Rhodiola rosea extract product as well as preparation method and application thereof

Abstract

The invention relates to the technical field of cosmetics, in particular to a rhodiola rosea extract product and a preparation method and application thereof. The rhodiola rosea extraction product is prepared from the following components in parts by mass: 114 to 164 parts of salidroside, 25 to 36 parts of tyrosol and 0.108 to 0.157 part of quercetin. The mass ratio of the salidroside to the total flavonoids in the rhodiola rosea extract product is (8-12): 1. The invention provides a rhodiola rosea extract product which contains salidroside, tyrosol and quercetin with higher concentration under the condition that the content of total flavonoids is not changed basically, so that the whitening effect, the safety and the synergistic interaction effect on nicotinamide and tranexamic acid of the product can be enhanced, and the problem that the application of plant extracts in cosmetics is limited is solved.

Description

Technical Field

[0001] The invention relates to the technical field of cosmetics, and in particular to a rhodiola rosea extract product and a preparation method and application thereof. Background Art

[0002] In recent years, natural plant extracts have been increasingly used in cosmetic raw materials due to their safety, mildness and effectiveness. The effective enrichment of active ingredients in plant extracts has also become one of the hot topics of concern. Traditional extraction methods include immersion, hot reflux extraction, ultrasonic extraction, microwave-assisted extraction, supercritical fluid extraction, bio-enzymatic hydrolysis, etc., but these methods have the disadvantages of low active ingredient content, high cost, and long time consumption. The main reason is that the active ingredients in plants often exist in the vacuoles and plant cell walls inside plant cells. Conventional extraction solvents are difficult to destroy the cell walls, and the active ingredients are difficult to dissolve from the plant cell walls. Therefore, the direct solvent extraction method is often difficult to achieve efficient extraction. At present, physical methods such as crushing are used in plant pretreatment processes, but due to the crushing capacity of the crushing equipment and the high toughness of plant fibers, it is often difficult to achieve significant results.

[0003] Rhodiola rosea is a perennial herb or shrub plant of the Crassulaceae family. Its medicinal part is the dried root of Rhodiola rosea. Due to its excellent UV resistance, Rhodiola rosea extract is widely used in whitening cosmetics. However, due to the low content of active ingredients in Rhodiola rosea extracts, and the fact that tyrosol, as the aglycone of salidroside, rarely exists in free form, the extraction rate is low; coupled with the limitation of the amount of addition, it cannot play a major whitening role in whitening cosmetics. Therefore, traditional whitening agents such as niacinamide and tranexamic acid are still the main whitening ingredients in whitening cosmetics, but these traditional whitening agents are often accompanied by skin irritation.

[0004] Therefore, it is of great significance to specifically increase the content of important active ingredients in Rhodiola rosea extract, improve the whitening effect, and alleviate the skin irritation of traditional whitening ingredients.

[0005] In view of this, the present invention is proposed. Summary of the invention

[0006] One object of the present invention is to provide a Rhodiola rosea extract product, in which the contents of salidroside, tyrosol and quercetin are significantly increased while the total flavonoids content remains substantially unchanged, thereby improving the efficacy and safety of the product.

[0007] Another object of the present invention is to provide a method for preparing a Rhodiola rosea extract product.

[0008] Another object of the present invention is to provide the use of Rhodiola rosea extract in the preparation of skin care products.

[0009] In order to achieve the above-mentioned object of the present invention, the present invention provides a Rhodiola rosea extract product, comprising the following components by mass:

[0010] 114-164 parts of salidroside, 25-36 parts of tyrosol and 0.108-0.157 parts of quercetin;

[0011] The mass ratio of the salidroside to the total flavonoids in the rhodiola rosea extract product is (8-12):1.

[0012] In a specific embodiment of the present invention, the Rhodiola rosea extract product includes the following components by mass:

[0013] 4.5-6.5 parts of Rhodiola rosea extract, 46-49 parts of butylene glycol and 46-49 parts of water.

[0014] Another aspect of the present invention provides a method for preparing a Rhodiola rosea extract product, comprising the following steps:

[0015] (a) treating Rhodiola rosea at 110-150°C and 0.145-0.5 MPa for 10-30 min;

[0016] (b) Using ethanol aqueous solution as the extraction solvent, with a solid-liquid ratio of 1:(20-50), extracting the Rhodiola rosea treated in step (a) at 40-90° C. for 1-4 h.

[0017] In a specific embodiment of the present invention, the method further comprises: concentrating the extract obtained by the extraction and re-dissolving it with a butanediol aqueous solution.

[0018] In a specific embodiment of the present invention, the volume fraction of the ethanol aqueous solution is 50% to 95% of the ethanol aqueous solution.

[0019] In a specific embodiment of the present invention, the mass fraction of butanediol in the butanediol aqueous solution is 45% to 55%.

[0020] In a specific embodiment of the present invention, during the re-dissolution, the mass of the butanediol aqueous solution is 10 to 50 times the mass of the material after the concentration treatment.

[0021] In a specific embodiment of the present invention, the process further comprises: filtering and sterilizing the reconstituted material.

[0022] In a specific embodiment of the present invention, in step (a), the particle size of Rhodiola rosea is 10 to 60 meshes.

[0023] Another aspect of the present invention provides the use of any one of the above-mentioned Rhodiola rosea extract products in the preparation of skin care products.

[0024] The present invention also provides a whitening composition, comprising any one of the above-mentioned Rhodiola rosea extract products and a whitening agent; the whitening agent comprises niacinamide and / or tranexamic acid.

[0025] Compared with the prior art, the present invention has the following beneficial effects:

[0026] (1) The present invention provides a Rhodiola rosea extract product, which contains higher concentrations of salidroside, tyrosol and quercetin while keeping the total flavonoid content substantially unchanged, and can enhance the whitening efficacy and safety of the product as well as the synergistic effect on niacinamide and tranexamic acid, thereby solving the problem of application limitations of plant extracts in cosmetics;

[0027] (2) The preparation method of the Rhodiola rosea extract product of the present invention adopts a high temperature and high pressure pretreatment process, which significantly increases the content of salidroside, tyrosol and quercetin in the extract while keeping the total flavonoid content basically unchanged, while ensuring the efficacy and safety of the product. BRIEF DESCRIPTION OF THE DRAWINGS

[0028] In order to more clearly illustrate the specific implementation methods of the present invention or the technical solutions in the prior art, the drawings required for use in the specific implementation methods or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are some implementation methods of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.

[0029] Figure 1 A photo of the Rhodiola rosea extract product provided in Example 1 of the present invention;

[0030] Figure 2 A photo of the Rhodiola rosea extract product provided in Example 2 of the present invention;

[0031] Figure 3 A photo of the Rhodiola rosea extract product provided in Example 3 of the present invention;

[0032] Figure 4 A photo of the Rhodiola rosea extract product provided in Example 4 of the present invention;

[0033] Figure 5 A photo of the Rhodiola rosea extract product provided in Example 5 of the present invention;

[0034] Figure 6 A photo of the Rhodiola rosea extract product provided in Example 6 of the present invention;

[0035] Figure 7 A photo of the Rhodiola rosea extract product provided in Example 7 of the present invention;

[0036] Figure 8 A photo of the Rhodiola rosea extract product provided in Example 8 of the present invention;

[0037] Fig. 9 A photo of the Rhodiola rosea extract product provided in Comparative Example 1;

[0038] Fig.10 A photo of the Rhodiola rosea extract product provided for Comparative Example 2;

[0039] Fig.11 The test results of the Rhodiola rosea extract product provided in Example 1 and Comparative Example 1 of the present invention on the inhibition of the inflammatory factor IL-6, wherein the right side is Example 1 and the left side is Comparative Example 1;

[0040] Fig.12 The test results of the Rhodiola rosea extract product provided in Example 1 and Comparative Example 1 of the present invention on the inhibition of inflammatory factor TNF-α, wherein the right side is Example 1 and the left side is Comparative Example 1;

[0041] Fig.13 The test results of the effect of the Rhodiola rosea extract product provided in Example 1 and Comparative Example 1 of the present invention on the viability of RAW264.7 cells, wherein the right side is Example 1 and the left side is Comparative Example 1;

[0042] Fig.14 The whitening effect comparison of the Rhodiola rosea extract product provided by Example 1 of the present invention and Comparative Example 1, wherein the right side is Example 1 and the left side is Comparative Example 1;

[0043] Fig.15 The whitening effect comparison of the Rhodiola rosea extract product provided in Example 1 of the present invention after compounding with niacinamide or tranexamic acid;

[0044] Fig.16 This is a comparison of the whitening effects of the Rhodiola rosea extract product provided in Comparative Example 1 of the present invention after compounding with niacinamide or tranexamic acid;

[0045] Fig.17 The results of the inhibition test on tyrosinase activity of the Rhodiola rosea extract product provided in Example 1 and Comparative Example 1 of the present invention;

[0046] Fig.18 These are the results of the inhibition test on melanin by the Rhodiola rosea extract products provided in Example 1 and Comparative Example 1 of the present invention. DETAILED DESCRIPTION

[0047] The technical scheme of the present invention will be clearly and completely described below in conjunction with the accompanying drawings and specific embodiments, but it will be understood by those skilled in the art that the following described embodiments are part of embodiments of the present invention, rather than all embodiments, and are only used to illustrate the present invention, and should not be considered as limiting the scope of the present invention. Based on the embodiments in the present invention, all other embodiments obtained by those of ordinary skill in the art without making creative work are within the scope of protection of the present invention. If specific conditions are not specified in the embodiments, they are carried out according to normal conditions or conditions recommended by the manufacturer. If the manufacturer is not specified in the reagents or instruments used, they are all conventional products that can be purchased commercially.

[0048] In one aspect, the present invention provides a Rhodiola rosea extract product, comprising the following components by mass:

[0049] 114-164 parts of salidroside, 25-36 parts of tyrosol and 0.108-0.157 parts of quercetin;

[0050] The mass ratio of the salidroside to the total flavonoids in the rhodiola rosea extract product is (8-12):1.

[0051] The Rhodiola rosea extract product of the present invention contains higher concentrations of salidroside, tyrosol and quercetin while keeping the total flavonoid content substantially unchanged, can enhance the whitening efficacy and safety of the product and the synergistic effect on niacinamide and tranexamic acid, and solves the problem of application limitations of plant extracts in cosmetics.

[0052] For example, in different embodiments, the mass fractions of each component in the Rhodiola rosea extract product can be exemplified as follows:

[0053] The amount of salidroside can be 114 parts, 120 parts, 130 parts, 140 parts, 150 parts, 160 parts, 164 parts or a range consisting of any two of them;

[0054] The amount of tyrosol can be 25 parts, 26 parts, 28 parts, 30 parts, 32 parts, 34 parts, 36 parts or a range consisting of any two of them;

[0055] The amount of quercetin can be 0.108, 0.11, 0.12, 0.13, 0.14, 0.15, 0.157, or a range consisting of any two thereof.

[0056] For example, in different embodiments, the mass ratio of the salidroside to the total flavonoids in the rhodiola rosea extract product can be 8:1, 8.5:1, 9:1, 9.5:1, 10:1, 10.5:1, 11:1, 11.5:1, 12:1 or a range consisting of any two of them.

[0057] In the Rhodiola rosea extract product of the present invention, the proportions of salidroside, tyrosol and quercetin in the Rhodiola rosea extract product are significantly increased. Taking salidroside as an example, its ratio to total flavonoids is significantly increased, which can enhance the whitening efficacy and safety of the product as well as the synergistic effect on niacinamide and tranexamic acid.

[0058] In a specific embodiment of the present invention, the Rhodiola rosea extract product includes the following components by mass:

[0059] 4.5-6.5 parts of Rhodiola rosea extract, 46-49 parts of butylene glycol and 46-49 parts of water.

[0060] The Rhodiola rosea extract comprises at least the following components by mass:

[0061] 114-164 parts of salidroside, 25-36 parts of tyrosol and 0.108-0.157 parts of quercetin;

[0062] Among them, the mass ratio of salidroside to total flavonoids in the rhodiola rosea extract product is (8-12):1.

[0063] For example, in different embodiments, the mass fractions of each component in the Rhodiola rosea extract product can be exemplified as follows:

[0064] The amount of the Rhodiola rosea extract can be 4.5 parts, 5 parts, 5.5 parts, 6 parts, 6.5 parts or a range consisting of any two of them;

[0065] The amount of butanediol can be 46 parts, 47 parts, 48 ​​parts, 49 parts or a range consisting of any two thereof;

[0066] The amount of water can be 46 parts, 47 parts, 48 ​​parts, 49 parts or a range consisting of any two of them.

[0067] In a specific embodiment of the present invention, the Rhodiola rosea extract product includes the following components by mass:

[0068] 5 parts of Rhodiola rosea extract, 47 parts of butylene glycol and 48 parts of water.

[0069] Another aspect of the present invention provides a method for preparing a Rhodiola rosea extract product, comprising the following steps:

[0070] (a) treating Rhodiola rosea at 110-150°C and 0.145-0.5 MPa for 10-30 min;

[0071] (b) using ethanol aqueous solution as the extraction solvent, with a solid-liquid ratio of 1:(20-50) (m / m), and extracting the Rhodiola rosea treated in step (a) at 40-90° C. for 1-4 h.

[0072] For example, in different embodiments, in step (a), the treatment temperature can be 110°C, 120°C, 130°C, 140°C, 150°C or a range consisting of any two thereof; the treatment time can be 10 min, 15 min, 20 min, 25 min, 30 min or a range consisting of any two thereof.

[0073] In actual operation, the treatment pressure may be 0.145-0.5 MPa, such as 0.145 MPa, 0.15 MPa, 0.2 MPa, 0.3 MPa, 0.4 MPa, 0.5 MPa, etc. The pressure here refers to absolute pressure, which refers to gauge pressure (relative pressure) + atmospheric pressure.

[0074] High pressure treatment under the above conditions can not only avoid dark color of the product, but also ensure the reduction of loss of active substances.

[0075] For example, in different embodiments, in step (b), the material-liquid ratio can be exemplarily 1:20 (m / m), 1:25 (m / m), 1:30 (m / m), 1:35 (m / m), 1:40 (m / m), 1:45 (m / m), 1:50 (m / m) or a range consisting of any two of them.

[0076] For example, in different embodiments, the extraction temperature may be illustratively 40° C., 50° C., 60° C., 70° C., 80° C., 90° C., or a range consisting of any two thereof.

[0077] For example, in different embodiments, the extraction time can be illustratively 1 h, 2 h, 3 h, 4 h, or a range consisting of any two thereof.

[0078] In a specific embodiment of the present invention, the method further comprises: concentrating the extract obtained by the extraction and re-dissolving it with a butanediol aqueous solution.

[0079] In actual operation, the butanediol used in the present invention may be 1,3-butanediol.

[0080] In a specific embodiment of the present invention, the volume fraction of the ethanol aqueous solution is 50% to 95% of the ethanol aqueous solution.

[0081] For example, in different embodiments, the volume fraction of the ethanol aqueous solution can be illustratively 50%, 60%, 70%, 80%, 90%, 95% or a range consisting of any two thereof.

[0082] In a specific embodiment of the present invention, the mass fraction of butanediol in the butanediol aqueous solution is 45% to 55%.

[0083] For example, in different embodiments, the mass fraction of butanediol in the butanediol aqueous solution may be 45%, 48%, 50%, 52%, 55% or a range consisting of any two thereof.

[0084] In a specific embodiment of the present invention, during the re-dissolution, the mass of the butanediol aqueous solution is 10 to 50 times the mass of the material after the concentration treatment.

[0085] For example, in different embodiments, during the re-dissolution, the mass of the butanediol aqueous solution can be 10 times, 15 times, 20 times, 25 times, 30 times, 35 times, 40 times, 45 times, 50 times the mass of the concentrated material, or a range consisting of any two of them.

[0086] In a specific embodiment of the present invention, the process further comprises: filtering and sterilizing the reconstituted material.

[0087] In a specific embodiment of the present invention, in step (a), the particle size of the Rhodiola rosea is 10-60 mesh, that is, the particle size below the 10 mesh sieve and above the 60 mesh sieve.

[0088] Another aspect of the present invention provides the use of any one of the above-mentioned Rhodiola rosea extract products in the preparation of skin care products.

[0089] The present invention also provides a whitening composition, comprising any one of the above-mentioned Rhodiola rosea extract products and a whitening agent; the whitening agent comprises niacinamide and / or tranexamic acid.

[0090] The Rhodiola rosea extract product of the present invention has a synergistic effect on the whitening effects of traditional whitening agents niacinamide and tranexamic acid.

[0091] Some of the raw material information used in the following specific embodiments may be as follows, but is not limited thereto:

[0092] Rhodiola rosea: Rhodiola rosea, Part used: Root, Origin: China.

[0093] Example 1

[0094] This embodiment provides a method for preparing a Rhodiola rosea extract product, comprising the following steps:

[0095] (1) Take coarse powder of Rhodiola rosea, pass it through a 10-mesh sieve, and high-pressure treat it at 0.2 MPa and 121°C for 20 min.

[0096] (2) The Rhodiola rosea treated with high pressure in step (1) was added to a 95% ethanol aqueous solution at a solid-liquid ratio of 1:20 (m / m) based on dry weight, and then extracted at 60° C. for 2 h.

[0097] (3) The material extracted in step (2) is allowed to stand and cool to about 40° C., filtered through gauze to obtain a coarse filtrate; the coarse filtrate is then placed in a rotary evaporator and concentrated under reduced pressure to an extract state (constant mass).

[0098] (4) Add 50% 1,3-butanediol aqueous solution (20 times the mass of the extract) to the extract and mix well; filter using H70 paperboard, and measure turbidity (control the turbidity of the liquid ≤ 5FNU), solid content, conductivity, and pH. Take photos to confirm the sample status.

[0099] (5) sterilizing the material obtained in step (4) at 80-85° C. for 40 min, cooling and mixing to obtain the Rhodiola rosea extract product.

[0100] Example 2

[0101] This embodiment provides a method for preparing a Rhodiola rosea extract product, comprising the following steps:

[0102] (1) Take coarse powder of Rhodiola rosea, pass it through a 10-mesh sieve, and high-pressure treat it at 0.2 MPa and 121°C for 20 min.

[0103] (2) The Rhodiola rosea treated with high pressure in step (1) was added to a 50% ethanol aqueous solution at a solid-liquid ratio of 1:20 (m / m) based on dry weight, and then extracted at 60° C. for 2 h.

[0104] (3) The material extracted in step (2) is allowed to stand and cool to about 40° C., filtered through gauze to obtain a coarse filtrate; the coarse filtrate is then placed in a rotary evaporator and concentrated under reduced pressure to an extract state (constant mass).

[0105] (4) Add 50% 1,3-butanediol aqueous solution (20 times the mass of the extract) to the extract and mix well; filter using H70 paperboard, and measure turbidity (control the turbidity of the liquid ≤ 5FNU), solid content, conductivity, and pH. Take photos to confirm the sample status.

[0106] (5) sterilizing the material obtained in step (4) at 80-85° C. for 40 min, cooling and mixing to obtain the Rhodiola rosea extract product.

[0107] Example 3

[0108] This embodiment provides a method for preparing a Rhodiola rosea extract product, comprising the following steps:

[0109] (1) Take coarse powder of Rhodiola rosea, pass it through a 10-mesh sieve, and high-pressure treat it at 0.2 MPa and 121°C for 20 min.

[0110] (2) The Rhodiola rosea treated with high pressure in step (1) was added to a 70% ethanol aqueous solution at a solid-liquid ratio of 1:20 (m / m) based on dry weight, and then extracted at 60° C. for 2 h.

[0111] (3) The material extracted in step (2) is allowed to stand and cool to about 40° C., filtered through gauze to obtain a coarse filtrate; the coarse filtrate is then placed in a rotary evaporator and concentrated under reduced pressure to an extract state (constant mass).

[0112] (4) Add 50% 1,3-butanediol aqueous solution (20 times the mass of the extract) to the extract and mix well; filter using H70 paperboard, and measure turbidity (control the turbidity of the liquid ≤ 5FNU), solid content, conductivity, and pH. Take photos to confirm the sample status.

[0113] (5) sterilizing the material obtained in step (4) at 80-85° C. for 40 min, cooling and mixing to obtain the Rhodiola rosea extract product.

[0114] Example 4

[0115] This embodiment provides a method for preparing a Rhodiola rosea extract product, comprising the following steps:

[0116] (1) Take coarse powder of Rhodiola rosea, pass it through a 10-mesh sieve, and high-pressure treat it at 0.2 MPa and 121°C for 20 min.

[0117] (2) The Rhodiola rosea treated with high pressure in step (1) was added to a 95% ethanol aqueous solution at a solid-liquid ratio of 1:20 (m / m) based on dry weight, and then extracted at 80° C. for 2 h.

[0118] (3) The material extracted in step (2) is allowed to stand and cool to about 40° C., filtered through gauze to obtain a coarse filtrate; the coarse filtrate is then placed in a rotary evaporator and concentrated under reduced pressure to an extract state (constant mass).

[0119] (4) Add 50% 1,3-butanediol aqueous solution (20 times the mass of the extract) to the extract and mix well; filter using H70 paperboard, and measure turbidity (control the turbidity of the liquid ≤ 5FNU), solid content, conductivity, and pH. Take photos to confirm the sample status.

[0120] (5) sterilizing the material obtained in step (4) at 80-85° C. for 40 min, cooling and mixing to obtain the Rhodiola rosea extract product.

[0121] Example 5

[0122] This embodiment provides a method for preparing a Rhodiola rosea extract product, comprising the following steps:

[0123] (1) Take coarse powder of Rhodiola rosea, pass it through a 10-mesh sieve, and high-pressure treat it at 0.2 MPa and 121°C for 20 min.

[0124] (2) The Rhodiola rosea treated with high pressure in step (1) was added to a 95% ethanol aqueous solution at a solid-liquid ratio of 1:20 (m / m) based on dry weight, and then extracted at 90° C. for 2 h.

[0125] (3) The material extracted in step (2) is allowed to stand and cool to about 40° C., filtered through gauze to obtain a coarse filtrate; the coarse filtrate is then placed in a rotary evaporator and concentrated under reduced pressure to an extract state (constant mass).

[0126] (4) Add 50% 1,3-butanediol aqueous solution (20 times the mass of the extract) to the extract and mix well; filter using H70 paperboard, and measure turbidity (control the turbidity of the liquid ≤ 5FNU), solid content, conductivity, and pH. Take photos to confirm the sample status.

[0127] (5) sterilizing the material obtained in step (4) at 80-85° C. for 40 min, cooling and mixing to obtain the Rhodiola rosea extract product.

[0128] Example 6

[0129] This embodiment provides a method for preparing a Rhodiola rosea extract product, comprising the following steps:

[0130] (1) Take coarse powder of Rhodiola rosea, pass it through a 10-mesh sieve, and high-pressure treat it at 0.145 MPa and 110°C for 20 min.

[0131] (2) The Rhodiola rosea treated with high pressure in step (1) was added to a 95% ethanol aqueous solution at a solid-liquid ratio of 1:20 (m / m) based on dry weight, and then extracted at 60° C. for 2 h.

[0132] (3) The material extracted in step (2) is allowed to stand and cool to about 40° C., filtered through gauze to obtain a coarse filtrate; the coarse filtrate is then placed in a rotary evaporator and concentrated under reduced pressure to an extract state (constant mass).

[0133] (4) Add 50% 1,3-butanediol aqueous solution (20 times the mass of the extract) to the extract and mix well; filter using H70 paperboard, and measure turbidity (control the turbidity of the liquid ≤ 5FNU), solid content, conductivity, and pH. Take photos to confirm the sample status.

[0134] (5) sterilizing the material obtained in step (4) at 80-85° C. for 40 min, cooling and mixing to obtain the Rhodiola rosea extract product.

[0135] Example 7

[0136] This embodiment provides a method for preparing a Rhodiola rosea extract product, comprising the following steps:

[0137] (1) Take coarse powder of Rhodiola rosea, pass it through a 10-mesh sieve, and high-pressure treat it at 0.32 MPa and 135°C for 20 min.

[0138] (2) The Rhodiola rosea treated with high pressure in step (1) was added to a 95% ethanol aqueous solution at a solid-liquid ratio of 1:20 (m / m) based on dry weight, and then extracted at 60° C. for 2 h.

[0139] (3) The material extracted in step (2) is allowed to stand and cool to about 40° C., filtered through gauze to obtain a coarse filtrate; the coarse filtrate is then placed in a rotary evaporator and concentrated under reduced pressure to an extract state (constant mass).

[0140] (4) Add 50% 1,3-butanediol aqueous solution (20 times the mass of the extract) to the extract and mix well; filter using H70 paperboard, and measure turbidity (control the turbidity of the liquid ≤ 5FNU), solid content, conductivity, and pH. Take photos to confirm the sample status.

[0141] (5) sterilizing the material obtained in step (4) at 80-85° C. for 40 min, cooling and mixing to obtain the Rhodiola rosea extract product.

[0142] Example 8

[0143] This embodiment provides a method for preparing a Rhodiola rosea extract product, comprising the following steps:

[0144] (1) Take coarse powder of Rhodiola rosea, pass it through a 10-mesh sieve, and high-pressure treat it at 0.5 MPa and 150°C for 20 min.

[0145] (2) The Rhodiola rosea treated with high pressure in step (1) was added to a 95% ethanol aqueous solution at a solid-liquid ratio of 1:20 (m / m) based on dry weight, and then extracted at 60° C. for 2 h.

[0146] (3) The material extracted in step (2) is allowed to stand and cool to about 40° C., filtered through gauze to obtain a coarse filtrate; the coarse filtrate is then placed in a rotary evaporator and concentrated under reduced pressure to an extract state (constant mass).

[0147] (4) Add 50% 1,3-butanediol aqueous solution (20 times the mass of the extract) to the extract and mix well; filter using H70 paperboard, and measure turbidity (control the turbidity of the liquid ≤ 5FNU), solid content, conductivity, and pH. Take photos to confirm the sample status.

[0148] (5) sterilizing the material obtained in step (4) at 80-85° C. for 40 min, cooling and mixing to obtain the Rhodiola rosea extract product.

[0149] Comparative Example 1

[0150] Comparative Example 1 provides a method for preparing a Rhodiola rosea extract product, comprising the following steps:

[0151] (1) Take the coarse powder of Rhodiola rosea and pass it through a 10-mesh sieve.

[0152] (2) The Rhodiola rosea obtained in step (1) was added to a 95% ethanol aqueous solution at a solid-liquid ratio of 1:20 (m / m), and then extracted at 60° C. for 2 h.

[0153] (3) The material extracted in step (2) is allowed to stand and cool to about 40° C., filtered through gauze to obtain a coarse filtrate; the coarse filtrate is then placed in a rotary evaporator and concentrated under reduced pressure to an extract state (constant mass).

[0154] (4) Add 50% 1,3-butanediol aqueous solution (20 times the mass of the extract) to the extract and mix well; filter using H70 paperboard, and measure turbidity (control the turbidity of the liquid ≤ 5FNU), solid content, conductivity, and pH. Take photos to confirm the sample status.

[0155] (5) sterilizing the material obtained in step (4) at 80-85° C. for 40 min, cooling and mixing to obtain the Rhodiola rosea extract product.

[0156] Comparative Example 2

[0157] Comparative Example 2 provides a method for preparing a Rhodiola rosea extract product, comprising the following steps:

[0158] (1) Take coarse powder of Rhodiola rosea, pass it through a 10-mesh sieve, and high-pressure treat it at 0.2 MPa and 121°C for 20 min.

[0159] (2) The Rhodiola rosea obtained in step (1) was added to a 95% ethanol aqueous solution at a solid-liquid ratio of 1:20 (m / m), and then extracted at 60° C. for 2 h.

[0160] (3) The material extracted in step (2) is allowed to stand and cool to about 40° C., filtered through gauze to obtain a coarse filtrate; the coarse filtrate is then placed in a rotary evaporator and concentrated under reduced pressure to an extract state (constant mass).

[0161] (4) Add 50% 1,3-propylene glycol aqueous solution (20 times the mass of the extract) to the extract and mix well; filter using H70 paperboard, and measure turbidity (control the turbidity of the liquid ≤ 5FNU), solid content, conductivity, and pH. Take photos to confirm the sample status.

[0162] (5) sterilizing the material obtained in step (4) at 80-85° C. for 40 min, cooling and mixing to obtain the Rhodiola rosea extract product.

[0163] Experimental Example 1

[0164] The products of Examples 1 to 6 and Comparative Examples 1 to 2 were tested, and the test results are shown in Table 1.

[0165] Table 1 Product process indicators of Examples 1 to 6 and Comparative Examples 1 to 2

[0166]

[0167]

[0168] Figures 1 to 10 The photos are respectively of the Rhodiola rosea extract products of Examples 1 to 8 and Comparative Examples 1 to 2.

[0169] The differences in the contents of total flavonoids and salidroside, tyrosol, and quercetin in the Rhodiola rosea extract products of Example 1 and Comparative Examples 1-2 are shown in Tables 2-3 below.

[0170] Table 2 Differences in ingredients between Example 1 and Comparative Example 1

[0171]

[0172] Table 3 Differences in ingredients between Example 1 and Comparative Example 2

[0173]

[0174]

[0175] From the above results, it can be seen that the preparation method of Example 1 of the present invention significantly increases the content of salidroside, tyrosol, and quercetin, which are 57.8%, 66.7%, and 49.5% respectively compared with the increase in Comparative Example 1; but it has no significant effect on the total flavonoid content. In the product obtained by replacing the re-dissolution solvent in Comparative Example 2, the content of salidroside, tyrosol, and quercetin is still low, indicating that the replacement of the re-dissolution solvent in Comparative Example 2 has no significant effect on the enrichment of the active ingredient content.

[0176] Experimental Example 2

[0177] Efficacy verification test

[0178] 1. Anti-inflammatory activity

[0179] (1) Experimental methods

[0180] MTT method to detect cytotoxicity: take the logarithmic growth phase digestion and inoculate it into a 96-well plate, place the culture plate in a 37°C, 5% CO2 incubator for 18 to 24 hours, discard the supernatant, add different amounts of the test substance, so that the sample mass concentration in the whole system is 0.0195%, 0.039%, 0.078%, 0.156%, 0.313%, 0.625%, 1.25%, 2.5%, 5%, and continue to culture in a 37°C, 5% CO2 incubator. After 18 to 24 hours of cell culture, discard the supernatant, add MTT solution (0.5 mg / mL), mix gently, and incubate at 37°C in the dark for 4 hours. After the incubation, discard the supernatant, add 150 μL of DMSO to each well, shake for 20 minutes, and measure the absorbance at 490nm with an enzyme marker. Among them, the sample concentration is calculated based on the total amount of the product of each embodiment or comparative example.

[0181] Detection of inflammatory factor content: cells in the logarithmic growth phase were inoculated into 24-well plates and incubated at 37°C, 5% CO2 incubator. Untreated cells were used as blank controls, and only LPS-treated cells were added as negative controls. The positive control was LPS+dexamethasone. The sample group was LPS+different concentrations of Rhodiola rosea extract. After 18-24 hours of cell culture, the cells were grouped and sampled. Cell culture medium was added to the blank and negative control groups, cell culture medium containing 0.001% dexamethasone was added to the positive control group, and cell culture medium with corresponding concentrations of Rhodiola rosea extract was added to the sample group. Three replicate wells were set for each treatment group. After 18-24 hours of culture, the culture medium in the plate was aspirated, and PBS was added to wash once. Cell culture medium was added to the blank control group, and cell culture medium containing LPS was added to the negative and positive control combination sample groups. The supernatant was collected after continued culture at 37°C, 5% CO2 incubator for 18-24 hours. According to the operating instructions of the ELISA kit, the content of cellular inflammatory factors IL-6 and TNF-α was detected.

[0182] (2) Experimental results

[0183] Fig.11 The test results of the inhibition test of the Rhodiola rosea extract product provided in Example 1 and Comparative Example 1 of the present invention on the inflammatory factor IL-6; Fig.12 The test results of the Rhodiola rosea extract product provided in Example 1 and Comparative Example 1 of the present invention on the inhibition of inflammatory factor TNF-α. From the above test results, it can be seen that the Rhodiola rosea extract product obtained in Comparative Example 1 significantly reduces the IL-6 content in RAW264.7 cells, but has no significant effect on the TNF-α content; the Rhodiola rosea extract product obtained in Example 1 significantly reduces the IL-6 and TNF-α contents in RAW264.7 cells, indicating that the Rhodiola rosea extract product obtained by the preparation method of Example 1 has the effect of inhibiting TNF-α. And at a high safety concentration, the inhibitory effect is better than that of Comparative Example 1.

[0184] Fig.13 The test results of the effect of the Rhodiola rosea extract product provided in Example 1 of the present invention and Comparative Example 1 on the viability of RAW264.7 cells. As can be seen from the figure, at a mass concentration of 0.156%, the Rhodiola rosea extract product of Example 1 has less toxicity to cells and a higher safe concentration. Therefore, the preparation method of Example 1 of the present invention can also improve the safety of plant extracts.

[0185] 2. Whitening effect and synergistic whitening effect

[0186] (1) Experimental methods

[0187] Randomly select zebrafish in a 6-well plate, 15 per well. Water-soluble samples were given, and a normal control group was set up at the same time, with a volume of 3 mL per well. Incubate at 28°C in the dark for 45 hours. Ten zebrafish were randomly selected from each experimental group and photographed under a dissecting microscope. Advanced image processing software was used to analyze and collect data, analyze the melanin signal intensity (S) of the zebrafish head, and calculate the whitening efficacy of the sample (statistical analysis p < 0.05, efficacy value ≥ 20%, determined to be effective).

[0188] The sample preparation includes:

[0189] 1%, 2%, and 4% Rhodiola rosea extract products are all prepared using water as the solvent;

[0190] The 2% tranexamic acid solution was prepared using water as solvent;

[0191] The preparation of 2% nicotinamide solution includes: firstly, mixing 5g nicotinamide and 35g water evenly to obtain a nicotinamide aqueous solution, then taking 2g of the nicotinamide aqueous solution and adding water to 100g;

[0192] Niacinamide compound solution: 5g niacinamide, 5g Rhodiola rosea extract, and 10g water are mixed and shaken to obtain a compound solution; 1g of the compound solution is added with water to 100g to obtain a 1% niacinamide compound solution; 2g of the compound solution is added with water to 100g to obtain a 2% niacinamide compound solution;

[0193] Tranexamic acid compound solution: 5g tranexamic acid and 5g Rhodiola rosea extract are mixed evenly to obtain a compound solution; 2g of the compound solution is added with water to 100g to obtain a 2% tranexamic acid compound solution; 4g of the compound solution is added with water to 100g to obtain a 4% niacinamide compound solution. All concentrations are mass concentrations.

[0194] (2) Experimental results

[0195] Fig.14The whitening efficacy of the Rhodiola rosea extract product provided in Example 1 of the present invention and Comparative Example 1 is compared. As can be seen from the figure, at the same concentration, the Rhodiola rosea extract product obtained in Example 1 has a better inhibitory effect on zebrafish melanin production, and the whitening efficacy can reach up to 72%, so the treatment method of Example 1 can significantly improve the whitening efficacy of the product.

[0196] Fig.15 The whitening effect comparison of the Rhodiola rosea extract product provided in Example 1 of the present invention after compounding with niacinamide or tranexamic acid; Fig.16 This is a comparison of the whitening effects of the Rhodiola rosea extract product provided in Comparative Example 1 of the present invention after being compounded with niacinamide or tranexamic acid. Fig.15 and Fig.16 It can be seen that according to the zebrafish test results (the lighter the color, the less melanin is formed and the stronger the whitening effect), it is found that the Rhodiola rosea extract product of Example 1 has a synergistic effect on the whitening effects of niacinamide and tranexamic acid.

[0197] 3. Tyrosinase inhibition test

[0198] (1) Experimental methods

[0199] The Rhodiola rosea extract was prepared into different mass concentrations (0.05%, 0.1%, 0.15%, 0.2%, 0.25%), α-arbutin was used as a positive control, and the reaction system was prepared according to the addition amounts of various reagents in Table 4. The reaction was carried out for a certain time, and the absorbance was measured at a wavelength of 475 nm.

[0200] Table 4 Reaction system

[0201]

[0202] Note: "+" in the table means added, "-" means not added.

[0203] (2) Experimental results

[0204] Fig.17 The results of the inhibition test of the Rhodiola rosea extract products on tyrosinase activity provided in Example 1 of the present invention and Comparative Example 1. As can be seen from the figure, within the concentration range of 0.05% to 0.25%, the inhibition rate of the Rhodiola rosea extract product obtained by Example 1 on tyrosinase increases with the increase of concentration. At a concentration of 0.25%, the inhibition rate reaches 81%, while the inhibition rate of the Rhodiola rosea extract product of Comparative Example 1 only reaches 80% at 2.5%, indicating that the method of the embodiment of the present invention can greatly improve the effect of the Rhodiola rosea extract product on inhibiting tyrosinase activity.

[0205] 4. Melanin production inhibition test

[0206] (1) Experimental methods

[0207] MTT method to detect cell activity: B16-F10 cells in the logarithmic growth phase were digested and inoculated into 96-well plates, and the culture plates were placed in a 37°C, 5% CO2 incubator for 18 to 24 hours. Negative control (culture medium), positive control (culture medium containing 5% DMSO) and zero well (PBS) were set up, and the Rhodiola rosea extract product sample group (mass concentrations were 0.039%, 0.078%, 0.156%, 0.313%, 0.625%, 1.25%, 2.5%, and 5%, respectively, with DMEM culture medium as the solvent, and 5% samples were prepared according to the mass concentration, and then diluted to the required concentration in sequence), cultured for 18 to 24 hours, discarded the supernatant, added the prepared and filtered MTT (0.5 mg / mL), gently mixed, and incubated at 37°C in the dark for 4 hours. After the incubation, the supernatant was discarded, 150 μL of DMSO was added to each well, shaken for 20 minutes, and the OD570nm value was read with an enzyme marker.

[0208] Melanin content detection: B16-F10 cells were inoculated into 6-well plates and incubated in a 37°C, 5% CO2 incubator for 18 to 24 hours. The experiment set up a blank control group (BC), a negative control group (NC, theophylline), a positive control group (PC, α-arbutin), and a Rhodiola rosea extract product sample group (mass concentration of 0.313%, 0.625%, 1.25%, DMEM medium as solvent). After the cells were administered and cultured for 3 days, the melanin content in the cell culture medium and cells was tested respectively.

[0209] (2) Fig.18 The results of the melanin inhibition test of the Rhodiola rosea extract products provided in Example 1 and Comparative Example 1 of the present invention. As can be seen from the figure, compared with the blank control group (culture medium), the Rhodiola rosea extract product of Example 1 has a significant inhibitory effect on the melanin production of B16-F10 cells at concentrations of 0.625% and 1.25%, and the inhibitory effect is better than that of the Rhodiola rosea extract product of Comparative Example 1.

[0210] The present invention realizes efficient enrichment of target active ingredients in the Rhodiola rosea extract product by adopting a certain pretreatment process, significantly increases the contents of salidroside, tyrosol and quercetin in the Rhodiola rosea extract product, enhances the whitening effect and safety, and simultaneously has a synergistic effect on nicotinamide and tranexamic acid, thereby significantly improving the applicability of the Rhodiola rosea extract product in cosmetics.

[0211] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit it. Although the present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that they can still modify the technical solutions described in the aforementioned embodiments, or replace some or all of the technical features therein with equivalents. However, these modifications or replacements do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of the present invention.

Claims

1. Rhodiola rosea extract product, characterized in that, It includes the following components by mass: 114-164 parts of salidroside, 25-36 parts of tyrosol and 0.108-0.157 parts of quercetin; The mass ratio of the salidroside to the total flavonoids in the rhodiola rosea extract product is (8-12):

1.

2. The Rhodiola rosea extract product according to claim 1, characterized in that It includes the following components by mass: 4.5-6.5 parts of Rhodiola rosea extract, 46-49 parts of butylene glycol and 46-49 parts of water.

3. The method for preparing the Rhodiola rosea extract product according to claim 1 or 2, characterized in that: The steps include: (a) treating Rhodiola rosea at 110-150°C and 0.145-0.5 MPa for 10-30 min; (b) Using ethanol aqueous solution as the extraction solvent, with a solid-liquid ratio of 1:(20-50), extracting the Rhodiola rosea treated in step (a) at 40-90° C. for 1-4 h.

4. The method for preparing the Rhodiola rosea extract product according to claim 3, characterized in that: The volume fraction of the ethanol aqueous solution is 50% to 95%.

5. The method for preparing the Rhodiola rosea extract product according to claim 3, characterized in that: Also includes: The extract obtained by the extraction is concentrated and redissolved with a butanediol aqueous solution.

6. The method for preparing the Rhodiola rosea extract product according to claim 5, characterized in that: In the butanediol aqueous solution, the mass fraction of butanediol is 45% to 55%.

7. The method for preparing the Rhodiola rosea extract product according to claim 5, characterized in that: During the re-dissolution, the mass of the butanediol aqueous solution is 10 to 50 times the mass of the material after the concentration treatment.

8. The method for preparing the Rhodiola rosea extract product according to claim 3, characterized in that: In step (a), the particle size of the Rhodiola rosea is 10 to 60 meshes.

9. Use of the Rhodiola rosea extract product according to any one of claims 1 to 2 or the Rhodiola rosea extract product prepared by the preparation method of the Rhodiola rosea extract product according to any one of claims 3 to 8 in the preparation of skin care products.

10. A whitening composition, characterized in that: Including Rhodiola rosea extract products and whitening agents; The Rhodiola rosea extract product is the Rhodiola rosea extract product according to any one of claims 1 to 2 or the Rhodiola rosea extract product prepared by the preparation method of the Rhodiola rosea extract product according to any one of claims 3 to 8; The whitening agent includes niacinamide and / or tranexamic acid.

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