Acne-removing composition with dual synergistic effect as well as preparation method and application of acne-removing composition

Abstract

The invention relates to an acne-removing composition with a dual synergistic effect as well as a preparation method and application thereof, and belongs to the technical field of cosmetics. The plant active ingredient composition comprises an aquilaria sinensis leaf extract and an acanthopanax trifoliatus leaf / stem extract composition, and the weight ratio of the aquilaria sinensis leaf extract to the acanthopanax trifoliatus leaf / stem extract is that the aquilaria sinensis leaf extract to the acanthopanax trifoliatus leaf / stem extract is (1-4): (1-3). The plant active ingredient composition disclosed by the invention has synergistic antibacterial and synergistic antioxidant effects. By resisting inflammation and oxidative damage caused by proliferation of propionibacterium acnes, acnes are repaired from two aspects of bacteriostasis and oxidative damage resistance. The cosmetic prepared from the plant active ingredient composition has the advantages that the acne improvement condition, the face redness improvement condition and the itching relieving condition are obviously improved, and the overall satisfaction degree is high.

Description

Technical Field

[0001] The present invention relates to the technical field of cosmetics, and in particular to an anti-acne composition with dual synergistic effects, and a preparation method and application thereof. Background Art

[0002] Acne, commonly known as pimples or acne, is a chronic inflammatory skin disease of the hair follicle sebaceous gland unit, characterized by polymorphic skin lesions such as comedones, papules, pustules and nodules, mostly formed in areas with abundant sebaceous glands. With the modern people's attention to skin health, the acne repair and acne removal market has expanded rapidly in recent years.

[0003] The colonization and invasion of Propionibacterium acnes play a vital role in the occurrence and development of acne. He Lisha et al. showed through clinical research that the total bacterial detection rate in facial lesions of acne is higher than that in normal facial skin. The bacteria isolated from facial lesions in acne are mainly Propionibacterium acnes, followed by Staphylococcus epidermidis; Zhang Liyuan et al. conducted in-depth research and found that Propionibacterium acnes exists in cysts and pustules of acne patients. This shows that there is a certain relationship between the onset of acne and Propionibacterium acnes. Propionibacterium acnes itself is pathogenic and can also cause three other pathological manifestations, namely significant inflammatory response, abnormal increase in sebum secretion, and excessive keratinocyte keratinization.

[0004] In addition, the imbalance of skin microorganisms, physiological state, and external stimuli can lead to oxidative stress, barrier dysfunction, and inflammatory response. Changes in the skin barrier will directly affect the colonization of microorganisms, leading to changes in local microbial diversity. At present, the main way to solve acne is to inhibit Propionibacterium acnes, ignoring the inflammation and barrier damage caused by the colonization and reproduction of Propionibacterium acnes, or the acne outbreak after the barrier is damaged. Therefore, fighting oxidative stress is also crucial in the prevention and treatment of acne.

[0005] There are many products for acne on the market, and they are effective, but most of them are irritating to a certain extent, and long-term use will cause skin damage. (1) Retinoids. Topical retinoids are the first choice for the treatment and maintenance of mild to moderate acne vulgaris patients, but all-trans retinoic acid is easily decomposed by light, and its side effects can cause local skin irritation reactions such as erythema, desquamation, itching and stinging, and are not suitable for sensitive skin. (2) Antibiotics. They can not only play an anti-inflammatory role, but also reduce the colonization of Propionibacterium acnes. Clindamycin preparations and erythromycin preparations are commonly used topical antibiotics for the treatment of acne, but due to the increase in the drug resistance of Propionibacterium acnes, their efficacy has gradually weakened. Antibiotics such as metronidazole and chloramphenicol have also been banned in cosmetics. (3) Glucocorticoids are acne treatment drugs. Although they bring a short-term acne-removing experience, long-term use will accumulate hormones on the skin, aggravate the sensitivity of the skin, and the skin will develop tolerance to such drugs, leading to hormone face. (4) The application of retinol in cosmetic formulas has limitations, such as being easily oxidized in the air and being insoluble in water, which results in the inability to fully exert the excellent acne-removing effect of retinol. Therefore, when developing a series of acne-suppressing products, it is necessary to ensure the acne-removing effect while pursuing a gentle soothing effect. It is crucial to find safe, effective, and naturally derived acne inhibitors.

[0006] In recent years, with the popularity of environmental protection, low carbon, green and natural trends, plant-derived acne-suppressing products have become a hot topic of research and are gaining more and more attention and popularity. The characteristics of mildness, small side effects, wide sources, low prices, less drug resistance, and suitability for long-term and preventive applications make the research and development of plant-derived acne-suppressing products have a good prospect.

[0007] Therefore, it is necessary to find skin care products that have both synergistic antibacterial and synergistic antioxidant effects, starting from both the microecological barrier and the antioxidant barrier to achieve the effect of inhibiting acne. Summary of the invention

[0008] The purpose of the present invention is to overcome the deficiencies of the prior art and provide an anti-acne composition with dual synergistic effects and a preparation method and application thereof.

[0009] To achieve the above object, the technical solution adopted by the present invention is:

[0010] In a first aspect, the present invention provides a plant active ingredient composition, comprising a composition of azelaic acid leaf extract and a balsam pear leaf / stem extract, wherein the weight ratio of the azelaic acid leaf extract to the balsam pear leaf / stem extract is azelaic acid leaf extract: balsam pear leaf / stem extract = (1-4): (1-3).

[0011] By selecting specific components for combination, the obtained plant active ingredient composition has the advantages of synergistic inhibition of Propionibacterium acnes and synergistic anti-oxidation.

[0012] Furthermore, the plant active ingredient composition also includes tea active ingredients, and the tea active ingredients include tea polyphenols and / or epigallocatechin gallate.

[0013] In a specific embodiment of the present invention, the weight ratio of the composition of the extract of Aquilaria sinensis leaves and the extract of the leaves / stems of Ampelopsis odoratis and the active ingredients of tea is the composition of the extract of Aquilaria sinensis leaves and the extract of the leaves / stems of Ampelopsis odoratis and the active ingredients of tea is 1: (3-5). The present invention combines the plant composition obtained by different weight ratios of the extract of Aquilaria sinensis leaves and the extract of the leaves / stems of Ampelopsis odoratis and the active ingredients of tea in a specific weight ratio, and the antibacterial and antioxidant synergistic index of each composition is less than 1, and has synergistic antibacterial and antioxidant effects, further enhancing the efficacy.

[0014] Furthermore, the preparation method of the Aquilaria sinensis leaf extract of the present invention is:

[0015] (1) First extraction: Mix the Aquilaria sinensis leaves and water, the weight ratio of Aquilaria sinensis leaves to water is Aquilaria sinensis leaves: water = 1:15-25, perform hot reflux extraction for 0.5-2h, remove the Aquilaria sinensis leaves residue, and obtain the first Aquilaria sinensis leaves extract;

[0016] (2) Second extraction: Take the Aquilaria sinensis leaf residue of step (1), mix the Aquilaria sinensis leaf residue and water, the weight ratio of the Aquilaria sinensis leaf residue and water is Aquilaria sinensis leaf residue: water = 1: 10-25, perform hot reflux extraction for 0.5-1.5h, remove the Aquilaria sinensis leaf residue, and obtain a second Aquilaria sinensis leaf extract;

[0017] (3) combining the first extract of Aquilaria sinensis leaves obtained in step (1) and the second extract of Aquilaria sinensis leaves obtained in step (2), centrifuging at 3000-7000 rpm for 8-30 min, and removing the residue; taking the supernatant and spray drying the supernatant to obtain an Aquilaria sinensis leaf extract.

[0018] In a specific embodiment of the present invention, the weight ratio of Aquilaria sinensis leaves to water is Aquilaria sinensis leaves: water = 1:22; and the hot reflux extraction time is 1 hour.

[0019] In a specific embodiment of the present invention, the weight ratio of Aquilaria sinensis leaf residue and water is Aquilaria sinensis leaf residue: water = 1:22; and the hot reflux extraction time is 1 hour.

[0020] In a specific embodiment of the present invention, centrifugation is performed at 4000 rpm for 10 min.

[0021] Furthermore, the preparation method of the Bletilla striata leaf / stem extract of the present invention is:

[0022] (1) First extraction: Mix the leaves / stems of Aglaonema odoratum and water, the weight ratio of the leaves / stems of Aglaonema odoratum to water is Aglaonema odoratum: water = 1:10-20, perform hot reflux extraction for 1.5-2.5 hours, remove the residue of the leaves / stems of Aglaonema odoratum, and obtain the first extract of the leaves / stems of Aglaonema odoratum;

[0023] (2) taking the white balsam pear leaf / stem residue of step (1), mixing the white balsam pear leaf / stem residue with water, wherein the weight ratio of the white balsam pear leaf / stem residue to water is white balsam pear leaf / stem residue: water = 1:8-15, performing hot reflux extraction for 1.0-2.0 h, removing the white balsam pear leaf / stem residue, and obtaining a second white balsam pear leaf / stem extract;

[0024] (3) The first extract of the white balsam pear leaf / stem of step (1) and the second extract of the white balsam pear leaf / stem of step (2) are combined and concentrated, the concentrated solution is filtered using a ceramic membrane (0.2 μm), the retentate is discarded, and the filtrate is retained; the filtrate is concentrated; the filtrate is sterilized by UHT instantaneous high temperature to obtain a sterilized solution; and then spray-dried to obtain a white balsam pear leaf / stem extract.

[0025] In a specific embodiment of the present invention, the weight ratio of the bracteatum leaf / stem to water is bracteatum leaf / stem: water = 1:15; and the hot reflux extraction time is 2 hours.

[0026] In a specific embodiment of the present invention, the weight ratio of the leaf / stem residue of Ampelopsis ulmoides and water is Ampelopsis ulmoides leaf / stem residue: water = 1:10; and the hot reflux extraction time is 1.5 h.

[0027] In a second aspect, the present invention seeks to protect the use of the plant active ingredient composition in the preparation of antibacterial products and / or antioxidant products.

[0028] In a specific embodiment of the present invention, the bacteria species include Propionibacterium acnes.

[0029] Furthermore, the product includes cosmetics.

[0030] In a third aspect, the present invention provides a cosmetic comprising the plant active ingredient composition.

[0031] Furthermore, the cosmetics also contain cosmetic accessories.

[0032] Furthermore, the cosmetic auxiliary material includes at least one of a solvent, a chelating agent, a moisturizer, a thickener, an antioxidant, an emollient, an emulsifier, a pH adjuster and a fragrance.

[0033] In a specific embodiment of the present invention, the solvent includes water; the chelating agent includes disodium EDTA; the humectant includes at least one of glycerin, hyaluronic acid, allantoin, butylene glycol and 1,2-hexanediol; the thickener includes at least one of xanthan gum, acrylic acid (ester) / C10-30 alkyl acrylate crosspolymer and cetearyl alcohol; the antioxidant includes p-hydroxyacetophenone; the emollient includes at least one of caprylic / capric triglyceride, polydimethylsiloxane and hydrogenated polyisobutene; the emulsifier includes PEG-100 glyceryl stearate and / or cetearyl glucoside; the pH adjuster includes arginine.

[0034] Furthermore, the cosmetic contains 0.5 to 2 parts of the plant active ingredient composition and 98 to 99.5 parts of cosmetic excipients by weight.

[0035] Furthermore, the cosmetic auxiliary material contains, by weight, 52.32 to 85.79 parts of water, 0.05 to 0.2 parts of disodium EDTA, 1 to 5 parts of glycerin, 0.03 to 0.1 parts of hyaluronic acid, 0.05 to 0.2 parts of xanthan gum, 0.05 to 0.3 parts of allantoin, 0.12 to 0.5 parts of acrylic acid (esters) / C10-30 alkyl acrylate cross-linked polymer, 4 to 10 parts of butylene glycol, glycol, 0.5-3 parts of 1,2-hexanediol, 0.3-0.8 parts of p-hydroxyacetophenone, 1-5 parts of cetearyl alcohol, 2-6 parts of caprylic / capric triglyceride, 0.5-2 parts of PEG-100 glyceryl stearate, 1-3 parts of cetearyl glucoside, 1-3 parts of polydimethylsiloxane, 2-6 parts of hydrogenated polyisobutene, 0.10-0.48 parts of arginine and 0.01-0.1 parts of fragrance.

[0036] Furthermore, by weight, the cosmetic excipient contains 70.62 parts of water, 0.1 parts of disodium EDTA, 3 parts of glycerin, 0.05 parts of hyaluronic acid, 0.1 parts of xanthan gum, 0.2 parts of allantoin, 0.2 parts of acrylates / C10-30 alkyl acrylate crosspolymer, 7 parts of butylene glycol, 1.5 parts of 1,2-hexanediol, 0.5 parts of p-hydroxyacetophenone, 3 parts of cetearyl alcohol, 4 parts of caprylic / capric triglyceride, 1 part of PEG-100 glyceryl stearate, 2 parts of cetearyl glucoside, 2 parts of polydimethylsiloxane, 4 parts of hydrogenated polyisobutene, 0.18 parts of arginine and 0.05 parts of fragrance.

[0037] The cosmetics have the functions of synergistically inhibiting Propionibacterium acnes and synergistically anti-oxidation. Consumer tests have shown that there are significant improvements in the improvement of acne, improvement of facial redness and anti-itching, and the overall satisfaction is high.

[0038] In a fourth aspect, the present invention also claims a method for preparing the cosmetic, comprising the following steps:

[0039] S1: Mix the components in phase A, adjust the temperature to 80-85°C, and disperse them completely;

[0040] S2: After dissolving phase B and phase C, add phase A in step S1 and homogenize and emulsify;

[0041] S3: Adjust the temperature of the homogenized and emulsified product in step S3 to 60-65°C, add phase D, and stir to dissolve evenly;

[0042] S4: adjusting the temperature of the product obtained by stirring and dissolving in step S3 to 40-45° C., adding phase E, stirring evenly, and adjusting the temperature to room temperature to obtain the cosmetic;

[0043] The phase A contains at least one of water, disodium EDTA, glycerin, hyaluronic acid, xanthan gum, allantoin and acrylic acid (esters) / C10-30 alkyl acrylate cross-linked polymer;

[0044] The phase B contains at least one of butanediol, 1,2-hexanediol and p-hydroxyacetophenone;

[0045] The phase C contains at least one of cetearyl alcohol, caprylic / capric triglyceride, PEG-100 glyceryl stearate, cetearyl glucoside, dimethicone and hydrogenated polyisobutene;

[0046] The D phase contains arginine;

[0047] The E phase contains the botanical active ingredient composition and a fragrance.

[0048] Furthermore, in step S2, phase B and / or phase C may be dissolved at 80-85°C.

[0049] Compared with the prior art, the present invention has the following beneficial effects:

[0050] 1. In the composite plant composition of the present invention, when the weight ratio of Aquilaria sinensis leaf extract: Aquilaria sinensis leaf / stem extract = (1-4): (1-3), the synergistic antibacterial index and the synergistic antioxidant index CI are both <1, which has both synergistic antibacterial and synergistic antioxidant effects.

[0051] 2. In the composite plant-active ingredient composition of the present invention, when the weight ratio of the plant composition obtained by different weight ratios of Aquilaria sinensis leaf extract and Bletilla striata leaf / stem extract to tea polyphenols is 1:(4-5), the antibacterial and antioxidant synergistic index of each composition is less than 1, and it has synergistic antibacterial and antioxidant effects.

[0052] 3. In the composite plant-active ingredient composition of the present invention, when the weight ratio of the plant composition obtained by different weight ratios of the Aquilaria sinensis leaf extract and the Aquilaria scabra leaf / stem extract to EGCG is 1:(3-5), the antibacterial and antioxidant synergistic index of each composition is less than 1, and it has synergistic antibacterial and antioxidant effects.

[0053] 4. The composition of the present invention not only has excellent synergistic antibacterial effect on Propionibacterium acnes, but also has synergistic anti-oxidation effect. It can repair acne from the two aspects of antibacterial and anti-oxidation damage by counteracting the inflammation and oxidative damage caused by the proliferation of Propionibacterium acnes.

[0054] 5. According to consumer tests, the cosmetics (anti-acne cream) prepared by the plant active ingredient composition of the present invention have significant improvements in the improvement of acne, improvement of facial redness and anti-itching, and the overall satisfaction is high. BRIEF DESCRIPTION OF THE DRAWINGS

[0055] Figure 1 The synergistic antioxidant test results of the plant composition obtained by different weight ratios of the Aquilaria sinensis leaf extract and the Aquilaria odorata leaf / stem extract obtained in Test Example 2 (the plant composition described in Example 1). Among them, A is: Aquilaria sinensis leaf extract; B is: Aquilaria sinensis leaf / stem extract; C is: Composition 1 (Aquilaria sinensis leaf extract: Aquilaria sinensis leaf / stem extract = 1:1); D is: Composition 2 (Aquilaria sinensis leaf extract: Aquilaria sinensis leaf / stem extract = 4:1); E is: Composition 3 (Aquilaria sinensis leaf extract: Aquilaria sinensis leaf / stem extract = 2:3); F is: Composition 4 (Aquilaria sinensis leaf extract: Aquilaria sinensis leaf / stem extract = 3:2). The above ratios are weight ratios.

[0056] Figure 2 This is a graph showing the synergistic antioxidant test results of a plant-active ingredient composition (the plant-active ingredient composition described in Example 2) compounded with a plant composition obtained by combining different weight ratios of the Aquilaria sinensis leaf extract and the Aquilaria odorifera leaf / stem extract obtained in Test Example 2 and different proportions of tea polyphenols. G is tea polyphenols; H is composition 6 [(Aquilaria sinensis leaf extract: Ampelopsis odoratus leaf / stem extract = 1:1): tea polyphenols = 1:3]; I is composition 10 [(Aquilaria sinensis leaf extract: Ampelopsis odoratus leaf / stem extract = 2:3): tea polyphenols = 1:3]; J is composition 7 [(Aquilaria sinensis leaf extract: Ampelopsis odoratus leaf / stem extract = 1:1): tea polyphenols = 1:4]; K is composition 11 [(Aquilaria sinensis leaf extract: Ampelopsis odoratus leaf / stem extract = 2:3): tea polyphenols = 1:4]; L is composition 8 [(Aquilaria sinensis leaf extract: Ampelopsis odoratus leaf / stem extract = 1:1): tea polyphenols = 1:5]; M is composition 12 [(Aquilaria sinensis leaf extract: Ampelopsis odoratus leaf / stem extract = 2:3): tea polyphenols = 1:5]. The above ratios are weight ratios.

[0057] Figure 3This is a graph showing the synergistic antioxidant test results of a plant composition obtained by combining different weight ratios of the Aquilaria sinensis leaf extract and the Aquilaria odorifera leaf / stem extract obtained in Test Example 2 with a plant-active ingredient composition (the plant-active ingredient composition described in Example 3) in different proportions of EGCG. Wherein, N is: EGCG; O is: composition 14 [(Aquilaria sinensis leaf extract: Ampelopsis odoratus leaf / stem extract = 1:1): EGCG = 1:3]; P is: composition 18 [(Aquilaria sinensis leaf extract: Ampelopsis odoratus leaf / stem extract = 2:3): EGCG = 1:3]; Q is: composition 15 [(Aquilaria sinensis leaf extract: Ampelopsis odoratus leaf / stem extract = 1:1): EGCG = 1:4]; R is: composition 19 [(Aquilaria sinensis leaf extract: Ampelopsis odoratus leaf / stem extract = 2:3): EGCG = 1:4]; S is: composition 16 [(Aquilaria sinensis leaf extract: Ampelopsis odoratus leaf / stem extract = 1:1): EGCG = 1:5]; T is: composition 20 [(Aquilaria sinensis leaf extract: Ampelopsis odoratus leaf / stem extract = 2:3): EGCG = 1:5]. The above ratios are weight ratios. DETAILED DESCRIPTION

[0058] To better illustrate the purpose, technical solutions and advantages of the present invention, the present invention will be further described below in conjunction with specific examples. Other materials, reagents, etc. used in the examples, unless otherwise specified, can be obtained from commercial sources.

[0059] Example 1

[0060] In this embodiment, plant compositions (compositions 1 to 4) were prepared by configuring Aquilaria sinensis leaf extract and Aquilaria odorifera leaf / stem extract in different weight ratios, and the specific ratios are shown in Table 1:

[0061] Table 1 Compositions of different weight ratios of Aquilaria sinensis leaf extract and Aquilaria sinensis leaf / stem extract

[0062]

[0063] According to the proportions of each composition in Table 1, weigh the costus root leaf extract and the umbelliferae leaf / stem extract powder, dissolve the costus root leaf extract and the umbelliferae leaf / stem extract powder with sterile enzyme-free water to obtain 200 mg / mL plant extract stock solution.

[0064] Example 2

[0065] In this example, the plant-active ingredient composition was obtained by compounding the compositions 1 and 3 with tea polyphenols in different weight ratios. The specific ratios are shown in Table 2:

[0066] Table 2 Composite compositions of compositions 1 and 3 with tea polyphenols at different weight ratios

[0067]

[0068]

[0069] The preparation method of compositions 5 to 12 comprises the following steps:

[0070] 1. According to the method of Example 1, according to the ratio of composition 1 and composition 3, 200 mg / mL of plant extract was prepared, and diluted with sterile enzyme-free water to obtain 6.25 mg / mL of plant extract stock solution.

[0071] 2. Dissolve tea polyphenols in sterile enzyme-free water and prepare a 6.25 mg / mL tea polyphenol stock solution.

[0072] 3. Use the above stock solution to compound so that the total concentration of the plant extract and tea polyphenols is 6.25 mg / mL. Do not change the total concentration and adjust the proportion of each drug. The specific formulation ratio is shown in Table 2.

[0073] Example 3

[0074] In this example, plant compositions 1 and 3 were compounded with EGCG (epigallocatechin gallate) in different weight ratios to obtain plant-active ingredient compositions (compositions 13 to 20), and the specific ratios are shown in Table 3:

[0075] Table 3 Composite compositions of plant compositions 1 and 3 with EGCG at different weight ratios

[0076]

[0077] Tea polyphenols were replaced with EGCG, and other preparation methods were the same as in Example 2.

[0078] Test Example 1

[0079] In this test example, the minimum inhibitory concentration (MIC) of the test samples was determined by the microbroth dilution method to evaluate the inhibitory effect of each test sample on Propionibacterium acnes; the synergistic antibacterial effect of each test sample was evaluated by exploring the synergistic effect index (CI) to screen for excellent combinations that inhibit Propionibacterium acnes.

[0080] 1. Test materials

[0081] Propionibacterium acnes (ATCC 11827) was purchased from Shanghai Microbiological Collection Center; BHI brain heart infusion broth was purchased from Qingdao High-Tech Industrial Park Haibo Biotechnology Co., Ltd.; purified agar powder was purchased from Shanghai Yuanye Biotechnology Co., Ltd.; sodium chloride Sinopharm Chemical Reagent Co., Ltd.; sterile enzyme-free water was purchased from Beijing Solebow Technology Co., Ltd.; anaerobic gas-generating bags and anaerobic sealed culture bags were purchased from Mitsubishi Gas Chemical Co., Ltd. of Japan; Aquilaria sinensis leaf extract and Acanthopanax odoratum leaf / stem extract were provided by Perfect; epigallocatechin gallate (EGCG 98%) and tea polyphenols (98%) were purchased from Xi'an Tianben Bioengineering Co., Ltd.

[0082] The preparation method of the extract of Aquilaria sinensis leaves is as follows:

[0083] (1) subjecting Aquilaria sinensis leaves and water to hot reflux extraction for 1 h at a solid-liquid ratio of 1:22 (weight ratio), removing the residue, and obtaining a first extract of Aquilaria sinensis leaves;

[0084] (2) taking the residue from step (1), performing hot reflux extraction on the residue and water at a solid-liquid ratio of 1:22 (weight ratio) for 1 hour, removing the residue, and obtaining a second extract of Aquilaria sinensis leaves;

[0085] (3) combining the first extract of Aquilaria sinensis leaves obtained in step (1) and the second extract of Aquilaria sinensis leaves obtained in step (2), centrifuging at 4000 rpm for 10 min, and removing the residue; taking the supernatant and spray drying the mixture to obtain an Aquilaria sinensis leaf extract.

[0086] The preparation method of the extract of balsam pear leaf / stem is as follows:

[0087] (1) subjecting the leaves / stems of the white calamus to hot reflux extraction with water at a solid-liquid ratio of 1:15 (weight ratio) for 2 h, removing the residue, and obtaining the first extract of the leaves / stems of the white calamus;

[0088] (2) taking the residue from step (1), performing hot reflux extraction with water at a solid-liquid ratio of 1:10 for 1.5 h, removing the residue, and obtaining a second extract of the leaves / stems of the white calamus;

[0089] (3) The first extract of the white balsam pear leaf / stem of step (1) and the second extract of the white balsam pear leaf / stem of step (2) are combined and concentrated, the concentrated solution is filtered using a ceramic membrane (0.2 μm), the retentate is discarded, and the filtrate is retained; the filtrate is concentrated; the filtrate is sterilized by UHT instantaneous high temperature to obtain a sterilized solution; and then spray-dried to obtain a white balsam pear leaf / stem extract.

[0090] 2. Test methods

[0091] (1) Preparation of BHI liquid and solid culture medium

[0092] Prepare according to the instructions, accurately weigh the culture medium particles and agar in a beaker, add 1000 mL of deionized water, stir with a glass rod until the culture medium particles are completely dissolved, heat and boil in a microwave oven until the agar is evenly dispersed, dispense into conical bottles, seal, autoclave at 121°C for 30 minutes, cool and store in a refrigerator at 4°C for later use, and obtain BHI solid culture medium. Agar does not need to be added when preparing BHI liquid culture medium.

[0093] (2) Preparation of bacterial suspension

[0094] Take out the glycerol tube of the tested bacteria stored in the -20℃ refrigerator, take 20μL of bacterial solution with an inoculation loop, inoculate it on the agar slant by streaking method, place it in a 37℃ constant temperature incubator and culture it for 48-72h, rinse the slant with physiological saline to obtain a high-concentration bacterial suspension; take another test tube, pour in an appropriate amount of raw salt, take an appropriate amount of high-concentration bacterial suspension to make its turbidity consistent with that of No. 5 McFarland turbidity tube, and obtain a final concentration of 1×10 6 CFU / mL bacterial suspension.

[0095] (3) Determination of MIC value

[0096] ①Cultivation method

[0097] Add 100 μL of BHI liquid medium to columns 2 to 11 of the 96-well plate, and add 200 μL of BHI liquid medium to column 12. Add 200 μL of each sample to be tested to column 1, and take 100 μL of the horizontal two-fold dilution to column 10 (discard the excess 100 μL of the drug solution). Then take 1×10 6 Add CFU / mL bacterial suspension to columns 1 to 11, 100 μL per well. The final volume of each well is 200 μL. Column 11 is the growth control well, and column 12 is the blank control well. Place the 96-well plate in an anaerobic constant temperature culture at 37°C for 36 to 72 hours.

[0098] ②Evaluation criteria

[0099] Visually observed, the concentration of the drug solution in the sterile growth hole is the minimum inhibitory concentration (MIC).

[0100] (4) Evaluation criteria

[0101] The Chou-Talalay model is a commonly used pharmacological model used to evaluate the synergistic and antagonistic effects of compound combinations during the onset of action. The synergistic effect index (CI) is calculated according to the Chou-Talalay formula, which is as follows:

[0102]

[0103] Note: C a, C b , C c , C d are the concentrations corresponding to the antibacterial effects of components A, B, C, and D when acting alone; C A , C B , C C , C D It indicates the inhibitory effect observed at the corresponding concentration when each component is compounded into a composite, C A-D Result = Composition MIC experimental data × C A-D The proportion of a component in a composition. If CI < 1, it indicates a synergistic effect; if CI = 1, it indicates no interaction; and if CI > 1, it indicates an antagonistic effect.

[0104] 3. Test results

[0105] (1) Table 4 shows the antibacterial results of the individual components of each sample to be tested

[0106] Table 4 Antibacterial results of individual components of each sample to be tested

[0107]

[0108]

[0109] As shown in Table 4, the extracts of Achyranthes bidentata leaves / stem, Aquilaria sabdariffa leaves, tea polyphenols and EGCG alone all had excellent antibacterial activity, with MICs of 10.416, 3.125, 0.098 and 0.098 mg / mL, respectively.

[0110] (2) Table 5 shows the synergistic antibacterial results of the plant compositions (compositions 1 to 4) obtained by using different weight ratios of the Aquilaria sinensis leaf extract and the Aquilaria sinensis leaf / stem extract in Example 1:

[0111] Table 5 Synergistic antibacterial results of compositions 1 to 4 of Example 1 (mg / mL)

[0112]

[0113] Table 5 shows the antibacterial results of compositions 1 to 4 described in Preparation Example 1. The MICs of the four ratios shown in the table are all 3.125 mg / mL, and the synergistic antibacterial index CI is all <1, indicating a synergistic effect. Among them, the synergistic indexes of composition 1 and composition 3 (optimal) are relatively small.

[0114] Therefore, composition 1 and composition 2 were subsequently compounded with tea polyphenols and EGCG.

[0115] (3) Table 6 shows the synergistic antibacterial results of plant-active ingredient compositions (compositions 5 to 12) obtained by compounding compositions 1 and 3 with tea polyphenols at different weight ratios in Example 2:

[0116] Table 6 Synergistic antibacterial results of compositions 5 to 12 of Example 2 (mg / mL)

[0117]

[0118] As shown in Table 6, when the weight ratio of the composition of Aquilaria sinensis leaf extract and Ampelopsis pilosula leaf / stem extract to tea polyphenols is 1:(3-5), i.e., compositions 6-8 and compositions 10-12, CI < 1, they have a synergistic antibacterial effect.

[0119] (4) Table 7 shows the synergistic antibacterial results of plant-active ingredient compositions (compositions 13 to 20) obtained by compounding compositions 1 and 3 with EGCG at different weight ratios in Example 3:

[0120] Table 7 Synergistic antibacterial results of compositions 13 to 20 of Example 3 (mg / mL)

[0121]

[0122] As shown in Table 7, when the weight ratio of the composition of Aquilaria sinensis leaf extract and Ampelopsis pilosula leaf / stem extract to EGCG is 1:(3-5), i.e., compositions 14-16 and compositions 18-20, CI < 1, they have a synergistic antibacterial effect.

[0123] Test Example 2

[0124] This test evaluates the antioxidant capacity of each sample by measuring its scavenging ability for DPPH free radicals, and obtains the IC 50 The synergistic antioxidant effect (synergistic effect against oxidative stress) was evaluated by the synergistic effect index (CI).

[0125] 1. Test materials: 1,1-diphenyl-2-trinitrophenylhydrazine (DPPH) was purchased from Shanghai MacLean Biochemical Technology Co., Ltd.

[0126] 2. Test methods

[0127] (1) Antioxidant test

[0128] The concentrations of Aquilaria sinensis leaf extract, Aquilaria odorata leaf / stem extract and plant composition were prepared to be 12.5-400 μg / mL, and the concentrations of tea polyphenols, EGCG and plant-active ingredient composition were prepared to be 0.78125-25 μg / mL to obtain the samples to be tested. 500 μL of the samples to be tested of different concentrations were taken into plastic centrifuge tubes with a pipette, and 500 μL of DPPH (0.2 mmol / L, prepared in ethanol) solution was added. After shaking and avoiding light for 30 minutes, ethanol was used as a blank control and VC as a positive control. The absorbance was measured at 517 nm, and three parallel experiments were performed. The specific calculation formula is as follows:

[0129]

[0130] Note: D1 is the absorbance of the test sample or positive control; D2 is the absorbance of the blank control.

[0131] (2) Drawing and IC 50 calculate

[0132] The concentration index of each sample to be tested (Log Drug Concentration) is used as the horizontal axis, and the scavenging rate of each sample to be tested on DPPH free radicals is used as the vertical axis (DPPH radical scavenging activity / %). Graphpadprism 9 is used to draw a curve and obtain the half inhibition rate IC 50 .

[0133] (3) Evaluation criteria

[0134] The synergy index (CI) was calculated according to the Chou-Talalay formula, which is as follows:

[0135]

[0136] Note: C a , C b , C c , C d The IC of components A, B, C, and D acting alone 50 ; C A , C B , C C , C D Indicates the IC corresponding to the compound when the test drug is compounded into a composite 50 , C A-D The result = composition IC 50 ×C A-D The proportion of a component in a composition. If CI < 1, it indicates a synergistic effect; if CI = 1, it indicates no interaction; and if CI > 1, it indicates an antagonistic effect.

[0137] 3. Test results

[0138] (1) Table 8 shows the synergistic antioxidant results of the plant composition obtained by using different weight ratios of the Aquilaria sinensis leaf extract and the Aquilaria sinensis leaf / stem extract described in Preparation Example 1:

[0139] Table 8 Synergistic antioxidant results of different proportions of the composition in Preparation Example 1

[0140] Aquilegia Sinensis Leaf Extract Balsam Pear Leaf / Stem Extract Composition 1 Composition 2 Composition 3 Composition 4 <![CDATA[Log(IC 50 )]]> 1.884 2.328 2.039 1.939 2.027 2.145 <![CDATA[IC 50 (μg / mL)]]> 76.560 212.814 109.396 86.896 106.414 97.274 CI - - 0.971 0.990 0.856 0.945 Collaboration or not - - Collaboration Collaboration Collaboration Collaboration

[0141] Table 8 and Figure 1The antioxidant results of the plant composition obtained by using different weight ratios of the Aquilaria sinensis leaf extract and the Aquilaria odorata leaf / stem extract described in Example 1. Figure 1 A is: Aquilaria sinensis leaf extract; Figure 1 B is: Bletilla striata leaf / stem extract; Figure 1 C is: Composition 1 (Aquilaria sinensis leaf extract: Ampelopsis pilosula leaf / stem extract = 1:1); Figure 1 D is: Composition 2 (Aquilaria sinensis leaf extract: Ampelopsis pilosula leaf / stem extract = 4:1); Figure 1 E is: Composition 3 (Aquilaria sinensis leaf extract: Ampelopsis pilosula leaf / stem extract = 2:3); Figure 1 F is: Composition 4 (Aquilaria sinensis leaf extract: Ampelopsis odorata leaf / stem extract = 3:2). The above ratios are weight ratios. The results showed that the IC 50 The IC values ​​of compositions 1 to 4 were 76.560 and 212.814 μg / mL, respectively. 50 They are 109.396, 86.896, 106.414 and 97.274 μg / mL respectively, and the antioxidant synergistic index CI is less than 1, which has a synergistic antioxidant effect.

[0142] Combined with the antibacterial results, it can be seen that when the weight ratio of Aquilaria sinensis leaf extract: Aquilaria sinensis leaf / stem extract = (1-4): (1-3), the composition has a synergistic antibacterial and antioxidant effect.

[0143] (2) Tables 9 to 11 show the synergistic antioxidant results of the plant-active ingredient compositions prepared by combining the Aquilaria sinensis leaf extract and the Aquilaria sinensis leaf / stem extract in different weight ratios in Example 2 with tea polyphenols in different proportions:

[0144] Table 9 Plant composition: tea polyphenols weight ratio = 1:3 Antioxidant results

[0145] Tea polyphenols Composition 6 Composition 10 <![CDATA[Log(IC 50 )]]> 0.5541 0.6373 0.6787 <![CDATA[IC 50 (μg / mL)]]> 3.5818 4.3381 4.7720 CI - 0.918 1.010 Collaboration or not - Collaboration Antagonism

[0146] Table 10 Plant composition: tea polyphenols weight ratio = 1:4 Antioxidant results

[0147] Tea polyphenols Composition 7 Composition 11 <![CDATA[Log(IC 50 )]]> 0.5541 0.5391 0.5692 <![CDATA[IC 50 (μg / mL)]]> 3.5818 3.4602 3.7085 CI - 0.779 0.835 Collaboration or not - Collaboration Collaboration

[0148] Table 11 Antioxidant results of plant composition: tea polyphenols weight ratio = 1:5

[0149] Tea polyphenols Composition 8 Composition 12 <![CDATA[Log(IC 50 )]]> 0.5541 0.5115 0.5067 <![CDATA[IC 50 (μg / mL)]]> 3.5818 3.2471 3.2114 CI - 0.760 0.752 Collaboration or not - Collaboration Collaboration

[0150] Tables 9 to 11 and Figure 2 The synergistic antioxidant results of the plant-active ingredient composition obtained by mixing the Aquilaria sinensis leaf extract and the Aquilaria sinensis leaf / stem extract in different weight ratios with tea polyphenols in different proportions as described in Example 2, Figure 2 G is: tea polyphenols; Figure 2 H is: Composition 6 [(Aquilaria sinensis leaf extract: Aquilaria sinensis leaf / stem extract = 1:1): tea polyphenols = 1:3]; Figure 2 I is: composition 10 [(Aquilaria sinensis leaf extract: Aquilaria sinensis leaf / stem extract = 2:3): tea polyphenols = 1:3]; Figure 2 J is: composition 7 [(Aquilaria sinensis leaf extract: Aquilaria sinensis leaf / stem extract = 1:1): tea polyphenols = 1:4]; Figure 2 K is: composition 11 [(Aquilaria sinensis leaf extract: Aquilaria sinensis leaf / stem extract = 2:3): tea polyphenols = 1:4]; Figure 2 L is: composition 8 [(Aquilaria sinensis leaf extract: Aquilaria sinensis leaf / stem extract = 1:1): tea polyphenols = 1:5]; Figure 2 M is: composition 12 [(Aquilaria sinensis leaf extract: Aquilaria sinensis leaf / stem extract = 2:3): tea polyphenols = 1:5]. The above ratios are weight ratios. When the weight ratio of composition 1 to tea polyphenols is 1: (3-5) and the weight ratio of composition 3 to tea polyphenols is 1: (4-5), the antioxidant synergistic index of each composition is <1, and all have synergistic antioxidant effects. As the content of tea polyphenols increases, the synergistic index decreases and the synergistic effect increases.

[0151] Combined with the antibacterial results, it can be seen that when the weight ratio of plant composition to tea polyphenols is 1:(4-5), it has a synergistic antibacterial and antioxidant effect.

[0152] (3) Tables 12 to 14 show the synergistic antioxidant results of the plant composition obtained by combining the Aquilaria sinensis leaf extract and the Aquilaria sinensis leaf / stem extract in different weight ratios with the plant-active ingredient composition prepared by combining EGCG in different proportions:

[0153] Table 12 Plant composition: EGCG = 1:3 Antioxidant results

[0154] EGCG Composition 14 Composition 18 <![CDATA[Log(IC 50 )]]> 0.4969 0.5110 0.5616 <![CDATA[IC 50 (μg / mL)]]> 3.1398 3.2434 3.6442 CI - 0.782 0.879 Collaboration or not - Collaboration Collaboration

[0155] Table 13 Plant composition: EGCG = 1:4 Antioxidant results

[0156] EGCG Composition 15 Composition 19 <![CDATA[Log(IC 50 )]]> 0.4969 0.5099 0.5051 <![CDATA[IC 50 (μg / mL)]]> 3.1398 3.2352 3.1996 CI - 0.830 0.821 Collaboration or not - Collaboration Collaboration

[0157] Table 14 Plant composition: EGCG = 1:5 Antioxidant results

[0158] EGCG Composition 16 Composition 20 <![CDATA[Log(IC 50 )]]> 0.4969 0.4950 0.4953 <![CDATA[IC 50 (μg / mL)]]> 3.1398 3.1260 3.1282 CI - 0.834 0.835 Collaboration or not - Collaboration Collaboration

[0159] Tables 12 to 14 and Figure 3 The synergistic antioxidant results of the plant composition obtained by mixing the Aquilaria sinensis leaf extract and the Aquilaria sinensis leaf / stem extract in different weight ratios with the plant-active ingredient composition in different proportions of EGCG as described in Example 3, Figure 3 N is: EGCG; Figure 3 O is: composition 14 [(Aquilaria sinensis leaf extract: Ampelopsis pilosula leaf / stem extract = 1:1): EGCG = 1:3]; Figure 3 P is: Composition 18 [(Aquilaria sinensis leaf extract: Aquilaria sinensis leaf / stem extract = 2:3): EGCG = 1:3]; Figure 3 Q is: Composition 15 [(Aquilaria sinensis leaf extract: Aquilaria sinensis leaf / stem extract = 1:1): EGCG = 1:4]; Figure 3 R is: composition 19 [(Aquilaria sinensis leaf extract: Aquilaria sinensis leaf / stem extract = 2:3): EGCG = 1:4]; Figure 3 S is: composition 16 [(Aquilaria sinensis leaf extract: Aquilaria sinensis leaf / stem extract = 1:1): EGCG = 1:5]; Figure 3 T is: Composition 20 [(Aquilaria sinensis leaf extract: Ampelopsis odoratum leaf / stem extract = 2:3): EGCG = 1:5]. The above ratios are weight ratios. When the weight ratio of Aquilaria sinensis leaf extract and Ampelopsis odoratum leaf / stem extract composition (compositions 1 and 3) to EGCG is 1:(3-5), the antioxidant synergistic index of each composition is <1, and all have synergistic antioxidant effects.

[0160] Combined with the antibacterial results, it can be seen that when the weight ratio of plant composition: EGCG = 1: (3-5), it has a synergistic antibacterial and antioxidant effect.

[0161] Application Example 1

[0162] This application example provides a plant composition anti-acne cream for inhibiting Propionibacterium acnes, the weight parts of each component are as shown in Table 15, wherein the plant composition is composition 3 of Example 1 (weight ratio of Aquilaria sinensis leaf extract: Aquilaria sinensis leaf / stem extract = 2:3). The preparation method thereof comprises the following steps:

[0163] 1. Add the water in phase A, and add the remaining components in phase A in sequence while stirring, heat to 80-85°C, homogenize and disperse completely, and keep constant temperature for use;

[0164] 2. Preheat phase B to 80-85°C to dissolve, then add it to phase A treated in step 1 and stir to dissolve evenly;

[0165] 3. Mix phase C and heat to 80-85℃ until dissolved, set aside;

[0166] 4. Add phase C treated in step 3 to the mixture of phase A and phase B treated in step 2, start homogenization and emulsification, and start cooling;

[0167] 5. Cool down to 60-65°C in step 4, add phase D, stir to dissolve evenly, and continue stirring to cool down;

[0168] 6. In step 5, cool down to 40-45°C, add phase E, stir evenly and cool down to room temperature.

[0169] Application Example 2

[0170] This application example provides a plant composition anti-acne cream for inhibiting Propionibacterium acnes, the weight parts of each component are as shown in Table 15, wherein the plant composition is the composition 11 of Example 2 [(Aquilaria sinensis leaf extract: Aquilaria sinensis leaf / stem extract = 2:3): tea polyphenols = 1:4]. Its preparation method is the same as that of Application Example 1.

[0171] Application Example 3

[0172] This application example provides a plant composition anti-acne cream for inhibiting Propionibacterium acnes, the weight parts of each component are as shown in Table 15, wherein the plant composition is composition 19 of Example 3 [(Aquilaria sinensis leaf extract: Aquilaria sinensis leaf / stem extract = 2:3): EGCG = 1:4]. Its preparation method is the same as that of Application Example 1.

[0173] Comparative Example 1

[0174] This comparative example provides a plant composition anti-acne cream for inhibiting Propionibacterium acnes. The weight proportions of the components are as shown in Table 16. The difference from Application Examples 1 to 3 is that there is no plant composition.

[0175] Comparative Example 2

[0176] This comparative example provides a plant composition anti-acne cream for inhibiting Propionibacterium acnes. The weight proportions of the components are shown in Table 16. The difference from Application Example 1 is that the plant composition contains only Aquilaria sinensis leaf extract.

[0177] Comparative Example 3

[0178] This comparative example provides a plant composition anti-acne cream for inhibiting Propionibacterium acnes. The weight proportions of the components are shown in Table 16. The difference from Application Example 1 is that the plant composition contains only the extract of the leaf / stem of Ampelopsis pilosula.

[0179] Comparative Example 4

[0180] This comparative example provides a plant composition anti-acne cream for inhibiting Propionibacterium acnes. The weight proportions of the components are shown in Table 16. The difference from Application Example 2 is that the plant composition contains only tea polyphenols (without a plant extract composition).

[0181] Comparative Example 5

[0182] This comparative example provides a plant composition acne cream for inhibiting Propionibacterium acnes. The weight proportions of the components are shown in Table 16. The difference from Application Example 3 is that the plant composition contains only EGCG (without plant extract composition).

[0183] Table 15 Application example formula of plant composition acne cream for inhibiting Propionibacterium acnes

[0184]

[0185] Table 16 Comparative formula of plant composition acne cream for inhibiting Propionibacterium acnes

[0186]

[0187] Test Example 3

[0188] 90 male and female volunteers aged 20 to 40 were selected (the inclusion criteria were facial lesions, the main lesions were acne, with a small number of pustules or papules, and a total number of lesions of 10 to 50), and randomly divided into 9 groups, 10 in each group (5 males and 5 females), and used the acne cream containing application examples 1 to 3 and the acne cream containing comparative examples 1 to 5 respectively, the use time was every night after facial cleaning, the use method remained consistent, and the subjects' satisfaction with the product and the effectiveness of inhibiting acne were tracked through a questionnaire after 28 days of use.

[0189] The research method of this experiment is self-control before and after, and the subjects make subjective evaluations. Satisfaction = number of satisfied evaluations / total number of subjects, where satisfied evaluations include very satisfied, relatively satisfied, and somewhat satisfied. During the trial, no subjects experienced adverse reactions, and no subjects withdrew from the test.

[0190] As shown in Table 17, which is the result of the consumer survey, Application Examples 1 to 3 are superior to Comparative Examples 1 to 5 in terms of improvement of acne, improvement of facial redness, anti-itching and overall product satisfaction.

[0191] Table 17 Consumer survey results

[0192]

[0193] Finally, it should be noted that the above embodiments are only used to illustrate the technical solution of the present invention rather than to limit the scope of protection of the present invention. Although the present invention has been described in detail with reference to the preferred embodiments, those skilled in the art should understand that the technical solution of the present invention can be modified or replaced by equivalents without departing from the essence and scope of the technical solution of the present invention.

Claims

1. A plant active ingredient composition, characterized in that: The invention comprises a composition of an extract of Aquilaria sinensis leaves and an extract of a leaf / stem of Glechoma longituba. The weight ratio of the extract of Aquilaria sinensis leaves to the extract of a leaf / stem of Glechoma longituba is: the extract of Aquilaria sinensis leaves: the extract of a leaf / stem of Glechoma longituba = (1-4): (1-3).

2. The plant active ingredient composition according to claim 1, characterized in that: The plant active ingredient composition further comprises tea active ingredients, and the tea active ingredients comprise tea polyphenols and / or epigallocatechin gallate.

3. The plant active ingredient composition according to claim 2, characterized in that: The weight ratio of the Aquilaria sinensis leaf extract and the Ampelopsis odoratum leaf / stem extract composition to the tea active ingredient is: the Aquilaria sinensis leaf extract and the Ampelopsis odoratum leaf / stem extract composition: the tea active ingredient = 1: (3-5).

4. Use of the plant active ingredient composition according to any one of claims 1 to 3 in the preparation of antibacterial products and / or antioxidant products.

5. The use according to claim 4, characterized in that: The species of bacteria include Propionibacterium acnes.

6. The use according to claim 5, characterized in that: The products include cosmetics.

7. A cosmetic, characterized in that: The cosmetic contains the plant active ingredient composition according to any one of claims 1 to 3.

8. The cosmetic according to claim 7, characterized in that: The cosmetics also contain cosmetic accessories.

9. The cosmetic according to claim 8, characterized in that: The cosmetic auxiliary material comprises at least one of a solvent, a chelating agent, a moisturizing agent, a thickening agent, an antioxidant, a moisturizing agent, an emulsifier, a pH value adjusting agent and a fragrance.

10. The method for preparing the cosmetic according to any one of claims 7 to 9, characterized in that: The following steps are involved: S1: Mix the components in phase A, adjust the temperature to 80-85°C, and disperse them completely; S2: After dissolving phase B and phase C, add phase A in step S1 and homogenize and emulsify; S3: Adjust the temperature of the homogenized and emulsified product in step S3 to 60-65°C, add phase D, and stir to dissolve evenly; S4: adjusting the temperature of the product obtained by stirring and dissolving in step S3 to 40-45° C., adding phase E, stirring evenly, and adjusting the temperature to room temperature to obtain the cosmetic; The phase A contains at least one of water, disodium EDTA, glycerin, hyaluronic acid, xanthan gum, allantoin and acrylic acid (esters) / C10-30 alkyl acrylate cross-linked polymer; The phase B contains at least one of butanediol, 1,2-hexanediol and p-hydroxyacetophenone; The phase C contains at least one of cetearyl alcohol, caprylic / capric triglyceride, PEG-100 glyceryl stearate, cetearyl glucoside, dimethicone and hydrogenated polyisobutene; The D phase contains arginine; The phase E contains the plant active ingredient composition according to any one of claims 1 to 3 and a fragrance.

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