Licorice plant sunscreen composition suitable for sensitive skin and preparation method thereof
By combining licorice extract with other plant extracts in a specific proportion, the existing sunscreen products have solved the problems of high irritation, low sunscreen index and narrow bands on sensitive skin, achieving high sunscreen index, wide band, stable and gentle sunscreen effects.
Patent Information
- Application Number
- CN202411196579.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-08-29
- Publication Date
- 2025-08-12
- Estimated Expiration
- 2044-08-29
AI Technical Summary
Existing sunscreen products are highly irritating to sensitive skin, have a low sunscreen index, narrow sunscreen band, and are prone to discoloration, which cannot provide comprehensive and stable ultraviolet protection.
Using a specific proportion of licorice extract, grey edamame seed extract and red axle extract, the synergistic action of the glycyrrhizone, the glycyrrhizone isomer and the glycyrrhizone derivative is used to absorb the ultraviolet light in different bands to form a stable plant sunscreen composition.
It provides a high sun protection index, wide sun protection band, is not easy to discolor, and is gentle and non-irritating to sensitive skin, improving the stability and protection ability of the sun protection composition.
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Figure CN119074607B_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of cosmetics, in particular to a liquorice plant sunscreen composition suitable for sensitive skin and a preparation method thereof. Background Art
[0002] Long-term exposure to ultraviolet rays can cause burns, redness, aging, and even increase the risk of skin cancer, so skin protection from the sun is necessary. Currently, most sunscreen products on the market use physical or chemical sunscreens. However, physical sunscreens, such as zinc oxide and titanium dioxide, are generally insoluble in water and require the addition of large amounts of oil to dissolve, resulting in a greasy feel on the skin, clogging pores, and causing skin inflammation and acne. Chemical sunscreens, on the other hand, present more safety risks, such as skin irritation and allergies. Furthermore, due to their small molecular weight, they may enter blood vessels, posing potential harm to the human body. In recent years, plant-based sunscreens have gradually entered the public eye, offering advantages such as being mild, safe, refreshing, non-irritating, and non-greasy. However, their disadvantages include a low SPF, yellowing and discoloration of the product, and the narrow protection band of a single sunscreen.
[0003] Therefore, a plant sunscreen composition with a high sun protection index, a wide sun protection band, not easy to change color, and mild and non-irritating to sensitive skin has broad application prospects. Summary of the Invention
[0004] Based on this, the purpose of the present invention is to overcome the shortcomings of the above-mentioned prior art and provide a licorice plant sunscreen composition suitable for sensitive skin and a preparation method thereof.
[0005] To achieve the above-mentioned object, the technical solution adopted by the present invention is as follows: a plant sunscreen composition, comprising the following components in parts by weight: 1-5 parts of licorice extract, 2-6 parts of glycyrrhiza uralensis seed extract, and 1-5 parts of red clover extract, wherein the mass percentage of the licorice extract in the plant sunscreen composition is 10-50%; the licorice extract includes glycyrrhizic acid, glycyrrhizic acid isomers, and glycyrrhizic acid derivatives, and the glycyrrhizic acid derivatives include 2'-oxymethyl glycyrrhizic acid;
[0006] The structural formula of the glycyrrhizinone is shown in formula (I),
[0007]
[0008] The structural formula of the glycyrrhizinatedione isomers is shown in formula (II),
[0009]
[0010] The structural formula of the 2'-oxymethyl glycyrrhizinatedione is shown in formula (III),
[0011]
[0012] The 2'-oxymethyl glycyrrhizinatedione is a glycyrrhizinatedione in which the phenolic hydroxyl group on the benzene ring is replaced by an oxymethyl group.
[0013] The present invention can prepare a plant sunscreen composition with a high sun protection index, a wide sun protection band, not easy to change color, and mild and non-irritating to sensitive skin by the synergy of licorice extract, gray hair soybean seed extract, and red clover extract in specific weight parts. And the inventor found in the actual experimental process that glycyrrhizic acid dione can absorb short-wave ultraviolet light in the 250-280nm segment, and has a certain protective effect on UVB, while the isomers of glycyrrhizic acid dione can absorb long-wave ultraviolet light in the 360-390nm segment, and have a strong protective effect on UVA. Under light-proof (weak light) conditions, glycyrrhizic acid dione will be partially converted into its isomers, and the isomers will be partially converted into glycyrrhizic acid dione after seeing light (strong light). The derivatives of glycyrrhizic acid dione also have similar light protection effects and structural transformations, but the protective power is slightly lower and the stability is stronger. Therefore, when the licorice extract includes glycyrrhizic acid dione, glycyrrhizic acid dione isomers and glycyrrhizic acid dione derivatives, the plant sunscreen composition system has better stability and better sun protection effect.
[0014] Preferably, the total mass percentage of glycyrrhizin, glycyrrhizin isomers and 2'-oxymethyl glycyrrhizin in the licorice extract is ≥80%, and the total mass percentage of glycyrrhizin and glycyrrhizin isomers in the licorice extract is ≥60%.
[0015] Preferably, the total mass percentage of glycyrrhizin, glycyrrhizin isomers and 2'-oxymethyl glycyrrhizin in the licorice extract is ≥95%, and the total mass percentage of glycyrrhizin and glycyrrhizin isomers in the licorice extract is 85-90%.
[0016] During actual experiments, the inventors found that the total mass percentage of glycyrrhizin, glycyrrhizin isomers, and 2'-oxymethyl glycyrrhizin dione in the licorice extract further affects the stability and sunscreen effect of the plant sunscreen composition system. When the mass percentage of glycyrrhizin, glycyrrhizin isomers, and 2'-oxymethyl glycyrrhizin dione in the licorice extract is within the above range, while ensuring the stability of the plant sunscreen composition system, the sunscreen effect can be greatly improved, achieving a better comprehensive protection effect.
[0017] Preferably, the weight ratio of glycyrrhizin to glycyrrhizin isomers in the licorice extract is (20-30): (60-70).
[0018] The inventors found in actual experiments that when the weight ratio of glycyrrhizin to glycyrrhizin isomers in the licorice extract is (20-30): (60-70), the sun protection effect can be greatly improved, achieving a better comprehensive protection effect.
[0019] Preferably, the mass percentage of the liquorice extract in the botanical sunscreen composition is 30-40%.
[0020] During actual experiments, the inventors found that when the mass percentage of licorice extract in the plant sunscreen composition is within the above range, while ensuring the stability of the plant sunscreen composition system, the sunscreen effect can be greatly improved to achieve a better comprehensive protection effect.
[0021] In addition, the present invention provides a preparation method of the licorice extract, and the preparation method is as follows:
[0022] S1, extracting the licorice flower powder by mixing it with an ethanol aqueous solution and collecting the supernatant;
[0023] S2. After concentrating the supernatant under reduced pressure, purifying it by chromatography to obtain a purified solution, and drying it to a constant weight to obtain the licorice extract.
[0024] Preferably, the extraction in S1 adopts ultrasonic extraction, the mass volume ratio of the licorice flower powder and the ethanol aqueous solution is 1g: (5-20)mL, the volume fraction of the ethanol aqueous solution is 60-90%, the ultrasonic extraction temperature is 25-45°C, the ultrasonic extraction time is 20-60min, and the ultrasonic extraction power is 100-250w.
[0025] Further preferably, the mass volume ratio of the licorice flower powder and the ethanol aqueous solution is 1g:(13-15)mL, the ultrasonic extraction temperature is 30-35°C, the ultrasonic extraction time is 35-45min, and the ultrasonic extraction power is 180-220w.
[0026] The inventors found in actual experiments that the parameters extracted in S1 would affect the final yield of the licorice extract. When the above-mentioned preferred parameters were used, the final yield of the licorice extract was higher.
[0027] Preferably, the chromatography purification in S2 is performed using an LH-20 gel chromatography column, the column volume is 100-150 mL, the eluent is 60-90% ethanol by volume, and the flow rate is 0.5-2 mL / min.
[0028] When using LH-20 gel chromatography column for purification, good purification effect can be achieved when the column volume is 100-150mL.
[0029] Further preferably, the eluent is ethanol with a volume fraction of 75-85%, and the flow rate is 0.8-1.2 mL / min.
[0030] Preferably, in S2, the purified solution is collected in a range of 200-700 mL. Further preferably, the purified solution is collected in a range of 290-400 mL.
[0031] Preferably, the licorice extract prepared by the present invention needs to be stored at low temperature and away from light, and the storage time at low temperature and away from light is 12-72 hours.
[0032] Furthermore, the present invention provides use of the plant sunscreen composition in the preparation of cosmetics.
[0033] The present invention provides a cosmetic comprising the following components in percentage by mass: 7-20% of the plant sunscreen composition, 5-40% of a cosmetic base, and the balance being water; the cosmetic base comprising at least one of an emollient, a film former, a humectant, a thickener, a preservative, and an emulsifier.
[0034] Preferably, the present invention provides a sunscreen product comprising the following components in percentage by mass: 7-20% plant sunscreen composition, 0.5-15% emollient, 0.1-5% film former, 5-12% humectant, 0.1-0.5% thickener, 0.5-2% preservative, 1-5% emulsifier, and the balance being water.
[0035] Optionally, the emollient includes at least one of dicaprylyl carbonate, propylene glycol carbonate, and diisopropyl sebacate; and / or the film-forming agent includes at least one of trimethylsiloxysilicate and cyclopentasiloxane; and / or the moisturizer includes at least one of glycerin, 1,3-butylene glycol, and 1,2-pentanediol; and / or the thickener includes xanthan gum; and / or the preservative includes at least one of parahydroxyacetophenone and hexylene glycol; and / or the emulsifier includes at least one of polyglyceryl-10 oleate, lauryl PEG-9 polydimethylsiloxyethyl polydimethicone, and steareth-21.
[0036] The present invention provides a method for preparing the sunscreen product, which comprises the following steps:
[0037] The emulsifier, film former and emollient are mixed, heated to 40-50°C, and homogenized into a uniform oil phase. Then, a moisturizer, a thickener and water are added at 20-30°C for emulsification. After the emulsification is completed, the plant sunscreen composition and the preservative are added and stirred to obtain a sunscreen product.
[0038] Compared with the prior art, the beneficial effects of the present invention are as follows: the present invention can prepare a plant sunscreen composition with a high sun protection index, a wide sun protection band, not easy to change color, and mild and non-irritating to sensitive skin through the synergy of licorice extract, glycyrrhiza uralensis seed extract, and red clover extract in specific weight portions. In addition, the inventors found in the actual experimental process that glycyrrhizic acid dione can absorb short-wave ultraviolet light in the 250-280nm segment and has a certain protective effect on UVB, while the isomers of glycyrrhizic acid dione can absorb long-wave ultraviolet light in the 360-390nm segment and have a strong protective effect on UVA. Under light-proof (weak light) conditions, glycyrrhizic acid dione will be partially converted into its isomers, and the isomers will be partially converted into glycyrrhizic acid dione after seeing light (strong light). The derivatives of glycyrrhizic acid dione also have similar light protection effects and structural transformations, but the protection power is slightly lower and the stability is stronger. Therefore, when the licorice extract includes glycyrrhizin, glycyrrhizin isomers and glycyrrhizin derivatives, the plant sunscreen composition system has better stability and better sunscreen effect. BRIEF DESCRIPTION OF THE DRAWINGS
[0039] Figure 1 This is a component diagram of licorice extract-1 analyzed by liquid chromatography;
[0040] Figure 2 Mass spectrometry identification of glycyrrhizin in licorice extract-1;
[0041] Figure 3 This is a diagram of the isomers of glycyrrhizinatedione identified by mass spectrometry in licorice extract-1;
[0042] Figure 4 Mass spectrometry identification of glycyrrhizinatedone derivatives in licorice extract-1;
[0043] Figure 5 This is the image of glycyrrhizinone identified in Licorice Extract-1 by H NMR spectroscopy;
[0044] Figure 6 This is a diagram of isomers of glycyrrhizinatedione in licorice extract-1 identified by H NMR spectroscopy;
[0045] Figure 7 This is a diagram showing the identification of glycyrrhizinone derivatives in licorice extract-1 by H NMR spectroscopy;
[0046] Figure 8 Images of the red area on the face of volunteers in Performance Test 6 before and after using the blank application example and application example 1 products. DETAILED DESCRIPTION
[0047] In order to better illustrate the purpose, technical solutions and advantages of the present invention, the present invention will be further described below with reference to the accompanying drawings and specific examples. Its purpose is to understand the content of the present invention in detail, rather than to limit the present invention. All other embodiments obtained by ordinary technicians in this field without making creative work are within the scope of protection of the present invention. Unless otherwise specified, the experimental reagents and instruments designed for the implementation and comparative examples of the present invention are all commonly used ordinary reagents and instruments, which can be obtained from commercial channels. In the implementation and comparative examples, the experimental methods used are all conventional methods unless otherwise specified; and unless otherwise specified, the raw materials used in parallel experiments are from the same batch of raw materials.
[0048] Glycine max seed extract: trade name Neurophroline TM , purchased from Givaudan, Switzerland;
[0049] Trifolium pratense extract: product number L2-SCB2727, purchased from Zhenghe (Guangzhou) Biotechnology Co., Ltd.
[0050] Commercially available licorice extract: product number L2-CY2078, purchased from Zhenghe (Guangzhou) Biotechnology Co., Ltd.
[0051] White lupin seed extract: product number L2-SCB2347, purchased from Zhenghe (Guangzhou) Biotechnology Co., Ltd.
[0052] Lysimachia sibiricum extract: product number L2-SCB2335, purchased from Zhenghe (Guangzhou) Biotechnology Co., Ltd.
[0053] Alfalfa extract: product number shsw240803, purchased from Xi'an Shouhe Biotechnology Co., Ltd.
[0054] Licorice flower powder: collected from the Chengxitan licorice planting base in Huamachi Town, Yanchi District, from June to July 2023. The collected licorice flowers were dried at room temperature to constant weight, ground into powder, and passed through an 80-200 mesh sieve to obtain licorice flower powder;
[0055] The licorice flower powder used in the licorice extracts 1-28 of the present invention was collected from the Chengxitan licorice planting base in Huamachi Town, Yanchi from June to July 2023. The collected licorice flowers were dried at room temperature to constant weight, ground into powder, and passed through an 80-mesh sieve to obtain licorice flower powder;
[0056] The licorice extract is a homemade product, and the preparation method of the licorice extract is as follows:
[0057] S1. Mixing licorice flower powder with ethanol aqueous solution and then ultrasonically extracting, collecting the supernatant; the mass volume ratio of the licorice flower powder and ethanol aqueous solution is 1g: (5-20)mL, the volume fraction of the ethanol aqueous solution is 60-90%, the ultrasonic extraction temperature is 25-45°C, the ultrasonic extraction time is 20-60min, and the ultrasonic extraction power is 100-250w;
[0058] S2. After concentrating the supernatant under reduced pressure, purify it using an LH-20 gel chromatography column to obtain a purified solution, collect 200-700 mL of the purified solution, and dry it to constant weight to obtain the licorice extract; the column volume is 100-150 mL, the eluent is 60-90% ethanol by volume, and the flow rate is 0.5-2 mL / min.
[0059] Further preferably, in S1, the mass volume ratio of licorice flower powder and ethanol aqueous solution is 1g: (13-15)mL, the temperature of ultrasonic extraction is 30-35°C, the time of ultrasonic extraction is 35-45min, and the power of ultrasonic extraction is 180-220w.
[0060] Further preferably, in S2, the eluent is ethanol with a volume fraction of 75-85%, and the flow rate is 0.8-1.2 mL / min.
[0061] More preferably, the purified solution is collected in a 290-400 mL segment.
[0062] Licorice Extract-1~Licorice Extract-29
[0063] (1) A method for preparing licorice extract-1, comprising the following steps:
[0064] S1. Mixing licorice flower powder with ethanol aqueous solution and performing ultrasonic extraction, collecting the supernatant; the mass volume ratio of the licorice flower powder and ethanol aqueous solution is 1g:13mL, the volume fraction of the ethanol aqueous solution is 80%, the ultrasonic extraction temperature is 35°C, the ultrasonic extraction time is 40min, and the ultrasonic extraction power is 200w;
[0065] S2. After concentrating the supernatant under reduced pressure, purifying it using an LH-20 gel chromatography column to obtain a purified solution, collecting 290-400 mL of the purified solution, and drying it to constant weight to obtain the licorice extract; the column volume is 130 mL, the eluent is 80% by volume ethanol, and the flow rate is 1 mL / min;
[0066] S3. Store in a cool and dark place for 48 hours before use.
[0067] (2) A method for preparing licorice extract-2, comprising the following steps:
[0068] Compared with the preparation method of licorice extract-1, only the mass-to-volume ratio of licorice flower powder and ethanol aqueous solution in S1 is different, that is, the mass-to-volume ratio of licorice flower powder and ethanol aqueous solution is 1g:15mL; the remaining components, weight parts and preparation method are exactly the same as those of licorice extract-1.
[0069] (3) A method for preparing licorice extract-3, comprising the following steps:
[0070] Compared with the preparation method of licorice extract-1, only the mass-to-volume ratio of licorice flower powder and ethanol aqueous solution in S1 is different, that is, the mass-to-volume ratio of licorice flower powder and ethanol aqueous solution is 1g:5mL; the remaining components, weight parts and preparation method are exactly the same as those of licorice extract-1.
[0071] (4) A method for preparing licorice extract-4, comprising the following steps:
[0072] Compared with the preparation method of licorice extract-1, only the mass-to-volume ratio of licorice flower powder and ethanol aqueous solution in S1 is different, that is, the mass-to-volume ratio of licorice flower powder and ethanol aqueous solution is 1g:20mL; the remaining components, weight parts and preparation method are exactly the same as those of licorice extract-1.
[0073] (5) A method for preparing licorice extract-5, comprising the following steps:
[0074] Compared with the preparation method of Licorice Extract-1, only the temperature of the ultrasonic extraction in S1 is different, which is 30° C.; the remaining components, weight parts and preparation method are exactly the same as those of Licorice Extract-1.
[0075] (6) A method for preparing licorice extract-6, comprising the following steps:
[0076] Compared with the preparation method of Licorice Extract-1, only the temperature of the ultrasonic extraction in S1 is different, which is 25° C.; the remaining components, weight parts and preparation method are exactly the same as those of Licorice Extract-1.
[0077] (7) A method for preparing licorice extract-7, comprising the following steps:
[0078] Compared with the preparation method of Licorice Extract-1, only the temperature of the ultrasonic extraction in S1 is different, which is 45° C.; the remaining components, weight parts and preparation method are exactly the same as those of Licorice Extract-1.
[0079] (8) A method for preparing licorice extract-8, comprising the following steps:
[0080] Compared with the preparation method of Licorice Extract-1, only the power of the ultrasonic extraction in S1 is different, and the power of the ultrasonic extraction is 220w; the remaining components, weight parts and preparation method are exactly the same as those of Licorice Extract-1.
[0081] (9) A method for preparing licorice extract-9, comprising the following steps:
[0082] Compared with the preparation method of Licorice Extract-1, only the power of the ultrasonic extraction in S1 is different, and the power of the ultrasonic extraction is 250w; the remaining components, weight parts and preparation method are exactly the same as those of Licorice Extract-1.
[0083] (10) A method for preparing licorice extract-10, comprising the following steps:
[0084] Compared with the preparation method of Licorice Extract-1, only the power of the ultrasonic extraction in S1 is different, and the power of the ultrasonic extraction is 100w; the remaining components, weight parts and preparation method are exactly the same as those of Licorice Extract-1.
[0085] (11) A method for preparing licorice extract-11, comprising the following steps:
[0086] Compared with the preparation method of Licorice Extract-1, only the ultrasonic extraction time in S1 is different, which is 20 minutes; the remaining components, weight parts and preparation method are exactly the same as those of Licorice Extract-1.
[0087] (12) A method for preparing licorice extract-12, comprising the following steps:
[0088] Compared with the preparation method of Licorice Extract-1, only the ultrasonic extraction time in S1 is different, which is 35 minutes; the remaining components, weight parts and preparation method are exactly the same as those of Licorice Extract-1.
[0089] (13) A method for preparing licorice extract-13, comprising the following steps:
[0090] Compared with the preparation method of Licorice Extract-1, only the ultrasonic extraction time in S1 is different, which is 60 minutes; the remaining components, weight parts and preparation method are exactly the same as those of Licorice Extract-1.
[0091] (14) A method for preparing licorice extract-14, comprising the following steps:
[0092] Compared with the preparation method of Licorice Extract-1, only the eluent in S2 is different, and the eluent is 75% ethanol by volume; the remaining components, weight parts and preparation method are exactly the same as those of Licorice Extract-1.
[0093] (15) A method for preparing licorice extract-15, comprising the following steps:
[0094] Compared with the preparation method of Licorice Extract-1, only the eluent in S2 is different, and the eluent is 85% ethanol by volume; the remaining components, weight parts and preparation method are exactly the same as those of Licorice Extract-1.
[0095] (16) A method for preparing licorice extract-16, comprising the following steps:
[0096] Compared with the preparation method of Licorice Extract-1, only the eluent in S2 is different, and the eluent is 60% ethanol by volume; the remaining components, weight parts and preparation method are exactly the same as those of Licorice Extract-1.
[0097] (17) A method for preparing licorice extract-17, comprising the following steps:
[0098] Compared with the preparation method of Licorice Extract-1, only the eluent in S2 is different, which is 90% ethanol by volume; the remaining components, weight parts and preparation method are exactly the same as those of Licorice Extract-1.
[0099] (18) A method for preparing licorice extract-18, comprising the following steps:
[0100] Compared with the preparation method of Licorice Extract-1, only the flow rate of the eluent in S2 is different, which is 1.2 mL / min; the remaining components, weight parts and preparation method are exactly the same as those of Licorice Extract-1.
[0101] (19) A method for preparing licorice extract-19, comprising the following steps:
[0102] Compared with the preparation method of Licorice Extract-1, only the eluent flow rate in S2 is different, which is 0.8 mL / min; the remaining components, weight parts and preparation method are exactly the same as those of Licorice Extract-1.
[0103] (20) A method for preparing licorice extract-20, comprising the following steps:
[0104] Compared with the preparation method of Licorice Extract-1, only the flow rate of the eluent in S2 is different, which is 0.5 mL / min; the remaining components, weight parts and preparation method are exactly the same as those of Licorice Extract-1.
[0105] (21) A method for preparing licorice extract-21, comprising the following steps:
[0106] Compared with the preparation method of Licorice Extract-1, only the flow rate of the eluent in S2 is different, which is 2 mL / min; the remaining components, weight parts and preparation method are exactly the same as those of Licorice Extract-1.
[0107] (22) A method for preparing licorice extract-22, comprising the following steps:
[0108] Compared with the preparation method of Licorice Extract-1, only the eluent and flow rate in S2 are different. The eluent is 60% ethanol by volume and the flow rate is 0.5 mL / min. The remaining components, weight parts and preparation method are exactly the same as those of Licorice Extract-1.
[0109] (23) A method for preparing licorice extract-23, comprising the following steps:
[0110] Compared with the preparation method of Licorice Extract-1, only the eluent and flow rate in S2 are different. The eluent is 90% ethanol by volume and the flow rate is 2 mL / min. The remaining components, weight parts and preparation method are exactly the same as those of Licorice Extract-1.
[0111] (24) A method for preparing licorice extract-24, comprising the following steps:
[0112] Compared with the preparation method of Licorice Extract-1, the only difference is the collection of the purified solution in S2, which is the 200-370 mL segment of the purified solution; the remaining components, weight parts and preparation method are exactly the same as those of Licorice Extract-1.
[0113] (25) A method for preparing licorice extract-25, comprising the following steps:
[0114] Compared with the preparation method of Licorice Extract-1, the only difference is the collection of the purified solution in S2, which is the 320-700 mL section of the purified solution; the remaining components, weight parts and preparation method are exactly the same as those of Licorice Extract-1.
[0115] (26) A method for preparing licorice extract-26, comprising the following steps:
[0116] Compared with the preparation method of Licorice Extract-1, only the low-temperature and dark storage time in S3 is different. After being stored at low temperature and dark for 0 hours, it is selected; the remaining components, weight parts and preparation method are exactly the same as Licorice Extract-1.
[0117] (27) A method for preparing licorice extract-27, comprising the following steps:
[0118] Compared with the preparation method of Licorice Extract-1, only the low-temperature and dark storage time in S3 is different. It is selected after being stored at low temperature and dark for 12 hours; the remaining components, weight parts and preparation method are exactly the same as Licorice Extract-1.
[0119] (28) A method for preparing licorice extract-28, comprising the following steps:
[0120] Compared with the preparation method of Licorice Extract-1, only the low-temperature and dark storage time in S3 is different. It is selected after being stored at low temperature and dark for 72 hours; the remaining components, weight parts and preparation method are exactly the same as Licorice Extract-1.
[0121] (29) A method for preparing licorice extract-29, comprising the following steps:
[0122] Compared with the preparation method of licorice extract-1, only the selection of licorice flower powder in S1 is different. The licorice flower powder selected was collected from the Chengxitan licorice planting base in Huamachi Town, Yanchi from June to July 2023. The collected licorice flowers were dried to constant weight at room temperature, ground into powder, and passed through a 150-mesh sieve to obtain licorice flower powder.
[0123] 1. Test Method: Accurately weigh 1 mg of licorice extract and dissolve it in 10 mL of methanol. After filtering through a 0.22 μm filter membrane, the content of the components in the extract was determined using LC-MS / MS. The chromatographic column used was a C18 column (100 mm × 2.1 mm, 3 μM), the mobile phase was 60% methanol, the flow rate was 0.5 mL / min, and the sample volume was 10 μL. The content of each component was calculated according to the following formula: Percentage of each component = Peak area of single component / Total peak area * 100%.
[0124] Figure 1-4 They are all targeting licorice extract-1, Figure 1 This is a component diagram of licorice extract-1 analyzed by liquid chromatography. Figure 2-3 For the mass spectrometric identification of licorice extract-1, Figure 5-7 This is a diagram for identifying glycyrrhizic acid dione, its isomers, and its derivatives in licorice extract-1 using hydrogen nuclear magnetic resonance spectroscopy. Figure 5-7 The identification was performed by H NMR spectroscopy after the single compound was isolated and purified from Licorice Extract-1 using gel chromatography.
[0125] from Figure 1 It can be seen that the licorice extract 1 mainly contains three active ingredients, glycyrrhizic acid dione: isomers: derivatives = 23:67:7, with a purity of 97%; Figure 2 It can be seen that the molecular weight of the purified glycyrrhizinatedone is 272.97; Figure 3 It can be seen that the molecular weight of the purified isomers of glycyrrhizinatedione is 272.98; Figure 4It can be seen that the molecular weight of the purified glycyrrhizinated derivative is 287.00; Figure 5-7 It can be seen that the three purified compounds were identified as glycyrrhizinone, an isomer of glycyrrhizinone, and 2'-oxymethylglycyrrhizinone, respectively.
[0126] Table 1
[0127]
[0128]
[0129] As shown in Table 1, the licorice extracts-1 to licorice extracts-13 differ only in the mass volume ratio of licorice flower powder to ethanol aqueous solution, extraction temperature, extraction time, and extraction power during the extraction process in step S1, which affect the final yield of the licorice extract.
[0130] Licorice extracts 14 to 23 differed only in the volume fraction and flow rate of the eluent during the chromatography purification process in step S2, which affected the proportions of glycyrrhizic acid dione, glycyrrhizic acid dione isomers, and glycyrrhizic acid dione derivatives in the final licorice extracts. However, in licorice extracts 14 to 23, the ratio of glycyrrhizic acid dione and glycyrrhizic acid dione isomers was basically stable.
[0131] Licorice Extracts 24 and 25 differ only in the fraction of the solution collected after the chromatography purification step S2. Collecting the purified solution in the early stages introduces impurities, while collecting the purified solution in the later stages increases the proportion of derivatives. Furthermore, different fractions of the solution collected also lead to varying yields of the final licorice extract. The ratios of glycyrrhizinone and glycyrrhizinone isomers in Glycyrrhizinone Extracts 24 and 25 are generally stable.
[0132] The only difference between licorice extract-26 and licorice extract-28 is the low-temperature dark storage time in step S3. The length of the low-temperature dark storage time will affect the ratio of glycyrrhizin and glycyrrhizin isomers. After 48 hours of low-temperature dark storage, the components in the licorice extract tend to be stable.
[0133] Licorice Extract-29 is made by using licorice flower powder with different mesh sizes during the extraction process, which has little effect on the final effect.
[0134] Examples and Comparative Examples
[0135] The present invention provides a plant sunscreen composition. The components and weight portions of the plant sunscreen composition are shown in Tables 2-3. The preparation method of the plant sunscreen composition comprises the following steps: licorice extract, ginkgo seed extract, and red clover extract are weighed according to weight, and no relevant components are added if not present, and the mixture is uniformly mixed to obtain the plant sunscreen composition.
[0136] Table 2
[0137]
[0138]
[0139] Table 3
[0140]
[0141]
[0142] Application Examples
[0143] Application Examples 1-22, Comparative Application Examples 1-10, and Blank Application Examples of the present invention provide a sunscreen product, the components (mass percentage) of which are shown in Table 4; wherein the plant sunscreen compositions in Application Examples 1-22 are respectively the plant sunscreen compositions prepared in Examples 1-22; the plant sunscreen compositions in Comparative Application Examples 1-10 are respectively the plant sunscreen compositions prepared in Comparative Examples 1-10; for example, the plant sunscreen composition used in Application Example 1 is the plant sunscreen composition in Example 1, the plant sunscreen composition used in Application Example 5 is the plant sunscreen composition in Example 5, the plant sunscreen composition used in Application Example 22 is the plant sunscreen composition in Example 22, and the same applies to other examples; the plant sunscreen composition used in Application Example 23 is the plant sunscreen composition prepared in Example 1.
[0144] Table 4
[0145]
[0146]
[0147] The preparation method of the sunscreen product provided in the application example is:
[0148] The emulsifier, film former and emollient are mixed, heated to 45°C, and homogenized into a uniform oil phase. Then, a moisturizer, a thickener and water are added at 25°C for emulsification. After the emulsification is completed, a plant sunscreen composition and a preservative are added and stirred to obtain a sunscreen product.
[0149] Performance Test-1
[0150] The effect examples of the present invention verify the anti-ultraviolet performance of the plant sunscreen compositions prepared in Examples 1-22 and Comparative Examples 1-10.
[0151] 1 mg of the plant sunscreen composition was dissolved in 1 mL of methanol, 200 μL of the sample was added to a 96-well plate, and the ultraviolet absorption values in the UVA (320-400 nm) and UVB (280-320 nm) bands were detected using a full-wavelength microplate reader (Thermo Fisher, Skyhigh). The ultraviolet absorption value of a certain band is the average ultraviolet absorption value within the band; the results are shown in Table 5.
[0152] Table 5
[0153]
[0154]
[0155] As can be seen from the above table, the UVA (320-400 nm) absorbance and UVB (280-320 nm) absorbance of the plant sunscreen composition prepared in the examples of the present invention are both above 1.1.
[0156] Examples 1-2 of the present application were used to test the sun protection effect of licorice extracts with different yields. The licorice extracts 1-13 of the present invention only differed in the mass volume ratio of licorice flower powder to ethanol aqueous solution, the extraction temperature, the extraction time, and the extraction power during the extraction process of step S1, which affected the yield of the final licorice extract. Examples 1-2 of the present application were used to test the sun protection effect of licorice extracts with different yields. There was almost no difference in the sun protection effect. Therefore, the other licorice extracts with different yields are not described one by one.
[0157] Example 3-17 of the present invention uses licorice extract-14 to licorice extract-28:
[0158] In Examples 1 and 3-12, the proportions of glycyrrhizin, glycyrrhizin isomers, and glycyrrhizin derivatives in the licorice extracts varied. In licorice extracts 14-23, the ratios of glycyrrhizin and glycyrrhizin isomers were essentially stable. The results showed that when the total mass percentage of glycyrrhizin, glycyrrhizin isomers, and 2'-oxymethylglycyrrhizin in the licorice extracts was ≥95%, and when the total mass percentage of glycyrrhizin and glycyrrhizin isomers in the licorice extracts was 85-90%, the sunscreen effect was better.
[0159] In Examples 1 and 13-14, the only difference was the collection period after chromatographic purification in step S2. Collecting the purified solution in the early stages introduced other impurities, while collecting the purified solution in the later stages increased the proportion of derivatives. Furthermore, different collection periods also resulted in different yields of the final licorice extract. Results showed that collecting the purified solution in the 290-400 mL range resulted in better sun protection.
[0160] Examples 1 and 15-17 differed only in the ratio of glycyrrhizin and glycyrrhizin isomers. The results showed that when the weight ratio of glycyrrhizin and glycyrrhizin isomers in the licorice extract was (20-30): (60-70), the sunscreen effect could be maximized, achieving better overall protection. When the ratio was outside the preferred range, Examples 15-16 had slightly lower UVA absorbance and a slightly narrower sunscreen width, resulting in slightly worse sunscreen effectiveness compared to Example 1.
[0161] Example 18 of the present invention uses licorice extract-29, and only the licorice flower powder in S1 is different. The licorice extract finally obtained is the same as that in Example 1, and the sun protection effect of Example 18 is similar to that of Example 1.
[0162] In Examples 1 and 19-22, only the weight proportions of licorice extract, glycyrrhiza uralensis seed extract, and clover extract are different. When the total mass percentage of licorice extract in the plant sunscreen composition is 30-40%, the sunscreen band is wider and the sunscreen effect is better.
[0163] In Comparative Examples 1-3, the weight percentages of licorice extract, ginkgo seed extract, and red clover extract are not within the specific scope of the present invention. Comparative Examples 4-7 do not contain any of licorice extract, ginkgo seed extract, and red clover extract, and are replaced with conventional extracts having a certain effect. Comparative Examples 8-10 do not contain any of licorice extract, ginkgo seed extract, and red clover extract. As can be seen from the table above, the plant sunscreen compositions prepared in Comparative Examples 1-2, 4-6, and 9-10 have either very poor UVA (320-400nm) absorbance or very poor UVB (280-320nm) absorbance, resulting in a narrow band of the sunscreen system and poor sunscreen effect. The plant sunscreen compositions prepared in Comparative Examples 3 and 7-8 have very poor UVA (320-400nm) absorbance and UVB (280-320nm) absorbance, and extremely poor sunscreen effect.
[0164] Performance Test-2
[0165] The effect examples of the present invention verify the cell protection performance of the plant sunscreen compositions prepared in Examples 1-22 and Comparative Examples 1-10 under ultraviolet irradiation.
[0166] The sample (1 mg / mL) was dissolved in DMEM medium (Gibco, 2105341) and co-cultured with human keratinocytes HaCaT. The cells were exposed to UVA and UVB irradiation at a dose of 200 mJ / cm 2 , continued to culture for 48 hours, and used a cell counter to detect cell viability. The results are shown in Table 6.
[0167] Table 6
[0168]
[0169]
[0170]
[0171] As can be seen from the above table, the survival rate of UVA-damaged cells and the survival rate of UVB-damaged cells of the plant sunscreen composition prepared in the embodiment of the present invention are both above 50%.
[0172] Examples 1-2 of the present application were used to test the cell viability of licorice extracts with different yields. The licorice extracts 1-13 of the present invention differed only in the mass volume ratio of licorice flower powder to ethanol aqueous solution, the extraction temperature, the extraction time, and the extraction power during the extraction process in step S1, which affected the final yield of the licorice extract. Examples 1-2 of the present application were used to test the cell viability of licorice extracts with different yields, and there was almost no difference. Therefore, the other licorice extracts with different yields are not described one by one.
[0173] Example 3-17 of the present invention uses licorice extract-14 to licorice extract-28:
[0174] In Examples 1 and 3-12, the proportions of glycyrrhizin, glycyrrhizin isomers, and glycyrrhizin derivatives in the licorice extracts varied. In licorice extracts 14-23, the ratios of glycyrrhizin and glycyrrhizin isomers were essentially stable. The results showed that when the total mass percentage of glycyrrhizin, glycyrrhizin isomers, and 2'-oxymethylglycyrrhizin in the licorice extracts was ≥95%, and when the total mass percentage of glycyrrhizin and glycyrrhizin isomers in the licorice extracts was 85-90%, the cell survival rate was higher.
[0175] In Examples 1 and 13-14, different sections of the solution collected after chromatographic purification in step S2 resulted in the introduction of impurities in the early stages of the purified solution, while collecting the solution in the later stages increased the proportion of derivatives. Furthermore, different sections of the solution collected also resulted in different yields of the final licorice extract. Results showed that collecting the purified solution between 290 and 400 mL resulted in higher cell survival rates.
[0176] In Examples 1 and 15-17, the ratio of glycyrrhizin and glycyrrhizin isomers was different. The results showed that when the weight ratio of glycyrrhizin and glycyrrhizin isomers in the licorice extract was (20-30): (60-70), the cell survival rate was higher, achieving a better overall protection effect. When the ratio was not within the preferred range, the survival rate of UVA-damaged cells in Examples 15-16 was too low, the sun protection width was slightly narrow, and the sun protection effect was slightly worse than that in Example 1.
[0177] Example 18 of the present invention uses licorice extract-29, and only the licorice flower powder in S1 is different. The final licorice extract obtained is the same as that in Example 1. The survival rate of damaged cells in Example 18 is similar to that in Example 1.
[0178] In Examples 1 and 19-22, only the weight proportions of licorice extract, glycyrrhiza uralensis seed extract, and clover extract are different. When the total mass percentage of licorice extract in the plant sunscreen composition is 30-40%, the cell survival rate is higher, the sunscreen band is wider, and the sunscreen effect is better.
[0179] In Comparative Examples 1-3, the weight percentages of licorice extract, ginkgo seed extract, and red clover extract are not within the specific scope of the present invention. Comparative Examples 4-7 do not contain any of licorice extract, ginkgo seed extract, and red clover extract, and are replaced with conventional extracts with a certain effect. Comparative Examples 8-10 do not contain any of licorice extract, ginkgo seed extract, and red clover extract. As can be seen from the table above, the plant sunscreen compositions prepared in Comparative Examples 1-2, 4-6, and 9-10 either have a very poor survival rate of UVA-damaged cells or a very poor survival rate of UVB-damaged cells, resulting in a narrow band of the sunscreen system and poor sunscreen effect. The plant sunscreen compositions prepared in Comparative Examples 3 and 7-8 have very poor survival rates of UVA-damaged cells and UVB-damaged cells, and their sunscreen effects are extremely poor.
[0180] Performance Test-3
[0181] The effectiveness examples of the present invention verify the stability of the sunscreen products prepared by Application Examples 1-23, Comparative Application Examples 1-10 and Blank Application Examples.
[0182] High temperature stability test: Place the test sample in a 40°C constant temperature box for 1 month and observe the color change of the sample.
[0183] Light stability test: Place the test sample in a light aging box for 12 hours and observe the color change of the sample.
[0184] After testing, the plant sunscreen compositions provided by the effectiveness verification application examples 1-23, comparative application examples 1-10 and blank application examples of the present invention showed no discoloration after stability testing, and the products had strong stability.
[0185] Performance Test-4
[0186] The effectiveness examples of the present invention verify the safety performance of the sunscreen products prepared by Application Examples 1-23, Comparative Application Examples 1-10 and Blank Application Examples.
[0187] Thirty volunteers (15 men and 15 women, aged 20-50 years) were recruited for a closed patch test. Equal amounts (0.020 mL to 0.025 mL) of the test sample were placed in a specific patch tester. The patch was then applied to the volunteer's arm with hypoallergenic tape, gently pressed to evenly adhere to the skin, and left for 24 hours. A blank control group received distilled water. After 24 hours, the patch tester was removed, and skin reactions were observed 0.5, 24, and 48 hours later, with the results recorded. The severity of adverse skin reactions is shown in Table 7 below.
[0188] Table 7
[0189]
[0190] After testing, the plant sunscreen compositions provided by Application Examples 1-23, Comparative Application Examples 1-10 and Blank Application Examples of the present invention all showed negative reactions after human patch tests, indicating that they are safe and non-irritating to human skin.
[0191] Performance Test-5
[0192] The effectiveness examples of the present invention verify the sunscreen performance of the sunscreen products prepared by Application Examples 1-23, Comparative Application Examples 1-10 and Blank Application Examples.
[0193] SPF value test: The test was conducted in accordance with the requirements of the "Safety Technical Specifications for Cosmetics" (2015 edition). 170 volunteers aged 32-60 were selected and divided into 34 groups, with 5 people in each group. The minimum erythema dose (MED) of the subjects' skin to ultraviolet radiation was predicted and the ultraviolet radiation dose was adjusted. 2 For normal skin area, (2.00±0.05)mg / cm 2 Apply the test substance or a blank sample evenly to the above-mentioned area using a specific dosage. Then, select the irradiation dose according to the standard and perform irradiation in three scenarios: ① No test substance applied to the subject's skin; ② Apply a control product (SPF 16.1±2.4, prepared according to the standard formula for high SPF standard P2 in the 2015 edition of the "Safety Technical Specifications for Cosmetics"); and ③ Apply the test substance. Observe the experimental results after 24 hours, and record the MED values for each of the three scenarios.
[0194] SPF value calculation method: The SPF value of the test substance or blank control protecting a single subject is expressed by the following formula: SPFi = MED value of protected skin / MED value of unprotected skin;
[0195] Calculate the arithmetic mean of the SPF values of all subjects protected by the test object, and round the result to one decimal place.
[0196] PFA value test: The test was conducted in accordance with the requirements of the "Safety Technical Specifications for Cosmetics" (2015 edition). 170 subjects aged 32 to 60 were selected and divided into 34 groups, with 5 subjects in each group. The minimum melanin dose (MPPD) of the subjects' skin was predicted to adjust the UV dose. A spot no less than 30 cm from the back of the subject was selected. 2 For normal skin area, (2.00±0.05)mg / cm 2 Apply the test substance or a blank sample evenly to the above-mentioned area using a specific dosage. Then, select the UVA exposure dose according to the specification and perform the exposure in three different conditions: ① No test substance applied to the subject's skin; ② Apply a control substance (PFA value 12.7±2.0, prepared according to the S2 formulation in ISO 24442); and ③ Apply the test substance. Observe the experimental results after 2-4 hours, and record the MPPD values for each of the three conditions.
[0197] PFA value calculation method: The PFA value of a single subject protected by the test substance or reference substance is expressed as follows: PFAi = MPPD value of protected skin / MPPD value of unprotected skin;
[0198] Calculate the arithmetic mean of the PFA values of all subjects protected by the test object, and round the result to one decimal place.
[0199] The test results are shown in Table 8.
[0200] Table 8
[0201]
[0202]
[0203] As can be seen from the above table, when the plant sunscreen composition prepared in the embodiment of the present invention is prepared into a sunscreen product, the SPF value is above 40 and the PFA value is above 12.
[0204] Application Examples 1-2 of this application use different licorice extracts. The only difference is the extraction yield. There is almost no difference in the sun protection test of licorice extracts with different yields. Therefore, the other licorice extracts with different yields are not described one by one.
[0205] In Application Examples 1 and 3-12, only the licorice extracts differed. The proportions of glycyrrhizic acid dione, glycyrrhizic acid dione isomers, and glycyrrhizic acid dione derivatives in the licorice extracts were different, and the ratios of glycyrrhizic acid dione and glycyrrhizic acid dione isomers were generally stable. The results showed that when the total mass percentage of glycyrrhizic acid dione, glycyrrhizic acid dione isomers, and 2'-oxymethyl glycyrrhizic acid dione in the licorice extracts was ≥95%, and when the total mass percentage of glycyrrhizic acid dione and glycyrrhizic acid dione isomers in the licorice extracts was 85-90%, the SPF value and PFA value were higher.
[0206] Application Examples 1 and 13-14 differ only in the licorice extracts. The collection of the solution after chromatographic purification in step S2 differs. Collecting the purified solution in the early stages introduces impurities, while collecting the purified solution in the later stages increases the proportion of derivatives. Furthermore, different collection stages also lead to different yields of the final licorice extract. Results show that collecting the purified solution in the 290-400 mL range yields higher SPF and PFA values.
[0207] Application Examples 1 and 15-17 differ only in the ratio of glycyrrhizin and glycyrrhizin isomers. The results show that when the weight ratio of glycyrrhizin and glycyrrhizin isomers in the licorice extract is (20-30): (60-70), the SPF and PFA values are higher, achieving better overall protection. When the ratio is not within the preferred range, the PFA values of Application Examples 15-16 are slightly lower, and the sun protection effect is slightly worse than that of Application Example 1.
[0208] Application Example 18 of the present invention uses licorice extract-29, and the licorice flower powder in S1 is selected differently. The final licorice extract obtained is the same as that in Application Example 1. The survival rate of damaged cells in Application Example 18 is similar to that in Application Example 1.
[0209] Application Examples 1 and 19-22 differ only in the weight proportions of licorice extract, glycyrrhiza uralensis seed extract, and clover extract. When the total mass percentage of licorice extract in the plant sunscreen composition is 30-40%, the SPF value and PFA value are higher, and the sunscreen effect is better.
[0210] In Comparative Application Examples 1-3, the weight percentages of licorice extract, ginkgo seed extract, and red clover extract are not within the specific scope of the present invention. Comparative Application Examples 4-7 do not contain any of licorice extract, ginkgo seed extract, and red clover extract, and are replaced with conventional extracts with a certain effect. Comparative Application Examples 8-10 do not contain any of licorice extract, ginkgo seed extract, and red clover extract. As can be seen from the table above, the plant sunscreen compositions prepared in Comparative Application Examples 1-2, 4-6, and 9-10 either have very poor SPF values or poor PFA values, resulting in a narrow band of the sunscreen system and poor sunscreen effect. The plant sunscreen compositions prepared in Comparative Application Examples 3 and 7-8 have very poor SPF and PFA values, and their sunscreen effects are extremely poor.
[0211] Performance Test-6
[0212] The effectiveness examples of the present invention verify the repairing and soothing effects of the sunscreen products prepared by Application Examples 1-23, Comparative Application Examples 1-10 and Blank Application Examples.
[0213] The test process involved selecting 170 volunteers aged 18-45. On the day of their visit, they did not apply any skincare products. After cleansing their faces, they sat quietly in a constant temperature and humidity room at 21±1°C and 50±10% humidity for 30 minutes. Facial images were taken using Visia-7, and image analysis of the red zone images was performed to obtain the a* value. A transepidermal water loss probe was used to measure the skin's transepidermal water loss. The TM Hex (Courage + Khazaka) test measures initial facial TEWL. Subjects were randomly divided into 34 groups, each with 5 participants. Each group randomly applied sunscreen products, including the blank application, application examples 1-23, and control application examples 1-10, to their entire faces. TEWL testing and Visia-7 photography were performed on days 7 and 14. Improvements in TEWL and a* values were analyzed at days 0, 7, and 14. Improvement was expressed as the improvement rate for each value, calculated as follows:
[0214] Improvement rate relative to the initial value = (X 使用前 -X 使用后 ) / X 使用前 ×100%;
[0215] The transepidermal water loss (TEWL) value is a commonly used indicator reflecting the barrier function of the stratum corneum. The lower the TEWL value, the better the skin barrier function and the better the repair effect of the product. The redness a* value reflects the degree of skin sensitivity and redness. The lower the a* value, the lower the skin stress level and the better the soothing effect of the product.
[0216] The test results are shown in Table 9;
[0217] Table 9
[0218]
[0219]
[0220] As can be seen from the table above, when the plant sunscreen composition prepared in the embodiment of the present invention is prepared into a sunscreen product, the TEWL improvement rate is more than 13% in 7 days and more than 24% in 14 days; the a* improvement rate is more than 10% in 7 days and more than 17% in 14 days, and has good repair and soothing effects. Figure 8 For volunteers, use blank application examples and application example 1 product before and after facial red area pictures. Figure 8 It can be seen that the degree of facial redness of the volunteers was significantly reduced after using the product of Application Example 1. The plant sunscreen composition provided by the present invention has a good soothing effect when prepared into a sunscreen product.
[0221] Application Examples 1-2 of this application use different licorice extracts. The only difference is the extraction yield. The repair and soothing tests on licorice extracts with different yields show almost no difference. Therefore, the other licorice extracts with different yields are not described one by one.
[0222] In Application Examples 1 and 3-12, only the licorice extracts differed. The proportions of glycyrrhizin, glycyrrhizin isomers, and glycyrrhizin derivatives in the licorice extracts were different, and the ratios of glycyrrhizin and glycyrrhizin isomers were generally stable. The results showed that when the total mass percentage of glycyrrhizin, glycyrrhizin isomers, and 2'-oxymethylglycyrrhizin in the licorice extract was ≥95%, and when the total mass percentage of glycyrrhizin and glycyrrhizin isomers in the licorice extract was 85-90%, the repair and soothing effects were better.
[0223] In Application Examples 1 and 13-14, the selection of the solution collection section after chromatographic purification in step S2 differed. Collecting the purified solution in the early stages introduced impurities, while collecting the purified solution in the later stages increased the proportion of derivatives. Furthermore, different collection sections also resulted in different yields of the final licorice extract. Results showed that collecting the purified solution between 290 and 400 mL resulted in greater repair and soothing effects.
[0224] In Application Examples 1 and 15-17, the ratios of glycyrrhizin and glycyrrhizin isomers varied. The results showed that a weight ratio of glycyrrhizin to glycyrrhizin isomers of (20-30):(60-70) in the licorice extract resulted in better repair and soothing effects. When the ratio was outside the optimal range, the repair and soothing effects were slightly poorer.
[0225] Application Example 18 of the present invention uses licorice extract-29, and the licorice flower powder in S1 is selected differently. The licorice extract finally obtained is the same as that in Application Example 1. The repairing and soothing effects of Application Example 18 are similar to those of Application Example 1.
[0226] In Application Examples 1 and 19-22, the weight proportions of licorice extract, ginkgo seed extract, and red clover extract are different. When the total mass percentage of licorice extract in the plant sunscreen composition is 30-40%, the repairing and soothing effects are better.
[0227] In Comparative Application Examples 1-3, the weight percentages of licorice extract, ginkgo seed extract, and red clover extract were outside the specific range of the present invention. Comparative Application Examples 4-7 did not contain any of the licorice extract, ginkgo seed extract, and red clover extract, and were replaced with conventional extracts with a certain effect. Comparative Application Examples 8-10 did not contain any of the licorice extract, ginkgo seed extract, and red clover extract. As can be seen from the table above, the products prepared in the comparative examples had extremely poor repair and soothing effects.
[0228] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention and are not intended to limit the scope of protection of the present invention. Although the present invention has been described in detail with reference to preferred embodiments, those skilled in the art should understand that the technical solutions of the present invention may be modified or replaced by equivalents without departing from the essence and scope of the technical solutions of the present invention.
Claims
1. A plant sunscreen composition, characterized in that: The plant sunscreen composition comprises the following components in parts by weight: 1-5 parts of licorice extract, 2-6 parts of ginkgo seed extract, and 1-5 parts of red clover extract. The mass percentage of the licorice extract in the plant sunscreen composition is 10-50%. The preparation method of the licorice extract is as follows: S1. Extracting the liquorice flower powder by mixing it with an ethanol aqueous solution and collecting the supernatant; wherein the mass volume ratio of the liquorice flower powder to the ethanol aqueous solution is 1 g: (5-20) mL, the volume fraction of the ethanol aqueous solution is 60-90%, the ultrasonic extraction temperature is 25-45° C., the ultrasonic extraction time is 20-60 min, and the ultrasonic extraction power is 100-250 W; S2. After concentrating the supernatant under reduced pressure, chromatographically purifying the supernatant using an LH-20 gel chromatography column to obtain a purified solution, collecting 200-700 mL of the purified solution, and drying to constant weight to obtain the licorice extract; The column volume is 100-150 mL, the eluent is 60-90% ethanol by volume, and the flow rate is 0.5-2 mL / min; The licorice extract includes glycyrrhizin, glycyrrhizin isomers and glycyrrhizin derivatives, and the glycyrrhizin derivatives include 2'-oxymethyl glycyrrhizin; The structural formula of the glycyrrhizinone is shown in formula (I), The structural formula of the glycyrrhizinatedione isomers is shown in formula (II), The structural formula of the 2'-oxymethyl glycyrrhizinatedione is shown in formula (III), 2. The plant sunscreen composition according to claim 1, wherein The total mass percentage of glycyrrhizin, glycyrrhizin isomers and 2'-oxymethyl glycyrrhizin in the licorice extract is greater than or equal to 95%, and the total mass percentage of glycyrrhizin and glycyrrhizin isomers in the licorice extract is 85-90%.
3. The plant sunscreen composition according to claim 2, wherein The weight ratio of glycyrrhizinone to glycyrrhizinone isomers in the licorice extract is (20-30): (60-70).
4. The plant sunscreen composition according to claim 1, wherein The total mass percentage of the liquorice extract in the plant sunscreen composition is 30-40%.
5. Use of the plant sunscreen composition according to any one of claims 1 to 4 in the preparation of cosmetics.
6. A cosmetic, characterized in that: The cosmetic comprises the following components in percentage by mass: 7-20% of the plant-based sunscreen composition according to any one of claims 1 to 4, 5-40% of a cosmetic base, and the balance being water; the cosmetic base comprising at least one of an emollient, a film former, a humectant, a thickener, a preservative, and an emulsifier.
Citation Information
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