach resin extract and karaya tree extract and by using the preparation process of the present invention, has synergistic effect, significant effects on oxidation resistance and free radical inhibition, and no great difference in oxidation resistance is found by using different hydrolyzed plant proteins or resin extracts.
Test example 2 measurement of moisturizing Effect
2.1 purpose of the experiment
Under the conditions that the temperature is 20 +/-2 ℃ and the humidity is 50 +/-10%, 150 subjects are selected, a blank control group is set, samples are smeared and tested on the two forearms of the subjects according to a double-blind principle, and the skin moisture content of the test samples is tested at T0, T30min and T2h, so that the moisturizing effect of the tested products on the skin surface layer is evaluated.
2.2 Experimental methods
According to the QB/T4256-2011 guide for evaluating the moisturizing efficacy of cosmetics in the light industry standard of the people's republic of China.
The instrument comprises the following steps: skin moisture tester Corneometer CM825, Courage + Khazaka, germany.
2.3 evaluation index
Table 5 evaluation indices: moisture value change rate of 2 hours
Dosage forms Not reaching the standard Reach the standard Is excellent in
Aqueous preparation ≤10% 10~30% ≥30%
2.4 results of the experiment
TABLE 6 moisture content variation value (%)
Figure BDA0003446255730000121
Figure BDA0003446255730000131
The data in table 6 show that both the application examples and the application comparative examples have a certain improvement effect on the moisture content of the skin, wherein the effect of the application examples is better than that of the application comparative examples. Through test, the hydrolyzed vegetable protein and resin extract of the invention has stronger water-holding effect. The raw materials are matched and prepared in a preparation mode, so that a good synergistic effect is brought, the composition is superior to other combination modes, and the moisturizing effect is good.
Experimental example 3 tightening test
3.1 purpose of the experiment
And (5) confirming the compact effect of the product through a direct use test of a consumer meeting the requirements. The tightening effect of the test product was evaluated by periocular sampling and testing on a double-blind basis.
3.2 Experimental methods
1) Sensory evaluation
Under the conditions that the temperature is 20 +/-2 ℃ and the humidity is 50 +/-10%, 78 subjects are selected and randomly divided into 13 groups, an application example group, an application comparative example group and a blank control group are set, 6 persons in each group use 1 time of corresponding test products in a half-face test mode after the subjects wash faces, skin tightening effect test is carried out at T5min, the test products are scored in a questionnaire survey mode, and the average value of the test products is taken.
2) Image acquisition
And selecting 20 subjects, continuously using the product of the application example 1 for 4 weeks according to experimental design, using the product for 1 time respectively in a half-face test mode after cleaning the face in the morning and evening, tracking and observing the eye skin of the subjects in the group, and acquiring skin photos at T5min, 2 nd week and 4 th week respectively. The subject was in a relaxed state with his head in a natural position, closed eyes were forward, and 2 front photographs of the subject before and after the skin care product was applied were taken with VISIA-CR.
The instrument comprises the following steps: skin analyzer VISIA-CR, Canfield, usa.
3.3 evaluation index
TABLE 7 evaluation index
Evaluation of Invalidation Slightly compact Moderately compact Apparent compactness Strong compactness
Score of 0 ≤1 1~2 2~3 ≥3
3.4 test results
1) Even compact effect scoring
Table 8 compactness scores
Figure BDA0003446255730000141
Figure BDA0003446255730000151
The data in Table 8 show that the application example and the application comparative example have a certain skin tightening effect, and the tightening effect of the hydrolyzed vegetable protein of the invention on the product is the most; in addition, the data of the application comparative example 7 and the comparison of the application examples show that the preparation method plays an important role in the tightening effect of the product.
2) The instant compact effect picture acquisition result is shown in fig. 1.
After testing by 20 volunteers, 18 subjects showed a distinct tightening sensation after 5min using application example 1, with a higher proportion of women than men and a stronger tightening sensation than men.
3) The long-acting compact effect picture acquisition result is shown in fig. 2.
After testing of 20 subjects, using application example 1, 11 volunteers showed a reduction in eye wrinkles after one month, and the composition of the present invention was effective in reducing the wrinkle condition.
Test example 4 elasticity test
4.1 purpose of the experiment
The improvement effect of the product on the skin elasticity is confirmed through a direct use test of a consumer meeting the requirements. The elastic effect of the test product was evaluated by double-blind sampling and testing of the subjects' faces.
4.2 Experimental methods
And (3) selecting 20 subjects, continuously using the product of the application example of the invention for 1-4 weeks according to experimental design, using the product for 1 time respectively in a half-face test mode after cleaning faces in the morning and evening, tracking and observing skin elasticity indexes of the subjects entering the group, and acquiring skin elasticity data in the 0 th, 2 th and 4 th weeks respectively. Skin elasticity data was collected 3 times on the cheek area of the subject and averaged.
Testing an instrument: cuto
Figure BDA0003446255730000161
Dual MPA 580
4.3 evaluation criteria
The value of the elasticity R2 represents the ratio of the amount of springback of the skin in the absence of negative pressure to the maximum amount of stretch in the presence of negative pressure, and a ratio closer to 1 indicates better skin elasticity.
4.4 results of the experiment
TABLE 9 skin elasticity score
Sample set W0 W2 W4 From the initial difference
Application example 1 0.5607±0.0534 0.6249±0.0497 0.6816±0.0371 0.1209
Application example 2 0.5620±0.0587 0.5860±0.0614 0.6224±0.0456 0.0604
Application example 3 0.5618±0.0348 0.6035±0.0574 0.6398±0.0315 0.0780
Application example 4 0.5636±0.0421 0.6104±0.0382 0.6521±0.0380 0.0885
Comparative application example 8 0.5617±0.0490 0.5626±0.06814 0.5638±0.0271 0.0021
Blank control group 0.5681±0.0361 0.5682±0.0634 0.5678±0.0178 -0.0003
The R2 values were measured using a skin elasticity tester, and the results are shown in Table 9, where the R2 value was the lowest at week 0 in the test group, and the elasticity score showed a gradual increase after 2 and 4 weeks using the product of example. Wherein, the elasticity score of the sample of example 1 is increased by 21.6 percent after 4 weeks, and the elasticity score of the sample of example 4 is increased by 15.8 percent, which shows that the skin elasticity is obviously improved, and the composition of the invention has better effect of improving the skin elasticity.
Comprehensively, tests of the test examples 1-4 prove that the composition and the essence containing the composition have better beneficial effects on resisting oxidation, moisturizing, tightening and improving the skin elasticity.
While the preferred embodiments of the present invention have been illustrated and described, it will be understood by those skilled in the art that the present invention is not limited to the details of the embodiments shown and described, but is capable of numerous equivalents and substitutions without departing from the spirit of the invention as set forth in the claims appended hereto.

Claims (10)

1. A composition with firming and anti-aging effects is characterized in that: the composition comprises the following components in parts by weight: 0.1-12 parts of hydrolyzed vegetable protein, 0.1-20 parts of resin extract, 1-50 parts of polyhydric alcohol and 30-90 parts of water.
2. The composition with tightening and anti-aging effects as claimed in claim 1, wherein: the composition comprises the following components in parts by weight: 3-10 parts of hydrolyzed vegetable protein, 8-15 parts of resin extract, 10-15 parts of polyhydric alcohol and 60-75 parts of water.
3. The composition with tightening and anti-aging effects as claimed in claim 1 or 2, wherein: the composition comprises the following components in parts by weight: 6-10 parts of hydrolyzed vegetable protein, 8-12 parts of resin extract, 11-13 parts of polyhydric alcohol and 66-72 parts of water.
4. The composition with tightening and anti-aging effects as claimed in any one of claims 1 to 3, wherein: the hydrolyzed vegetable protein comprises at least one of hydrolyzed sesame protein, hydrolyzed soybean protein, hydrolyzed lupin protein and hydrolyzed hazelnut protein.
5. The composition with tightening and anti-aging effects as claimed in any one of claims 1 to 3, wherein: the resin extract is a mixture of peach resin extract and karaya extract according to the mass ratio of 1 (0.5-2).
6. The composition with tightening and anti-aging effects as claimed in any one of claims 1 to 3, wherein: the polyhydric alcohol comprises at least one of glycerol, dipropylene glycol, butylene glycol, propylene glycol, 1, 2-pentanediol, 1, 2-hexanediol, and ethylhexylglycerol.
7. The method for preparing the composition with tightening and anti-aging effects as claimed in any one of claims 1 to 6, wherein: the method comprises the following steps: respectively preparing hydrolyzed vegetable protein and resin extract, dissolving in water, filtering with ceramic membrane, adding polyalcohol into the filtrate, stirring, and sterilizing to obtain composition with tightening and antiaging effects.
8. The process for preparing the composition with tightening and anti-aging effects as claimed in claim 7, wherein:
the preparation steps of the hydrolyzed vegetable protein comprise:
1) pre-treating plants: drying the plant components at 60-65 ℃, extracting for 2-3 times in a screw oil press for degreasing at the rotating speed of 20-60 r/min, and crushing the extracted plant cake to 10-200 meshes to obtain plant powder;
2) extracting crude plant protein: putting the plant powder into water according to the mass ratio of 1 (1-15) to liquid, adjusting the pH value to 8-11, carrying out ultrasonic extraction for 1-3 h for 1-3 times, wherein the ultrasonic power is 100-500W, filtering, and collecting a plant crude protein extracting solution;
3) preparing hydrolyzed vegetable protein: adjusting the pH value of the crude plant protein extract to 9-12, adjusting the temperature to 40-60 ℃, adding papain with the mass of 0.005-0.1% of that of the crude plant protein extract for enzymolysis for 1-4 h, adjusting the temperature to 70-80 ℃, and inactivating the enzyme for 10-30 min; adjusting the pH value to 3-5, centrifuging, collecting precipitate, and drying to obtain hydrolyzed vegetable protein;
the preparation method of the resin extract comprises the following steps:
1) pretreatment of resin: soaking the resin with water at 30-50 ℃ according to the mass ratio of the material to the liquid of 1 (1-5), removing bark and silt after full swelling, draining, drying, and crushing to 10-200 meshes to obtain resin powder;
2) extracting a crude resin extraction solution: putting the resin powder into water according to the mass ratio of material to liquid of 1 (1-15), adjusting the temperature to 70-80 ℃, performing ultrasonic extraction for 1-4 h with the ultrasonic power of 100-300W, filtering, and collecting the crude resin extraction liquid;
3) preparing a resin extract: adjusting the pH value of the resin crude extract to 3-6.5, adding mixed enzyme accounting for 0.001-0.02% of the mass of the resin crude extract for enzymolysis for 10-60 min, wherein the enzymolysis temperature is 45-60 ℃, then heating to 70-80 ℃, and inactivating the enzyme for 10-30 min; filtering, centrifuging the filtrate, collecting supernatant, and drying to obtain resin extract; the mixed enzyme is a mixture of pectinase and cellulase according to the mass ratio of 5: 2.
9. Use of the composition having tightening and anti-aging effects according to any one of claims 1 to 6 for the preparation of cosmetics.
10. The cosmetic is characterized by comprising the composition with the firming and anti-aging effects and auxiliary materials of any one of 1 to 6.
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