CN110946782A - Application of codonopsis pilosula oligosaccharide in preparation of cosmetics - Google Patents

Application of codonopsis pilosula oligosaccharide in preparation of cosmetics Download PDF

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CN110946782A
CN110946782A CN201911373187.9A CN201911373187A CN110946782A CN 110946782 A CN110946782 A CN 110946782A CN 201911373187 A CN201911373187 A CN 201911373187A CN 110946782 A CN110946782 A CN 110946782A
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parts
water
codonopsis pilosula
oligosaccharide
stirring
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胡芳弟
周静
李文
李雪
白瑞斌
王燕萍
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Lanzhou University
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Lanzhou University
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/60Sugars; Derivatives thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/73Polysaccharides
    • 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
    • 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
    • A61K2800/80Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
    • A61K2800/84Products or compounds obtained by lyophilisation, freeze-drying

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  • Gerontology & Geriatric Medicine (AREA)
  • Cosmetics (AREA)

Abstract

The invention discloses an application of codonopsis pilosula oligosaccharide in preparing cosmetics, wherein the content of the codonopsis pilosula oligosaccharide is 1-20%; the preparation method of the codonopsis pilosula oligosaccharide comprises the following steps: reflux-extracting radix Codonopsis coarse powder with ethanol, decocting the residue with water, mixing filtrates, concentrating, adding ethanol, sealing, centrifuging, concentrating the supernatant under reduced pressure to dry, and freeze-drying in refrigerator to obtain radix Codonopsis crude oligosaccharide; dissolving crude oligosaccharide in water, purifying, and eluting with distilled water; preparing a curve, merging the eluates according to the curve, concentrating under reduced pressure to dryness, and freeze-drying in a refrigerator to obtain the purified codonopsis pilosula oligosaccharide component. The invention has the beneficial effects that: the application of the codonopsis pilosula oligosaccharide in preparing cosmetics such as anti-aging cosmetics and whitening cosmetics can reduce skin melanin, make skin white and moist, achieve the effects of whitening and protecting skin, effectively prevent skin relaxation and skin surface wrinkle increase caused by excessive active oxygen in vivo, and have the advantages of stable property, small irritation and the like.

Description

Application of codonopsis pilosula oligosaccharide in preparation of cosmetics
Technical Field
The invention relates to the technical field of cosmetics, in particular to application of codonopsis pilosula oligosaccharide in preparation of cosmetics.
Background
The radix Codonopsis is dried root of radix Codonopsis Codonpis pilosula (Franch.) Nannf, radix Codonopsis Pilosulae Codonpis Nannf, var. modesta (Nannf.) L.T.Shen or radix Codonopsis Codonopsistsgshen Oliv. Has the functions of invigorating spleen, benefiting lung, nourishing blood and promoting fluid production. Can be used for treating deficiency of spleen-lung qi, anorexia, listlessness, cough, asthma, deficiency of qi and blood, sallow complexion, palpitation, short breath, thirst due to body fluid consumption, and internal heat. The Council of national health service committee of 11 months 1 and 2018 records the codonopsis pilosula as 'homology of medicine and food', which shows that the codonopsis pilosula can be played more greatly in more fields. The codonopsis pilosula oligosaccharide is extracted from codonopsis pilosula, has the molecular weight of 173-1384 and consists of glucose, fructose mannose, rhamnose and arabinose; has in vitro antioxidant activity comparable to that of Vc, and can scavenge free radicals, thereby achieving antioxidant effect.
Free radicals are important factors causing skin aging, air pollution, stress, drugs and the like all cause the body to generate free radicals, and ultraviolet rays are main inducers of the free radicals of the skin. Free radicals have a tendency to pair with molecules or parts of molecules that contain one or more unpaired electrons. Most radicals are therefore very reactive and have a high degree of chemical activity. Under normal conditions, free radicals in the human body are in a dynamic equilibrium with constant production and elimination. However, the free radicals are excessively generated or slowly eliminated, and can cause various damages to the body by attacking vital macromolecular substances and various cells, accelerate the aging process of the body, and show gradual aging changes, such as senile pigmentation, skin wrinkling and the like. Therefore, it is very important to strengthen the radical resistance.
Aging is also called aging, and generally refers to the phenomenon that after the organism is matured under normal conditions, the organism can decline in function, the internal environment stability and the stress ability are reduced, the structure and components gradually degenerate, and the organism tends to die and can not be reversible. Skin aging is the prevention of gradual functional and organic degenerative changes in the skin over time, manifested by the prevention of wrinkles, dryness, scaling, sagging and discolorations.
Oriental women 'beautiful white' have become iron law, and since ancient times, there is a saying 'one white covers three ugly'. Therefore, cosmetic science and technology workers invent various whitening cosmetics, and the cosmetic whitening agent also becomes the focus of industrial attention. With the development of cosmetic science, numerous whitening agents are developed and applied in succession, such as: arbutin, kojic acid, azelaic acid, niacinamide, and the like. However, the primary concern of whitening cosmetics is "safety", people gradually recognize the protective effect of melanin on human skin, such as protection against ultraviolet injury, skin photoaging and the like, and if the melanin formation is excessively intervened, the protective effect of melanin on skin is reduced while whitening skin, and skin health is influenced. In recent years, natural plant compositions have received wide attention from the industry because of their green, natural, and safe properties.
The codonopsis pilosula oligosaccharide has certain medicinal value and health care effect, but the application of the codonopsis pilosula oligosaccharide in cosmetics is rarely reported at present, and particularly, the effect on the aspects of aging resistance, whitening and the like is not reported yet.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides the application of codonopsis pilosula oligosaccharide in preparing cosmetics.
In order to achieve the purpose, the technical scheme provided by the invention is as follows: the application of the codonopsis pilosula oligosaccharide in preparing cosmetics comprises the following components in percentage by weight of 1-20%; the cosmetic is in the form of cream, lotion, emulsion, paste, powder or spray; the preparation method of the codonopsis pilosula oligosaccharide comprises the following steps: adding 10 times of 95% ethanol by mass into the coarse codonopsis pilosula powder, performing reflux extraction for 2 times for degreasing, wherein the reflux extraction time is 1 hour each time, drying alcohol extraction residues, decocting and extracting for 3 times by using 12, 10 and 10 times of water by mass, wherein the decoction extraction time is 1 hour each time, combining filtrates, concentrating until the content of medicinal materials is 1g/ml, slowly adding 95% ethanol until the final concentration of the ethanol is 80%, hermetically placing for 24 hours, centrifuging at the rotating speed of 10600 Xg for 15min, concentrating supernatant at 50 ℃ and 60rpm under reduced pressure until the supernatant is dry, adding a small amount of water, placing in a refrigerator at-80 ℃ for 4 hours, and performing freeze drying for 24 hours to obtain crude codonopsis pilosula oligosaccharides; dissolving crude oligosaccharide in a small amount of water, purifying with Sephadex G-25 of 2.6 × 70cm, eluting with distilled water at flow rate of 1mL/min, and collecting 5mL per tube; detecting with phenol-sulfuric acid method 490nm, taking test tube number as abscissa and sugar content as ordinate, making curve, mixing eluates according to curve, concentrating under reduced pressure at 50 deg.C and 60rpm to dry, dissolving with small amount of water, placing in refrigerator at-80 deg.C for 4h, and freeze drying for 24h to obtain purified radix Codonopsis oligosaccharide component.
The preparation method of the codonopsis pilosula oligosaccharide has the following principle: reflux-extracting radix Codonopsis coarse powder to obtain radix Codonopsis ethanol extract (CPEE), decocting the residue with water to obtain water extract (CPWE), extracting the water extract with water and precipitating with ethanol to obtain crude radix Codonopsis polysaccharide (CPP), volatilizing solvent from the upper layer of ethanol solution to obtain crude radix Codonopsis oligosaccharide (RCPO), and purifying with Sephadex G-25 to obtain purified radix Codonopsis oligosaccharide (PCPO).
Further, in the application, the skin cream comprises the following components in parts by weight:
1-10 parts of codonopsis pilosula oligosaccharide, 0-1 part of 1618 alcohol, 0-5 parts of lanolin, 0-6 parts of caprylic capric acid glyceride, 0-3 parts of 72/721 emulsifier, 0-5 parts of glycerin monostearate, 0-8 parts of isooctyl palmitate, 1-5 parts of glycerin, 0-5 parts of 1, 3-butanediol, 0-1.5 parts of hydroxyethyl cellulose, 0-1.5 parts of carbomer, 0-0.5 part of sodium hyaluronate, 0-0.5 part of glutathione, 0-1 part of trehalose, 0-1 part of EDTA disodium, 0-0.1 part of natural mink oil, 0-0.7 part of nylon auromethyl ester, 0-1 part of phenoxy ethanol, 0-0.1 part of essence and 44.1-98 parts of water.
Further, in the application, the skin cream comprises the following components in parts by weight:
5 parts of codonopsis pilosula oligosaccharide, 0.6 part of 1618 alcohol, 2 parts of lanolin, 3 parts of caprylic capric glyceride, 3 parts of 72/721 emulsifier, 3 parts of glyceryl monostearate, 2 parts of isooctyl palmitate, 3 parts of glycerol, 1.1 parts of hydroxyethyl cellulose, 0.3 part of carbomer sodium hyaluronate, 0.02 part of glutathione, 0.05 part of trehalose, 0.05 part of EDTA disodium, 0.02 part of natural mink oil, 0.3 part of platinum methyl nicotinate, 0.2 part of phenoxyethanol, 0.01 part of essence and 76.32 parts of water.
Further, the application and the preparation method of the moisturizer comprise the following steps:
1) putting lanolin, caprylic capric glyceride, isooctyl palmitate, glyceryl monostearate and natural mink oil into an oil phase pot according to a ratio, heating for dissolving, and stirring uniformly to obtain an oil phase; wherein the heating temperature is 70-80 ℃, and the stirring speed is 20-40 rpm; 2) heating 1618 alcohol, 72/721 emulsifier, glycerol, sodium hyaluronate, trehalose, EDTA disodium and water to dissolve, stirring uniformly, keeping the temperature, independently preparing hydroxyethyl cellulose and carbomer, dissolving them in water, stirring fully at room temperature to make them uniformly swell, and mixing to obtain transparent water phase; wherein the heating temperature is 70-80 ℃, the heat preservation time is 0.4-0.6 h, and the stirring speed is 20-40 rpm;
3) sequentially adding the oil phase prepared in the step 1) and the water phase prepared in the step 2) into an emulsifying pot, homogenizing, uniformly stirring, cooling for the first time, adding codonopsis pilosula oligosaccharide, glutathione, essence, nipagin methyl ester and phenoxyethanol according to the proportion, uniformly stirring, cooling for the second time, and discharging; wherein the homogenizing time is 3-4 min; the stirring speed is 2000-4000 rpm; the temperature is reduced to 68-72 ℃ for the first time, and the stirring speed is 20-40 rpm; and cooling to room temperature for the second time.
Further, in the application, the skin lotion comprises the following components in parts by weight:
1-5 parts of codonopsis pilosula oligosaccharide, 1-5 parts of glycerol, 0-5 parts of 1, 3-propylene glycol, 0-0.5 part of sodium hyaluronate, 0-1.5 parts of carbomer, 0-0.5 part of glutathione, 0-1 part of trehalose, 0-1 part of EDTA disodium, 0-1 part of phenoxyethanol, 0-0.1 part of essence and 79.4-98 parts of water.
Further, in the application, the skin lotion comprises the following components in parts by weight:
3 parts of codonopsis pilosula oligosaccharide, 4 parts of glycerol, 3 parts of 1, 3-propylene glycol, 0.1 part of sodium hyaluronate, 0.1 part of carbomer, 0.2 part of glutathione, 0.1 part of trehalose, 0.05 part of EDTA disodium, 1 part of phenoxyethanol, 0.01 part of essence and 88.44 parts of water.
Further, the application and the preparation method of the emollient water comprise the following steps:
adding glycerol, EDTA disodium, 1, 3-propylene glycol, carbomer, sodium hyaluronate, trehalose and deionized water into a stirring pot with the temperature controlled between 80 and 85 ℃ according to the proportion, and stirring at the stirring speed of 1500-2000r/min for 0.4 to 0.6 hours; then cooling to 40-45 ℃, adding the glutathione, the codonopsis pilosula oligosaccharide, the phenoxyethanol and the essence with the proportion in turn, continuing to pass through a stirrer, stirring at the speed of 500 plus 2000r/min, cooling to room temperature, and discharging.
Further, in the application, the emulsion comprises the following components in parts by weight:
1-8 parts of codonopsis pilosula oligosaccharide, 0-5 parts of squalane, 0-10 parts of PEG-60 hydrogenated castor oil, 0-3 parts of A165 emulsifier, 0-1.5 parts of hydroxyethyl cellulose, 0-1.5 parts of carbomer, 0-5 parts of glycerol, 0-5 parts of 1, 3-propylene glycol, 0-0.5 part of sodium hyaluronate, 0-0.5 part of glutathione, 0-1 part of trehalose, 0-1 part of EDTA disodium, 0-5 parts of ethanol, 0-0.1 part of essence, 0-0.7 part of platinum methyl ester, 0-1 part of phenoxyethanol and 63.2-99 parts of water.
Further, in the application, the emulsion comprises the following components in parts by weight:
6 parts of codonopsis pilosula oligosaccharide, 3 parts of squalane, 5 parts of PEG-60 hydrogenated castor oil, 1 part of hydroxyethyl cellulose, 2 parts of A165 emulsifier, 0.2 part of carbomer, 3 parts of glycerol, 2 parts of 1, 3-propylene glycol, 0.2 part of sodium hyaluronate, 0.1 part of glutathione, 0.1 part of trehalose, 0.2 part of EDTA disodium, 4 parts of ethanol, 0.01 part of essence, 0.3 part of platinum methyl ester, 0.2 part of phenoxyethanol and 72.69 parts of water.
Further, the application and the preparation method of the emulsion comprise the following steps:
1) adding squalane, PEG-60 hydrogenated castor oil and A165 emulsifier into an oil phase pot according to the proportion, heating to dissolve, and uniformly stirring to obtain an oil phase; wherein the heating temperature is 70-80 ℃, and the stirring speed is 20-40 rpm;
2) heating and dissolving 1, 3-propylene glycol, sodium hyaluronate, trehalose, glycerol, EDTA disodium, ethanol and water according to a ratio, uniformly stirring, preserving heat, independently preparing hydroxyethyl cellulose and carbomer, dissolving the hydroxyethyl cellulose and the carbomer in the water, fully stirring at room temperature to uniformly swell the materials, and mixing to obtain a transparent water phase; wherein the heating temperature is 75-85 ℃, the heat preservation time is 0.2-0.4 hour, and the stirring speed is 20-40 rpm;
3) sequentially adding the oil phase prepared in the step 1) and the water phase prepared in the step 2) into an emulsifying pot, homogenizing, uniformly stirring, cooling for the first time, adding the codonopsis pilosula oligosaccharide, glutathione, essence, nipagin methyl ester and phenoxyethanol in the matched amount, uniformly stirring, cooling for the second time, and discharging; wherein, the homogenizing time is 3-4min, and the stirring speed is 2000-; the temperature is reduced to 68-72 ℃ for the first time, and the stirring speed is 20-40 rpm; and cooling to room temperature for the second time.
The invention has the beneficial effects that: the application of the codonopsis pilosula oligosaccharide in preparing cosmetics such as anti-aging cosmetics and whitening cosmetics can reduce skin melanin, make skin white and moist, achieve the effects of whitening and protecting skin, effectively prevent skin relaxation and skin surface wrinkle increase caused by excessive active oxygen in vivo, and have the advantages of stable property, small irritation and the like.
Drawings
FIG. 1 shows the DPPH scavenging effect curve of Codonopsis oligosaccharide.
FIG. 2 is a graph showing the scavenging effect of Codonopsis pilosula oligosaccharide on superoxide anion.
FIG. 3 shows the results of the activities of SOD, GSH-Px, CAT and MDA in the serum of rats in each group under the action of Codonopsis pilosula oligosaccharide.
FIG. 4 shows the levels of SOD and CAT activity in liver tissues of rats in each group under the action of Codonopsis pilosula oligosaccharide.
Detailed Description
The application of the codonopsis pilosula oligosaccharide in preparing cosmetics comprises the following components in percentage by weight of 1-20%; the cosmetic is in the form of cream, lotion, emulsion, paste, powder or spray; the preparation method of the codonopsis pilosula oligosaccharide comprises the following steps: adding 10 times of 95% ethanol by mass into the coarse codonopsis pilosula powder, carrying out reflux extraction for 2 times for degreasing, wherein the reflux extraction time is 1h each time, airing alcohol extraction dregs, decocting and extracting for 3 times by using 12, 10 and 10 times of water by mass, wherein the decoction extraction time is 1h each time, combining filtrates, concentrating until the content of medicinal materials is 1g/ml, slowly adding 95% ethanol until the final concentration of the ethanol is 80%, hermetically placing for 24h, centrifuging (10600 Xg, 15min), concentrating supernate under reduced pressure (50 ℃,60rpm) until the supernate is dry, adding a small amount of water, placing in a refrigerator at minus 80 ℃ for 4h, and carrying out freeze drying (24h) to obtain the crude codonopsis pilosula oligosaccharide. Dissolving crude oligosaccharide in a small amount of water, purifying with SephadexG-25(2.6 × 70cm), eluting with distilled water at an elution flow rate of 1mL/min, and collecting 5mL per tube; detecting with phenol-sulfuric acid method 490nm, taking test tube number as abscissa and sugar content as ordinate, making curve, mixing eluates according to curve, concentrating under reduced pressure (50 deg.C, 60rpm) to dry, dissolving with small amount of water, placing in refrigerator at-80 deg.C for 4h, and freeze drying (24h) to obtain purified radix Codonopsis oligosaccharide component.
Example 1:
the skin cream prepared from the codonopsis pilosula oligosaccharide contains the following components in parts by weight:
1-10g of codonopsis pilosula oligosaccharide, 0-1g of 1618 alcohol, 0-5g of lanolin, 0-6g of caprylic capric glyceride, 0-3g of 72/721 emulsifier, 0-5g of glyceryl monostearate, 0-8g of isooctyl palmitate, 1-5g of glycerol, 0-5g of 1, 3-butanediol, 0-1.5g of hydroxyethyl cellulose, 0-1.5g of carbomer, 0-0.5g of sodium hyaluronate, 0-0.5g of glutathione, 0-1g of trehalose, 0-1g of EDTA disodium, 0-0.1g of natural mink oil, 0-0.7g of Niplatin methyl ester, 0-1g of phenoxy ethanol, 0-0.1g of essence and 44.1-98g of water.
Wherein, the most preferred technical scheme is as follows:
5g of codonopsis pilosula oligosaccharide, 0.6g of 1618 alcohol, 2g of lanolin, 3g of caprylic capric glyceride, 3g of 72/721 emulsifier, 3g of glyceryl monostearate, 2g of isooctyl palmitate, 3g of glycerol, 1.1g of hydroxyethyl cellulose, 0.3g of carbomer, 0.03g of sodium hyaluronate, 0.02g of glutathione, 0.05g of trehalose, 0.05g of disodium EDTA (ethylene diamine tetraacetic acid), 0.02g of natural mink oil, 0.3g of methyl nicotinplatinum, 0.2g of phenoxyethanol, 0.01g of essence and 76.32g of water.
The preparation method of the codonopsis pilosula oligosaccharide moisturizer comprises the following steps:
1) putting lanolin, caprylic capric glyceride, isooctyl palmitate, glyceryl monostearate and natural mink oil into an oil phase pot according to a ratio, heating for dissolving, and stirring uniformly to obtain an oil phase; wherein the heating temperature is 70-80 ℃, and the stirring speed is 20-40 rpm; 2) heating 1618 alcohol, 72/721 emulsifier, glycerol, sodium hyaluronate, trehalose, EDTA disodium and water to dissolve, stirring uniformly, keeping the temperature, independently preparing hydroxyethyl cellulose and carbomer, dissolving them in water, stirring fully at room temperature to make them uniformly swell, and mixing to obtain transparent water phase; wherein the heating temperature is 70-80 ℃, the heat preservation time is 0.4-0.6 h, and the stirring speed is 20-40 rpm;
3) sequentially adding the oil phase prepared in the step 1) and the water phase prepared in the step 2) into an emulsifying pot, homogenizing, uniformly stirring, cooling for the first time, adding codonopsis pilosula oligosaccharide, glutathione, essence, nipagin methyl ester and phenoxyethanol according to the proportion, uniformly stirring, cooling for the second time, and discharging; wherein the homogenizing time is 3-4 min; the stirring speed is 2000-4000 rpm; the temperature is reduced to 68-72 ℃ for the first time, and the stirring speed is 20-40 rpm; and cooling to room temperature for the second time.
Example 2:
the skin lotion prepared from the codonopsis pilosula oligosaccharide contains the following components in parts by weight:
1-5g of codonopsis pilosula oligosaccharide, 1-5g of glycerol, 0-5g of 1, 3-propylene glycol, 0-0.5g of sodium hyaluronate, 0-1.5g of carbomer, 0-0.5g of glutathione, 0-1g of trehalose, 0-1g of EDTA disodium, 0-1g of phenoxyethanol, 0-0.1g of essence and 79.4-98g of water.
Wherein, the most preferred technical scheme is as follows:
3g of codonopsis pilosula oligosaccharide, 4g of glycerol, 3g of 1, 3-propylene glycol, 0.1g of sodium hyaluronate, 0.1g of carbomer, 0.2g of glutathione, 0.1g of trehalose, 0.05g of EDTA disodium, 1g of phenoxyethanol, 0.01g of essence and 88.44g of water.
The preparation method of the codonopsis pilosula oligosaccharide skin lotion comprises the following steps:
adding glycerol, EDTA disodium, 1, 3-propylene glycol, carbomer, sodium hyaluronate, trehalose and deionized water into a stirring pot with the temperature controlled between 80 and 85 ℃ according to the proportion, and stirring at the stirring speed of 1500-2000r/min for 0.4 to 0.6 hours; then cooling to 40-45 ℃, adding the glutathione, the codonopsis pilosula oligosaccharide, the phenoxyethanol and the essence with the proportion in turn, continuing to pass through a stirrer, stirring at the speed of 500 plus 2000r/min, cooling to room temperature, and discharging.
Example 3:
the emulsion prepared from the codonopsis pilosula oligosaccharide contains the following components in parts by weight:
1-8g of codonopsis pilosula oligosaccharide, 0-5g of squalane, 0-10g of PEG-60 hydrogenated castor oil, 0-3g of A165 emulsifier, 0-1.5g of hydroxyethyl cellulose, 0-1.5g of carbomer, 0-5g of glycerol, 0-5g of 1, 3-propylene glycol, 0-0.5g of sodium hyaluronate, 0-0.5g of glutathione, 0-1g of trehalose, 0-1g of EDTA disodium, 0-5g of ethanol, 0-0.1g of essence, 0-0.7g of Niplatinum methyl ester, 0-1g of phenoxyethanol and 63.2-99g of water.
Wherein, the most preferred technical scheme is as follows:
6g of codonopsis pilosula oligosaccharide, 3g of squalane, 5g of PEG-60 hydrogenated castor oil, 1g of hydroxyethyl cellulose, 2g of A165 emulsifier, 0.2g of carbomer, 3g of glycerol, 2g of 1, 3-propylene glycol, 0.2g of sodium hyaluronate, 0.1g of glutathione, 0.1g of trehalose, 0.2g of EDTA disodium, 4g of ethanol, 0.01g of essence, 0.3g of platinum methyl ester, 0.2g of phenoxyethanol and 72.69g of water.
The preparation method of the codonopsis pilosula oligosaccharide emulsion comprises the following steps:
1) adding squalane, PEG-60 hydrogenated castor oil and A165 emulsifier into an oil phase pot according to the proportion, heating to dissolve, and uniformly stirring to obtain an oil phase; wherein the heating temperature is 70-80 ℃, and the stirring speed is 20-40 rpm;
2) heating and dissolving 1, 3-propylene glycol, sodium hyaluronate, trehalose, glycerol, EDTA disodium, ethanol and water according to a ratio, uniformly stirring, preserving heat, independently preparing hydroxyethyl cellulose and carbomer, dissolving the hydroxyethyl cellulose and the carbomer in the water, fully stirring at room temperature to uniformly swell the materials, and mixing to obtain a transparent water phase; wherein the heating temperature is 75-85 ℃, the heat preservation time is 0.2-0.4 hour, and the stirring speed is 20-40 rpm;
3) sequentially adding the oil phase prepared in the step 1) and the water phase prepared in the step 2) into an emulsifying pot, homogenizing, uniformly stirring, cooling for the first time, adding the codonopsis pilosula oligosaccharide, glutathione, essence, nipagin methyl ester and phenoxyethanol in the matched amount, uniformly stirring, cooling for the second time, and discharging; wherein, the homogenizing time is 3-4min, and the stirring speed is 2000-; the temperature is reduced to 68-72 ℃ for the first time, and the stirring speed is 20-40 rpm; and cooling to room temperature for the second time.
Comparative example 1:
the skin cream comprises the following components:
1618 g of alcohol 0.6g, lanolin 2g, caprylic capric glyceride 3g, 72/721 g of emulsifier 3g, glyceryl monostearate 3g, isooctyl palmitate 2g, glycerin 3g, hydroxyethyl cellulose 1.1g, carbomer 0.3g, sodium hyaluronate 0.03g, glutathione 0.02g, trehalose 0.05g, EDTA disodium 0.05g, natural mink oil 0.02g, platinum methyl nicotinate 0.3g, phenoxyethanol 0.2g, essence 0.01g and water 81.33 g.
The preparation method of the skin cream comprises the following steps:
1) putting lanolin, caprylic capric glyceride, isooctyl palmitate, glyceryl monostearate and natural mink oil into an oil phase pot according to a ratio, heating for dissolving, and stirring uniformly to obtain an oil phase; wherein the heating temperature is 70-80 ℃, and the stirring speed is 20-40 rpm;
2) heating 1618 alcohol, 72/721 emulsifier, glycerol, sodium hyaluronate, trehalose, EDTA disodium and water to dissolve, stirring uniformly, keeping the temperature, independently preparing hydroxyethyl cellulose and carbomer, dissolving them in water, stirring fully at room temperature to make them uniformly swell, and mixing to obtain transparent water phase; wherein the heating temperature is 70-80 ℃, the heat preservation time is 0.4-0.6 h, and the stirring speed is 20-40 rpm;
3) sequentially adding the oil phase prepared in the step 1) and the water phase prepared in the step 2) into an emulsifying pot, homogenizing, uniformly stirring, cooling for the first time, adding glutathione, essence, nipagin methyl ester and phenoxyethanol according to the proportion, uniformly stirring, cooling for the second time, and discharging; wherein the homogenizing time is 3-4 min; the stirring speed is 2000-4000 rpm; the temperature is reduced to 68-72 ℃ for the first time, and the stirring speed is 20-40 rpm; and cooling to room temperature for the second time.
Comparative example 2:
the skin lotion comprises the following components:
4g of glycerol, 3g of 1, 3-propylene glycol, 0.1g of sodium hyaluronate, 0.1g of carbomer, 0.2g of glutathione, 0.1g of trehalose, 0.05g of EDTA disodium, 1g of phenoxyethanol, 0.01g of essence and 91.45g of water.
The preparation method of the emollient water comprises the following steps:
adding glycerol, EDTA disodium, 1, 3-propylene glycol, carbomer, sodium hyaluronate, trehalose and deionized water into a stirring pot with the temperature controlled between 80 and 85 ℃ according to the proportion, and stirring at the stirring speed of 1500-2000r/min for 0.4 to 0.6 hours; then the temperature is reduced to 40-45 ℃, the glutathione, the phenoxyethanol and the essence with the proportion are sequentially added, the mixture is continuously stirred by a stirrer at the stirring speed of 500 plus 2000r/min, the temperature is reduced to the room temperature, and the material is discharged.
Comparative example 3:
the emulsion comprises the following components:
3g of squalane, 5g of PEG-60 hydrogenated castor oil, 1g of hydroxyethyl cellulose, 2g of A165 emulsifier, 0.2g of carbomer, 3g of glycerol, 2g of 1, 3-propylene glycol, 0.2g of sodium hyaluronate, 0.1g of glutathione, 0.1g of trehalose, 0.2g of EDTA disodium, 4g of ethanol, 0.01g of essence, 0.3g of platinum methyl nicotinate, 0.2g of phenoxyethanol and 78.70g of water.
A method of preparing an emulsion comprising the steps of:
1) adding squalane, PEG-60 hydrogenated castor oil and A165 emulsifier into an oil phase pot according to the proportion, heating to dissolve, and uniformly stirring to obtain an oil phase; wherein the heating temperature is 70-80 ℃, and the stirring speed is 20-40 rpm;
2) heating and dissolving 1, 3-propylene glycol, sodium hyaluronate, trehalose, glycerol, EDTA disodium, ethanol and water according to a ratio, uniformly stirring, preserving heat, independently preparing hydroxyethyl cellulose and carbomer, dissolving the hydroxyethyl cellulose and the carbomer in the water, fully stirring at room temperature to uniformly swell the materials, and mixing to obtain a transparent water phase; wherein the heating temperature is 75-85 ℃, the heat preservation time is 0.2-0.4 hour, and the stirring speed is 20-40 rpm;
3) sequentially adding the oil phase prepared in the step 1) and the water phase prepared in the step 2) into an emulsifying pot, homogenizing, uniformly stirring, cooling for the first time, adding glutathione, essence, methyl nicotinovolvate and phenoxyethanol in the ratio amount, uniformly stirring, cooling for the second time, and discharging; wherein, the homogenizing time is 3-4min, and the stirring speed is 2000-; the temperature is reduced to 68-72 ℃ for the first time, and the stirring speed is 20-40 rpm; and cooling to room temperature for the second time.
The whitening effect of the codonopsis pilosula oligosaccharide is evaluated by adopting the in-vitro antioxidant capacity and the skin melanin reduction rate.
The invention adopts skin texture and elasticity tests and an aging model of the SD rat induced by D-galactose to directly evaluate the anti-aging activity of the codonopsis pilosula oligosaccharide, and the SD rat induced by the D-galactose has the following advantages:
d-galactose is a reducing sugar that is converted at high levels to aldoses and hydrogen peroxide catalyzed by galactose oxidase, producing superoxide anions and oxygen radicals. These changes are very similar to the normal aging process and also to the model of natural aging, manifested by neurological dysfunction, decreased antioxidant enzyme activity and poor immune response.
Effect verification:
1. determination of antioxidant capacity of codonopsis pilosula oligosaccharide
1.1 reagents and instruments
DPPH (Chishiai chemical industry development Co., Ltd.), pyrogallol (Tianjin Mao chemical reagent factory), and water as double distilled water; other reagents are analytically pure reagents;
759S ultraviolet and visible spectrophotometer (Shanghai prismatic light technology, Inc.); HH-2 constant temperature water bath (Guohua electric appliance Co., Ltd.)
1.2 Experimental methods
1.2.1DPPH free radical scavenging experiment comprises the following specific steps:
preparing radix Codonopsis oligosaccharide by the above method, and adding water to obtain solutions to be detected with different concentrations;
the specific steps of the DPPH free radical scavenging experiment are as follows:
mixing the same volume (2mL) of the solution to be detected with 0.2mmol/L DPPH solution (A)Sample (A));
Mixing equal volume (2mL) of anhydrous ethanol with 0.2mmol/L of DPPH solution (A)Air conditioner);
After 30min of light shielding, A is measured at 517nmSample (A)、AAir conditionerAn absorbance value.
Clearance calculation formula: clearance (%) ═ aSample (A)-AAir conditioner)/AAir conditioner
The removal effect curve of Codonopsis oligosaccharide on DPPH is prepared by taking Codonopsis oligosaccharide concentration as abscissa and DPPH removal rate as ordinate, and is shown in FIG. 1.
1.2.2 specific procedures for superoxide anion scavenging experiments were:
preparing the extract of the decoction for invigorating middle-jiao and replenishing qi according to the above preparation method, and adding water to obtain solutions to be tested with different concentrations;
taking 3.8mL of Tris-HCl buffer solution with the pH value of 8.2 and 0.5mmol/L of Tris-HCl buffer solution with the pH value of 8.2, placing the Tris-HCl buffer solution in a test tube, respectively placing 0.1mL of solution to be detected, uniformly mixing, and placing in a water bath at the temperature of 25 ℃ for 10 min;
taking out, rapidly adding 0.1mL (10mmol/L) of pyrogallol with the temperature of 25 deg.C kept for 10min, shaking, standing for 30min, and measuring absorbance A1 at 320 nm.
The absorbance A2 is measured by replacing pyrogallol with distilled water, and the absorbance A3 is measured by replacing a sample with distilled water;
clearance calculation formula: clearance (%) ═ 1- (A1-A2)/A3
The concentration of the codonopsis pilosula oligosaccharide is used as an abscissa, and the superoxide anion removal rate is used as an ordinate, so that a curve of the effect of the codonopsis pilosula oligosaccharide on removing superoxide anions is prepared, and the curve is shown in figure 2.
1.3 analysis of results
As can be seen from figure 1, the removal rate of the codonopsis pilosula oligosaccharide to DPPH is very obvious, and the DPPH removal rate reaches 93% when the concentration of the codonopsis pilosula oligosaccharide is 3mg/ml, which indicates that the codonopsis pilosula oligosaccharide has very strong oxidation resistance and can scavenge free radicals, promote cellular metabolism, enhance cellular activity, improve the structure and function of an organism and improve the vitality of the organism, so that the aging of cells is delayed and the anti-aging effect of the codonopsis pilosula oligosaccharide is exerted.
As can be seen from FIG. 2, the dangshen oligosaccharide has a certain scavenging effect on superoxide anions, and the scavenging effect is gradually enhanced along with the increase of the concentration of the dangshen oligosaccharide, which shows that the capability of the dangshen oligosaccharide in scavenging superoxide anions and the concentration thereof have an energy-effect relationship, when the concentration of the dangshen oligosaccharide is 12mg/ml, the DPPH scavenging rate reaches 99%, and 50% of the superoxide anions need to be scavenged by dangshen micromolecule sugar with the concentration of 4.5 mg/ml.
2. Determination of anti-aging capability of codonopsis pilosula oligosaccharide to D-galactose-induced SD rat
2.1 Experimental materials and instruments
2.1.1 Experimental animals
72 SD rats, female, 6-8 weeks old, were provided by the laboratory animal center, Lanzhou university.
2.1.2 drugs and reagents
Codonopsis Pilosula Oligosaccharide (PCPO), Codonopsis pilosula is provided by Weiyuan county of Gansu province, Codonopsis pilosula oligosaccharide is prepared by this subject group: extracting radix Codonopsis coarse powder with 10 times of 95% ethanol under reflux twice (1 h/time) for defatting, air drying the residue, decocting with 12, 10 times of water for three times (1 h/time), mixing filtrates, concentrating to 1g/ml (each ml is equivalent to 1g of medicinal material, slowly adding 95% ethanol until the final concentration of ethanol is 80%, sealing, standing for 24h, centrifuging, precipitating, freeze drying to obtain radix Codonopsis polysaccharide, concentrating the supernatant under reduced pressure to obtain radix Codonopsis oligosaccharide, D-galactose (Shanghai Michelin Biotechnology Co., Ltd.), vitamin E (Beijing Sorbao Tech technologies Co., Ltd.), SOD, GSH-Px, CAT, and MDA detection kit (Nanjing institute of bioengineering research).
2.2 Experimental methods
2.2.1 pharmaceutical formulation
(1) D-galactose preparation: dissolving D-galactose in 0.9% physiological saline to obtain a volume concentration of 40mg/ml, and storing in a refrigerator at 4 deg.C for use.
(2) Preparing PCPO: before the experiment, each reagent is prepared into the required concentration (23mg/mL, 40mg/mL and 70mg/mL distilled water) by using distilled water and stored in a refrigerator at 4 ℃ for later use.
(3) Vit E preparation: the solution was prepared in 20mg/mL vegetable oil. Storing in a refrigerator at 4 deg.C for use.
2.2.2 Experimental animal groups and dosing
(1) Healthy birth-age SD rats are purchased from Lanzhou university animal center, female, and the weight of the SD rats is 180-. The animal was acclimated for 7 days before the behavioral screening experiment.
(2) The pre-screened SD rats were randomly divided into a normal control group (Normal), a Model group (Model), a PCPO treatment group of 12 rats each, a low dose group (PCPO-L), a medium dose group (PCPO-M), a high dose group (PCPO-H), and a positive control Vitamin E (VE) group. Except for the control group, the mice of other groups are injected with 200mg/kg of D-galactose per day (the injection volume is 10mL/kg) in an intraperitoneal mode 1 time per day for 14 consecutive days, and the normal control group is injected with the same volume of normal saline subcutaneously. While the PCPO treatment group and the positive control group continue to inject D-galactose, 3 PCPO (230mg/kg/D, 400mg/kg/D, 700mg/kg/D) and vitamin E (200mg/kg/D) with different dosages are respectively gavaged, and distilled water with the same amount as that of the normal control group and the model group is gavaged for 28 days continuously.
2.2.3 preparation of homogenate
(1) Serum preparation: the abdominal aorta of the rat is used for blood taking, a non-anticoagulation blood collection tube is moved into the abdominal aorta, after standing for 2 hours, the abdominal aorta is centrifuged for 15min in a low-speed centrifuge (3000r/min) to separate serum.
(2) Liver tissue: after the rats were sacrificed, the abdominal cavity was quickly cut open, the liver tissues of the rats were separated and taken out, washed with ice physiological saline at 4 ℃ to remove blood, and blotted with filter paper. A10% liver homogenate was prepared with 4 ℃ pre-cooled physiological saline. Centrifuging 10% of the homogenate for 10-15min at 4 deg.C at 2000r/min, and collecting supernatant.
2.2.4 index detection
The content of Malondialdehyde (MDA), superoxide dismutase (SOD) activity, hydrogen peroxide (CAT) and glutathione peroxidase (GSH-PX) in rat serum were measured. The superoxide dismutase (SOD) activity and glutathione peroxidase (GSH-PX) activity in rat liver tissues were measured.
2.3 analysis of results
And (4) processing and analyzing experimental data by adopting SPSS19.0 software. The results are as follows
FIG. 3 shows the results of SOD, GSH-Px, CAT and MDA activities in the serum of rats in each group (wherein # P <0.05# # P <0.01# # P <0.001 in comparison with the normal control group; P <0.05 × P <0.01 × P <0.001 in comparison with the model group). The Model group was significantly different from the Normal group. GSH-Px and CAT of the groups except PCPO-L have no significant difference with the Model group, and compared with the Model group, SOD, GSH-Px and CAT activities of the rest dose groups of the VE group and the PCPO are all increased and have significant difference. The MDA content in the serum of the rats in each group is reduced compared with that in the Model group, and the statistical significance is achieved.
The levels of SOD and CAT activity in liver tissues of mice in each group are shown in FIG. 4 (wherein # P <0.05# # P <0.01# # P <0.001 in comparison with the normal control group; and <0.05 × P <0.01 × P <0.001 in comparison with the model group). Each index was reduced in the Model group compared to the Normal group. Compared with the Model group, the dose groups of the VE group and the PCPO group are increased, and the difference is significant.
The result shows that the codonopsis pilosula oligosaccharide has a protective effect on a D-galactose-induced peroxidation damage model mouse, and the increase of the activity of the antioxidant enzyme can promote the body to be free from oxidative damage, so that the codonopsis pilosula oligosaccharide has a protective effect.
3. Evaluation of product index
The comparative example differs from the examples in that: it does not contain dangshen oligosaccharide.
The codonopsis pilosula oligosaccharide cosmetics prepared in the examples 1 to 3 are tested:
3.1 stability test
(1) Heat resistance test: the heat resistance of the samples of examples 1 to 3 was evaluated by placing the samples in a 40 ℃ thermostat for 24 hours, and observing whether oil-water separation occurred after the samples were cooled to room temperature.
(2) Cold resistance test: the cold resistance of the steel is evaluated by placing the steel of examples 1 to 3 in a refrigerator at-5 to 10 ℃ for 24 hours, and observing whether oil-water separation occurs after the steel is cooled to room temperature.
(3) Cold-hot cycling test: in examples 1 to 3, "constant temperature at 40 ℃ for 12h → constant temperature at 25 ℃ for 12h → constant temperature at-20 ℃ for 12h → constant temperature at 25 ℃ for 12 h", respectively, was continued for two cycles. The operation is the same as the heat and cold resistance test.
(4) Determination of pH: accurately weighing 30.1000 g of example 1 and example respectively, adding 10mL of boiled and cooled secondary water, heating to 40 ℃, continuously stirring to be uniform, cooling to room temperature, and measuring by a pH meter (pH 4.0-8.5); an appropriate amount of example 2 was accurately weighed into a beaker and measured by a pH meter (pH 4.0-8.5).
(5) And (3) centrifugal test: an appropriate amount of the mixture obtained in example 1 and example 3 was placed in a centrifuge tube, centrifuged at 2000r/min for 30min, and then whether or not the stratification phenomenon occurred was observed.
3.2 sanitary requirements
According to a standard detection method of microorganisms in cosmetics in the cosmetic hygiene Specification (2015 edition), the total number of bacteria, the total number of mold and yeast, faecal coliform bacteria, staphylococcus aureus and pseudomonas aeruginosa in the cosmetics are detected according to the relevant requirements of skin moistening cream QB/T1857 + 2013, cosmetic water GB/T2660 + 2004 and skin care emulsion GB/T29665 + 2013.
3.3 analysis of results
Table 1 shows the stability tests of the examples.
TABLE 1
Heat resistance Cold-resistant Alternating cold and hot Centrifugation pH value Whether it is qualified or not
Example 1 - - - - 6.7 Is that
Example 2 - - - 7.7 Is that
Example 3 - - - - 7.0 Is that
"+" indicates delamination, and "-" indicates no delamination
As can be seen from the results in Table 1, the stability tests in examples 1 to 3 respectively meet the relevant requirements of skin moistening cream QB/T1857-2013, cosmetic water GB/T2660-2004 and skin care emulsion GB/T29665-2013.
Table 2 shows the detection of microorganisms in the examples.
TABLE 2
Microbiological indicator Limit amount Example 1 Example 2 Example 3
Total number of colonies (CFU/g or CFU/mL) ≤1000 Not detected out Not detected out Not detected out
Fecal coliform bacteria/g (or mL) Cannot be detected Not detected out Not detected out Not detected out
Staphylococcus aureus/g (or mL) Cannot be detected Not detected out Not detected out Not detected out
Pseudomonas aeruginosa/g (or mL) Cannot be detected Not detected out Not detected out Not detected out
Mold, Yeast (CFU/g or CFU/mL) ≤100 Not detected out Not detected out Not detected out
As is clear from Table 2, the total number of bacteria, the total number of mold and yeast, the fecal coliform group, the Staphylococcus aureus group, and the Pseudomonas aeruginosa in examples 1 to 3 meet the regulations of the cosmetic hygiene Specification (2015).
4. Skin texture, elasticity test and melanin test
4.1 test population
120 wrinkled persons with average age of 25-55 years old. Wherein 30 men and 90 women have no damage to skin health. Each example and comparative example 20 subjects.
4.2 Experimental materials and instruments
Skin image analysis System (Skin Visimeter SV600), Skin elasticity tester (Cutomer duolMPA 580) Skin melanin tester (Cutomer MPA580, Germany)
4.3 Experimental methods
4.3.1 skin texture test
The test areas were selected from the same amount of the cosmetics of examples and comparative examples, and the test areas were selected from the left and right cheekbones of the face, the left and right cheeks of the intersection of the nose tip and the pupil, and the left and right sides of the intersection of the temple and the mouth corner. Applied twice daily, morning and evening, during the experiment, the subject was unable to apply any other cosmetic. The texture of the Skin at the test site was measured five times per spot and averaged by a technician using a Skin image analysis system (Skin visualizer SV 600). Subjects after four weeks of continuous application of the cosmetics, Skin texture was tested using a Skin image analysis system (Skin visiomerer sv 600).
The number of each measurement at the test site of the subject was counted, and the skin texture change rate was compared and analyzed on the basis of week 0 to evaluate the improvement of the skin texture by the cosmetic preparations of examples and comparative examples. (each subject was measured by the same technician) four weeks (28 days) after using the product, Table 3 shows the statistics of skin texture changes due to Codonopsis oligosaccharide.
TABLE 3
Figure BDA0002340243280000131
4.3.2 skin elasticity test.
Taking the cosmetics of examples and comparative examples, the test areas of the left and right cheekbones of the face, the left and right cheeks at the intersection of the nose tip and the pupil, and the left and right sides at the intersection of the temple and the mouth corner are selected and applied twice a day in the morning and evening, and the test subjects can not apply any other cosmetics during the test period. The changes in the elasticity values of the applied areas were measured by a test population using the example and comparative cosmetics and then using a skin elasticity tester (current meter dual MPA580) under the direction of the skilled person. (Each subject was measured by the same technician each time)
The values measured at each time of the test sites of the subjects were counted, and the skin elasticity change rates were compared and analyzed on the basis of week 0 to evaluate the improvement of the skin elasticity by the cosmetics of examples and comparative examples. After four weeks (28 days) of use of the product, Table 4 shows the statistics of the skin elasticity changes under the effect of the Codonopsis oligosaccharides.
TABLE 4
Figure BDA0002340243280000141
4.3.3 skin melanin test
Taking the cosmetics of examples and comparative examples, the test areas of the left and right cheekbones of the face, the left and right cheeks at the intersection of the nose tip and the pupil, and the left and right sides at the intersection of the temple and the mouth corner are selected and applied twice a day in the morning and evening, and the test subjects can not apply any other cosmetics during the test period. The changes in the melanin values at the application sites were determined by a panel of test persons using the example and comparative cosmetics and then using a skin melanin tester (Cutometer MPA580, germany) under the direction of the skilled person. (Each subject was measured by the same technician each time)
The number of each measurement at the test site of the subject was counted, and the skin melanin change rate was compared and analyzed on the basis of week 0 to evaluate the improvement of skin melanin in the cosmetic preparations of examples and comparative examples. The test results of 20 subjects per group were averaged, and the melanin reduction rate was calculated according to the following formula. The higher the melanin reduction rate, the more obvious the whitening effect. The melanin reduction rate was calculated by the following formula. The higher the melanin reduction rate, the more obvious the whitening effect. The melanin reduction rate is (melanin content before use for 1 day-melanin content after 28 consecutive days) ÷ melanin content before use for 1 day × 100%. After four weeks (28 days) of use of the above product, Table 5 shows the statistics of skin melanin changes under the effect of Codonopsis oligosaccharide.
TABLE 5
Melanin reduction ratio (%)
Example 1 79.9
Example 2 68.3
Example 3 77.2
Comparative example 1 39.3
Comparative example 2 23.1
Comparative example 3 40.1
4.4 analysis of results
The results in tables 3 and 4 show that: the subjects of the comparative examples showed a general improvement in skin elasticity and texture after 4 weeks of use, while the subjects of the examples showed a significant improvement in skin elasticity and texture after 4 weeks of use, especially the skin elasticity and texture of example 1 was significantly improved compared to that of comparative example 1, indicating that the anti-aging effect of the product was significantly improved. As can be seen from table 5, the skin melanin reduction rate of the test subjects in the comparative examples is general after 4 weeks of use, while the melanin reduction rate of the test subjects in the examples is obvious after 4 weeks of use, which indicates that the whitening effect of the product is obviously improved.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (10)

1. The application of the codonopsis pilosula oligosaccharide in preparing cosmetics is characterized in that the content of the codonopsis pilosula oligosaccharide in the cosmetics is 1-20% by weight; the cosmetic is in the form of cream, lotion, emulsion, paste, powder or spray; the preparation method of the codonopsis pilosula oligosaccharide comprises the following steps: adding 10 times of 95% ethanol by mass into the coarse codonopsis pilosula powder, performing reflux extraction for 2 times for degreasing, wherein the reflux extraction time is 1 hour each time, drying alcohol extraction residues, decocting and extracting for 3 times by using 12, 10 and 10 times of water by mass, wherein the decoction extraction time is 1 hour each time, combining filtrates, concentrating until the content of medicinal materials is 1g/ml, slowly adding 95% ethanol until the final concentration of the ethanol is 80%, hermetically placing for 24 hours, centrifuging at the rotating speed of 10600 Xg for 15min, concentrating supernatant at 50 ℃ and 60rpm under reduced pressure until the supernatant is dry, adding a small amount of water, placing in a refrigerator at-80 ℃ for 4 hours, and performing freeze drying for 24 hours to obtain crude codonopsis pilosula oligosaccharides; dissolving crude oligosaccharide in a small amount of water, purifying with Sephadex G-25 of 2.6 × 70cm, eluting with distilled water at flow rate of 1mL/min, and collecting 5mL per tube; detecting with phenol-sulfuric acid method 490nm, taking test tube number as abscissa and sugar content as ordinate, making curve, mixing eluates according to curve, concentrating under reduced pressure at 50 deg.C and 60rpm to dry, dissolving with small amount of water, placing in refrigerator at-80 deg.C for 4h, and freeze drying for 24h to obtain purified radix Codonopsis oligosaccharide component.
2. The use according to claim 1, wherein the cream comprises the following components in parts by weight: 1-10 parts of codonopsis pilosula oligosaccharide, 0-1 part of 1618 alcohol, 0-5 parts of lanolin, 0-6 parts of caprylic capric acid glyceride, 0-3 parts of 72/721 emulsifier, 0-5 parts of glycerin monostearate, 0-8 parts of isooctyl palmitate, 1-5 parts of glycerin, 0-5 parts of 1, 3-butanediol, 0-1.5 parts of hydroxyethyl cellulose, 0-1.5 parts of carbomer, 0-0.5 part of sodium hyaluronate, 0-0.5 part of glutathione, 0-1 part of trehalose, 0-1 part of EDTA disodium, 0-0.1 part of natural mink oil, 0-0.7 part of nylon auromethyl ester, 0-1 part of phenoxy ethanol, 0-0.1 part of essence and 44.1-98 parts of water.
3. The use according to claim 2, wherein the cream comprises the following components in parts by weight: 5 parts of codonopsis pilosula oligosaccharide, 0.6 part of 1618 alcohol, 2 parts of lanolin, 3 parts of caprylic capric glyceride, 3 parts of 72/721 emulsifier, 3 parts of glyceryl monostearate, 2 parts of isooctyl palmitate, 3 parts of glycerol, 1.1 parts of hydroxyethyl cellulose, 0.3 part of carbomer sodium hyaluronate, 0.02 part of glutathione, 0.05 part of trehalose, 0.05 part of EDTA disodium, 0.02 part of natural mink oil, 0.3 part of platinum methyl nicotinate, 0.2 part of phenoxyethanol, 0.01 part of essence and 76.32 parts of water.
4. The use according to claim 2 or 3, wherein the preparation method of the skin cream comprises the following steps:
1) putting lanolin, caprylic capric glyceride, isooctyl palmitate, glyceryl monostearate and natural mink oil into an oil phase pot according to a ratio, heating for dissolving, and stirring uniformly to obtain an oil phase; wherein the heating temperature is 70-80 ℃, and the stirring speed is 20-40 rpm;
2) heating 1618 alcohol, 72/721 emulsifier, glycerol, sodium hyaluronate, trehalose, EDTA disodium and water to dissolve, stirring uniformly, keeping the temperature, independently preparing hydroxyethyl cellulose and carbomer, dissolving them in water, stirring fully at room temperature to make them uniformly swell, and mixing to obtain transparent water phase; wherein the heating temperature is 70-80 ℃, the heat preservation time is 0.4-0.6 h, and the stirring speed is 20-40 rpm;
3) sequentially adding the oil phase prepared in the step 1) and the water phase prepared in the step 2) into an emulsifying pot, homogenizing, uniformly stirring, cooling for the first time, adding codonopsis pilosula oligosaccharide, glutathione, essence, nipagin methyl ester and phenoxyethanol according to the proportion, uniformly stirring, cooling for the second time, and discharging; wherein the homogenizing time is 3-4 min; the stirring speed is 2000-4000 rpm; the temperature is reduced to 68-72 ℃ for the first time, and the stirring speed is 20-40 rpm; and cooling to room temperature for the second time.
5. The use according to claim 1, wherein the emollient water comprises the following components in parts by weight: 1-5 parts of codonopsis pilosula oligosaccharide, 1-5 parts of glycerol, 0-5 parts of 1, 3-propylene glycol, 0-0.5 part of sodium hyaluronate, 0-1.5 parts of carbomer, 0-0.5 part of glutathione, 0-1 part of trehalose, 0-1 part of EDTA disodium, 0-1 part of phenoxyethanol, 0-0.1 part of essence and 79.4-98 parts of water.
6. The use according to claim 5, wherein the emollient water comprises the following components in parts by weight: 3 parts of codonopsis pilosula oligosaccharide, 4 parts of glycerol, 3 parts of 1, 3-propylene glycol, 0.1 part of sodium hyaluronate, 0.1 part of carbomer, 0.2 part of glutathione, 0.1 part of trehalose, 0.05 part of EDTA disodium, 1 part of phenoxyethanol, 0.01 part of essence and 88.44 parts of water.
7. The use according to claim 5 or 6, wherein the emollient water is prepared by a method comprising the steps of: adding glycerol, EDTA disodium, 1, 3-propylene glycol, carbomer, sodium hyaluronate, trehalose and deionized water into a stirring pot with the temperature controlled between 80 and 85 ℃ according to the proportion, and stirring at the stirring speed of 1500-2000r/min for 0.4 to 0.6 hours; then cooling to 40-45 ℃, adding the glutathione, the codonopsis pilosula oligosaccharide, the phenoxyethanol and the essence with the proportion in turn, continuing to pass through a stirrer, stirring at the speed of 500 plus 2000r/min, cooling to room temperature, and discharging.
8. The use according to claim 1, wherein the emulsion comprises the following components in parts by weight:
1-8 parts of codonopsis pilosula oligosaccharide, 0-5 parts of squalane, 0-10 parts of PEG-60 hydrogenated castor oil, 0-3 parts of A165 emulsifier, 0-1.5 parts of hydroxyethyl cellulose, 0-1.5 parts of carbomer, 0-5 parts of glycerol, 0-5 parts of 1, 3-propylene glycol, 0-0.5 part of sodium hyaluronate, 0-0.5 part of glutathione, 0-1 part of trehalose, 0-1 part of EDTA disodium, 0-5 parts of ethanol, 0-0.1 part of essence, 0-0.7 part of platinum methyl ester, 0-1 part of phenoxyethanol and 63.2-99 parts of water.
9. The use according to claim 8, wherein the emulsion comprises the following components in parts by weight: 6 parts of codonopsis pilosula oligosaccharide, 3 parts of squalane, 5 parts of PEG-60 hydrogenated castor oil, 1 part of hydroxyethyl cellulose, 2 parts of A165 emulsifier, 0.2 part of carbomer, 3 parts of glycerol, 2 parts of 1, 3-propylene glycol, 0.2 part of sodium hyaluronate, 0.1 part of glutathione, 0.1 part of trehalose, 0.2 part of EDTA disodium, 4 parts of ethanol, 0.01 part of essence, 0.3 part of platinum methyl ester, 0.2 part of phenoxyethanol and 72.69 parts of water.
10. Use according to claim 8 or 9, characterized in that the preparation of said emulsion comprises the following steps:
1) adding squalane, PEG-60 hydrogenated castor oil and A165 emulsifier into an oil phase pot according to the proportion, heating to dissolve, and uniformly stirring to obtain an oil phase; wherein the heating temperature is 70-80 ℃, and the stirring speed is 20-40 rpm;
2) heating and dissolving 1, 3-propylene glycol, sodium hyaluronate, trehalose, glycerol, EDTA disodium, ethanol and water according to a ratio, uniformly stirring, preserving heat, independently preparing hydroxyethyl cellulose and carbomer, dissolving the hydroxyethyl cellulose and the carbomer in the water, fully stirring at room temperature to uniformly swell the materials, and mixing to obtain a transparent water phase; wherein the heating temperature is 75-85 ℃, the heat preservation time is 0.2-0.4 hour, and the stirring speed is 20-40 rpm;
3) sequentially adding the oil phase prepared in the step 1) and the water phase prepared in the step 2) into an emulsifying pot, homogenizing, uniformly stirring, cooling for the first time, adding the codonopsis pilosula oligosaccharide, glutathione, essence, nipagin methyl ester and phenoxyethanol in the matched amount, uniformly stirring, cooling for the second time, and discharging; wherein, the homogenizing time is 3-4min, and the stirring speed is 2000-; the temperature is reduced to 68-72 ℃ for the first time, and the stirring speed is 20-40 rpm; and cooling to room temperature for the second time.
CN201911373187.9A 2019-12-27 2019-12-27 Application of codonopsis pilosula oligosaccharide in preparation of cosmetics Pending CN110946782A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2006134409A2 (en) * 2005-06-13 2006-12-21 Jaszberenyi Csaba Jozsef Synergistic prebiotic compositions
CN109223808A (en) * 2018-09-29 2019-01-18 兰州大学 Application of the Radix Codonopsis oligosaccharides of the 000Da of Fen Liang≤5 in the antioxidant activity drug that DPPH free radical is removed in preparation
CN109350621A (en) * 2018-09-29 2019-02-19 兰州大学 Application of the Radix Codonopsis extract in the antioxidant activity drug that DPPH free radical is removed in preparation

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2006134409A2 (en) * 2005-06-13 2006-12-21 Jaszberenyi Csaba Jozsef Synergistic prebiotic compositions
CN109223808A (en) * 2018-09-29 2019-01-18 兰州大学 Application of the Radix Codonopsis oligosaccharides of the 000Da of Fen Liang≤5 in the antioxidant activity drug that DPPH free radical is removed in preparation
CN109350621A (en) * 2018-09-29 2019-02-19 兰州大学 Application of the Radix Codonopsis extract in the antioxidant activity drug that DPPH free radical is removed in preparation

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