Plant extract as well as preparation method and application thereof

By using a combination of oil and ethanol as extraction solvents, combined with shock extraction and ultrasonic extraction technology, the problem of low extraction rate of fat-soluble active ingredients in traditional methods is solved, achieving more efficient extraction and more stable extracts, suitable for multiple A skin care formula.

CN119385859APending Publication Date: 2025-02-07GUANGZHOU CADLIN COSMETICS
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Patent Information

Application Number
CN202411734171.7
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-11-29
Publication Date
2025-02-07

AI Technical Summary

Technical Problem

Traditional plant extraction methods use water or alcohol as extraction solvents, resulting in a low extraction rate of fat-soluble active ingredient and the extract is not easy to store when compounded into complexes.

Method used

The combination of oil and fat and ethanol is used as the extraction solvent, and the extraction rate of the active ingredient is improved by vibration extraction and ultrasonic extraction, and a co-solvent is added after the deethanol treatment to maintain the stability of the extract.

Benefits of technology

It improves the extraction rate of fat-soluble active ingredients, expands the scope of use of extracts, makes them more stable in the complex, and reduces the irritation and volatility of ethanol to the skin.

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Abstract

The invention relates to the technical field of skin care products, in particular to a plant extract and a preparation method and application thereof. The preparation method comprises the steps that a solvent composition is used as an extraction solvent to extract plant raw materials, an obtained extraction product is subjected to or not subjected to ethanol removal treatment, the plant extract is prepared, and the solvent composition comprises grease and ethanol; the grease is prepared from one or more of C12-15 alcohol benzoate and caprylic acid / capric triglyceride. In the preparation process of the plant extract, the solvent composition serves as an extraction solvent, the extraction rate of active ingredients can be increased, and therefore the fat-soluble plant extract with the skin care effect can be prepared.
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Description

Technical Field

[0001] The present application relates to the technical field of skin care products, and in particular to a plant extract and a preparation method and application thereof. Background Art

[0002] At present, chemical moisturizers such as glycerin, butylene glycol, ceramide, and hyaluronic acid are mainly used in skin care products for moisturizing. However, the use of chemical moisturizers not only fails to maintain long-term moisturizing, but also puts a burden on the skin. Extracting active moisturizing ingredients from natural plants can alleviate the irritation caused by chemical moisturizers to a certain extent. For example, the skin care composition recorded in application number 202410248816.X includes ginseng root water, ginseng root extract, sodium hyaluronate and ceramide NP, wherein the preparation method of ginseng root extract includes the following steps: (1) taking dried ginseng roots, extractants and water, mixing and crushing to obtain ginseng roots; (2) extracting ginseng roots to obtain extracts; (3) filtering, desalting, decolorizing and sterilizing the extracts in turn to obtain.

[0003] However, traditional methods mostly use water or alcohol as extraction solvents to extract active ingredients from natural plants, and the extraction rate of active ingredients (such as fat-soluble active ingredients) is low. Summary of the invention

[0004] Based on this, one or more embodiments of the present application provide a plant extract and a preparation method and application thereof, including the following technical solutions:

[0005] One or more embodiments of the present application provide a solvent composition, which includes oil and ethanol; the oil includes one or more of C12-15 alcohol benzoate and caprylic / capric triglyceride.

[0006] In some embodiments of the present application, the volume ratio of the oil to the ethanol is 1:(1.5-3).

[0007] In some embodiments of the present application, the oil comprises C12-15 alcohol benzoate and caprylic / capric triglyceride in a volume ratio of 1:(1.5-4).

[0008] One or more embodiments of the present application also provide a method for preparing a plant extract, the preparation method comprising: extracting a plant raw material using the solvent composition as an extraction solvent, and preparing the plant extract with or without deethanol treatment of the obtained extract product.

[0009] In some embodiments of the present application, the usage ratio of the plant raw material and the solvent composition is 1 g: (10-100) mL.

[0010] In some embodiments of the present application, the preparation method comprises the following steps: mixing the solvent composition and the plant raw material for vibration extraction and ultrasonic extraction, centrifuging, and collecting the supernatant as the extraction product.

[0011] In some embodiments of the present application, the conditions for the oscillation extraction include: a temperature of 40°C-50°C, a time of 10 min-60 min, and a frequency of 100 r / min-150 r / min.

[0012] In some embodiments of the present application, the conditions for ultrasonic extraction include: temperature of 35°C-65°C, time of 30min-60min, and power of 400W-600W.

[0013] In some embodiments of the present application, the centrifugal conditions include: a temperature of 20°C-30°C and a rotation speed of 7000r / min-9000r / min.

[0014] In some embodiments of the present application, the ethanol removal treatment is carried out by rotary evaporation;

[0015] Optionally, the method further comprises adding a co-solvent to the residue obtained by rotary evaporation;

[0016] Optionally, the cosolvent includes one or more of polysorbate-85, polyglyceryl-2 isostearate, PEG-6 caprylic / capric glycerides, sorbitan sesquioleate and cetyl PEG / PPG-10 / 1 polydimethylsiloxane;

[0017] Optionally, 7g-9g of the co-solvent is added to every 100g of the residue.

[0018] In some embodiments of the present application, the plant raw material includes one or more of Rosa roxburghii, mango pit, evening primrose and Trumpet creeper.

[0019] In some embodiments of the present application, the plant material is sized to pass through a 20-80 mesh sieve.

[0020] One or more embodiments of the present application also provide a plant extract prepared by the preparation method.

[0021] One or more embodiments of the present application also provide a skin care product, comprising the plant extract.

[0022] In some embodiments of the present application, the skin care product includes a complex of a roxburghii extract, a squirrel mango kernel extract, and a trumpet creeper extract;

[0023] Optionally, the complex comprises 1-10 parts of mango seed extract, 1-10 parts of trumpet creeper extract and 1-10 parts of roxburghii roxburghii extract;

[0024] Optionally, the skin care product comprises 5wt%-10wt% of the complex.

[0025] One or more embodiments of the present application also provide a method for preparing the skin care product, the method comprising the following steps:

[0026] The plant extract is prepared by the preparation method; and

[0027] A skin care product comprising the plant extract is prepared.

[0028] In some embodiments of the present application, the preparation method comprises:

[0029] Separately preparing the roxburghii roxburghii extract, the mango seed extract and the trumpet creeper extract, and mixing them to prepare the composite; and

[0030] The skin care product comprising the complex is prepared.

[0031] The details of one or more embodiments of the present application are set forth in the description which follows, and other features, objects, and advantages of the present application will be apparent from the description and its claims. BRIEF DESCRIPTION OF THE DRAWINGS

[0032] In order to more clearly illustrate the technical solutions in the embodiments of the present application and to more completely understand the present application and its beneficial effects, the following is a brief introduction to the drawings required for the description of the embodiments. Obviously, the drawings described below are only some embodiments of the present application, and those skilled in the art can obtain other drawings based on these drawings without creative work.

[0033] Figure 1 The standard curve of DPPH free radical scavenging rate and VE equivalent was drawn;

[0034] Figure 2 It is the statistical chart of VE equivalent corresponding to the selected plant raw materials;

[0035] Figure 3 This is a diagram of Roselle extract under different conditions;

[0036] Figure 4 It is a statistical chart of VE equivalent of different plant extracts obtained by using different solvents;

[0037] Figure 5 This is a statistical chart of VE equivalent of mango kernel extracts obtained using different solvents;

[0038] Figure 6 This is the statistical chart of VE equivalent of mango kernel extract obtained from single factor experiment;

[0039] Figure 7 The effects of three-way interaction on plant extracts;

[0040] Figure 8 This is a statistical chart of VE equivalents of mango seed extract, roxburghii extract and trumpet creeper extract at different compounding ratios;

[0041] Fig. 9 The 10% compound plant extract lotion has a moisturizing and repairing effect on the human body. DETAILED DESCRIPTION

[0042] The present application will be further described in detail below in conjunction with the accompanying drawings, embodiments and examples. It should be understood that these embodiments and examples are only used to illustrate the present application and are not used to limit the scope of the present application. The purpose of providing these embodiments and examples is to make the understanding of the disclosure of the present application more thorough and comprehensive. It should also be understood that the present application can be implemented in many different forms, is not limited to the embodiments and examples described herein, and those skilled in the art can make various changes or modifications without violating the connotation of the present application, and the equivalent form obtained also falls within the protection scope of the present application. In addition, in the description below, a large number of specific details are given in order to provide a more comprehensive understanding of the present application, and it should be understood that the present application can be implemented without one or more of these details.

[0043] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as those commonly understood by those skilled in the art to which this application belongs. The terms used herein in the specification of this application are only for the purpose of describing implementation modes and embodiments and are not intended to limit this application.

[0044] the term

[0045] Unless otherwise specified or incompatible herewith, the terms and phrases used herein shall have the following meanings:

[0046] The terms "and / or", "or / and", and "and / or" used in this article include any one of two or more related listed items, and also include any and all combinations of related listed items, and the arbitrary and all combinations include any two related listed items, any more related listed items, or a combination of all related listed items. It should be noted that when at least three items are connected by at least two conjunctions selected from "and / or", "or / and", and "and / or", it should be understood that in this application, the technical solution undoubtedly includes technical solutions that are all connected by "logical and", and undoubtedly includes technical solutions that are all connected by "logical or". For example, "A and / or B" includes three parallel solutions of A, B and A+B. For example, the technical solution of "A, and / or, B, and / or, C, and / or, D" includes any one of A, B, C, and D (that is, the technical solution that is all connected by "logical OR"), and also includes any and all combinations of A, B, C, and D, that is, the combination of any two or any three of A, B, C, and D, and also includes the combination of four of A, B, C, and D (that is, the technical solution that is all connected by "logical AND").

[0047] In the present application, "plurality", "multiple", "multiple times", "multiples", etc., unless otherwise specified, refer to a number greater than 2 or equal to 2. For example, "one or more" means one or greater than or equal to two.

[0048] As used herein, "combination thereof", "any combination thereof", "any combination thereof" etc. include all suitable combinations of any two or more of the listed items.

[0049] Herein, the “suitable” mentioned in “suitable combination”, “suitable method”, “any suitable method”, etc., shall be based on the ability to implement the technical solution of this application, solve the technical problems of this application, and achieve the expected technical effects of this application.

[0050] Herein, “preferred”, “better”, “more preferred” and “suitable” are merely used to describe implementation methods or examples with better effects, and it should be understood that they do not constitute limitations on the scope of protection of this application.

[0051] In the present application, "further", "further", "particularly" and the like are used for descriptive purposes to indicate differences in content, but should not be construed as limiting the scope of protection of the present application.

[0052] In this application, "optionally", "optional", and "optional" mean optional or dispensable, that is, any one of the two parallel schemes of "yes" or "no". If multiple "options" appear in a technical solution, unless otherwise specified and there is no contradiction or mutual restriction, each "optional" is independent.

[0053] In the present application, the terms "first", "second", "third", "fourth", etc. in "the first aspect", "the second aspect", "the third aspect", "the fourth aspect", etc. are used only for descriptive purposes and cannot be understood as indicating or implying relative importance or quantity, nor can they be understood as implicitly indicating the importance or quantity of the indicated technical features. Moreover, "first", "second", "third", "fourth", etc. only serve the purpose of non-exhaustive enumeration and description, and it should be understood that they do not constitute a closed limitation on quantity.

[0054] In the present application, the technical features described in an open manner include closed technical solutions composed of the listed features, and also include open technical solutions containing the listed features.

[0055] In the present application, when it comes to numerical intervals (i.e., numerical ranges), unless otherwise specified, the optional numerical distribution is considered continuous within the above numerical interval, and includes the two numerical endpoints (i.e., the minimum and maximum values) of the numerical range, and each numerical value between the two numerical endpoints. Unless otherwise specified, when the numerical interval only refers to the integers within the numerical interval, it includes the two endpoint integers of the numerical range, and each integer between the two endpoints. In this article, it is equivalent to directly listing each integer, such as t is an integer selected from 1-10, indicating that t is any integer selected from the integer group consisting of 1, 2, 3, 4, 5, 6, 7, 8, 9 and 10. In addition, when multiple ranges are provided to describe features or characteristics, these ranges can be combined. In other words, unless otherwise specified, the ranges disclosed herein should be understood to include any and all sub-ranges included therein.

[0056] The temperature parameters in this application, unless otherwise specified, are allowed to be either constant temperature treatment or to vary within a certain temperature range. It should be understood that the constant temperature treatment allows the temperature to fluctuate within the accuracy range controlled by the instrument. Fluctuations within the range of ±5°C, ±4°C, ±3°C, ±2°C, and ±1°C are allowed.

[0057] In the present application, % (w / w) and wt% both represent weight percentage, % (v / v) refers to volume percentage, and % (w / v) refers to mass volume percentage.

[0058] All documents mentioned in this application are cited as references in this application, just as each document is cited as reference separately. Unless they conflict with the application purpose and / or technical solution of this application, the cited documents involved in this application are cited with all contents and all purposes. When the cited documents are involved in this application, the definitions of relevant technical features, terms, nouns, phrases, etc. in the cited documents are also cited. When the cited documents are involved in this application, the examples and preferred methods of the cited relevant technical features can also be incorporated into this application as references, but are limited to the implementation of this application. It should be understood that when the cited content conflicts with the description in this application, the present application shall prevail or be modified adaptively according to the description of this application.

[0059] In a first aspect of an embodiment of the present application, a solvent composition is provided, wherein the solvent composition comprises oil and ethanol; the oil comprises one or more of C12-15 alcohol benzoate and caprylic / capric triglyceride.

[0060] The embodiments of the present application provide a solvent composition with a specific formula. Using the solvent composition as an extraction solvent during the preparation of a plant extract can increase the extraction rate of active ingredients, thereby enabling the preparation of a fat-soluble plant extract with moisturizing and repairing effects.

[0061] Traditional plant extraction generally uses water or ethanol as extraction solvent, in which case a part of important fat-soluble active substances in plants such as sterols, oil-soluble vitamins, etc. are difficult to extract and utilize. However, the present application uses a combination of oil and ethanol as extraction solvent, and can extract that part of fat-soluble substances by the method of oil-soluble oil, breaking the limitation of traditionally often using water extraction or alcohol extraction to prepare plant extracts. In addition, general natural active substances are obtained by water extraction or alcohol extraction, and most of them cannot be applied to oil phase products. Using the solvent composition of the present application as extraction solvent can expand the scope of use of the obtained plant extracts and can be applied to more types of formulas. Furthermore, the natural plant extracts prepared with water or ethanol as extraction solvents are not easy to store when compounded into a composite, but the present application uses oil and ethanol extraction, and only a small amount of cosolvent is added on the basis of the overall composite without adding preservatives to keep stable.

[0062] In some of the examples, the volume ratio of the oil to the ethanol is 1:(1-3), for example, 1:1.5, 1:1.6, 1:1.8, 1:2, 1:2.2, 1:2.4, 1:2.6, 1:2.8, and 1:3.

[0063] In some examples, the oil includes C12-15 alcohol benzoate and caprylic / capric triglyceride in a volume ratio of 1:(1.5-4) (e.g., 1:1.5, 1:2, 1:2.2, 1:2.4, 1:2.6, 1:2.8, 1:3, 1:3.2, 1:3.4, 1:3.6, 1:3.8, 1:4).

[0064] The second aspect of the embodiment of the present application provides a method for preparing a plant extract, the preparation method comprising: extracting a plant raw material with the solvent composition described in the first aspect as an extraction solvent, and preparing a plant extract with or without removing ethanol from the obtained extract product. Optionally, the obtained extract product is treated with ethanol removal, and removing ethanol can make the extract more stable in a cosmetic formula (such as an emulsion) system and reduce the volatilization of ethanol, and can also reduce the irritation and damage of ethanol to the skin.

[0065] In some examples, the ratio of the plant material to the solvent composition is 1 g:(10-100) mL, for example, 1:10, 1:15, 1:20, 1:25, 1:30, 1:35, 1:40, 1:45, 1:50, 1:55, 1:60, 1:65, 1:70, 1:75, 1:80, 1:85, 1:90, 1:95, or 1:100.

[0066] In some examples, the preparation method includes the following steps: mixing the solvent composition and the plant material for shaking extraction and ultrasonic extraction, centrifuging, and collecting the supernatant as the extraction product. In the embodiment of the present application, the extraction efficiency is improved by combining the shaking extraction and ultrasonic assisted extraction.

[0067] In some of the examples, the conditions for the oscillation extraction include: a temperature of 40°C-50°C (for example, 40, 41, 42, 43, 44, 45, 46, 47, 48, 49, 50°C), a time of 10min-60min (for example, 10, 15, 20, 25, 30, 35, 40, 45, 50, 55, 60min), and a frequency of 100r / min-150r / min (for example, 100, 105, 110, 115, 120, 125, 130, 135, 140, 145, 150r / min).

[0068] In some of the examples, the conditions for ultrasonic extraction include: temperature of 35°C-65°C (for example, 35, 40, 45, 50, 55, 60, 65°C), time of 30min-60min (for example, 30, 35, 40, 45, 50, 55, 60min), and power of 400W-600W (for example, 400, 450, 500, 550, 600W).

[0069] In some examples, the centrifugal conditions include: a temperature of 20°C-30°C (for example, 20, 21, 22, 23, 24, 25, 26, 27, 28, 29, 30°C), a rotation speed of 7000r / min-9000r / min (for example, 7000, 7100, 7200, 7300, 7400, 7500, 7600, 7700, 7800, 7900, 8000, 8100, 8200, 8300, 8400, 8500, 8600, 8700, 8800, 8900, 9000r / min).

[0070] In some of these examples, the ethanol removal was performed by rotary evaporation;

[0071] Optionally, the method further comprises adding a co-solvent to the residue obtained by rotary evaporation;

[0072] Optionally, the cosolvent includes one or more of polysorbate-85, polyglyceryl-2 isostearate, PEG-6 caprylic / capric glycerides, sorbitan sesquioleate and cetyl PEG / PPG-10 / 1 polydimethylsiloxane;

[0073] Optionally, 7.0 g to 9.0 g (e.g., 7.0, 7.1, 7.2, 7.3, 7.4, 7.5, 7.6, 7.7, 7.8, 7.9, 8, 8.1, 8.2, 8.3, 8.4, 8.5, 8.6, 8.7, 8.8, 8.9, 9.0 g) of the co-solvent is added to every 100 g of the residue.

[0074] In some embodiments of the present application, the plant raw material includes one or more of Rosa roxburghii, mango pit, evening primrose and Trumpet creeper.

[0075] In some embodiments of the present application, the plant material is sized to pass through a 20-80 mesh sieve.

[0076] Optionally, the antioxidant capacity of natural plant extracts is used as an evaluation index, and the compounding ratio is determined by uniform design. Except for plant extracts that have been deethanolized, a small amount of co-solvent can be added to make them more stable without adding preservatives.

[0077] The third aspect of the embodiments of the present application provides a plant extract prepared by the preparation method described in the second aspect.

[0078] A fourth aspect of the embodiments of the present application provides a skin care product, which includes the plant extract described in the third aspect.

[0079] In some of these examples, the skin care product includes a complex of prickly pear extract, squirrel mango kernel extract, and trumpet creeper extract;

[0080] Optionally, the complex comprises 1-10 parts of mango seed extract, 1-10 parts of trumpet creeper extract and 1-10 parts of roxburghii roxburghii extract;

[0081] Optionally, the skin care product comprises 5 wt%-10 wt% (eg, 5%, 6%, 7%, 8%, 9%, 10%) of the complex.

[0082] A fifth aspect of the embodiments of the present application provides a method for preparing the skin care product described in the fourth aspect, the method comprising the following steps:

[0083] The plant extract is prepared by the preparation method described in the second aspect; and

[0084] A skin care product comprising the plant extract is prepared.

[0085] In the process of preparing the skin care product, the preparation method described in the second aspect can be referred to first, and the extracts of mango pit, trumpet creeper and roxburghii can be prepared respectively, and then the ethanol removal treatment is performed after mixing. Compared with the ethanol removal treatment, the situation where the amount of co-solvent used is too large and is not conducive to use in the formulation system can be avoided.

[0086] The embodiments of the present application will be described in detail below in conjunction with examples. It should be understood that these examples are only used to illustrate the present application and are not intended to limit the scope of the present application. The experimental methods for which specific conditions are not specified in the following examples are preferably referred to the guidance provided in the present application, and can also be based on the experimental manual or normal conditions in this area, can also be based on the conditions recommended by the manufacturer, or refer to experimental methods known in the art.

[0087] In the following specific embodiments, the measured parameters of raw material components may have slight deviations within the range of weighing accuracy unless otherwise specified. For temperature and time parameters, acceptable deviations caused by instrument test accuracy or operation accuracy are allowed.

[0088] In order to further illustrate the present application, the following examples are used to provide a detailed description. The raw materials used in the following examples of the present application are all commercially available products. The raw materials used in the examples of the present application are commercially available products.

[0089] In the following embodiments: wherein,

[0090] DPPH free radical scavenging rate determination method

[0091] Accurately weigh DPPH, make up to volume with ethanol solution to prepare a DPPH working solution with a concentration of 101 μmoL / L, take 200 μL of the test solution and mix it thoroughly with 3.0 mL of DPPH working solution, let it stand at room temperature in the dark for 20 min, use anhydrous ethanol as a blank control, measure the absorbance at a wavelength of 517 nm, and measure each sample in parallel 3 times.

[0092] Clearance rate / % = [(A control -A sample ) / A control ]×100%

[0093] A control is the absorbance value of blank control, A sample Sample absorbance

[0094] Determination method of VE standard curve

[0095] VE was diluted to concentrations of 0.0, 15.0, 30.0, 60.0, 120.0, 240.0, and 480.0 μmol / L. A certain amount of VE solution was mixed with 3.0 mL of DPPH working solution and allowed to stand at room temperature in the dark for 20 min. The absorbance was measured at a wavelength of 517 nm. A standard curve was drawn with VE concentration as the abscissa (X) and absorbance value (Y as the ordinate). The linear relationship between VE concentration and absorbance within the range of 0.0-5.0 μmol / L was good, and the linear fitting equation was y=0.1775x+0.0166(R 2 =0.9977).

[0096] The DPPH free radical scavenging rate of the extract was referenced to the standard curve ( Figure 1 ) is expressed as VE equivalent, and all samples were measured three times.

[0097] The content of the embodiment is as follows:

[0098] 1. Screening methods for raw materials and extraction solvents

[0099] 1.1 Screening of plant raw materials

[0100] Plants are rich in active substances, such as terpenes, flavonoids, phenolic acids, sterols, carotenoids, vitamin A, organic acids, polyunsaturated fatty acids, etc., which not only have strong antioxidant and anti-aging abilities, but also have certain moisturizing and skin-emollient abilities. In this example, the antioxidant ability of the extract is used as the evaluation standard to screen plant raw materials rich in such substances and select the raw materials of the composite plant extract.

[0101] 1.1.1 Preparation of plant materials

[0102] The selected plant raw materials (coconut meat, roxburghii, mango kernel, peony seed, schisandra chinensis, roselle, evening primrose or trumpet creeper) are dried at 45° C., crushed, and sieved (40 meshes), and the prepared powder is stored for later use.

[0103] 1.1.2 Screening of plant raw materials

[0104] The above-prepared raw materials are further screened, and the screening steps include:

[0105] Weigh a certain amount of powder → shake and extract at 45℃ for 30min → ultrasonic extraction at 45℃ for 45min → centrifuge to obtain supernatant.

[0106] Among them, the material-liquid ratio is 1:50 (g:mL), the shaking frequency of the shaking table is 120r / min, the ultrasonic extraction power is 500W, the centrifugal speed is 8000r / min at room temperature, and the extraction solvent is a mixture of oil (the volume ratio of oil A to oil E is 1:3) and ethanol with a volume ratio of 1:2.

[0107] The results are expressed in VE equivalents.

[0108] 1.2 Screening of extraction solvent

[0109] 1.2.1 Selection of polar grease

[0110] Commonly used oils in laboratories are roughly classified into high, medium and low polarity oils, such as C12-15 alcohol benzoate, ethylhexyl palmitate, triethylhexanoin, and caprylic / capric triglyceride.

[0111] Referring to Table 1, oil and ethanol are mixed in a certain ratio (volume ratio of oil to ethanol is 1:2), and the obtained mixture is used as the extraction solvent to extract the plant material. The extraction steps are as described in Item 1.1.2, and the plant material is mango pit. The results are calculated in VE equivalent.

[0112] 1.2.2 Compounding of polar oils

[0113] Referring to Table 3, the polar oils screened were compounded, the oils were matched in different proportions, and then the mixed oils were mixed with ethanol in a certain proportion (the volume ratio of oil to ethanol was 1:2), and the obtained mixture was used as the extraction solvent to extract the plant raw material. The extraction steps were recorded in Item 1.1.2, and mango kernels were selected as the plant raw material for extraction. The results are calculated in VE equivalent.

[0114] 1.2.3 Compounding of polar oils and ethanol

[0115] Referring to Table 4, the selected polar oils and ethanol were compounded in a certain ratio (polar oil: ethanol = 1:1, 1:2, 1:3), and the obtained mixture was used as the extraction solvent for plant extraction. The extraction steps were recorded in Item 1.1.2. Mango kernels were selected as the extraction raw material, and the results were calculated in VE equivalents.

[0116] 2. Experimental results

[0117] 2.1 Screening results of plant raw materials

[0118] The prepared plant materials are extracted under the same extraction conditions, as described in Item 1.1.2.

[0119] result Figure 2 As shown. Figure 2 It can be seen that the clearance rates of sea buckthorn, evening primrose, roxburghii, trumpet creeper, mango seed and roselle are relatively high, among which mango seed extract has the highest VE equivalent. Figure 3 As shown in the results, Roselle contains a large amount of anthocyanins, which will change color under high temperature and light conditions, affecting its activity. Therefore, in the subsequent experiments, this raw material was discarded in order to ensure the stability of the extract. Finally, Rosa roxburghii, mango kernel and trumpet creeper were used as the raw materials for the composite extract.

[0120] 2.2 Screening results of extraction solvents

[0121] 2.2.1 Screening results of polar oils and fats

[0122] Table 1. Selection of oils with different polarity (volume ratio)

[0123]

[0124] Table 2 (corresponding Figure 4 ), the effect of different polarity oils on raw material extraction (results in VE equivalent / μmol)

[0125] Experiment number Mango pit Rosa roxburghii Trumpet creeper 1 21.56 19.63 4.44 2 12.35 16.23 3.13 3 15.14 13.87 3.60 4 18.53 18.38 3.65 5 20.73 21.79 4.35

[0126] Table 2 and Figure 4 The results show that in the extraction process of mango kernel, experiment number 1 was found to have the best effect, and its VE equivalent could reach 21.56 μmol; in the extraction process of roxburghii, experiment 5 was found to have the best effect, and its VE equivalent was 21.79 μmol; in the extraction process of trumpet creeper, experiment 1 had the best extraction effect, and the clearance rate could reach 88.84%, and the VE equivalent was 4.44 μmol. Therefore, the combination of A and E oils was considered comprehensively to explore their extraction capacity after compounding.

[0127] 2.2.2 Compounding results of polar oils

[0128] The oils and fats were compounded according to the compounding ratio shown in Table 3 and then compounded with ethanol at a volume ratio of 1:2. The extraction was performed according to the description under 1.1.2 and the obtained extracts were tested. The results are shown in the following table and Figure 5 shown.

[0129] Table 3. Preferred oils and fats (volume ratio)

[0130] Experiment number A E Clearance rate / % VE / μmoL 1 0.75 0.25 40.38 19.28 2 1 0 45.71 22.45 3 0.25 0.75 52.10 25.36 4 0.5 0.5 44.95 21.89 5 0 1 48.19 20.73

[0131] According to the above experimental results, when the ratio of oil A to E is 1:3, the DPPH clearance rate of the obtained extract is the highest, and the VE equivalent is 25.36 μmol. Therefore, the subsequent experiments choose the ratio of A:E=1:3 for extraction.

[0132] 2.2.3 Results of compounding polar oils and ethanol

[0133] The ratio of compounded oil and ethanol is shown in Table 4. Extraction is performed according to the description under 1.1.2, and the extract is tested. The results are shown in the following table.

[0134] Table 4. Compounding of mixed oils and ethanol (volume ratio)

[0135] Experiment number Mixed Grease Ethanol Clearance VE / μmoL 1 1 1 36.27 17.61 2 1 2 52.21 25.35 3 1 3 51.73 25.12

[0136] According to the above experimental results, when the ratio of compounded oil and ethanol is 1:2, the DPPH removal rate of the obtained extract is the highest, and the VE equivalent is 25.35 μmol. Therefore, the subsequent experiments choose the ratio of oil: ethanol = 1:2 for subsequent experiments.

[0137] 2. Preparation of natural plant extracts (process optimization using mango kernel raw materials)

[0138] 2.1 Extraction process optimization

[0139] Traditional extraction methods are generally water extraction or alcohol extraction, but they will waste some oil-soluble substances in plant species. Therefore, this application uses oil and alcohol composite extraction in the extraction. The oil-soluble oil extraction method is added to the traditional extraction method, which can extract effective active ingredients to a greater extent; in addition, in the ultrasonic extraction method, it can promote the expansion of plant cell wall pores, increase the speed and frequency of material molecular movement, and thus increase the speed at which the target component enters the solvent. This application also adds high-temperature shaking and high-temperature ultrasonic extraction to the traditional extraction method, which saves time and improves efficiency. The DPPH clearance rate and VE equivalent of the extract are used as evaluation indicators, and the process is optimized.

[0140] 2.1.1 Single factor experiment of extracts

[0141] Initial conditions for single factor experiment:

[0142] Accurately weigh the plant raw materials of roxburghii, mango core and trumpet creeper powder, add oil and ethanol in a volume ratio of 1:2, and the volume ratio of A oil:E oil in the oil is 1:3 for extraction. The extraction steps refer to the steps recorded in 1.1.2, and set up a single factor variable experiment.

[0143] Under the initial conditions, the effects of solid-liquid ratio, ultrasonic time, ultrasonic temperature and extraction time on the scavenging rate of DPPH free radicals in the extract were investigated.

[0144] in,

[0145] The material-liquid ratio (g:mL) was set at five levels: 1:10, 1:50, 1:100, and 1:200;

[0146] Ultrasonic time (min) was set at four levels: 15, 30, 45, and 60;

[0147] The ultrasonic temperature (°C) was set at four levels: 35, 45, 55, and 65;

[0148] The extraction time (min) can be set to four levels: 15, 30, 45, and 60.

[0149] 2.1.2 Response surface analysis of extraction process

[0150] On the basis of single factor experiments, the solid-liquid ratio, ultrasonic time, ultrasonic temperature and extraction time were selected for response surface analysis to determine the optimal extraction conditions. The response surface experimental scheme is shown in Table 5.

[0151] Table 5. Response surface test factor design table

[0152] serial number A: Material-Liquid Ratio B: Ultrasonic time / min C: Ultrasonic temperature / ℃ D: Extraction time / min -1 1:10 30 35 15 0 1:50 45 45 30 1 1:100 60 55 45

[0153] 2.1.3 Response surface experiment verification

[0154] Accurately weigh the roxburghii, mango kernel, and trumpet creeper powder, extract them according to the optimal extraction conditions of the response surface experiment, and record their DPPH scavenging rates.

[0155] 2.1.4 Calculation of synergistic effect (SE) of compound components

[0156] The actual antioxidant value (EAC) of a single component is expressed as an IC50 value (TE), and the theoretical antioxidant capacity (TAC) of a mixed component is related to the antioxidant capacity of a single component.

[0157] TAC=W a ×T a +W b ×T b +W c ×T c

[0158] Ta-Tc represent the antioxidant capacity of single components using the same fixed dose, and Wa-Wc represent the weight of the antioxidant capacity of each extract in the single component of the sample.

[0159] The synergistic effect (SE) is the ratio of the theoretical effect to the actual effect:

[0160]

[0161] In the formula: SE>1 represents synergistic effect, SE<1 represents antagonism, and SE=1 represents additive effect.

[0162] 2.1.5 Human Experiment Evaluation Methods

[0163] Participants: Healthy women or men aged 18-60, with dull, dry and rough facial skin; no allergic diseases, no history of allergies to cosmetics or other topical preparations; no history of photosensitivity diseases, and no recent use of drugs that affect photosensitivity; the skin of the test area should be free of inflammation.

[0164] Experimental products:

[0165] Sample A: Emulsion-based formula, with 10% compound plant extract added.

[0166] Control B: Emulsion-based formula without adding compound plant extract.

[0167] Usage: D0-D28: Use sample A once in the morning and evening in the product area (do not use in the morning on D1); use control B in the control area. D0, H24, D7, D14 and D28 respectively represent: before use, 24 hours after use, 7 days after use, 14 days after use and 28 days after use.

[0168] Research design: 5-10 volunteers use the experimental product on their faces for 14 days, and the moisture content of the stratum corneum, skin gloss, skin elasticity and a value are measured before the test and 24 hours, 7 days and 14 days after using the experimental product. The location of each test area for each volunteer is as consistent as possible, with the left and right face skin of the volunteer as the product area (experimental group) and the control area (control group) (left A and right B). All operations are completed by the same person to reduce accidental errors. On the day of the test, the volunteers do not use the product. After cleaning the test area, it needs to be balanced for at least 30 minutes at a room temperature of 21±1℃ and a relative humidity of 55%±5% before testing.

[0169] Determination of efficacy indicators: Before using the product, and 24 hours, 7 days, 14 days and 28 days after using the product, the moisture content of the skin stratum corneum, skin gloss, skin elasticity and a value were measured using a CK probe and a VISIA-CR instrument respectively.

[0170] 2.2 Experimental Results

[0171] 2.2.1 Single factor experimental results

[0172] The effects of various factors on the DPPH of the extracts are shown in Table 6 and Figure 6 As shown in the figure, the antioxidant capacity of plant extracts is different under different conditions. When the solid-liquid ratio is 1:50, its antioxidant capacity reaches its peak, and the antioxidant capacity first increases and then decreases with the ultrasonic time and extraction time. However, it can be seen from the figure that the antioxidant capacity also increases with the increase of ultrasonic temperature. However, considering the energy consumption and efficiency issues, the solid-liquid ratio of 1:10-100, ultrasonic time of 30-60min, ultrasonic temperature of 35-55℃ and extraction time of 45min were selected for subsequent experiments.

[0173] Table 6. Effects of various factors on DPPH of extracts

[0174]

[0175]

[0176] 2.2.2 Establishment of response surface model and significance test

[0177] The experimental software used was Design-Expert8, and the Box-Behnhen experimental principle was applied to complete the response surface experimental design. The results are shown in Table 7. The experimental data were subjected to multiple regression analysis, and the variance analysis results of the regression model of Y were obtained, as shown in Table 8. Then, the multiple linear regression equation was used for fitting, and the results were as follows:

[0178] Y=25.41+0.21A+0.70B+0.57C-0.049AB+0.15AC+0.76BC-2.65A 2 -4.72B 2 -1.75C 2 .

[0179] Table 7. Response surface design results

[0180] Experiment number Material-liquid ratio Ultrasound time Ultrasonic temperature DPPH / % VE / μmoL 1 10 30 45 62.51 17.60 2 100 30 45 64.13 18.05 3 10 60 45 64.32 18.11 4 100 60 45 65.25 18.36 5 10 45 35 72.61 20.45 6 100 45 35 73.33 20.64 7 10 45 55 74.80 21.07 8 100 45 55 77.71 21.88 9 55 30 35 63.32 17.83 10 55 60 35 66.42 18.70 11 55 30 55 62.75 17.66 12 55 60 55 76.61 21.57 13 55 45 45 88.90 25.04 14 55 45 45 89.31 25.15 15 55 45 45 91.45 25.74 16 55 45 45 92.16 25.94 17 55 45 45 89.41 25.18

[0181] As shown in Table 7, the regression model significance result of VE equivalent (μmoL) (Y) in the extract indicated P < 0.0001, showing a significant difference. The lack of fit term is usually used to evaluate the reliability of the equation. If it is significant, the equation simulation is poor, otherwise it is good. The lack of fit term of Y is > 0.05, and the analysis is not significant, so the experimental model is reliable. 2(Y) = 0.9831, indicating that the model is consistent with the actual experiment with a high degree of fit. The regression equation of this experiment can be used to replace the actual experimental points, and speculation and analysis can be performed based on the VE equivalent in the plant extract.

[0182] According to the significant results of the regression model, the first-order terms are not significant; the second-order term A 2 , B 2 The differences were all very significant, C 2 The difference is not significant, so the degree of factor influence on extraction is: A=B>C.

[0183] Table 8. Analysis of variance of regression model

[0184] Sources of variance Degrees of Freedom sum of squares Mean Square F-number P-value Significance Model 9 158.57 17.62 45.29 <0.0001 *** A 1 0.37 0.37 0.95 0.3625 B 1 3.93 3.93 10.10 0.0155 C 1 2.60 2.60 6.69 0.0361 AB 1 9.72 9.720E-003 0.025 0.8789 AC 1 0.096 0.096 0.25 0.6345 BC 1 2.31 2.31 5.95 0.0448 <![CDATA[A 2 ]]> 1 29.66 29.66 76.26 <0.0001 *** <![CDATA[B 2 ]]> 1 93.99 93.99 241.62 <0.0001 *** <![CDATA[C 2 ]]> 1 12.83 12.83 32.99 0.0007 Residual 7 2.72 0.39 Lack of Fit 3 2.07 0.69 4.25 0.0987 Pure Error 4 0.65 0.16 Total difference 16 161.29

[0185] 2.2.3 Response surface three-factor interaction analysis

[0186] The effects of the interaction of A, B, and C on plant extracts Figure 7 As shown in the figure, the slope of the response surface formed by AB and BC is relatively steep, and the contour lines are elliptical and relatively dense, indicating that the AB and AC factors have a relatively large impact on it; however, the AC response surface is relatively flat, and the contour lines are nearly circular, indicating that their interaction is not significant and their impact on it is not significant.

[0187] 2.2.4 Verification Experiment

[0188] The analysis software Design-Expert8, the corresponding optimal conditions are a solid-liquid ratio of 55g / mL, an ultrasonic time of 45min, and an ultrasonic temperature of 45°C. However, for actual operation, the conditions were adjusted to a solid-liquid ratio of 50g / mL, an ultrasonic time of 45min, and an ultrasonic temperature of 45°C, and 3 groups of repeated experiments under the same conditions were performed. The average value was 91.40%, which was 0.70% lower than the actual theory and within an acceptable range.

[0189] 2.3 Mixture design method for compounding extracts and antioxidant evaluation method

[0190] 2.3.1 Uniform Experimental Design

[0191] The core idea of ​​uniform experiment is to use a deterministic method to find a set of points evenly distributed in space to achieve uniform distribution in the entire experimental factor space; more information can be obtained with fewer experiments. The uniform design table is shown in Table 9.

[0192] Table 9. Uniform experimental design and results

[0193] Experimental Coding X1 mango core X2 Rosa roxburghii X3 Trumpet Creeper DPPH removal rate / % VE / μmoL / mL 1 10(1.0) 6(0.6) 7(0.7) 88.25 13.96 2 3(0.3) 10(1.0) 6(0.6) 77.75 4.45 3 7(0.7) 1(0.1) 5(0.5) 82.18 15.95 4 8(0.8) 8(0.8) 9(0.9) 85.45 6.98 5 6(0.6) 9(0.9) 2(0.2) 83.82 10.67 6 2(0.2) 2(0.2) 8(0.8) 83.53 3.20 7 1(0.1) 7(0.7) 4(0.4) 72.64 2.98 8 9(0.9) 3(0.3) 3(0.3) 91.23 61.33 9 4(0.4) 5(0.5) 1(0.1) 87.48 5.52 10 5(0.5) 4(0.4) 10(1.0) 84.87 4.12

[0194] According to the optimal extraction conditions obtained from the above experiment (method under 1.1.2), the three plants of mango pit, roxburghii and trumpet creeper were extracted respectively, and then centrifuged to obtain the supernatant for later use, and then mixed according to the uniform design table in Table 9, and the DPPH free radical scavenging rate and VE equivalent per unit volume were determined as the evaluation criteria.

[0195] Depend on Figure 8 It can be seen that the DPPH scavenging rate of the eighth group of complexes is the highest, that is, the antioxidant capacity is strongest when the ratio of mango kernel extract: roxburghii extract: trumpet creeper extract is 3:1:1.

[0196] 2.3.2 Synergy Analysis

[0197] Table 10. Synergistic effect experiment of plant extracts

[0198] Experimental Coding X1 mango core X2 Rosa roxburghii X3 Trumpet Creeper Practical Effects Theoretical Effect SE 1 10(1.0) 6(0.6) 7(0.7) 9.75 65.18 6.68 2 3(0.3) 10(1.0) 6(0.6) 30.57 58.71 1.92 3 7(0.7) 1(0.1) 5(0.5) 8.53 39.71 4.65 4 8(0.8) 8(0.8) 9(0.9) 19.50 50.60 2.59 5 6(0.6) 9(0.9) 2(0.2) 12.77 49.27 3.86 6 2(0.2) 2(0.2) 8(0.8) 42.53 57.82 1.36 7 1(0.1) 7(0.7) 4(0.4) 45.76 62.39 1.36 8 9(0.9) 3(0.3) 3(0.3) 2.22 36.89 16.62 9 4(0.4) 5(0.5) 1(0.1) 24.69 46.96 1.90 10 5(0.5) 4(0.4) 10(1.0) 33.03 53.21 1.61

[0199] The application of single-ingredient extracts in cosmetics has the characteristics of single efficacy and insufficient functions. Therefore, the three plant extracts were compounded to test the synergistic effect after compounding, and the results are shown in Table 10. In the DPPH oxidation model, all compound components showed synergistic effects (SE>1), among which the experimental numbers 8, 1, 3, and 5 had the best synergistic effects, with SEs of 16.62, 6.68, 4.65, and 3.86, respectively.

[0200] 3. Evaluation of the moisturizing and repairing efficacy of the compound extract

[0201] 3.1 Preparation of compound extracts

[0202] Referring to the description under 1.1.2, accurately weigh mango kernel, roxburghii and trumpet creeper powder respectively for extraction, centrifuge, collect the supernatant, and prepare mango kernel extract, roxburghii extract and trumpet creeper extract accordingly;

[0203] Then, the mango seed extract: the roxburghii extract: the trumpet creeper extract were mixed in a volume ratio of 3:1:1 to prepare a mixed extract;

[0204] Next, the ethanol was evaporated by rotary evaporation, and 9% of the cosolvent polysorbate-85 was added to the residue (9 g of cosolvent was added per 100 g of the residue) to prevent the components from leaching out.

[0205] Test of moisturizing and repairing effect: The compounded plant extract was added to the basic formula of the lotion at an addition amount of 10wt%, recorded as sample A (containing 10wt% compounded plant extract), and a long-term human experiment was carried out. At the same time, the basic formula of the lotion without adding the compounded plant extract was used as a control, recorded as control B.

[0206] Table 11. Emulsion basic formula

[0207] raw material Addition amount / % PEG-20 Methyl Glucose Sesquistearate, Tocopherol (Vitamin E) 2.00 Methyl Glucose Sesquistearate 1.00 Dimethicone 10.00 Tocopheryl acetate 2.00 Cetearyl Alcohol 0.60 Deionized water 70.51 Paraben 0.10 EDTA-Disodium 0.10 Butanediol 3.00 2% Acrylates / C10-30 Alkyl Acrylate Crosspolymer 10.00 Triethanolamine 0.15 Phenoxyethanol, Ethylhexylglycerin 0.44 essence 0.10

[0208] 3.2 Human moisturizing and repair test

[0209] Five volunteers with dry, dull facial skin and damaged skin barrier were recruited. They were treated with a lotion containing 10% compound plant extracts (i.e., sample A) and a lotion without compound plant extracts (i.e., control B) on their left and right faces for 4 weeks, respectively. Follow-up visits were conducted on the 1st, 7th, 14th and 28th days according to the test indicators in Table 12.

[0210] Table 12. Human experimental determination indicators

[0211]

[0212] The moisturizing and repairing effects of lotions with 10% compound plant extracts and lotions without compound plant extracts on the human body Fig. 9 As shown, in the same period of time, the stratum corneum water content, skin gloss and skin elasticity of the skin using the lotion added with 10% compound plant extract were significantly higher than those of the skin using the lotion without adding compound plant extract, and in the same period of time, the a value of the skin using the lotion added with 10% compound plant extract was significantly lower than that using the lotion without adding compound plant extract, indicating that the extracted plant extract has certain effects on moisturizing and alleviating skin sensitivity on human skin.

[0213] The technical features of the above-mentioned implementation modes and examples can be combined in any appropriate manner. To make the description concise, not all possible combinations of the technical features in the above-mentioned implementation modes and examples are described. However, as long as there is no contradiction in the combination of these technical features, they should be considered to be within the scope of this specification.

[0214] The above-described embodiments only express several implementation methods of the present application, which is convenient for understanding the technical solution of the present application in detail, but it cannot be understood as a limitation on the scope of protection of the patent application. It should be pointed out that for ordinary technicians in this field, without departing from the concept of the present application, several deformations and improvements can be made, which all belong to the protection scope of the present application. In addition, it should be understood that after reading the above-mentioned teaching content of the present application, the technicians in this field can make various changes or modifications to the present application, and the equivalent forms obtained also fall within the protection scope of the present application. It should also be understood that the technical solutions obtained by the technicians in this field through logical analysis, reasoning or limited experiments on the basis of the technical solutions provided in the present application are all within the protection scope of the claims attached to the present application. Therefore, the protection scope of the patent of the present application shall be based on the content of the attached claims, and the description and drawings can be used to explain the content of the claims.

Claims

1. A solvent composition, characterized in that The solvent composition comprises oil and ethanol; the oil comprises one or more of C12-15 alcohol benzoate and caprylic / capric triglyceride.

2. The solvent composition according to claim 1, characterized in that The volume ratio of the oil to the ethanol is 1:(1.5-3).

3. The solvent composition according to any one of claims 1 to 2, characterized in that The oil comprises C12-15 alcohol benzoate and caprylic / capric triglyceride in a volume ratio of 1:(1.5-4).

4. A method for preparing a plant extract, characterized in that: The preparation method comprises: extracting plant raw materials using the solvent composition described in any one of claims 1 to 3 as an extraction solvent, and preparing a plant extract with or without deethanol treatment of the obtained extraction product.

5. The method for preparing the plant extract according to claim 4, characterized in that: The usage ratio of the plant raw material and the solvent composition is 1 g: (10-100) mL.

6. The method for preparing the plant extract according to claim 5, characterized in that: The preparation method comprises the following steps: mixing the solvent composition and the plant raw material for vibration extraction and ultrasonic extraction, centrifuging, and collecting the supernatant as the extraction product.

7. The method for preparing the plant extract according to claim 6, characterized in that: The preparation method satisfies one or more of the following conditions (1) to (3): (1) The conditions for oscillation extraction include: temperature of 40°C-50°C, time of 10 min-60 min, frequency of 100 r / min-150 r / min; (2) The conditions of ultrasonic extraction include: temperature of 35°C-65°C, time of 30 min-60 min, power of 400 W-600 W; and, (3) The centrifugal conditions include: temperature of 20°C-30°C and rotation speed of 7000 r / min-9000 r / min.

8. The method for preparing a plant extract according to any one of claims 4 to 7, characterized in that: The ethanol removal was carried out by rotary evaporation; Optionally, the method further comprises adding a co-solvent to the residue obtained by rotary evaporation; Optionally, the cosolvent includes one or more of polysorbate-85, polyglyceryl-2 isostearate, PEG-6 caprylic / capric glycerides, sorbitan sesquioleate and cetyl PEG / PPG-10 / 1 polydimethylsiloxane; Optionally, 7g-9g of the co-solvent is added to every 100g of the residue.

9. The method for preparing a plant extract according to any one of claims 4 to 7, characterized in that: The plant raw materials include one or more of roxburghii, mango pit, evening primrose and trumpet creeper.

10. The method for preparing a plant extract according to any one of claims 4 to 7, characterized in that: The plant raw material is sieved through a 20-80 mesh sieve.

11. The plant extract prepared by the preparation method according to any one of claims 4 to 10.

12. A skin care product, characterized in that: The skin care product comprises the plant extract according to claim 11.

13. The skin care product according to claim 12, characterized in that: The skin care product includes a complex of roxburghii extract, squirrel mango kernel extract and trumpet creeper extract; Optionally, the complex comprises 1-10 parts of mango seed extract, 1-10 parts of trumpet creeper extract and 1-10 parts of roxburghii roxburghii extract; Optionally, the skin care product comprises 5wt%-10wt% of the complex.

14. The method for preparing the skin care product according to any one of claims 12 to 13, characterized in that: The preparation method comprises the following steps: The plant extract is prepared by the preparation method according to any one of claims 4 to 10; and A skin care product comprising the plant extract is prepared.

15. The method for preparing a skin care product according to claim 14, characterized in that: The preparation method comprises: Separately preparing the roxburghii roxburghii extract, the mango seed extract and the trumpet creeper extract, and mixing them to prepare the composite; and The skin care product comprising the complex is prepared.

Citation Information

Patent Citations

  • Skin nourishing composition and application thereof in preparation of cosmetics with moisturizing and / or soothing effects

    CN118304229A