CN116725927B - Spatial structure composition containing peony active ingredient and preparation method and application thereof - Google Patents
Spatial structure composition containing peony active ingredient and preparation method and application thereof Download PDFInfo
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- CN116725927B CN116725927B CN202310996465.6A CN202310996465A CN116725927B CN 116725927 B CN116725927 B CN 116725927B CN 202310996465 A CN202310996465 A CN 202310996465A CN 116725927 B CN116725927 B CN 116725927B
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- polysaccharide
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- peony
- skin
- mixture
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- UHVMMEOXYDMDKI-JKYCWFKZSA-L zinc;1-(5-cyanopyridin-2-yl)-3-[(1s,2s)-2-(6-fluoro-2-hydroxy-3-propanoylphenyl)cyclopropyl]urea;diacetate Chemical compound [Zn+2].CC([O-])=O.CC([O-])=O.CCC(=O)C1=CC=C(F)C([C@H]2[C@H](C2)NC(=O)NC=2N=CC(=CC=2)C#N)=C1O UHVMMEOXYDMDKI-JKYCWFKZSA-L 0.000 description 1
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Abstract
The application discloses a composition with a space structure and containing peony active ingredients, and a preparation method and application thereof, and belongs to the technical field of daily chemical products. The product disclosed by the application has the advantages that through mutual collocation of the high-molecular space structural components and the peony active components with specific compositions, the product not only has excellent adsorptivity, can be used for a long time and is not fallen off, and has high safety to skin, but also has excellent effects of improving the problems of low skin glossiness and large pores, can play a good barrier role in the use process, and can improve the water retention of the skin; meanwhile, the anti-sensibility of the skin can be effectively improved, and the skin-soothing agent has a soothing effect on the skin.
Description
Technical Field
The application relates to the technical field of daily chemical products, in particular to a space structure composition containing peony active ingredients, and a preparation method and application thereof.
Background
Skin color darkness and pores are easy to cause skin to have loose feel and dullness, and at present, more cosmetics mainly solve the two problems through optical effects and compound actions, wherein the optical effects mainly refer to that the lightening components such as pearl powder and the like contained in the cosmetics can reflect and refract external light rays so as to enable the skin to have higher gloss and brightness when being observed by naked eyes; the compound is effective in promoting skin metabolism and inhibiting melanin generation, so that skin smoothness and glossiness can be improved, and skin compactness can be improved by some compounds such as collagen.
However, these existing cosmetics have certain defects that the cosmetics for inhibiting skin darkness by optical effect cannot fundamentally solve the skin problem, are easy to fall off during use, and have damage to the skin after long-term use; most of the active compounds in cosmetics have small action range and short action time, and meanwhile, the microbial environment balance of the skin can be changed, the sensitivity is changed, and even adverse reactions such as allergy are caused after long-term use.
Disclosure of Invention
Based on the defects existing in the prior art, the application aims to provide a composition product with a space structure, which has excellent adsorptivity, can be used for a long time without falling off, has high safety to skin, has excellent effect of improving the problems of low skin glossiness and large pores, can play a good barrier role in the use process and improves the water retention of the skin by matching high molecular space structure components with peony active components with specific components; meanwhile, the anti-sensibility of the skin can be effectively improved, and the skin-soothing agent has a soothing effect on the skin.
In order to achieve the above purpose, the application adopts the following technical scheme:
the space structure composition comprises the following components in parts by weight:
0.01-2 parts of a polymer space structure mixture and 0.01-100 parts of peony fermentation filtrate;
the high molecular space structure mixture comprises a polysaccharide mixture, wherein the polysaccharide mixture has a core-shell structure, the inner core is plant polysaccharide, and the molecular weight is more than 1000000 daltons; the plant polysaccharide is at least one of astragalus polysaccharide, peony polysaccharide, sodium hyaluronate, tremella polysaccharide, cassia seed polysaccharide, guar gum, starch, coumarone gum, agar, spiny marble gum, carrageenan, sclerotium gum, kappaphycus alvarezii and the like; the shell is at least one of bentonite, a methacryloxyethyl phosphorylcholine monomer, a polymer and a glycerylethanolamide methacrylate/stearyl methacrylate copolymer;
the peony fermentation filtrate is obtained by fermenting fermentation liquor containing NaDES solvent.
In the prior art, in order to improve the functional diversity and durability of skin care cosmetic products, people research the microstructure of the products and find that when some active ingredients in the products have a layered structure or a net structure, the active ingredients can better play a role in skin contact and protection, in the scheme of the application, the products select polysaccharide mixtures with space structures, and as the polysaccharide mixtures have further modified core-shell structures, after being matched with peony fermentation filtrate containing plant macromolecules, the space structures of the whole products are higher in crosslinking degree, the fluffiness of the products is higher, the effects of immediately improving the skin glossiness can be obtained, and meanwhile, the adsorption strength is higher, the products are not easy to fall off, and good skin barriers are formed, so that the moisture retention of the skin is improved; the peony fermentation filtrate is a product obtained by adopting fermentation culture solution containing NaDES solvent for fermentation, and the NaDES solvent has good biocompatibility, strong solubility for plant components and is beneficial to improving the stability of natural compounds, so that peony active substances can be synchronously converted in the fermentation process of the peony fermentation filtrate, and hydrogen bonds exist in acting force among molecules, so that the obtained product has the advantages of richer skin care component types, higher activity, better spatial structure, capability of improving the condition of large skin pores and regulating skin sensitivity after long-term use, and good relieving effect on skin.
Another object of the present application is to provide a method for preparing the composition for spatial structure, comprising the steps of:
the components are subjected to micro-jet homogenization treatment to form a space structure composition.
It is still another object of the present application to provide a skin care product comprising the spatial structure composition.
Preferably, the components of the skin care product further comprise at least one of a solvent, a humectant, a preservative and a thickener;
more preferably, the solvent is water, the humectant is at least one of caprylic/capric triglyceride, butanediol and 1, 2-hexanediol, the preservative is p-hydroxyacetophenone, and the thickener is at least one of acrylamide dimethyl taurate/VP copolymer and polyacrylate crosslinked polymer-6.
More preferably, the skin care product comprises the following components in parts by weight based on 100 parts by weight:
8-12 parts of caprylic/capric triglyceride, 2-5 parts of butanediol, 0.5-1.5 parts of 1, 2-hexanediol, 0.2-1 part of p-hydroxyacetophenone, 0.1-0.5 part of acrylamide dimethyl taurate/VP copolymer, 0.2-1 part of polyacrylate crosslinked polymer-6, 0.01-2 parts of high molecular space structure mixture, 0.01-100 parts of peony fermentation filtrate and the balance of water.
According to the viscosity, stability and functional requirements of the actual prepared product, a person skilled in the art can introduce proper processing aids into the preparation raw materials, and after verification, when the product is prepared by the raw materials with the types and proportions, the stability of the product is better, and the use effect is better.
Preferably, the polymer space structure mixture is a polysaccharide mixture.
Preferably, the plant polysaccharide is a peony polysaccharide.
Preferably, the inner shell of the plant polysaccharide mixture is peony polysaccharide and the outer shell is bentonite.
The peony polysaccharide is different from other compounds such as flavone compounds extracted from peony, the active compounds mainly contained in the peony polysaccharide have better effects of resisting oxidization and scavenging free radicals, meanwhile, the spatial structure complexity of molecules is higher, the peony polysaccharide can be effectively dispersed in a water solvent, after the peony polysaccharide is wrapped by bentonite to form a core-shell structure, the peony polysaccharide cannot inhibit the oxidization resistance, and the contact effect of the whole component and skin is better due to good thixotropy and viscosity of the bentonite, so that the removal of free radicals on the skin surface by the peony polysaccharide is facilitated, and the effects of whitening and the like are realized.
More preferably, the preparation method of the peony polysaccharide comprises the following steps:
(1) Rolling and crushing peony peel, and extracting with ethanol as an extractant in an ultrasonic environment;
(2) Freezing and thawing the extracting solution obtained in the step (1) for 7-8 times at the temperature of-20 ℃, and centrifuging the obtained mixture to separate protein;
(3) And (3) decolorizing the mixture obtained after protein separation in the step (2) by an alkaline chromatographic column, and then carrying out electrophoresis treatment for 5-7 hours under the voltage of 1.2-1.8V, thereby separating to obtain the peony polysaccharide.
The process can effectively separate macromolecular polysaccharide from the peony pericarp, has high separation efficiency, and can not obviously damage the structure of polysaccharide molecules.
Preferably, the method for preparing the polysaccharide mixture comprises the following steps:
(1) Uniformly dispersing plant polysaccharide, bentonite, at least one of a methacryloxyethyl phosphorylcholine monomer and a polymer and a glycerylethanolamide methacrylate/stearyl methacrylate copolymer in water, and carrying out micro-jet homogenization treatment to obtain a viscous mixture;
(2) The polysaccharide thickening mixture is subjected to freeze-drying treatment to obtain a polysaccharide mixture.
When the existence form of the plant polysaccharide in the skin care product has great influence on the space structure of the product, if the preparation process of the polysaccharide mixture is not properly selected, the product cannot realize the expected space structure, the viscosity of the product is extremely low, and finally, good skin attaching effect and anti-falling performance cannot be realized.
Preferably, the mass ratio of the plant polysaccharide to at least one of bentonite, methacryloxyethyl phosphorylcholine monomer and polymer, glycerylethanolamide methacrylate/stearyl methacrylate copolymer (plant polysaccharide): (at least one of methacryloyloxyethyl phosphorylcholine monomer and polymer, glycerylethanol methacrylate/stearyl alcohol methacrylate copolymer) =1: (2.5 to 3.5).
The plant polysaccharide mainly plays a role in enhancing the spatial molecular structure and caring skin in the polysaccharide mixture, and if the content is too small, the functions are difficult to play, but if the content is too large, the viscosity of a viscous mixture with changed quality is possibly unsuitable, the ideal final structure is difficult to realize, and the adhesive force and the component uniformity of the product are not ideal.
Preferably, the temperature of the micro-jet homogenization treatment is 33-37 ℃ and 450+/-50 m/s.
Preferably, the step of freeze-drying is: pre-freezing at-12 to-18 ℃ for 4.5 to 5.5 hours, performing primary drying treatment at-35 to-45 ℃ for 9.5 to 10.5 hours under the pressure of 0.05 to 0.1MPa, performing secondary drying treatment at-2 to 2 ℃ for 4.5 to 5.5 hours, and performing tertiary drying at 36 to 40 ℃ for 9.5 to 10.5 hours.
Preferably, the peony fermentation filtrate is a peony seed meal fermentation filtrate.
The peony seed meal contains active ingredients with high antioxidant, water supplementing and other effects, such as paeoniflorin, carotene and the like, and the low-activity macromolecular substances in the peony seed meal can be effectively converted into high-biological active substances by adopting a fermentation process, and compared with an unfermented pure extract product, the peony seed meal has higher compatibility and better stability with other raw materials in the product, particularly a polysaccharide mixture; meanwhile, due to the existence of the NaDES solvent, the peony seed meal has higher fermentation efficiency and more complete fermentation degree.
Preferably, the preparation method of the peony fermentation filtrate comprises the following steps:
adding NaDES into a fermentation culture solution, then transferring peony seed meal powder and lactobacillus to ferment for 9-11 days at 30-40 ℃, sterilizing the obtained mixed solution, and centrifuging to obtain supernatant, thus obtaining peony fermentation filtrate.
Preferably, the NaDES solvent comprises the following components in parts by weight: 0.8-1.2 parts of lactobionic acid, 0.8-1.2 parts of fructose, 0.8-1.2 parts of sorbitol and 4.5-5.5 parts of water.
More preferably, the preparation method of the NaDES solvent comprises the following steps: and mixing the components, heating at 46-50 ℃ for 2.5-3.5 h, and then drying at 58-62 ℃ for 71-73 h to obtain the NaDES solvent.
Preferably, the fermentation broth comprises the following components in parts by weight: 1.5-2.5 parts of NaDES solvent, 1.5-2.5 parts of glucose, 0.5-1.5 parts of urea and 14-16 parts of water.
Preferably, the addition amount of the peony seed meal powder in the fermentation culture solution is 4-6 g/100mL.
Preferably, the inoculation amount of the lactobacillus is 0.15-0.25vol%, and the viable count of the lactobacillus liquid is 10 9 CFU/mL。
Preferably, the skin care product further comprises 4-6 parts of water-soluble thickening ionic compound;
more preferably, the water-soluble thickening ionic compound is at least one of vitamin C, vitamin C derivatives, decarboxylated carnosine salts, 4-methoxysalicylic acid potassium, tranexamic acid, zinc sulfate, salicylic acid and fruit acid.
More preferably, the water-soluble thickening ionic compound is vitamin C.
The inventor experiments show that some water-soluble thickening ionic compounds have certain skin activity functions such as whitening, moisturizing and the like, but the viscosity influence degree of the components on skin care products is extremely high, the stability and usability of the products can be possibly influenced, meanwhile, the components have high skin irritation, and the polysaccharide mixture and the peony fermentation filtrate in the composition with the space structure have obvious inhibition effect on the side effects of the components, so that when the water-soluble thickening ionic compounds are introduced into the skin care products, the viscosity and the mildness of the products are not greatly influenced, and the skin care effect of the products can be further improved.
Another object of the present application is to provide a method for preparing the skin care product, comprising the steps of:
(1) Carrying out micro-jet homogenization treatment on each component of the space structure composition to obtain a component a;
(5) Heating and uniformly mixing a solvent, a humectant, a preservative and a thickener, and cooling to 40-50 ℃ to obtain a component A;
(6) And adding the component a and the water-soluble thickening ionic compound into the component A, uniformly mixing, and cooling to 25-30 ℃ to obtain the skin care product.
The inventor finds through experiments that in the water-based skin care product system, more thickening agents are generally required to be introduced in order to realize the ideal skin pasting effect, but the thickening agents are chemical substances, the safety and stability of the product are easy to change when the product is used in a large amount, and meanwhile, the production cost is also improved.
The composition product containing the peony active ingredient and having a space structure has the advantages that through mutual collocation of the high-molecular space structural ingredient and the peony active ingredient with a specific composition, the composition product has excellent adsorptivity, can be used for a long time without falling off, has high safety to skin, has excellent effect of improving the problems of low skin glossiness and large pores, can play a good barrier role in the use process, and improves the water retention of the skin; meanwhile, the anti-sensibility of the skin can be effectively improved, and the skin-soothing agent has a soothing effect on the skin.
Drawings
FIG. 1 is a schematic representation of the product of example 2 diluted with 50 times the mass of water.
FIG. 2 is a schematic representation of the product of comparative example 2 diluted with 50 times the mass of water.
Fig. 3 is a raman image of the product of example 4 of effect example 3 in use test, and from left to right is a block diagram of tests 0.5h, 1h, 2h and 4h in sequence.
Fig. 4 is a raman image of the product of comparative example 4 of effect example 3 in use, showing the structure of tests 0.5h, 1h, 2h and 4h in sequence from left to right.
FIG. 5 is a graph showing test results of the model control group in effect example 4.
FIG. 6 is a graph showing the results of the positive control test in effect example 4.
FIG. 7 is a graph showing the results of the test set 3 in effect example 4.
Detailed Description
The present application will be further described with reference to specific examples and comparative examples for better illustrating the objects, technical solutions and advantages of the present application, and the object of the present application is to be understood in detail, not to limit the present application. All other embodiments, which can be made by those skilled in the art without the inventive effort, are intended to be within the scope of the present application. The experimental reagents and instruments involved in the practice of the present application are common reagents and instruments unless otherwise specified.
Example 1
In one embodiment of the spatial structure composition, the preparation method and the application thereof, the spatial structure composition and the raw material components of the prepared skin care product are shown in table 1, and the preparation method of the skin care product comprises the following steps:
(1) Uniformly dispersing 2g of peony polysaccharide and bentonite in 200mL of water according to a mass ratio of 1:3, and carrying out micro-jet homogenization treatment for 5 times at 35 ℃ under the condition of 500m/s rate for 5min each time to obtain a viscous mixture; the preparation method of the peony polysaccharide comprises the following steps:
(a) Grinding 100g of peony peel, soaking and extracting for 3 times with 900mL of ethanol as an extracting agent in an ultrasonic environment at 40 ℃ for 90min each time;
(b) Freezing and thawing the extracting solution obtained in the step (a) for 8 times at the temperature of-20 ℃, and centrifuging the obtained mixture at the speed of 4800r/min for 60min to separate protein;
(c) Decolorizing the mixture obtained after separating the protein in the step (b) by using a commercial alkaline DEAE cellulose chromatographic column, stirring glass powder into colloid by using water, filling the colloid into the column, balancing the colloid for 3 days by using a borax water solution with the pH value of 9 and 0.05mol/L, adding the decolorized solution at the upper end of the column, carrying out electrophoresis treatment for 6 hours under the voltage of 1.5V and the current of 32mA, and separating to obtain the peony polysaccharide; the molecular weight of the peony polysaccharide is more than 1000000 daltons;
(2) Freeze drying the viscous mixture to obtain polysaccharide mixture; the freeze drying steps are as follows: pre-freezing at-15deg.C for 5 hr, drying at-40deg.C under 0.08MPa for 10 hr, drying at 0deg.C for 5 hr, and drying at 38deg.C for 10 hr;
(3) Adding NaDES into fermentation culture solution, transferring into addition amount of 6g of impurity-removed broken peony seed meal powder and 0.2vol% of lactobacillus for fermentation at 35+ -5deg.C for 10 days, sterilizing the obtained mixed solution, centrifuging at 4000r/min for 40min, and collecting supernatant to obtain peony fermentation filtrate; the NaDES solvent comprises the following components in parts by weight: 1 part of lactobionic acid, 1 part of fructose, 1 part of sorbitol and 5 parts of water; the preparation method of the NaDES solvent comprises the following steps: mixing the components, heating at 48 ℃ for 3 hours, and then drying at 60 ℃ for 72 hours to obtain the NaDES solvent; the fermentation culture solution comprises the following components in parts by weight: 2.5 parts of NaDES solvent, 2 parts of glucose, 1 part of urea and 15 parts of water;
(4) Mixing the polysaccharide mixture and the peony fermentation filtrate, and carrying out micro-jet homogenization treatment for 10min at the speed of 450+/-50 m/s at the temperature of 35 ℃ to obtain the space structure composition (component a);
(5) Heating solvent water, humectant caprylic/capric triglyceride, butanediol, 1, 2-hexanediol, preservative p-hydroxyacetophenone, thickener acrylamide dimethyl taurate/VP copolymer and polyacrylate crosslinked polymer-6 to 85 ℃, homogenizing and mixing for 3min at 2500rpm until uniformity, and cooling to 45 ℃ to obtain a component A;
(6) And adding the component a and the water-soluble thickening ionic compound into the component A, stirring and mixing the components at a rotating speed of 20rpm until the components are uniform, and cooling the components to 30 ℃ to obtain the skin care product containing the space structure composition.
Examples 2 to 4
The difference between this example and example 1 is only that the composition and the ratio of the raw materials for preparing the skin care product are different, as shown in table 1.
TABLE 1
Examples 5 to 6
The difference between examples 5-6 and example 4 is that in the preparation process of the product, the preparation raw materials of the plant polysaccharide in the polysaccharide mixture are different, and in example 5, the peony pericarp for preparing the peony polysaccharide in example 4 is replaced by commercial astragalus root, and the prepared plant polysaccharide is astragalus root polysaccharide; example 5 the peony pericarp of the peony polysaccharide prepared in example 4 was replaced with the commercially available tremella, the prepared plant polysaccharide was tremella polysaccharide, and the preparation process of the two plant polysaccharides was identical to that of the peony polysaccharide described in examples 1-4.
Comparative examples 1 to 4
A skin care product differing from examples 1 to 4 only in the component formulations as shown in Table 2.
TABLE 2
Comparative example 5
The skin care product only differs from example 4 in that the preparation method of the peony polysaccharide comprises the following steps:
(a) Grinding and crushing tree peony peel, soaking and extracting for 3 times by taking ethanol as an extracting agent in an ultrasonic environment at 40 ℃ for 90min each time;
(b) Freezing and thawing the extracting solution obtained in the step (a) for 8 times at the temperature of-20 ℃, and centrifuging the obtained mixture at the speed of 4800rpm to separate protein;
(c) And (3) decolorizing the mixture obtained after separating the proteins in the step (b) by an alkaline DEAE cellulose chromatographic column to obtain the peony polysaccharide. The molecular weight of the peony polysaccharide is less than 1000000 daltons.
Comparative example 6
The skin care product is different from the embodiment 4 only in that the preparation method of the skin care product comprises the following steps (1): uniformly dispersing 0.5g of peony polysaccharide and bentonite in 20mL of water according to a mass ratio of 1:3, and then stirring at 15rpm for 2 hours at 35 ℃ to obtain a viscous mixture. The peony polysaccharide mixture particles prepared in the comparative example show larger non-uniformity in color shade and size.
Comparative example 7
The skin care product is different from the embodiment 4 only in that the preparation method of the skin care product comprises the following steps (2): and drying the polysaccharide thickening mixture for 72 hours in a 65 ℃ oven at normal pressure to obtain the peony polysaccharide mixture. The peony polysaccharide mixture exhibits severe agglomeration.
Comparative example 8
A skin care product differing from example 4 only in that the skin care product preparation method comprises the steps of:
(1) Uniformly mixing 0.5g of peony polysaccharide with bentonite according to a mass ratio of 1:3 to obtain a peony polysaccharide mixture; the preparation method of the peony polysaccharide is the same as that of examples 1-4;
(2) Preparing peony fermentation filtrate according to the same method as in examples 1-4;
(4) Mixing the peony polysaccharide mixture and peony fermentation filtrate, homogenizing at a speed of 450+/-50 m/s for 10min at 35 ℃ to obtain a component a;
(5) Final skin care products were prepared in the same manner as in examples 1-4.
Comparative example 9
A skin care product differing from example 4 only in that the NaDES solvent was replaced with purified water.
Effect example 1
To verify the adhesion of the skin care products of the present application, the products of each example and comparative example were tested for viscosity at 25℃with a Brookfield DV-2T RV viscometer at 4#5rpm for 30 seconds, and the results are shown in Table 3.
TABLE 3 Table 3
It can be seen from table 3 that the products of the examples of the present application have desirable viscosities, particularly the product of example 4, and that vitamin C in the product will significantly inhibit the viscosity of the product when the peony polysaccharide mixture and peony fermentation filtrate are not introduced, and the viscosity reduction effect of vitamin C is significantly inhibited when both components are introduced, as compared to the product of comparative example 4. Examples 5 to 6 also show that other polysaccharide mixtures which form a spatial structure also significantly inhibit the reduction of the viscosity of the vitamin C product. On the other hand, according to the viscosity of the products of comparative examples 5-8, when the peony polysaccharide mixture and the peony fermentation filtrate adopt other conventional processes in the preparation process, even the core-shell structure design of the peony polysaccharide mixture is not performed, the viscosity of the products is greatly reduced, and the expected adhesiveness cannot be achieved.
After the products of example 2 and comparative example 2 are diluted with 50 times of water, the results are shown in fig. 1 and 2, and it can be seen that when the peony fermentation filtrate is contained in the products, the whole structure is more fluffy, and the components also have synergistic enhancement effect on the space structure of the products.
Effect example 2
In order to preliminarily verify the synergistic skin care effect of the peony polysaccharide composition and the peony fermentation filtrate in the spatial structure composition, the products of examples 1-3 and comparative examples 1-3 are subjected to preliminary user experience screening, and the specific method is as follows:
selecting 48 volunteers with 17-50 years old and obvious facial skin darkness and pore coarseness characteristics, randomly dividing the volunteers into 6 groups, wherein 8 people in each group respectively correspond to products of examples 1-3 or comparative examples 1-3 at the positions of facial darkness and pore coarseness, continuously using for 1 month and 3 times per week, uniformly coating the products when the volunteers are used, and performing self-evaluation on skin glossiness after using for 15 minutes, wherein the evaluation is divided into: three grades of significant improvement, slight improvement and no improvement (or deterioration), the number of evaluators of each group of three grades was counted, and then after completion of the test for 1 month, the self-evaluation of each volunteer in terms of skin glossiness and skin pores was investigated by a return visit, and the number of evaluators was evaluated and counted in the same three grades, and the structure is shown in table 4.
TABLE 4 Table 4
As can be seen from the table, the products in examples 1-3 all contain peony polysaccharide mixture and peony fermentation filtrate, but one of comparative examples 1 and 2 lacks, and comparative example 3 does not contain two substances, and when short-term test is carried out, the products in examples 1-3 show the effect of rapidly improving skin glossiness, and when the content of the components of the two substances is higher, 7 persons in the corresponding product group in example 3 evaluate that the product has obviously improved skin glossiness after use, and after long-term use, the improvement degree of the products in examples 1-3 with low content or high content is higher than that of the product in comparative example, which shows the effect of synergistically improving skin glossiness when the two components in the product are clinically used; on the other hand, the products of each example, especially the product of example 3, also showed the effect of significantly improving the skin pores, the number of significantly improved evaluation was up to 6, and the number of significantly improved evaluation of the products of comparative examples 1 to 3 was only 2 at most.
Further, in order to verify that the skin care product of the application does not cause irritation to human skin when used in a closed state, the products of examples 1 to 4 are subjected to a 24-hour closed human skin patch test according to 2015 edition of cosmetic safety technical specification: selecting 128 volunteers with ages 18-59 and meeting the standard, and dividing into 4 groups, wherein each group comprises 25 women and 7 men, and the selected area is not more than 50mm 2 A suitable patch tester with a depth of about 1mm was used, and about 0.020 to 0.025g of the product obtained in examples 1 to 4 was added to the patch tester by a closed patch test method. The patch tester is applied to the front curved side of a subject, the test object is removed after 24 hours, skin reactions are observed after 0.5 hour, 24 hours and 48 hours respectively, and the results are recorded according to the skin reaction grading standard in cosmetic safety technical Specification 2015 (specifically, the skin reaction grading standard of the human body skin patch test skin closed patch test in chapter 2 of cosmetic safety technical Specification 2015). While volunteers set up negative controls (blank, i.e., different test area skin of the same volunteer).
The results are shown in Table 5.
TABLE 5
As can be seen from Table 5, the tested grades of the products of the examples of the present application were all 0 points, and the products were 0 points after 24h and 48h of patch removal, and the skin mildness of the products was high.
Effect example 3
After human body evaluation, in order to verify the low-irritation effect of the skin care product based on the action of each component, referring to a chick embryo chorioallantoic membrane test of SNT 2329-2009 cosmetic eye irritation corrosiveness, the products of examples 1-4 and comparative examples 1-9 were tested by adopting the chick embryo chorioallantoic membrane blood vessel irritation test: (1) The chick embryos at age 0d were purchased, incubated to age 9d, and the defective chick embryos were inspected and discarded. Marking the position of an air chamber on the surface of a normal eggshell, stripping off eggshell parts and exposing white egg membranes; carefully remove the intima with forceps to ensure that the vascular membrane is not damaged; (2) evaluation by endpoint scoring: at least 6 chick embryos in each group are taken, the products of the examples and the comparative examples are prepared, namely, 0.3. 0.3 mL is directly dripped on the surface of the CAM, the reaction condition of the CAM is observed, after the CAM is acted for 3min, the test is gently washed by normal saline to remove the test, and 3 reactions and degrees of bleeding, coagulation and vascular thawing are observed within about 30s after washing. If the observation shows that the score of at least 1 reaction of all 6 chick embryos is above moderate (total score is not less than 12), the test should be repeated once. Endpoint Scoring (ES): score per chick embryo = sum of extent of bleeding, coagulation and vascular thawing observed per chick embryo; endpoint Score (ES) =number sum of 6 chick embryo scores.
The following table shows:
the test results are shown in Table 6.
TABLE 6
As can be seen from table 6, in the product of the example of the present application, the components except for vitamin C have substantially no apparent irritation, whereas the product of example 4 did not show irritation or comfort in use in the test of the above-mentioned effect example 2 because the irritation of vitamin C in the product of example 4 was significantly reduced due to the effect of the peony polysaccharide mixture and the peony fermentation filtrate in the product; in contrast, the product of comparative example 4 has higher irritation of vitamin C due to the absence of the above two components, and although the component has good whitening and moisturizing effects, the negative effect of skin irritation may occur when used alone; however, in examples 5 to 6 of the polysaccharide mixture prepared from the plant polysaccharide defined by the technical scheme of the application, the irritation of vitamin C can be obviously reduced, and as can be seen from the test results of comparative examples 5 to 9, the preparation process of the spatial structure composition and the skin care product which do not completely adopt the application has the effect of reducing the irritation of vitamin C, but the irritation reduction rate is obviously inferior to that of example 4.
Subsequently, the products of example 3, example 4 and comparative example 4 were subjected to whitening evaluation tests to verify that the synergistic whitening effect of the peony polysaccharide mixture, the peony fermentation filtrate and the vitamin C is achieved under the condition that the irritation of the vitamin C in the products of examples is significantly improved: selecting 165 subjects with chloasma and dark complexion on skin of 17-50 years old, randomly dividing the subjects into 5 groups of 33 subjects, using the products of examples 3-6 and comparative example 4 on the face respectively, using the products for 1.5 g/time, 2 times/day (1 time each in the morning and evening), continuously using the products for one month, and then carrying out self-judging standard by referring to the method of effect example 2, evaluating the whitening effect of the products, wherein the results are shown in Table 7, and the comparative example 4 groups have 2 subjects to give up midway and do not include statistics.
TABLE 7
As can be seen from table 7, when the products of example 4 and comparative example 4 containing vitamin C were used, the problem of darkening of skin color caused by chloasma of the skin was improved, but the whitening effect of vitamin C in example 4 was significantly increased compared with the products of example 3 and comparative example 4 due to the synergistic effect with the peony polysaccharide mixture and peony fermentation filtrate in the product components. When the products of examples 5-6 containing the polysaccharide mixture prepared from vitamin C and other plant polysaccharide are used, the synergistic whitening effect on vitamin C is achieved, and the peony polysaccharide effect is optimal.
Further, the vitamin C transdermal penetration rate test was performed on the products of example 4 and comparative examples 4 to 9: fresh pig back skin was cut to size for use by removing hair and subcutaneous tissue. Using Franz horizontal diffusion cells (effective diffusion area 1.5 cm) 2 ) Skin permeation studies were performed. Pig back skin is fixed between two diffusion tanks, the receiving liquid is isotonic PBS (pH=7.0-7.4), the test liquid is the liquid of example 4 and comparative example 4 respectively, a transdermal test is carried out in triplicate by circulating water bath at 37 ℃, 0.5mL of sample is taken at 24h after the start of the test, the sample is filtered by a 0.22 μm filter membrane and is used as a detection sample, and the content of vitamin C is detected by liquid chromatography respectively, so that the cumulative transmittance of vitamin C in the sample is calculated (the same steps as those of other comparative example products are treated). As shown in table 8.
The cumulative transmittance or retention (%) of the active material is calculated by the formula:
cumulative transmittance (%) = total transmission in receiving fluid/total in test fluid diffusion cell 100%
TABLE 8
Through tests, the cumulative transmittance of the product of the example 4 is 80.8%, but the cumulative transmittance of the product of the comparative example 4 is only 45.6%, which shows that in the product of the example 4, the effect of vitamin C penetrating through the skin is obviously increased under the action of the rest components, the vitamin C can be more effectively contacted with the deep skin and has active effect, and the vitamin C in the product of the comparative example 4 is difficult to achieve similar effect; from the results of examples 5 to 6, the space composition formed by the other polysaccharide mixture also has better permeation promotion effect on the active substances, while from the results of comparative examples 5 to 9, the permeation effect is lower than that of example 4 due to the fact that the product preparation process of the application is not fully adopted.
And the application of the product in human body test further confirms the conclusion: determining characteristic peaks of a test sample by using a Raman spectrum method, determining permeation behaviors of the sample by using a Raman imaging chart, analyzing permeation conditions of the test sample in the skin at the same time points of 0.5h, 2h, 4h and the like of a subject by using a Raman image, comparing the concentration of a standard sample of the test sample with the drawing of a Raman spectrum intensity curve, and calculating the permeation result of the sample on the skin of the subject.
The testing process comprises the following steps:
cleaning skin of a test area by using clear water after visiting, standing in a constant temperature and humidity room for 30 minutes after cleaning, carrying out product use on the test subjects taking part in the test according to test requirements after 30 minutes (taking three test areas of 1X 1 square centimeter at the front end of the arm and the forearm of each test subject, applying 5mg of sample to each test area of 1X 1 square centimeter, starting timing after clockwise uniform-speed smearing for 5 circles, calculating permeation time), and carrying out human body in-vivo Raman test (LabRAM Odyssey high-speed high-resolution microscopic confocal Raman spectrometer, 800 mm focal length, 0.35 cm) by using samples to be tested for 0.5h, 1h, 2h and 4h -1 Resolution (HORIBA)), test time is 3-5min, and raman spectral imaging data are processed and analyzed to show the distribution of the substance in human skin. Human raman test three 1 x 1 square centimeter areas inside the forearm were selected for three average tests per area to eliminate biological individual differences with the average.
The results are shown in fig. 3, fig. 4 and table 9.
TABLE 9
Similar to animal skin test, the component collocation of the product of example 4 can effectively improve the permeation effect of vitamin C contained in the product in the human skin test process, and can reach 55.67% high permeability after 4 hours.
Effect example 4
In order to verify the soothing efficacy of the product of the application, a zebra fish embryo in vivo experiment is used for testing: and (3) testing by using a model of neutrophil aggregation caused by copper sulfate-induced nerve dome cell injury in the embryonic side line region of the zebra fish. 24 fish embryos are exposed to 0.16mg/L copper sulfate pentahydrate and 5g/L sample solution of example 3, a model control group and a positive control group are simultaneously arranged, the fish embryos are fixed and sudan black stained after 40 minutes of exposure, the number of neutrophils in a lateral line area is counted and statistical analysis is carried out, and the results are shown in table 10 and fig. 5-7. From Table 10, it can be seen that the product of the application can cause the aggregation of the neutrophils in the zebra fish embryo due to the combined action of the peony polysaccharide mixture and the peony fermentation filtrate, i.e. has a relieving effect on organisms.
Table 10
Effect example 5
To verify the skin barrier effect of the skin care products containing the spatial structured composition of the present application, human body use tests were performed on the products of example 3 and comparative example 3: 10 skin-sensitive volunteers were screened, faces were selected as test sites, the test period was 14 days, and the volunteer face condition was observed and evaluated 1 day before and 14 days after the use of the samples. The test was preceded by a 1 week washout period during which the subjects used basic moisturizing water and moisturizing milk without any actives, no other products were used during the test, and subjects used example 3 (left face) and comparative example 3 (right face) half-face 14 consecutive days, respectively, with samples applied on the face after washing the face before sleeping each morning and evening, at about 0.2 g/time. The evaluation mode is that professional facial evaluation specialists evaluate the skin sensitivity condition of the faces of volunteers in 1-10 points, and the sensitivity degree change trend of the facial skin is evaluated according to the score before and after the test. The results are shown in Table 11. As can be seen from Table 11, the sensitivity of 10 volunteers to facial skin is reduced after two weeks of use, indicating that the product can establish a skin barrier on the skin surface to improve skin sensitivity, whereas the product of comparative example 3 has no similar effect, and even the sensitivity of 3 volunteers is increased after use, indicating that the components exerting the skin barrier effect in the product of the present application are peony polysaccharide mixture and peony fermentation filtrate.
TABLE 11
Finally, it should be noted that the above embodiments are only for illustrating the technical solution of the present application and not for limiting the scope of the present application, and although the present application has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that the technical solution of the present application may be modified or substituted equally without departing from the spirit and scope of the technical solution of the present application.
Claims (9)
1. The space structure composition is characterized by comprising the following components in parts by weight:
0.1-2 parts of a polymer space structure mixture and 1-100 parts of peony fermentation filtrate;
the high molecular space structure mixture comprises a polysaccharide mixture, wherein the polysaccharide mixture has a core-shell structure, the inner core is plant polysaccharide, and the molecular weight is more than 1000000 daltons; the plant polysaccharide is at least one of astragalus polysaccharide, peony polysaccharide and tremella polysaccharide; the shell is bentonite;
the preparation method of the polysaccharide mixture comprises the following steps:
(1) Uniformly dispersing plant polysaccharide and bentonite in water, and performing micro-jet homogenization treatment to obtain a viscous mixture;
(2) Freeze drying the polysaccharide thickening mixture to obtain a polysaccharide mixture;
the mass ratio of the polysaccharide to bentonite (plant polysaccharide): (bentonite) =1: (2.5-3.5);
the peony fermentation filtrate is obtained by fermenting fermentation liquor containing NaDES solvent;
the preparation method of the peony fermentation filtrate comprises the following steps:
adding NaDES into a fermentation culture solution, then transferring peony seed meal powder and lactobacillus to ferment for 9-11 days at 30-40 ℃, sterilizing the obtained mixed solution, and centrifuging to obtain supernatant to obtain peony fermentation filtrate;
the NaDES solvent comprises the following components in parts by weight: 0.8-1.2 parts of lactobionic acid, 0.8-1.2 parts of fructose, 0.8-1.2 parts of sorbitol and 4.5-5.5 parts of water.
2. The spatial structure composition of claim 1, wherein the outer shell of the polysaccharide mixture is bentonite and the plant polysaccharide is peony polysaccharide; the preparation method of the peony polysaccharide comprises the following steps:
(1) Rolling and crushing peony peel, and extracting with ethanol as an extractant in an ultrasonic environment;
(2) Freezing and thawing the extracting solution obtained in the step (1) for 7-8 times at the temperature of-20 ℃, and centrifuging the obtained mixture to separate protein;
(3) And (3) decolorizing the mixture obtained after protein separation in the step (2) by an alkaline chromatographic column, and then carrying out electrophoresis treatment for 5-7 hours under the voltage of 1.2-1.8V, thereby separating to obtain the peony polysaccharide.
3. The space-frame composition of claim 1, wherein the fermentation broth comprises the following components in parts by weight: 1.5-2.5 parts of NaDES solvent, 1.5-2.5 parts of glucose, 0.5-1.5 parts of urea and 14-16 parts of water.
4. A method of preparing a space structure composition according to any one of claims 1 to 3, comprising the steps of:
the components are subjected to micro-jet homogenization treatment to form a space structure composition.
5. A skin care product comprising the spatial structure composition of any one of claims 1 to 3.
6. The skin care product of claim 5, wherein the components of the skin care product further comprise at least one of a solvent, a humectant, a preservative, and a thickener; the solvent is water, the humectant is at least one of caprylic/capric triglyceride, butanediol and 1, 2-hexanediol, the preservative is p-hydroxyacetophenone, and the thickener is at least one of ammonium acryloyldimethyl taurate/VP copolymer and polyacrylate crosslinked polymer-6.
7. The skin care product according to claim 6, which comprises the following components in parts by weight based on 100 parts by weight:
8-12 parts of caprylic/capric triglyceride, 2-5 parts of butanediol, 0.5-1.5 parts of 1, 2-hexanediol, 0.2-1 part of p-hydroxyacetophenone, 0.1-0.5 part of acrylamide dimethyl taurate/VP copolymer, 0.2-1 part of polyacrylate crosslinked polymer-6, 0.01-2 parts of high molecular space structure mixture, 0.01-100 parts of peony fermentation filtrate and the balance of water.
8. The skin care product according to claim 7, wherein the components of the skin care product further comprise 4-6 parts of water-soluble thickening ionic compound; the water-soluble thickening ion compound is at least one of vitamin C, vitamin C derivatives, decarboxylated carnosine salts, 4-methoxysalicylic acid potassium, tranexamic acid, zinc sulfate, salicylic acid and fruit acid.
9. The method of preparing a skin care product according to claim 8, comprising the steps of:
(1) Mixing and homogenizing all components of the space structure composition to obtain a component a;
(2) Heating and uniformly mixing a solvent, a humectant, a preservative and a thickener, and cooling to 40-50 ℃ to obtain a component A;
(3) And adding the component a and the water-soluble thickening ionic compound into the component A, uniformly mixing, and cooling to 25-30 ℃ to obtain the skin care product.
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