A plant extract multi-effect composition and its preparation method and application
By combining the extracts of ginkgo leaves, gardenia fruit and blackberry with extracts of pomelo peel and white willow bark, a plant-extract multi-effect composition is formed, which solves the skin problems and inhibition caused by chemical preservatives in traditional cosmetics. The problem of insufficient bacterial effect has achieved efficient, safe and natural anticorrosion effects.
Patent Information
- Application Number
- CN202410552603.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-05-07
- Publication Date
- 2025-02-25
- Estimated Expiration
- 2044-05-07
AI Technical Summary
Traditional chemical preservatives used in existing cosmetics are prone to cause skin problems and have limited antibacterial effects, making it difficult to meet the needs of modern cosmetics for natural, safe and efficient anti-corrosion.
By using plant extracts such as ginkgo leaf extract, gardenia fruit extract and blackberry extract as antibacterial agents, combined with pomelo peel extract and white willow bark extract as synergistic agents, a plant extraction multi-effect effect is formed. Compositions used in cosmetics as natural preservatives.
The plant-extracted multi-effect composition significantly improves the antibacterial and antioxidant effects, has the ability to quickly and long-term antibacterial, and is low in dosage, safe and effective, naturally low irritation, and will not cause skin allergic reactions.
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Abstract
Description
Technical Field
[0001] The invention belongs to the field of cosmetics, and in particular relates to a plant extract multi-effect composition and a preparation method and application thereof. Background Art
[0002] In recent years, with the improvement of living standards, people pay more and more attention to the maintenance of their skin, and the use of cosmetics and skin care products has become more frequent. Preservatives are an indispensable ingredient in cosmetics. Adding preservatives can inhibit the growth of microorganisms in cosmetics. Selecting efficient and safe preservatives is one of the keys to the development of cosmetic formulas. However, traditional chemical preservatives, such as methylparaben and ethylparaben, are prone to cause skin problems. Therefore, the importance of developing natural extract preservatives is becoming increasingly prominent.
[0003] Ginkgo biloba is also known as the maidenhair tree and the ginkgo tree. Its leaves are also called ginkgo leaves. They are bitter, sweet and astringent, and neutral in nature. The chemical composition of ginkgo biloba is very complex. More than 170 compounds have been discovered so far, mainly flavonoids, terpenes, alcohols, alkaloids, polyisoprenes, polysaccharides and other active ingredients with pharmacological effects. Ginkgo biloba extract has certain antibacterial ability and is a potential natural preservative. It will not irritate the skin too much and cause allergies, and has good preservative effects.
[0004] Gardenia, also known as Gardenia jasminoides, is a shrub with a height of 0.3 to 3 meters. It grows in the wilderness, hills, valleys, slopes, shrubs or forests beside streams at an altitude of 10 to 1500 meters. It is a major traditional Chinese medicinal material in my country. The active ingredient in the fruit of Gardenia jasminoides, iridoid glycosides, can protect the liver and gallbladder, clear away heat and detoxify, and have antibacterial and anti-inflammatory effects. However, when Gardenia jasminoides is used alone, the antibacterial effect is weak.
[0005] Blackberry is a berry plant belonging to the genus Rubus of the Rosaceae family. Blackberry has a deep color and rich anthocyanins. Blackberry anthocyanins have multiple functions such as antibacterial, anti-inflammatory, anti-infection, antioxidant, anti-mutation, anti-cancer, lowering blood sugar, lowering blood pressure, lowering blood lipids, protecting blood vessels, and slowing down aging. Blackberry fruits are rich in sugar, acid, and various amino acids, vitamins and other nutrients. Blackberry berries also contain biologically active substances such as SOD, vitamin E, isocitric acid, γ-aminobutyric acid and flavonoids. They are rich in nutrients and have medicinal functions, but blackberry fruits are rarely used in cosmetics. Summary of the invention
[0006] In view of the deficiencies in the above-mentioned prior art, the present invention can significantly improve the antibacterial and antioxidant effects by giving full play to the synergistic effect between the extracts, and can achieve the purpose of rapid and long-term antibacterial. The plant extract multi-effect composition can be used in cosmetics and has the advantages of low dosage, safety and effectiveness, and natural low irritation.
[0007] The object of the present invention is to provide a plant extract multi-effect composition, comprising the following raw materials in percentage by weight: 20-60% of an antibacterial agent and 1-10% of a synergist, wherein the antibacterial agent comprises a mixture of at least two of ginkgo leaf extract, gardenia fruit extract and blackberry fruit extract, and the synergist comprises at least one of a grapefruit peel extract and a white willow bark extract.
[0008] In some embodiments of the present invention, the plant extract multi-effect composition includes the following raw materials in percentage by weight: 35% antibacterial agent and 5% synergist, wherein the antibacterial agent includes a mixture of at least two of ginkgo leaf extract, gardenia fruit extract, and blackberry fruit extract, and the synergist includes at least one of grapefruit peel extract and white willow bark extract.
[0009] In some embodiments of the present invention, the mass ratio of the gardenia fruit extract to the blackberry fruit extract is 3-5:2-5.
[0010] In some embodiments of the present invention, the mass ratio of the gardenia fruit extract to the blackberry fruit extract is 4:3.
[0011] In some embodiments of the present invention, the mass ratio of the gardenia fruit extract to the ginkgo leaf extract is 3-5:2-4.
[0012] In some embodiments of the present invention, the mass ratio of the gardenia fruit extract to the ginkgo leaf extract is 4:3.
[0013] In some embodiments of the present invention, the mass ratio of the blackberry extract to the ginkgo leaf extract is 2-5:2-4.
[0014] In some embodiments of the present invention, the mass ratio of the blackberry fruit extract to the ginkgo leaf extract is 4:3.
[0015] In some embodiments of the present invention, the mass ratio of the gardenia fruit extract, the blackberry fruit extract and the ginkgo leaf extract is 2-5:1-4:1-4.
[0016] In some embodiments of the present invention, the mass ratio of the gardenia fruit extract, the blackberry fruit extract and the ginkgo leaf extract is 3:2:2.
[0017] In some embodiments of the present invention, the extraction process of the ginkgo leaf extract comprises the following steps:
[0018] The ginkgo leaf extract is obtained by solvent extraction, impurity removal, concentration and drying.
[0019] In some preferred embodiments of the present invention, the solvent is selected from an ethanol aqueous solution with a mass concentration of 50-80%.
[0020] In some preferred embodiments of the present invention, the extraction is reflux extraction.
[0021] In some preferred embodiments of the present invention, the process further includes crushing and sieving the ginkgo leaves before the solvent extraction to obtain ginkgo leaf powder.
[0022] In some preferred embodiments of the present invention, the mass ratio of the ginkgo leaf powder to the solvent is 1:8-10.
[0023] In some embodiments of the present invention, the extraction process of the gardenia fruit extract comprises the following steps:
[0024] The gardenia fruit is subjected to solvent extraction, impurity removal, concentration and drying to obtain the gardenia fruit extract.
[0025] In some preferred embodiments of the present invention, the solvent is selected from an ethanol aqueous solution with a mass concentration of 40-80%.
[0026] In some embodiments of the present invention, the extraction is reflux extraction.
[0027] In some preferred embodiments of the present invention, the process further comprises crushing and sieving the gardenia fruit before the gardenia fruit is extracted with the solvent to obtain the gardenia fruit powder.
[0028] In some preferred embodiments of the present invention, the mass ratio of the gardenia fruit powder to the solvent is 1:6-10.
[0029] In some embodiments of the present invention, the extraction process of the blackberry fruit extract comprises the following steps:
[0030] The blackberry fruit is subjected to solvent extraction, impurity removal, concentration and drying to obtain a blackberry fruit extract.
[0031] In some preferred embodiments of the present invention, the solvent is selected from an ethanol aqueous solution with a mass concentration of 50-80%.
[0032] In some embodiments of the present invention, the extraction is ultrasonic extraction, the temperature of the ultrasonic extraction is 50-70° C., and the pressure is normal pressure.
[0033] In some preferred embodiments of the present invention, the process further includes crushing and sieving the black berry fruits before the black berry fruits are extracted with solvent to obtain black berry fruit powder.
[0034] In some preferred embodiments of the present invention, the mass ratio of the blackberry powder to the solvent is 1:6-10.
[0035] In some embodiments of the present invention, the extraction process of the pomelo peel extract comprises the following steps:
[0036] The pomelo peel is subjected to solvent extraction, impurity removal, concentration and drying to obtain the pomelo peel extract.
[0037] In some preferred embodiments of the present invention, the solvent is selected from an ethanol aqueous solution with a mass concentration of 20-50%.
[0038] In some embodiments of the present invention, the extraction is reflux extraction.
[0039] In some preferred embodiments of the present invention, the pomelo peel is crushed and sieved before the solvent extraction to obtain pomelo peel powder.
[0040] In some preferred embodiments of the present invention, the mass ratio of the pomelo peel powder to the solvent is 1:8-10.
[0041] In some embodiments of the present invention, the extraction process of the willow bark extract comprises the following steps:
[0042] The white willow bark is subjected to solvent extraction, impurity removal, concentration and drying to obtain the white willow bark extract.
[0043] In some preferred embodiments of the present invention, the solvent is selected from lime water, and the pH value of the lime water is 9-10.
[0044] In some embodiments of the present invention, the extraction temperature is 40-60°C.
[0045] In some preferred embodiments of the present invention, the process further includes crushing and sieving the willow bark before the solvent extraction to obtain willow bark powder.
[0046] In some preferred embodiments of the present invention, the mass ratio of the white willow bark powder to the solvent is 1:8-12.
[0047] In some embodiments of the present invention, the plant extract multi-effect composition further comprises 30-79% solvent.
[0048] In some embodiments of the present invention, the plant extract multi-effect composition further comprises 60% solvent.
[0049] In some embodiments of the present invention, the solvent includes at least one of 1,2-propylene glycol, 1,3-propylene glycol, 1,2-butylene glycol, 1,3-butylene glycol, 1,4-butylene glycol, 1,2-pentanediol, 1,5-pentanediol, isopentyl glycol, isohexanediol, 1,2-hexanediol, dipropylene glycol, water, glycerol, and methylpropanediol.
[0050] Another object of the present invention is to provide a method for preparing a plant extract multi-effect composition, comprising the following steps:
[0051] The antibacterial agent and the synergistic enhancer are mixed, a solvent is added, the temperature is increased, and the mixture is stirred to obtain a plant extract multi-effect composition.
[0052] In some embodiments of the present invention, the heating temperature is 35-45°C.
[0053] In some embodiments of the present invention, the stirring time is 20 to 40 minutes.
[0054] Another object of the present invention is to provide an application of a plant extract multi-effect composition in the preparation of cosmetics, wherein the cosmetics contain the plant extract multi-effect composition, and the cosmetics include at least one of a facial mask liquid, an emulsion, a cream, a toner, an essence, a stock solution, a facial cleanser, a lotion, a perfume, a makeup remover, a foundation liquid, a foundation cream, a concealer cream, a rouge, a lipstick, an eye shadow, and a blush.
[0055] In some embodiments of the present invention, the amount of the plant extract multi-effect composition is 0.5%-5% by mass.
[0056] Compared with the prior art, the present invention has the following beneficial effects:
[0057] (1) The components of the plant extract multi-effect composition provided by the present invention are all common plant extracts, which can replace traditional preservatives and have the advantages of being safe, mild and non-irritating, and will not cause skin allergic reactions.
[0058] (2) The components of the plant extract multi-effect composition provided by the present invention have a synergistic effect, which can not only improve the antibacterial and antioxidant effects, but also have a wide antibacterial spectrum, fast onset, long antibacterial effect, and can remove ABTS . +Free radicals.
[0059] (3) The present invention adds synergistic enhancers such as grapefruit peel extract and / or white willow bark extract to plant extract antibacterial agents such as ginkgo leaf extract, gardenia fruit extract and blackberry fruit extract. During the preparation, storage and use of cosmetics, the synergistic enhancers can effectively improve the efficacy of the plant extract antibacterial agents; at the same time, the plant extract antibacterial agents have a synergistic effect, which can significantly improve the antibacterial and antioxidant properties of the plant extract multi-effect composition. DETAILED DESCRIPTION
[0060] In order to enable those skilled in the art to better understand the technical solutions of the present invention, the technical solutions of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work should fall within the scope of protection of the present invention.
[0061] Example 1
[0062] This embodiment provides an extraction process for the Gardenia fruit extract, and the specific extraction process is as follows:
[0063] 55 kg of gardenia fruit is taken, crushed by a traditional Chinese medicine crusher, and passed through a 50-mesh sieve to obtain gardenia fruit powder; 50 kg of the sieved gardenia fruit powder is taken, 6-10 times of a 40-80% ethanol aqueous solution is added, mixed evenly, and then leached, generally leaching for 1-2 hours, the temperature is maintained at about 55 DEG C; after leaching, the extraction mixture is transferred to an ultrasonic extraction device, ultrasonically extracted for 2 hours by a high-power dual-frequency ultrasonic device; after the extraction is completed, the extract is filtered to remove impurities, and water and ethanol are removed under an environment not higher than 60 DEG C; the remaining gardenia fruit extract is further ultrafiltered to remove impurities and refined to obtain a gardenia fruit extract.
[0064] Example 2
[0065] This embodiment provides an extraction process for blackberry fruit extract, and the specific extraction process is as follows:
[0066] 55 kg of dried blackberry fruit is taken, crushed by a traditional Chinese medicine crusher, and then passed through an 80-mesh sieve for standby use; 50 kg of the sieved blackberry fruit powder is taken and added into an extraction container; 6-10 times of a 50-80% ethanol aqueous solution is added; ultrasonic extraction is performed 2-3 times at a temperature of 50-70° C. and normal pressure, each time for 1-2 hours; the extracts are combined, 1-5% of activated carbon is added, and the extracts are heated to reflux for decolorization for 0.5-2 hours; the extracts are filtered while hot, and the extracts are concentrated under reduced pressure at 65° C. to obtain a blackberry fruit extract concentrate; the concentrate is adsorbed by a macroporous resin, eluted with 60-70% ethanol, and the eluate is spray-dried to obtain a blackberry fruit extract.
[0067] Example 3
[0068] This embodiment provides an extraction process for ginkgo leaf extract, and the specific extraction process is as follows:
[0069] Take 55kg of ginkgo leaf, crush it with a Chinese medicine grinder, pass it through an 80-mesh sieve to obtain ginkgo leaf powder. Take 50kg of the sieved ginkgo leaf powder, add 8-10 times the amount of 50-80% ethanol aqueous solution, mix evenly, heat and reflux to extract 2-3 times, each time for 1-2 hours, and the extraction temperature is about 50°C. Combine the extracts, reduce pressure and vacuum concentrate at 65°C to obtain a ginkgo leaf extract concentrate, disperse it with an appropriate amount of pure water, adjust the pH to 4-5 with acid, extract it with ethyl acetate, and concentrate the ethyl acetate layer to obtain an extract; the extract is adsorbed by a macroporous resin, eluted with 95% ethanol by volume, and the eluate is concentrated and dried to obtain a ginkgo leaf extract.
[0070] Example 4
[0071] This embodiment provides an extraction process for pomelo peel extract, and the specific extraction process is as follows:
[0072] 55 kg of pomelo peel is taken, crushed by a traditional Chinese medicine crusher, and passed through a 50-mesh sieve to obtain pomelo peel powder; 50 kg of the sieved pomelo peel powder is taken, 8-10 times of a 20-50% ethanol aqueous solution is added, mixed evenly, and then heated under reflux for extraction 2-3 times, each time for 1-2 hours, the extraction temperature is about 50°C, the extracts are combined, and vacuum concentrated at 65°C to obtain a pomelo peel extract concentrate; after being dispersed with an appropriate amount of pure water, stirred evenly, and centrifuged; the supernatant is taken for adsorption by a macroporous resin, desorbed by 50-70% ethanol, activated carbon is added to the desorbed solution, stirred, heated, decolorized, cooled, and filtered; the filtrate is concentrated under reduced pressure, dried, and the pomelo peel extract is obtained.
[0073] Example 5
[0074] This embodiment provides an extraction process of white willow bark extract, and the specific extraction process is as follows:
[0075] 55 kg of white willow bark is taken, crushed by a traditional Chinese medicine crusher, and passed through a 50-mesh sieve to obtain white willow bark powder; 50 kg of the sieved pomelo peel powder is taken, 8-12 times of lime water is added, the pH value of the lime water is between 9 and 10, the temperature is controlled at about 50°C, mixed and stirred evenly for leaching, generally leaching for 1-2 hours, after leaching, the extraction mixture is transferred to an ultrasonic extraction device, ultrasonically extracted for 2 hours by a high-power dual-frequency ultrasonic device, and filtered; the filtrate is adsorbed by a resin column, the saturated resin column is rinsed with water, and then eluted with ethanol, a desorption liquid is collected, the desorption liquid is concentrated under reduced pressure to recover ethanol, and then spray-dried to obtain a white willow bark extract.
[0076] Preparation of plant extract multi-effect composition:
[0077] Table 1. Raw material composition of plant extract multi-effect composition.
[0078]
[0079]
[0080] According to the raw materials and mass percentages in Table 1, the above extracts and 1,3-butanediol were added to a 250 mL flask equipped with a thermometer and a stirrer, the temperature was raised to 40°C, and stirred for 30 to 50 minutes until completely mixed. After cooling to room temperature, insoluble impurities were filtered out to obtain a plant extract multi-effect composition.
[0081] Minimum inhibitory concentration test:
[0082] Test bacteria: The bacteria used in this experiment were Pseudomonas aeruginosa ATCC9027, Escherichia coli ATCC8739 and Staphylococcus aureus ATCC6538; the fungi were Candida albicans ATCC10231 and Aspergillus niger ATCC16404, all of which were from Guangdong Provincial Microbial Culture Collection Center.
[0083] Test culture medium: nutrient broth, malt extract broth.
[0084] Preparation of bacterial suspension:
[0085] (1) Preparation of bacterial suspension: Aseptically add sterile 0.9% sodium chloride aqueous solution to the bacterial slant to wash out a certain amount of bacteria. Then add the washed bacteria to a sterile container of the same size as the No. 2 turbidity standard tube and dilute with sterile 0.9% sodium chloride aqueous solution until the turbidity is the same as that of the No. 2 turbidity standard tube (corresponding to the approximate bacterial concentration of 6×10 8 cfu / ml) were the same.
[0086] (2) Preparation of yeast suspension: Aseptically add sterile 0.9% saline to the Candida albicans slant to wash out a certain amount of bacteria. Then add the washed bacteria to a sterile test tube of the same diameter (size) as the No. 3 and No. 4 turbidimetric standard tubes. Finally, add sterile 0.9% saline to dilute until the bacterial suspension contains about 10 8 cfu / ml, for future use.
[0087] (3) Preparation of Aspergillus niger suspension: Aspergillus niger spores were eluted with a sterile 0.9% sodium chloride aqueous solution containing 0.05% Tween-80 to prepare an Aspergillus niger spore suspension, and the Aspergillus niger spore suspension was filtered to remove mycelium until the Aspergillus niger spore suspension contained about 10 8 cfu / ml, for future use.
[0088] Test operation steps:
[0089] (1) Preparation of culture medium containing antimicrobial agent: Prepare the antimicrobial (inhibitory) solution into test solutions of different concentrations with distilled water. Take 2.5 ml of the test solution of each dilution and add it to a test tube containing 2.5 ml of double-concentration nutrient broth.
[0090] (2) Take 0.1ml and the bacterial content is about 10 8 cfu / ml bacterial suspension was inoculated into a test tube containing nutrient broth containing antibacterial (inhibitory) agents as the test group sample.
[0091] (3) Use the same method to inoculate a test tube containing nutrient broth without antimicrobial (inhibitory) agents as a positive control sample.
[0092] (4) Take two test tubes containing nutrient broth as negative control group samples.
[0093] (5) Place the test group samples, positive control group samples, and negative control group samples in a 37°C incubator for 48 hours and observe the results.
[0094] (6) The test bacterial suspension should be cultured and counted for viable bacteria, and the effective concentration should be 5×10 5 cfu / ml~5×10 6 cfu / ml.
[0095] Judging rules: When there is bacterial growth in the positive control tube (turbidity) and no bacterial growth in the negative control tube (transparent), the concentration of the test bacterial suspension is 5×10 5 cfu / ml~5×10 6 cfu / ml, the concentration of antibacterial (inhibitory) agent corresponding to the highest dilution of sterile growth in the test group is the minimum inhibitory concentration of the sample to the test bacteria.
[0096] Table 2. Minimum inhibitory concentration determination results.
[0097]
[0098]
[0099] As shown in Table 2, by comparing the data of Examples 6, 7, and 8 with Comparative Examples 1, 2, 4, 5, 7, and 8, it can be seen that there is an obvious synergistic antibacterial effect between the gardenia fruit extract and the blackberry fruit extract, and between the mixture of the two and the synergistic enhancers, the white willow bark extract and the grapefruit peel extract; by comparing the data of Examples 9, 10, and 11 with Comparative Examples 1, 3, 4, 6, 7, and 8, it can be seen that there is an obvious synergistic antibacterial effect between the gardenia fruit extract and the ginkgo leaf extract, and between the mixture of the two and the synergistic enhancers, the white willow bark extract and the grapefruit peel extract; Comparison of the data of Examples 12, 13, and 14 with Comparative Examples 2, 3, 5, 6, 7, and 8 shows that there is an obvious synergistic antibacterial effect between blackberry fruit extract and ginkgo leaf extract, and between the mixture of the two and the synergistic enhancers, white willow bark extract and grapefruit peel extract; Comparison of the data of Examples 15, 16, and 17 with Comparative Examples 1 to 8 shows that there is an obvious synergistic antibacterial effect between gardenia fruit extract, blackberry and ginkgo leaf extract, and between the mixture of the three and the synergistic enhancers, white willow bark extract and grapefruit peel extract.
[0100] Antiseptic efficacy test:
[0101] The microbial antiseptic challenge experiment was carried out in accordance with the ISO11930-2019 antiseptic efficacy test method. The bacteria used in this experiment were a mixed strain of Pseudomonas aeruginosa ATCC9027, Escherichia coli ATCC8739 and Staphylococcus aureus ATCC6538; the fungi were Candida albicans ATCC10231 and Aspergillus niger ATCC16404, all of which were from the Guangdong Provincial Microbiological Culture Collection Center.
[0102] The initial inoculum volume of the mixed bacteria used in the test was 10 5 ~10 6 CFU / g, the initial inoculum of Candida albicans and Aspergillus niger was 10 4 ~10 5 CFU / g, the bacterial content was measured on the 7th, 14th and 28th days, and the logarithmic value of the reduction in the number of various microorganisms at the corresponding time nodes was calculated. The preservatives in Table 3 were the compositions of Examples 6 to 17 and Comparative Examples 1 to 8 respectively; the test system was a facial mask liquid, and the formula and production process were shown in Table 3.
[0103] Table 3. Facial mask liquid ingredients and production process.
[0104]
[0105] The test results were judged as follows: the number of bacteria decreased by 3 orders of magnitude on the 7th day, and decreased by 3 orders of magnitude on the 14th and 28th days without increasing; the number of Candida albicans decreased by 1 order of magnitude on the 7th day, and decreased by one order of magnitude on the 14th and 28th days without increasing; the number of Aspergillus niger did not increase on the 14th day, and decreased by one order of magnitude on the 28th day, which was considered passed. The results are shown in Table 4.
[0106] Table 4. Test data of antiseptic efficacy of facial mask liquid.
[0107]
[0108]
[0109] As can be seen from Table 3, the facial mask liquids of Examples 18 to 29 containing the plant extract multi-effect compositions prepared by Examples 6 to 17 have all passed the antiseptic efficacy test and have a strong antiseptic effect. As time goes by, the total number of bacteria, yeasts and Aspergillus niger in the facial mask liquids of Comparative Examples 9 to 14, which are single-component compositions prepared by Comparative Examples 1 to 6, has decreased, indicating that they all have a certain antiseptic effect, but none of them have passed the antiseptic efficacy test. The bacteria, Candida albicans and Aspergillus niger in Comparative Examples 15 to 16 did not decrease during the test, and the antiseptic performance was very poor. It can be seen that the plant extract multi-effect composition has a synergistic antiseptic effect.
[0110] Antioxidant capacity test:
[0111] The antioxidant capacity can be reflected by the free radical scavenging ability of 2,2-azino-bis(3-ethyl-benzothiazole-6-sulfonic acid) diammonium salt (ABTS). The higher the ABTS free radical scavenging rate, the stronger the antioxidant capacity, and vice versa. Refer to GB / T39100-2020 Determination of Peptide Antioxidant Activity DPPH and ABTS Method. ABTS can be oxidized by K2S2O8 to generate blue-green free radical cation ABTS . +,ABTS . + appears blue-green, and has the maximum absorption peak at 734nm. When free radicals are removed, the number decreases and the solution color becomes lighter, resulting in a decrease in absorbance at 734nm. From this, the sample can be calculated to remove ABTS . + ability.
[0112] The specific operations are as follows:
[0113] Weigh a certain amount of ABTS . +, prepared with anhydrous ethanol to make ABTS . + Prepared to a concentration with an absorbance of 0.7±0.02 at 734nm, this is ABTS . + working solution. The test is divided into solvent background group (T a ), solvent reaction well group (T b ), sample background group (T c ), sample reaction group (T d ). Solvent background group (T a ) is solvent, anhydrous ethanol; solvent reaction hole group (T b ) is ABTS . + working solution, solvent; sample background group (T c ) is anhydrous ethanol, sample; sample reaction group (T d ) is ABTS . + working solution, sample. Three replicates per group. . + Working solution, prepared solutions of various examples and comparative examples (1%), anhydrous ethanol, and solvent were added to a 96-well plate in the amounts in Table 5 and mixed evenly. The mixture was reacted at 30°C for 10 minutes and the absorbance was measured at 734 nm using an ELISA reader. VC was used as a positive control. Samples for ABTS . + The free radical scavenging rate was calculated using the following formula:
[0114]
[0115] In formula (1):
[0116] A a ——average absorbance of solvent background wells;
[0117] Ab ——Average absorbance of solvent reaction wells;
[0118] A c ——Average absorbance of background wells of samples;
[0119] A d ——Absorbance of sample background well.
[0120] Table 5. ABTS free radical scavenging capacity sample addition table
[0121]
[0122] Table 6. Test results of ABTS free radical scavenging rate.
[0123] sample ABTS free radical scavenging rate (%) Example 6 72 Example 7 71 Example 8 78 Example 9 76 Example 10 74 Embodiment 11 81 Example 12 75 Embodiment 13 77 Embodiment 14 76 Embodiment 15 80 Example 16 80 Embodiment 17 84 Comparative Example 1 64 Comparative Example 2 60 Comparative Example 3 63 Comparative Example 4 54 Comparative Example 5 55 Comparative Example 6 57 Comparative Example 7 48 Comparative Example 8 45
[0124] From the results in Table 6, it can be seen that the antioxidant effect of the combination of any two or more of the gardenia fruit extract, blackberry fruit extract, and ginkgo leaf extract is better than the effect of using any of the above components alone, among which the combination formed by the three extracts has the best antioxidant effect, indicating that there is a synergistic antioxidant effect between the above two or three components.
[0125] Human skin patch test:
[0126] The irritation and safety of the emulsion containing the plant extract multi-effect composition prepared in Examples 6 to 17 were tested. The preservatives in Table 7 were the compositions of Examples 6 to 17 and Comparative Examples 1 to 8, respectively. The test system was the emulsion. The formula and production process of the emulsion are shown in Table 7.
[0127] Table 7. Emulsion ingredients and production process
[0128]
[0129] Test method: Refer to Chapter 7, Section 2, 6.1 Skin occluded patch test of the 2015 edition of the "Technical Specifications for Safety of Cosmetics". Weigh 0.02 mL of different emulsion products into the patch tester, and set up a blank control group at the same time. The control is the diluent of the cosmetic. 600 healthy volunteers were selected and divided into 12 groups, with 50 in each group, aged 18 to 24 years old, and had no history of allergies. After cleaning the inner side of the subject's forearm, take 0.02 mL of sample and add it to the filter paper attached to the patch tester. Apply the patch tester to the inner side of the subject's forearm with non-irritating tape. After pasting, press it lightly with your fingers to make it evenly attached to the skin for 24 hours. Instruct the subject to keep the patch site dry within 24 hours, avoid intense exercise, scratching the patch site, and long-term sunlight exposure. After 24 hours, remove the tester and mark it. Observe the skin reaction according to the standards in Table 8 at 30 minutes, 24 hours and 48 hours after removing the test patch tester, and record the observation results.
[0130] Table 8. Skin reaction grading standards for occlusive patch test
[0131]
[0132] Table 9. Skin patch test results
[0133]
[0134]
[0135]
[0136] As can be seen from Table 9, the emulsions of Examples 30 to 41 containing the plant extract multi-effect composition prepared in Examples 6 to 17 had no serious adverse reactions, and the subjects basically had negative reactions. The results show that the emulsions of Examples 30 to 41 containing the plant extract multi-effect composition prepared in Examples 6 to 17 have low irritation and high safety.
[0137] The mass percentage of the antibacterial agent in the plant extract multi-effect composition of the present invention is 20-60%, the mass percentage of the synergist is 1-10%, and the mass percentage of the solvent is 30-79% (for example, the mass percentage of the antibacterial agent is 20%, 25%, 30%, 40%, 45%, 50%, 55%, 60%, the mass percentage of the synergist is 1%, 2%, 3%, 4%, 6%, 7%, 8%, 9%, 10%, and the mass percentage of the solvent is 30%, 35%, 40%, 45%, 50%, 55%, 65%, 70%, 75%, 79%, etc.), and / or other solvents are used to extract ginkgo leaves, gardenia fruits, blackberries, grapefruit peels, and white willow barks (for example, ethanol, methanol, petroleum ether, ethyl acetate The plant extract multi-effect composition uses other solvents (such as 1,2-propylene glycol, 1,3-propylene glycol, 1,2-butylene glycol, 1,4-butylene glycol, 1,2-pentanediol, 1,5-pentanediol, isopentyl glycol, isohexanediol, 1,2-hexanediol, dipropylene glycol, water, glycerin, methyl propanediol, etc.), and / or the mass ratio of gardenia fruit extract to blackberry fruit extract is 3-5:2-5, and / or the mass ratio of gardenia fruit extract to ginkgo leaf extract is 3-5:2-4, and / or the mass ratio of blackberry fruit extract to ginkgo leaf extract is 2-5:2-4, and / or the mass ratio of gardenia fruit extract, blackberry fruit extract and ginkgo leaf extract is 2-5:1-4:1-4. The obtained plant extract multi-effect compositions all have synergistic antibacterial, synergistic preservative and synergistic antioxidant effects among the antibacterial agents, and the synergistic enhancers have obvious synergistic enhancing effects on the antibacterial agents. The plant extract multi-effect compositions are used to prepare cosmetics with low irritation and high safety.
[0138] 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 it. Although the present invention has been described in detail with reference to the above embodiments, ordinary technicians in the relevant field should understand that after reading the specification of this application, the technicians can still modify or replace the specific implementation mode of the present invention with equivalents, but these modifications or changes do not deviate from the scope of protection of the pending claims of the present application.
Claims
1. A plant extract multi-effect composition, characterized in that: The invention comprises the following raw materials in percentage by weight: 20-60% of an antibacterial agent and 1-10% of a synergist, wherein the antibacterial agent comprises a mixture of at least two of ginkgo leaf extract, gardenia fruit extract and blackberry fruit extract, and the synergist comprises at least one of a grapefruit peel extract and a white willow bark extract; The mass ratio of the gardenia fruit extract to the blackberry fruit extract is 3-5:2-5; The mass ratio of the gardenia fruit extract to the ginkgo leaf extract is 3-5:2-4; The mass ratio of the blackberry extract to the ginkgo leaf extract is 2-5:2-4; The mass ratio of the gardenia fruit extract, the blackberry fruit extract and the ginkgo leaf extract is 2-5:1-4:1-4; The extraction process of the ginkgo leaf extract comprises the following steps: Ginkgo biloba leaves are extracted with a first solvent, impurities are removed, concentrated, and dried to obtain a ginkgo biloba leaf extract; the first solvent is selected from an ethanol aqueous solution with a mass concentration of 50-80%; The extraction process of the gardenia fruit extract comprises the following steps: The gardenia fruit is extracted with a second solvent, impurities are removed, concentrated, and dried to obtain a gardenia fruit extract; the second solvent is selected from an ethanol aqueous solution with a mass concentration of 40-80%; The extraction process of the blackberry fruit extract comprises the following steps: The blackberry fruit is extracted with a third solvent, impurities are removed, concentrated, and dried to obtain a blackberry fruit extract; the third solvent is selected from an ethanol aqueous solution with a mass concentration of 50-80%; The extraction process of the pomelo peel extract comprises the following steps: The pomelo peel is extracted with a fourth solvent, impurities are removed, concentrated, and dried to obtain a pomelo peel extract; the fourth solvent is selected from an ethanol aqueous solution with a mass concentration of 20-50%; The extraction process of the white willow bark extract comprises the following steps: The willow bark is extracted with a fifth solvent, impurities are removed, concentrated and dried to obtain a willow bark extract; the fifth solvent is selected from lime water, and the pH value of the lime water is 9-10.
2. The plant extract multi-effect composition according to claim 1, characterized in that: The plant extract multi-effect composition also includes 30-79% of solvent.
3. The plant extract multi-effect composition according to claim 2, characterized in that: The solvent includes at least one of 1,2-propylene glycol, 1,3-propylene glycol, 1,2-butylene glycol, 1,3-butylene glycol, 1,4-butylene glycol, 1,2-pentanediol, 1,5-pentanediol, isopentyl glycol, isohexylene glycol, 1,2-hexanediol, dipropylene glycol, water, glycerol, and methylpropylene glycol.
4. Use of a plant extract multi-effect composition according to any one of claims 1 to 3 in the preparation of cosmetics, characterized in that: The cosmetics contain the plant extract multi-effect composition, and the cosmetics include at least one of lotion, cream, toner, stock solution, cleanser, lotion, perfume, rouge, lipstick, eye shadow and blush.
5. Use of a plant extract multi-effect composition according to any one of claims 1 to 3 in the preparation of cosmetics, characterized in that: The cosmetics contain the plant extract multi-effect composition, and the cosmetics include at least one of a facial mask liquid, an essence liquid, a makeup remover, a foundation liquid, a foundation cream, and a concealer cream.
6. The use according to claim 4, characterized in that In terms of mass percentage, the amount of the plant extract multi-effect composition is 0.5%-5%.
7. The use according to claim 5, characterized in that In terms of mass percentage, the amount of the plant extract multi-effect composition is 0.5%-5%.
Citation Information
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