Acne-removing composition, use and acne-removing product
By applying the combination of Panax notoginseng extract, yellow bark tree bark extract, Sophora root extract and lotus seed extract to acne removal products, the problem of difficult to achieve gentle acne removal effects in the prior art is solved, and a variety of acne removal effects have been achieved, including oil control, antibacterial and healing promotion.
Patent Information
- Application Number
- CN202510014050.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2025-01-06
- Publication Date
- 2025-03-18
- Estimated Expiration
- 2045-01-06
AI Technical Summary
It is difficult to develop a fully implantable formula to achieve mild acne removal effect in the prior art.
The combination of Panax notoginseng extract, yellow bark tree bark extract, Sophora root extract and lotus seed extract is used to achieve the effects of inhibiting dermatitis, enhancing skin resistance, controlling oil, antibacterial and promoting healing through synergy.
It achieves a gentle and rapid acne removal effect, reduces the redness and swelling and pain of acne, inhibits the growth of acne-causing bacteria, and promotes skin repair and health.
Smart Images

Figure CN119405574B_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the field of new daily chemical materials, and in particular to an acne-removing composition, uses and acne-removing products. Background Art
[0002] The occurrence of acne is related to many factors. Excessive secretion of the cortical glands can lead to clogged pores, forming blackheads, which further develop into acne. At the same time, the high-sugar, high-fat diet habits of contemporary young people, as well as bad living habits such as stress, lack of sleep, and lack of exercise also affect skin health and lead to acne.
[0003] The following literature is available on plant extracts as active ingredients for acne treatment:
[0004] Prior art 1: Publication number CN114642617A, the subject of the patent application is an acne repair essence patch and its preparation method, which discloses that extracts such as Panax notoginseng extract, dandelion extract, and Sophora flavescens root extract can inhibit dermatitis and enhance the skin's resistance through synergistic effects to fight inflammation and neutralize histamine.
[0005] Prior art 2: Publication No. CN107213098A, the subject of the patent application is a longan seed acne-removing mask and its preparation method, which discloses an acne-removing formula composed of longan seed dry powder, calendula extract, lotus seed powder, houttuynia cordata extract, saffron extract, Panax notoginseng powder and other components; the relevant effects of lotus seed powder are not recorded in the text.
[0006] In the relevant experiments of this application, it was found that the reasonable application of lotus seed extract can further improve the acne removal effect.
[0007] Therefore, the technical problem solved by the present invention is: how to develop a full plant extract formula to achieve a mild acne removal effect. Summary of the invention
[0008] The purpose of the present invention is to provide an acne-removing composition, which adopts a combination of Panax notoginseng extract, Phellodendron chinense bark extract, Sophora flavescens root extract and Lotus seed extract to achieve a mild and rapid acne-removing effect.
[0009] Meanwhile, the invention also provides application of the composition and cosmetics.
[0010] To achieve the above objectives, this application discloses:
[0011] An acne-removing composition comprising the following components in parts by weight:
[0012] 0.1-10 parts of Panax notoginseng extract;
[0013] 0.1-10 parts of Phellodendron chinense bark extract;
[0014] 0.5-15 parts of Sophora flavescens root extract;
[0015] 0.1-10 parts of lotus seed extract.
[0016] Panax notoginseng extract mainly contains notoginseng saponins, which have strong anti-inflammatory effects. They can reduce inflammatory reactions and relieve skin discomfort caused by acne. At the same time, they can promote wound healing, shorten skin repair time, and reduce the possibility of scar formation.
[0017] The extract of the bark of the yellow pine tree is rich in alkaloids and has a strong antibacterial effect. It can inhibit the growth and reproduction of bacteria that cause acne. At the same time, the extract of the bark of the yellow pine tree helps regulate oil secretion, reduce the greasy feeling of the skin, and help prevent the occurrence of acne. In addition, it has a good cleansing effect and can deeply clean the pores, remove dirt and blockages, prevent the formation of acne, and reduce the expansion of pores.
[0018] Sophora flavescens root extract is rich in matrine and other alkaloids, and has a good antibacterial effect, especially against acne pathogens such as penicillin-resistant Staphylococcus aureus. It can reduce the reproduction of pathogens and help slow down the occurrence and deterioration of acne. At the same time, other active ingredients have the function of regulating oil secretion and improving the oil condition of the skin. It helps to tighten pores, reduce the possibility of pore blockage and inflammation, and is conducive to preventing the formation of acne.
[0019] Lotus seed extract contains rich alkaline components, including liensinine and paraliensinine, which have good antibacterial and antiviral activities. At the same time, it also has the functions of anti-oxidation and scavenging free radicals, which helps to maintain skin health. In addition, lotus seed extract contains anti-inflammatory and anti-allergic components, which have good therapeutic effects on inflammatory skin diseases such as acne, eczema and dermatitis. In addition, the combination of lotus seed polyphenols and proteins can produce a sense of convergence. This combination is the result of the combined action of hydrophobic and hydrogen bonds. This property makes it have good adhesion to the skin under waterproof conditions, and can shrink large pores and reduce excessive sebum secretion in greasy skin.
[0020] The mechanism by which the above four achieve synergistic acne removal is:
[0021] The four ingredients act on the acne removal process from multiple aspects such as oil control, anti-inflammatory, antibacterial and healing promotion, forming a comprehensive treatment mechanism that enhances each other's effects. Among them, the coptis bark extract and lotus seed extract work together to reduce excessive sebum secretion, thereby avoiding pore blockage. At the same time, Panax notoginseng extract can improve microcirculation and promote the overall health of the skin. It can also synergize with the antioxidant ingredients in lotus seed extract to repair damaged skin and reduce pigmentation and scar formation after acne healing. The antibacterial and anti-inflammatory effects of Sophora flavescens root extract and Panax notoginseng extract can effectively reduce the redness, swelling and pain caused by acne and inhibit the growth of acne-causing bacteria.
[0022] The above-mentioned acne-removing composition further comprises bitter orange flower extract and / or dandelion extract.
[0023] Bitter orange flower extract contains a variety of flavonoids, which have anti-inflammatory properties and can reduce the skin's inflammatory response, relieve the redness and discomfort caused by acne. In addition, it can inhibit the growth of a variety of skin pathogens, including bacteria associated with acne formation (such as Propionibacterium acnes). By inhibiting the growth of these bacteria, the occurrence of acne can be reduced. At the same time, it also contains rich vitamins that can participate in cell repair and skin protection, promoting skin healing.
[0024] Dandelion extract is rich in flavonoids and polyphenols, and has significant antioxidant and anti-inflammatory activity and antioxidant properties. It can inhibit the release of inflammatory mediators, reduce the inflammatory response of the skin, and relieve symptoms such as pain caused by acne. It is also rich in antioxidants, which can neutralize the effects of free radicals, reduce the impact of oxidative stress in acne formation, and improve the overall health of the skin. The various vitamins and minerals contained in dandelions can promote the renewal and regeneration of skin cells and help improve skin color and texture. In addition, its diuretic effect may also help to excrete toxins from the body and further improve skin conditions.
[0025] The mechanism of the above two ingredients and Panax notoginseng extract, Phellodendron chinense bark extract, Sophora flavescens root extract, and Lotus seed extract to synergistically remove acne is:
[0026] The six active ingredients can synergize each other in acne removal through various mechanisms. Among them, the extracts from the bark of the yellow pine tree, the root of the sophora flavescens, and the dandelion extract are rich in anti-inflammatory substances, which can relieve the redness and swelling caused by acne and relieve the inflammatory response of the skin. At the same time, they also have antibacterial effects to a certain extent and can effectively inhibit the formation of Propionibacterium acnes. The astringent effect of lotus seed extract and the bark of the yellow pine tree can tighten pores and prevent pore blockage. At the same time, the extracts of Panax notoginseng and dandelion can promote wound healing and skin regeneration, and have a repairing effect on the skin.
[0027] In the above-mentioned acne-removing composition, the bitter orange flower extract is used in an amount of 0.1 to 10 parts and / or the dandelion extract is used in an amount of 0.1 to 10 parts.
[0028] The above-mentioned anti-acne composition includes the following components in parts by weight:
[0029] 0.5-5 parts of Panax notoginseng extract;
[0030] 0.5-5 parts of Phellodendron chinense bark extract;
[0031] 1-10 parts of Sophora flavescens root extract;
[0032] 0.5-5 parts of lotus seed extract;
[0033] 0.5-5 parts of bitter orange flower extract;
[0034] 0.5-5 parts of dandelion extract.
[0035] In the above-mentioned acne-removing composition, the Panax notoginseng extract, the Phellodendron chinense bark extract, and the Sophora flavescens root extract are obtained by an alcohol extraction method, and the lotus seed extract is obtained by a water extraction method.
[0036] In the above-mentioned acne-removing composition, the bitter orange flower extract is obtained by an alcohol extraction method, and the dandelion extract is obtained by a water extraction method.
[0037] Specifically, the extraction method of the above extract is:
[0038] Preparation of Panax notoginseng extract: crush the raw material of Panax notoginseng into powder of a certain coarseness and fineness, add a certain concentration of ethanol for extraction, filter after extraction, purify the filtrate with HP-20 macroporous resin column, and then concentrate the Panax notoginseng extract to complete dryness to obtain the Panax notoginseng extract;
[0039] The raw material of Panax notoginseng was washed with water and added to a wet material grinder, crushed into particles of about 40 mesh, added to an extraction tank, 5 to 7 times the amount of 45 to 60wt% ethanol solution was added to the extraction tank, stirred and extracted at 60 to 70°C for 1 to 2 hours, then filtered, and 2 to 4 times the amount of 45 to 60wt% ethanol solution was added to the raw material extraction tank, stirred and extracted at 60 to 70°C for 1 to 2 hours. After the extraction was completed, it was filtered, and the filtrate was added to a tubular centrifuge, the speed was controlled at 10000 to 12000 rpm, and the centrifugal speed was controlled at 3 to 5L / min. Then, the centrifuge was loaded into an LX-100B resin column, the ratio of the centrifuge to the resin was controlled at 5 to 9:1, and the loading speed was controlled at 10 to 20wt% of the original volume of 1-2 column volumes. The concentrated solution was placed in a vacuum drying device, the temperature was controlled at 50 to 60°C, the pressure was -0.07MPa to -0.09MPa, and it was vacuum dried to a powder state to obtain a Panax notoginseng extract.
[0040] Preparation of the Huangpi Tree Bark Extract: crush the Huangpi Tree bark into powder of a certain coarseness and fineness, then add high concentration ethanol to continuously reflux extract until it is almost colorless, centrifuge the filtrate after the extraction is completed, concentrate the filtrate to remove ethanol, and vacuum dry it to a powder state to obtain the Huangpi Tree Bark Extract;
[0041] The bark of the yellow-peeled tree is washed and added to a wet material grinder, crushed into particles of about 40 mesh, added to an extraction tank, and 8 to 10 times the amount of 70 to 90 wt% ethanol solution is added to the extraction tank for continuous reflux extraction until colorless. After the extraction is completed, filter the solution, and concentrate the filtrate with a single-effect concentrator. The concentration temperature is controlled at 50 to 60°C and the concentration pressure is -0.07 MPa to -0.09 MPa. The solution is concentrated until there is no alcohol. The concentrate is placed in a vacuum drying device. The vacuum drying conditions are the same as those of the concentrator to obtain the yellow-peeled tree bark extract.
[0042] Preparation of Sophora flavescens root extract: crush the Sophora flavescens root raw material into powder of a certain coarseness and fineness, add high concentration ethanol for extraction, filter after the extraction is completed, purify and decolorize the filtrate using a neutral alumina column, and then concentrate the Sophora flavescens root extract to complete dryness to obtain the Sophora flavescens root extract;
[0043] The raw material of Sophora flavescens root is directly added to the pulverizer, crushed into powder of about 30 meshes, added to the extraction tank, and 7 to 9 times the amount of 70 to 90wt% ethanol solution is added to the extraction tank, stirred and extracted for 1 to 2 hours, the temperature is controlled at 50 to 60°C, and filtered after the stirring extraction is completed. 3 to 5 times the amount of 70 to 90wt% ethanol solution is continued to be added to the extraction tank, stirred and extracted for 1 to 2 hours, the temperature is controlled at 50 to 60°C, and the stirring extraction is completed. Filter, the filtrate is decolorized by a neutral alumina column, wherein the ratio of the extract to alumina is controlled between 6 and 8:1, and the filtration rate is controlled at 1 to 1.5 times the column volume / h. After the extract is filtered, 70 to 90wt% ethanol solution is added to wash the neutral alumina column for 1 to 2 column volumes, and the extract filtrate and ethanol washing liquid are collected. The extract is added to a concentrator, the concentration temperature is controlled at 60-70°C, the concentration pressure is -0.07MPa to -0.09MPa, and after concentrating to 10-20wt% of the original volume, vacuum drying is performed under the same vacuum drying conditions as the concentrator conditions to obtain the Sophora flavescens root extract.
[0044] Preparation of lotus seed extract: crush the lotus seed raw material into powder of a certain coarseness and fineness, add pure water for heating extraction, centrifuge after the extraction is completed, and then concentrate the lotus seed extract until it is completely dry to obtain the lotus seed extract;
[0045] The lotus seed raw material is directly added to the grinder, crushed into powder of about 30 mesh, added to the extraction tank, 10 to 12 times the amount of pure water is added to the extraction tank, stirred and extracted for 1 to 2 hours, the temperature is controlled at 55 to 75°C, and filtered after the stirring and extraction is completed, and 5 to 6 times the amount of pure water is added to the extraction tank, stirred and extracted for 1 to 2 hours, the temperature is controlled at 55 to 75°C, and filtered after the stirring and extraction is completed. The extract is added to the concentrator, the concentration temperature is controlled at 60 to 70°C, the concentration pressure is -0.07MPa to -0.09MPa, and vacuum dried after concentrating to 10 to 20wt% of the original volume. The vacuum drying conditions are the same as those of the concentrator to obtain the lotus seed extract.
[0046] Preparation of bitter orange flower extract: crush the bitter orange flower into powder of a certain coarseness and fineness, then add high concentration ethanol to continuously reflux extract until it is almost colorless, centrifuge the filtrate after the extraction is completed, concentrate the filtrate to remove ethanol, and vacuum dry it to a powder state to obtain the bitter orange flower extract;
[0047] Wash the bitter orange flower and add it to a wet material grinder to grind it into particles of about 40 mesh. Add it to an extraction tank, add 6 to 8 times the amount of 70 to 90 wt% ethanol solution to the extraction tank, and continuously reflux and extract until it is colorless. After the extraction is completed, filter it, and concentrate the filtrate with a single-effect concentrator. Control the concentration temperature at 50 to 60°C and the concentration pressure at -0.07 MPa to -0.09 MPa. Concentrate until there is no alcohol. Place the concentrate in a vacuum drying device. The vacuum drying conditions are the same as those of the concentrator to obtain the bitter orange flower extract.
[0048] Preparation of dandelion extract: crush the dandelion raw material into powder of a certain coarseness and fineness, add pure water to heat and reflux for extraction, centrifuge after the extraction is completed, and then concentrate the dandelion extract to an extract, add water to the extract to suspend it, purify it with a polyamide resin column, and then reduce the pressure to concentrate the eluate to complete dryness to obtain the dandelion extract;
[0049] The dandelion raw material is directly added to the grinder, crushed into a powder of about 40 mesh, added to the extraction tank, and 10 to 12 times the amount of pure water is added to the extraction tank, and the temperature is controlled at 75 to 85°C for reflux extraction for 8 to 10 hours. The extract is added to the concentrator, the concentration temperature is controlled at 60 to 70°C, the concentration pressure is -0.07MPa to -0.09MPa, and it is concentrated to 10 to 20wt% of the original volume and then vacuum dried. The vacuum drying conditions are the same as those of the concentrator. After concentrating to an extract, it is suspended with water and purified by a polyamide resin column, wherein the ratio of the suspension to the polyamide resin is controlled between 1 and 3:1, and the filtration rate is controlled at 1 to 1.5 times the column volume / h. After the suspension is filtered, an ethanol-water solution gradient elution is added, 1 to 2 column volumes, and the 10% ethanol eluate is collected and concentrated under reduced pressure to complete dryness, and the concentration temperature is controlled at 60 to 70°C, and the concentration pressure is -0.07MPa to -0.09MPa to obtain a dandelion extract.
[0050] At the same time, the present invention also discloses the use of any of the above-mentioned acne-removing compositions in preparing cosmetics.
[0051] Finally, the present invention also discloses an acne-removing product, comprising any one of the above-mentioned acne-removing compositions.
[0052] In the above-mentioned acne-removing product, the content of the acne-removing composition is 0.1 to 30 wt %.
[0053] This application has at least the following beneficial effects:
[0054] The present invention uses a combination of Panax notoginseng extract, Phellodendron chinense bark extract, Sophora flavescens root extract and Lotus seed extract to act on the acne removal process from multiple aspects such as oil control, anti-inflammation, antibacterial and promoting healing, forming a comprehensive treatment mechanism so that the effects are mutually enhanced.
[0055] The combined effects of Phellodendron bark extract and lotus seed extract can reduce excessive sebum secretion, thus avoiding pore blockage. At the same time, Panax notoginseng extract can improve microcirculation and promote overall skin health. It can also work with the antioxidant ingredients in lotus seed extract to repair damaged skin and reduce pigmentation and scar formation after acne heals. The antibacterial and anti-inflammatory effects of Sophora flavescens root extract and Panax notoginseng extract can effectively reduce the redness, swelling and pain caused by acne and inhibit the growth of acne-causing bacteria.
[0056] Through the above combined effects, a gentle and effective acne removal effect is achieved. BRIEF DESCRIPTION OF THE DRAWINGS
[0057] Figure 1 This is a chicken embryo observation picture before using the anti-acne composition of Example 2 at a concentration of 5% of the present invention;
[0058] Figure 2 This is a chicken embryo observation picture after using the anti-acne composition of Example 2 at a concentration of 5% of the present invention. DETAILED DESCRIPTION
[0059] The present invention will be described clearly and completely below in conjunction with the embodiments of the present invention. In the description of the present invention, it should be noted that, if no specific conditions are specified in the embodiments, the conditions are carried out according to conventional conditions or conditions recommended by the manufacturer. If the manufacturer of the reagents or instruments used is not specified, they are all conventional products that can be purchased commercially.
[0060] Part I Preparation of Plant Extracts
[0061] 1.1 Preparation of Panax notoginseng extract
[0062] Preparation of Panax notoginseng extract 1
[0063] The raw material of Panax notoginseng is crushed into powder of a certain coarseness and fineness, and a certain concentration of ethanol is added for extraction. After extraction, the filtrate is filtered, and the filtrate is purified by using an HP-20 macroporous resin column. After that, the Panax notoginseng extract is concentrated to complete dryness to obtain a Panax notoginseng extract;
[0064] The Panax notoginseng raw material was washed with water and added to a wet material grinder, crushed into particles of about 40 mesh, and added to an extraction tank. Six times the weight of a 50wt% ethanol solution was added to the extraction tank, and the mixture was stirred and extracted at 65°C for 2 hours. The mixture was then filtered, and three times the weight of a 50wt% ethanol solution was added to the raw material extraction tank. The mixture was stirred and extracted at 65°C for 2 hours. After the extraction was completed, the mixture was filtered and the filtrate was added to a tubular centrifuge. The speed was controlled at 10000-12000 rpm and the centrifugal speed was controlled at 3-5L / min. The centrifugal liquid was then loaded onto an LX-100B resin column. The ratio of the centrifugal liquid to the resin was controlled at 6:1. The loading speed was controlled at 15wt% of the original volume of 1-2 column volumes. The concentrated liquid was placed in a vacuum drying device, the temperature was controlled at 50-60°C, the pressure was -0.07MPa to -0.09MPa, and the mixture was vacuum dried to a powder state to obtain a Panax notoginseng extract.
[0065] Preparation of Panax notoginseng extract 2
[0066] The preparation method is basically the same as that of Panax notoginseng extract 1, except that the ethanol used is a 60wt% ethanol solution, 7 times the weight of the ethanol solution is used during the first extraction process, and 4 times the weight of the ethanol solution is used during the second extraction process.
[0067] Preparation of Panax notoginseng extract 3
[0068] The preparation method is basically the same as that of Panax notoginseng extract 1, except that the ethanol used is a 45wt% ethanol solution, 5 times the weight of the ethanol solution is used during the first extraction process, and 2 times the weight of the ethanol solution is used during the second extraction process.
[0069] 1.2 Preparation of Phellodendron chinense bark extract
[0070] Preparation of Phellodendron chinense bark extract 1
[0071] The bark of the yellow-peeled tree is crushed into a powder of a certain coarseness and fineness, and then a high concentration of ethanol is added to continuously reflux and extract until it is almost colorless. After the extraction is completed, the filtrate is centrifuged, the filtrate is concentrated to remove the ethanol, and the filtrate is vacuum dried to a powder state to obtain the yellow-peeled tree bark extract;
[0072] The bark of the yellow-peeled tree is washed and added to a wet material grinder, crushed into particles of about 40 mesh, added to an extraction tank, and 9 times the weight of an 80wt% ethanol solution is added to the extraction tank for continuous reflux extraction until colorless. After the extraction is completed, the filtrate is concentrated in a single-effect concentrator, the concentration temperature is controlled at 50-60°C, and the concentration pressure is -0.07MPa to -0.09MPa. It is concentrated until there is no alcohol, and the concentrate is placed in a vacuum drying device. The vacuum drying conditions are the same as those of the concentrator to obtain the yellow-peeled tree bark extract.
[0073] Preparation of Phellodendron chinense bark extract 2
[0074] The preparation method is substantially the same as that of the Phellodendron chinense bark extract 1, except that the ethanol solution is 90 wt % and the amount of the ethanol solution is 10 times the weight.
[0075] Preparation of Phellodendron chinense bark extract 3
[0076] The preparation method is substantially the same as that of the Phellodendron chinense bark extract 1, except that the ethanol solution is 70 wt % and the amount of the ethanol solution is 8 times the weight.
[0077] 1.3 Preparation of Sophora flavescens root extract
[0078] Preparation of Sophora flavescens root extract 1
[0079] The raw material of Sophora flavescens root is crushed into powder of a certain coarseness and fineness, and high concentration ethanol is added for extraction. After the extraction is completed, the filtrate is filtered, and the filtrate is purified and decolorized using a neutral alumina column, and then the Sophora flavescens root extract is concentrated to complete dryness to obtain the Sophora flavescens root extract;
[0080] The raw material of Sophora flavescens root is directly added to the pulverizer, crushed into powder of about 30 mesh, added to the extraction tank, 8 times the weight of 80wt% ethanol solution is added to the extraction tank, stirred and extracted for 2 hours, the temperature is controlled at 60℃, and the stirring extraction is completed. Filter, continue to add 4 times the weight of 80wt% ethanol solution to the extraction tank, stir and extract for 2 hours, control the temperature at 60℃, and filter after the stirring extraction is completed. The filtrate is decolorized by a neutral alumina column, wherein the ratio of the extract to alumina is controlled between 6-8:1, and the filtration rate is controlled at 1-1.5 times the column volume / h. After the extraction solution is filtered, 80wt% ethanol solution is added to wash the neutral alumina column for 1-2 column volumes, and the extract filtrate and ethanol washing solution are collected. The extract is added to the concentrator, the concentration temperature is controlled at 60-70℃, the concentration pressure is -0.07MPa to -0.09MPa, and it is concentrated to 10-20wt% of the original volume and then vacuum dried. The vacuum drying conditions are the same as those of the concentrator to obtain the Sophora flavescens root extract.
[0081] Preparation of Sophora flavescens root extract 2
[0082] The preparation method is generally the same as the preparation method of Sophora flavescens root extract 1, except that the concentration of the ethanol solution is 90wt%, the amount of the ethanol solution used in the first extraction is 9 times the weight; and the amount of the ethanol solution used in the second extraction is 5 times the weight.
[0083] Preparation of Sophora flavescens root extract 3
[0084] The preparation method is generally the same as the Sophora flavescens root extract 1, except that the concentration of the ethanol solution is 70wt%, the amount of the ethanol solution used in the first extraction is 7 times by weight, and the amount of the ethanol solution used in the second extraction is 3 times by weight.
[0085] 1.4 Preparation of lotus seed extract
[0086] Preparation of lotus seed extract 1
[0087] The lotus seed raw material is crushed into powder of a certain coarseness and fineness, and pure water is added for heating extraction. After the extraction is completed, the lotus seed extract is centrifuged, and then the lotus seed extract is concentrated to be completely dry to obtain the lotus seed extract;
[0088] The lotus seed raw material is directly added to the grinder, crushed into a powder of about 30 mesh, added to the extraction tank, 10 times the amount of pure water is added to the extraction tank, stirred and extracted for 2 hours, the temperature is controlled at 70°C, and the stirring extraction is completed and filtered, and 5 times the amount of pure water is added to the extraction tank, stirred and extracted for 1 hour, the temperature is controlled at 70°C, and the stirring extraction is completed and filtered. The extract is added to the concentrator, the concentration temperature is controlled at 60-70°C, the concentration pressure is -0.07MPa to -0.09MPa, and vacuum dried after concentrating to 10-20wt% of the original volume. The vacuum drying conditions are the same as those of the concentrator to obtain the lotus seed extract.
[0089] Preparation of lotus seed extract 2
[0090] The preparation method is generally the same as that of lotus seed extract 1, except that the amount of pure water used in the first extraction is 12 times by weight; the amount of pure water used in the first extraction is 6 times by weight.
[0091] Preparation of lotus seed extract 3
[0092] The preparation method is generally the same as that of lotus seed extract 1, except that the extraction temperature is controlled at 75°C.
[0093] 1.5 Preparation of bitter orange flower extract
[0094] Preparation of bitter orange flower extract 1
[0095] The bitter orange flower is crushed into powder of a certain coarseness and fineness, and then a high concentration of ethanol is added to continuously reflux and extract until it is almost colorless. After the extraction is completed, the filtrate is centrifuged, the filtrate is concentrated to remove the ethanol, and vacuum dried to a powder state to obtain the bitter orange flower extract;
[0096] Wash the bitter orange flower and add it to a wet material grinder to grind it into particles of about 40 mesh. Add it to an extraction tank, add 8 times the amount of 80wt% ethanol solution to the extraction tank and continuously reflux and extract until it is colorless. After the extraction is completed, filter it and concentrate the filtrate with a single-effect concentrator. Control the concentration temperature at 50-60°C and the concentration pressure at -0.07MPa to -0.09MPa until there is no alcohol. Place the concentrate in a vacuum drying device. The vacuum drying conditions are the same as those of the concentrator to obtain the bitter orange flower extract.
[0097] Preparation of bitter orange flower extract 2
[0098] The preparation method is substantially the same as that of the bitter orange flower extract 1, except that 6 times the amount of 90 wt % ethanol solution is added.
[0099] Preparation of bitter orange flower extract 3
[0100] The preparation method is substantially the same as that of the bitter orange flower extract 1, except that 8 times the amount of 90 wt % ethanol solution is added.
[0101] 1.6 Preparation of dandelion extract
[0102] Preparation of Dandelion Extract 1
[0103] The dandelion raw material is crushed into powder of a certain coarseness and fineness, and pure water is added to perform heating reflux extraction. After the extraction is completed, the dandelion extract is centrifuged, and then the dandelion extract is concentrated to an extract. Water is added to the extract to suspend it, and after purification with a polyamide resin column, the eluate is concentrated under reduced pressure to complete dryness to obtain a dandelion extract.
[0104] The dandelion raw material is directly added to the grinder, crushed into a powder of about 40 mesh, added to the extraction tank, 10 times the amount of pure water is added to the extraction tank, and the temperature is controlled at 80°C for reflux extraction for 8 hours. The extract is added to the concentrator, the concentration temperature is controlled at 60-70°C, the concentration pressure is -0.07MPa to -0.09MPa, and it is concentrated to 10-20wt% of the original volume and then vacuum dried. The vacuum drying conditions are the same as the concentrator conditions. After concentrating to the extract, it is suspended with water and purified by a polyamide resin column, wherein the ratio of the suspension to the polyamide resin is controlled between 1-3:1, and the filtration rate is controlled at 1-1.5 times the column volume / h. After the suspension is filtered, an ethanol-water solution gradient elution is added, 1-2 column volumes, and the 10% ethanol eluate is collected and concentrated under reduced pressure to complete dryness, and the concentration temperature is controlled at 60-70°C, and the concentration pressure is -0.07MPa to -0.09MPa to obtain a dandelion extract.
[0105] Preparation of Dandelion Extract 2
[0106] The preparation method is basically the same as that of dandelion extract 1, except that 10 times the amount of pure water is added and the temperature is controlled at 75°C for reflux extraction for 10 hours.
[0107] Preparation of Dandelion Extract 3
[0108] The preparation method is basically the same as that of dandelion extract 1, except that 12 times the amount of pure water is added, and the temperature is controlled at 85°C for reflux extraction for 8 hours.
[0109] The moisture content of the raw materials is 12% for Panax notoginseng, 9% for Sophora flavescens, 12% for Phellodendron chinense bark, 2% for Lotus seeds, 8% for Taraxacum officinale, and 12% for Citrus aurantium.
[0110] Part II Examples and Comparative Examples
[0111] The plant extracts prepared in the above scheme are mixed, and butanediol is used as a solvent to obtain the composition of the present invention; the mixing can be carried out mechanically in a laboratory flask to keep the solution in a uniform phase.
[0112] The formula is shown in Table 1 below;
[0113] Table 1 Formulation Unit: wt%
[0114] Panax notoginseng extract 1 Phellodendron chinense bark extract1 Sophora flavescens root extract 1 Lotus seed extract 1 Bitter Orange Flower Extract1 Dandelion Extract 1 Butanediol Example 1 0.1 0.1 0.5 0.1 0 0 to 100 Example 2 1 1 2 1 0 0 to 100 Example 3 2 1 1 1 0 0 to 100 Example 4 0.8 1.5 2 1.5 0 0 to 100 Example 5 10 10 15 10 0 0 to 100 Example 6 0.1 0.1 0.5 0.1 0.1 0 to 100 Example 7 1 1 2 1 1 0 to 100 Example 8 10 10 15 10 10 0 to 100 Example 9 0.1 0.1 0.5 0.1 0 0.1 to 100 Example 10 1 1 2 1 0 1 to 100 Embodiment 11 10 10 15 10 0 10 to 100 Example 12 0.1 0.1 0.5 0.1 0.1 0.1 to 100 Embodiment 13 1 1 2 1 1 1 to 100 Embodiment 14 10 10 15 10 10 10 to 100 Comparative Example 1 1.5 1.5 2 0 0 0 to 100 Comparative Example 2 1.5 0 2 1.5 0 0 to 100 Comparative Example 3 1.5 1.5 2 0 1 0 to 100 Comparative Example 4 1.5 1.5 2 0 0 1 to 100 Comparative Example 5 1.5 1.5 2 0 1 1 to 100 Comparative Example 6 1.5 0 2 1.5 1 0 to 100 Comparative Example 7 1.5 0 2 1.5 0 1 to 100 Comparative Example 8 1.5 0 2 1.5 1 1 to 100
[0115] Embodiment 15
[0116] The formula and dosage are the same as those in Example 12, except that the extracts are: 2 pieces of Panax notoginseng extract, 2 pieces of Phellodendron chinense bark extract, 2 pieces of Sophora flavescens root extract, 2 pieces of lotus seed extract, 2 pieces of bitter orange flower extract, and 2 pieces of dandelion extract.
[0117] Example 16
[0118] The formula and dosage are the same as those in Example 13, except that the extracts are: 3 notoginseng extract, 3 phellodendron chinense bark extract, 3 sophora flavescens root extract, 3 lotus seed extract, 3 bitter orange flower extract, and 3 dandelion extract.
[0119] Part III Efficacy Test
[0120] Antibacterial rate (Propionibacterium acnes) efficacy test
[0121] Test method:
[0122] 1 Experimental materials and methods
[0123] Instruments and equipment: anaerobic incubator, vertical high-pressure steam sterilizer, reagents, phosphate buffer, reinforced Clostridium medium (RCM), Propionibacterium acnes.
[0124] 2 Experimental methods
[0125] 2.1 Sample processing
[0126] Sample: Dilute with sterile water to a sample concentration of 5%;
[0127] Blank control: phosphate buffer;
[0128] Control sample group: Propionibacterium acnes suspension + phosphate buffer.
[0129] 2.2 Test steps
[0130] Take the suspension of Propionibacterium acnes, add it to each sample solution and control solution, mix it evenly, start timing, and when the specified action time is reached, make appropriate dilutions. Take 2-3 dilutions, respectively pipette the sample solution and control solution into two plates, pour the reinforced Clostridium medium (RCM) and mix evenly. After it solidifies, turn the plate over, put it in an anaerobic incubator and culture it for 48 hours, and count the live bacteria.
[0131] 3 Calculation formula
[0132] Antibacterial rate = (AB) / A×100%;
[0133] Where: A-average colony count of control samples; B-average colony count of test samples.
[0134] 4 Data Analysis
[0135] Evaluation criteria: If the antibacterial rate is ≥50% -90%, the product has antibacterial effect; if the antibacterial rate is ≥90%, the product has a strong antibacterial effect.
[0136] 5 Test results
[0137] The anti-acne compositions obtained in Examples 1-16 and Comparative Examples 1-8 were tested according to the above method, and the results are shown in Table 2;
[0138] Table 2 Test results of antibacterial rate of acne-removing compositions obtained from Examples 1-16 and Comparative Examples 1-8 at 5% concentration
[0139]
[0140] Result analysis:
[0141] Through the comparison of all the embodiments and comparative examples, it can be seen that the various material combinations of the present invention can achieve good antibacterial effects (for the industry, an antibacterial rate of more than 80% means a good antibacterial state, and an antibacterial rate of 90% means a satisfactory antibacterial state); specifically, in each implementation case and comparative case, as the concentration of Examples 1 to 5 increases, the antibacterial ability gradually increases. When the concentration is 5wt%, the antibacterial level of the ratio of Example 2 reaches the best state.
[0142] From the results of Examples 6 to 8, when the bitter orange flower extract 1 is added to the composition in a trace amount and the composition is maintained at a low concentration, it can improve the antibacterial properties of the composition. When the bitter orange flower extract 1 is added to the composition at a higher concentration, it cannot improve the antibacterial properties of the composition or inhibit the antibacterial properties of the composition.
[0143] From the results of Examples 9 to 11, it can be seen that the dandelion extract 1 has little effect on the antibacterial property of the composition. The possible reason is that the antibacterial activity itself is relatively poor. Examples 12 to 14 show a similar trend.
[0144] The experimental results of Example 15 and Example 16 can prove that different extraction methods have some differences in antibacterial properties.
[0145] From Comparative Example 1 and Comparative Example 2, when the Phellodendron chinense bark extract 1 and the lotus seed extract 1 are missing, the total concentration is kept consistent and the antibacterial performance is reduced to a certain extent, indicating that the Phellodendron chinense bark extract 1 and the lotus seed extract 1 show relatively important antibacterial effects in the composition of the present invention.
[0146] From Comparative Examples 3 to 8, bitter orange flower extract 1 and dandelion extract 1 both showed a certain degree of antibacterial synergistic effect on the basis of the compositions of Comparative Examples 1 and 2. In particular, a more obvious synergistic effect was shown in the composition of Comparative Example 1. However, the formulas of Example 2 and Example 5 of the present invention did not show obvious synergistic results under the same conditions. In the composition of Example 1, bitter orange flower extract 1 and dandelion extract 1 showed obvious synergistic results. The possible reason is that bitter orange flower extract 1 and dandelion extract 1 can better exert their effects only under the premise that the antibacterial performance of the composition has room for improvement.
[0147] 2. Acne removal efficacy test
[0148] Test method:
[0149] 1. Experimental purpose and principle
[0150] Macrophages can be used as a cell model to study the anti-acne efficacy of cosmetics. By stimulating with bacterial lipopolysaccharide (LPS), the content of inflammatory factor TNF-α in the negative control and test sample groups is determined to evaluate whether the test samples are effective in inhibiting the content of inflammatory factor TNF-α. The content of TNF-α is determined by enzyme-linked immunosorbent assay (ELISA).
[0151] This test refers to the laboratory method and compares the results of the cellular TNF-α inflammatory factor content determination of the test sample with that of the negative control. If the cellular TNF-α inflammatory factor content of the test sample is lower than that of the negative control and there is a significant difference (P < 0.05), it can be considered that the test sample has a certain acne-removing effect.
[0152] This test method is an in vitro method, which provides a method for detecting the content of TNF-α inflammatory factor in macrophages, and can be used as one of the evidence supports for the claim of acne-removing efficacy of cosmetic raw materials and finished products.
[0153] 2 Test indicators, refer to Table 3;
[0154] Table 3 Test indicators
[0155] Test indicators Criteria Relative content of TNF-α inflammatory factor The relative content of TNF-α inflammatory factor is lower than that of the negative control and has a significant difference with the negative control, which reflects that the sample has a certain acne-removing effect.
[0156] 3 Experimental materials and methods
[0157] 3.1 Instruments: RT-6100 ELISA analyzer;
[0158] 3.2 Cells used in the experiment
[0159] Macrophages: RAW264.7 cells;
[0160] 3.3 Test methods
[0161] (1) Treatment of test samples
[0162] Sample group: The sample was diluted with pure water to a solution with a volume fraction of 4%, and then filtered with a 0.22 μm filter, and the filtrate was collected as the sample mother solution.
[0163] Negative control: basal culture medium (cell activity test): basal culture medium containing LPS (TNF-α inflammatory factor content determination).
[0164] (2) Test operation steps
[0165] Cell activity test: RAW264.7 cells were plated in 96-well plates. After 24 hours, the culture medium was discarded and basal culture medium containing different concentrations of test samples was added. After 24 hours, the OD was detected by MTT method. 490nm The effects of the test samples on the activity of RAW264.7 cells were analyzed by t-test.
[0166] Determination of TNF-α inflammatory factor content: RAW264.7 cells were plated in 96-well plates and cultured for 24 hours, then replaced with basal culture medium containing different concentrations of test samples. After 24 hours, the cell supernatant was collected and centrifuged. The supernatant was aspirated and the TNF-α content in the cell culture supernatant was determined using an ELISA kit to obtain the effect of the test samples on the TNF-α content of macrophages.
[0167] (3) Calculation formula
[0168] TNF-α relative content (%) = (TNF-α content in sample / TNF-α content in negative control) * 100%;
[0169] (4) Data analysis
[0170] The statistical analysis software was SPSS, and the comparison between the test sample and the negative control was performed using the independent sample t test. The above statistical analyses were all two-tailed tests, and the significance level was α = 0.05. P>0.05 indicated that there was no significant difference between the two groups; P<0.05 indicated that there was a significant difference between the two groups.
[0171] 4 Test results
[0172] 4.1 Cell viability assay
[0173] Before testing the TNF-α inflammatory factor content in the sample cells, cell activity screening is performed to obtain the optimal test concentration.
[0174] 4.2 Cellular TNF-α inflammatory factor content test
[0175] After the concentration was screened by cell activity, the best test concentration was selected to determine the content of TNF-α inflammatory factor in RAW264.7 cells, and the effect of the sample on the content of TNF-α inflammatory factor in RAW264.7 cells was obtained. The test results are shown in Table 4.
[0176] Table 4 0.25% concentration acne removal test results of the acne removal compositions obtained from Examples 1-16 and Comparative Examples 1-8
[0177] Inhibition rate of TNF-α content in cells / % P-value Example 1 20.49 <0.05 Example 2 25.29 <0.05 Example 3 26.44 <0.05 Example 4 23.10 <0.05 Example 5 28.75 <0.05 Example 6 23.48 <0.05 Example 7 32.63 <0.05 Example 8 31.15 <0.05 Example 9 29.76 <0.05 Example 10 31.43 <0.05 Embodiment 11 28.62 <0.05 Example 12 34.15 <0.05 Embodiment 13 31.84 <0.05 Embodiment 14 31.76 <0.05 Embodiment 15 29.81 <0.05 Example 16 30.26 <0.05 Comparative Example 1 19.26 <0.05 Comparative Example 2 17.48 <0.05 Comparative Example 3 24.34 <0.05 Comparative Example 4 21.89 <0.05 Comparative Example 5 21.07 <0.05 Comparative Example 6 19.18 <0.05 Comparative Example 7 18.09 <0.05 Comparative Example 8 20.28 <0.05
[0178] According to the results in Table 4:
[0179] According to the data of Examples 1-5, the composition obtained by compounding Panax notoginseng extract, Phellodendron chinense bark extract, Sophora flavescens root extract and Lotus seed extract in the present invention has a certain inhibitory effect on cell TNF-α content at a concentration of 0.25%, achieving a good acne removal effect. Among them, after comprehensively considering the balance between dosage and effect, the TNF-α inhibitory effect is best when compounded in the ratio of Example 3.
[0180] According to the data of Examples 6-8 and Examples 1, 2 and 5, the TNF-α inhibitory effect can be significantly improved by adding different concentrations of bitter orange flower extract.
[0181] According to the data of Examples 9-11 and Examples 1, 2 and 5, the TNF-α inhibitory effect can be significantly improved by adding dandelion extracts of different concentrations.
[0182] According to the data of Examples 12-14 and Examples 1, 2 and 5, adding bitter orange flower extract and dandelion extract to the composition obtained by compounding Panax notoginseng extract, Phellodendron chinense bark extract, Sophora flavescens root extract and lotus seed extract can also significantly improve the TNF-α inhibitory effect.
[0183] According to the data comparison between Example 2 and Comparative Examples 1-2, compared with Example 2, in the absence of either the Phellodendron chinense bark extract or the lotus seed extract, the TNF-α content inhibition effect of Comparative Examples 1-2 was greatly reduced even if the dosage of other extracts was increased, indicating that the present invention uses a compound of Panax notoginseng extract, Phellodendron chinense bark extract, Sophora flavescens root extract and lotus seed extract to synergistically enhance the TNF-α inhibition effect.
[0184] Similarly, according to the data comparison between Comparative Example 1 and Comparative Examples 3-5, and the data comparison between Comparative Example 2 and Comparative Examples 6-8, it can be seen that both the bitter orange flower extract 1 and the dandelion extract 1 can improve the TNF-α inhibitory effect, but the degree of improvement is not as great as that of the compound composition of the present invention.
[0185] Acne test
[0186] Test Method
[0187] 1. Purpose of the experiment
[0188] This experiment verifies the acne-removing effect of the sample by testing the changes in the skin a* value and acne volume of 10 healthy male and female subjects before and after using the test sample.
[0189] 2 Test plan
[0190] 2.1 Subject screening criteria
[0191] The subjects were screened from the subject information database of Huamiao Efficacy Testing Laboratory, and healthy subjects who met the inclusion and exclusion criteria were selected.
[0192] 2.2 Subject Information
[0193] Gender of subjects: 8 females, 2 males;
[0194] Age of subjects: 20-40 years old.
[0195] Subject skin quality requirements: The facial skin must have a certain amount of acne and pimples, and must not have nodules or cysts that are difficult to improve with clinical preparations;
[0196] This test included 10 healthy subjects aged 20-40 years old, and the final valid data were 10 people.
[0197] 2.3 Sample information
[0198] The above information refers to Table 5;
[0199] Table 5 Samples, items, number of people, and testing basis information
[0200] serial number Sample name Test items Number of people Detection basis Remark 1 Example 2 2% solution Cosmetic acne-removing efficacy test 10 people TGDCDC 023-2022 "Test Methods for Anti-Acne Efficacy of Cosmetics" /
[0201] 2.4 Sample Usage
[0202] Application area: face;
[0203] Frequency of use: Use in the morning and evening;
[0204] Usage cycle: 3 weeks (use the product as required in the first and second weeks, and stop using the product in the third week);
[0205] How to use: After cleansing your face, apply an appropriate amount of sample all over your face.
[0206] 2.5 Test Method
[0207] 2.5.1 Instrument measurement parameters and related equipment refer to Table 6;
[0208] Table 6 Instrument measurement parameters and related equipment information
[0209] Serial number Measurement parameters Instrument Name Test time Test site Parameter Description 1 Skin a* value Skin color probe (ColorimeterCL 400) D0, D3, D7, D14, D21 Face The larger the measurement value, the higher the skin redness value 2 Acne volume Multifunctional 3D Skin Imaging Analyzer (Antera3D CS) D0, D3, D7, D14, D21 Face The larger the measurement value, the larger the skin acne
[0210] 2.5.2 Statistics
[0211] The statistical analysis software was SPSS, and the statistical methods all adopted two-tailed tests, with a test level of a=0.050. Descriptive statistics were performed on the data of each group: quantity, mean, standard deviation, etc., and the difference (rate of change) between each test area and the benchmark value was calculated. The Shapiro-Wilk Test was used to test the significance of the normal distribution of the data improvement value. If Sig. (two-sided)>0.050, it was normally distributed, and a T test was performed. If Sig. (two-sided)<0.050, it was non-normally distributed, and a Wilcoxon test was performed; the comparison of the graded data before and after use used the two-related sample rank sum test; the comparison between the test product and the control group used the independent sample T test or rank sum test. The above statistical analyses were all two-tailed tests, with a significance level of a=0.05. “ns” indicates no statistical difference, P>0.050; “*” indicates significant difference, 0.010≤P≤0.050, noted as “*”; 0.001≤P≤0.010, noted as “**”; P<0.001, noted as “***”.
[0212] 2.5.3 Result determination basis
[0213] Sample before and after comparison:
[0214] If the statistical method significance level P<0.050, it means that there is a statistically significant difference between the subjects before and after using the sample;
[0215] If the statistical method significance level P≥0.050, it means that there is no statistically significant difference between the subjects before and after using the samples.
[0216] Compared with the initial value, the analysis of the moisture content index of the stratum corneum of the sample area increased significantly after using the sample (P<0.050), and the skin a* value, skin oil content, acne volume or red zone area index analysis decreased significantly (P<0.050), indicating that the sample has an acne-removing effect.
[0217] 2.6 Test steps, see Table 7;
[0218] Table 7 Test steps
[0219] Visit Schedule Process Project Before using the sample (D0) The subjects come for a visit and are visually evaluated by trained professional testers. Subjects who meet the inclusion criteria are enrolled; Clean face and wait: the subjects clean their faces with a cleansing product and dry their skin with dry facial tissues, and sit quietly in a laboratory at a temperature of 21±1℃ and 50±10% RH for 30 minutes; Data collection of the basic value of the skin of the test subjects: laboratory technicians operate a multi-functional 3D skin imaging analyzer (Antera3D CS) and a skin color probe (Colorimeter CL400) to measure the relevant basic value indicators of the test parts of the subjects; laboratory technicians instruct the subjects to use the product according to the product usage requirements and the use parts, and provide written test precautions and product instructions; the subjects receive the samples and leave the laboratory. 3 days after using the sample (D3) Subjects return for a visit, clean their face and wait: clean their face with a cleansing product, dry their skin with a dry facial tissue, and sit quietly for 30 minutes in a laboratory at a temperature of 21±1°C and 50±10% RH; D3 data collection of the test subjects' skin: laboratory technicians operate a multifunctional 3D skin imaging analyzer (Antera3DCS) and a skin color probe (Colorimeter CL400) to measure relevant indicators of the test parts of the subjects; staff check the subjects' usage records and return the products to the subjects after weighing them. 7 days after using the sample (D7) Subjects return for a visit, clean their face and wait: clean their face with a cleansing product, dry their skin with a dry facial tissue, and sit quietly for 30 minutes in a laboratory at a temperature of 21±1°C and 50±10% RH; D3 data collection of the test subjects' skin: laboratory technicians operate a multifunctional 3D skin imaging analyzer (Antera3DCS) and a skin color probe (Colorimeter CL400) to measure relevant indicators of the test parts of the subjects; staff check the subjects' usage records and return the products to the subjects after weighing them. 14 days after using the sample (D14) Subjects return for a visit, clean their face and wait: clean their face with a cleansing product, dry their skin with a dry facial tissue, and sit quietly for 30 minutes in a laboratory at a temperature of 21±1°C and 50±10% RH; D3 data collection of the test subjects' skin: laboratory technicians operate a multifunctional 3D skin imaging analyzer (Antera3DCS) and a skin color probe (Colorimeter CL400) to measure relevant indicators of the test parts of the subjects; staff check the subjects' usage records and return the products to the subjects after weighing them. 21 days after using the sample (D21) The subjects returned for a visit, cleansed their faces and waited: cleansed their faces with cleansing products, dried their skin with dry facial tissues, and sat quietly in a laboratory at a temperature of 21±1℃ and 50±10% RH for 30 minutes; D3 data collection of the test subjects' skin: laboratory technicians operated the multi-functional 3D skin imaging analyzer (Antera3DCS) and skin color probe (Colorimeter CL400) to measure relevant indicators of the test parts of the subjects; staff checked the subjects' usage records and weighed the products; the test process ended.
[0220] 3 Test Results
[0221] 3.1 Skin a* value (Colorimeter CL400), statistical table see Table 8;
[0222] Table 8 Descriptive statistics of skin a* values (n=10)
[0223]
[0224] Note: ① Normality test P value>0.050, that is, the data obeys the normal distribution, and the paired T test is used; if it does not obey the normal distribution, the rank sum test is used.
[0225] ②“n” indicates the number of people using the product. Due to the small sample size, the P value is for reference only. The difference analysis is shown in Table 9;
[0226] Table 9 Analysis of skin a* value differences (n=10)
[0227]
[0228] Note: ①Significant P value <0.050, that is, there is a significant difference between before and after use;
[0229] The significant P value is ≥0.050, that is, there is no significant difference between before and after use.
[0230] ②“n” represents the number of people using the product. Due to the small sample size, the P value is for reference only.
[0231] The instrument test and evaluation results show that:
[0232] After using the samples for 3 days, the skin a* value of the 10 subjects decreased by 2.42%, which was not significantly different from before using the samples (P>0.050); after using the samples for 7 days, the skin a* value decreased by 6.01%, which was significantly different from before using the samples (P<0.010); after using the samples for 14 days, the skin a* value decreased by 13.34%, which was significantly different from before using the samples (P<0.001); after using the samples for 21 days, the skin a* value decreased by 11.54%, which was significantly different from before using the samples (P<0.001), indicating that the samples have an improving effect on the degree of skin acne inflammation.
[0233] 3.2 Acne volume (Antera3D CS), volume description statistics are shown in Table 10;
[0234] Table 10 Descriptive statistics of acne volume (n=10)
[0235]
[0236] Note: ① Normality test P value>0.050, that is, the data obeys the normal distribution, and the paired T test is used; if it does not obey the normal distribution, the rank sum test is used.
[0237] ② "n" indicates the number of people using the product. Due to the small sample size, the P value is for reference only. The difference analysis is shown in Table 11;
[0238] Table 11 Analysis of differences in acne volume (n=10)
[0239]
[0240] Note: ①Significant P value <0.050, that is, there is a significant difference between before and after use;
[0241] The significant P value is ≥0.050, that is, there is no significant difference between before and after use.
[0242] ②“n” represents the number of people using the product. Due to the small sample size, the P value is for reference only.
[0243] The instrument test and evaluation results show that:
[0244] After 10 subjects used the samples for 3 days, the volume of acne decreased by 3.29%, which was not significantly different from before using the samples (P>0.050); after using the samples for 7 days, the volume of acne decreased by 34.21%, which was not significantly different from before using the samples (P>0.050); after using the samples for 14 days, the volume of acne decreased by 53.95%, which was significantly different from before using the samples (P<0.010); after using the samples for 21 days, the volume of acne decreased by 59.21%, which was significantly different from before using the samples (P<0.010), indicating that the samples have an improvement effect on the acne area of the skin.
[0245] 4. Irritation test
[0246] Test Method
[0247] 1. Experimental purpose and principle
[0248] The chicken embryo chorioallantoic membrane test is an early in vitro eye irritation assessment method. The chorioallantoic membrane (CAM) is a respiratory membrane that surrounds the chicken embryo. This test uses the characteristics of the intact, clear and transparent vascular system of the chorioallantoic membrane of the mid-stage incubated chicken embryo. A certain amount of the test substance is directly exposed to the chicken embryo chorioallantoic membrane. After a period of exposure, the changes in the toxic effect indicators of the chorioallantoic membrane (such as bleeding, coagulation and vascular melting) are observed. These indicators reflect the changes in the morphological structure, color and permeability of the blood vessels and vascular networks, as well as the phenomena such as the denaturation of the chorioallantoic membrane proteins and the degree of damage. Then a score is obtained by combining them to evaluate the eye irritation of the test substance.
[0249] The purpose of this test is to test the ability of the test substance to cause toxic changes in the chicken embryo chorioallantoic membrane and to evaluate the elements and processes of the potential eye irritation of the evaluated substance.
[0250] This test method is an in vitro method and is suitable for the detection of cosmetics and cosmetic raw materials.
[0251] 2 Test indicators
[0252] CAMVA irritation test: ES≤4, non-irritating; 4<ES≤12, mild irritating; 12<ES<16, moderate irritating; ES≥16, strong irritating / corrosive.
[0253] 3 Experimental materials and methods
[0254] 3.1 Instruments and equipment: fully automatic incubator, stereo microscope, SPF chicken embryos;
[0255] 3.2 Reagents: sodium chloride, sodium dodecyl sulfate (SDS);
[0256] 3.3 Incubation conditions
[0257] Room temperature 20℃~25℃, relative humidity 45%~70%. Incubation temperature 37.5℃±0.5℃, relative humidity 55%~70%, turntable 3 times / h~6 times / h. Rotation is not necessary when incubating 9-day-old chick embryos.
[0258] 3.4 Test methods
[0259] (1) Test operation steps
[0260] In this test, 6 embryos were selected for each group, and the conditions of the chorioallantoic membrane were recorded with a camera. A polytetrafluoroethylene resin ring was placed on the chorioallantoic membrane of the chicken embryo and photographed. The sample to be tested was added to the polytetrafluoroethylene resin ring, the time of adding the sample was recorded, and the air chamber was covered with a moistened plastic wrap. The chicken embryo was moved to a constant temperature and humidity chamber for culture, and the degree of change of each toxic effect was observed.
[0261] (2) Observation of results
[0262] Bleeding, coagulation, and vascular melting were observed and recorded, and scored according to their severity.
[0263] (3) Data analysis
[0264] The scoring criteria are shown in Table 12;
[0265] Table 12 Scoring criteria
[0266]
[0267] The endpoint evaluation method was used to conduct the test and calculate the endpoint evaluation (ES), with the result retained to two decimal places; the score of each chicken embryo = the sum of the bleeding, coagulation and vascular melting observed in each chicken embryo; ES = the average of the mathematical sums obtained for 6 chicken embryos.
[0268] According to the above test method, Examples 1-16 and Comparative Examples 1-8 were diluted into 2% aqueous solutions and tested for samples. The results showed that they were non-irritating.
[0269] Wherein, the chicken embryo result of embodiment 2 is as follows Figure 1-Figure 2 As shown, Figure 1 This is a chicken embryo observation picture before using the sample of Example 2. Figure 2 This is a chicken embryo observation diagram after using the sample of Example 2. The test result of the sample of Example 2 is ES=3.00;
[0270] This proves that the technical solution of the present invention is mild and non-irritating.
[0271] Application Examples
[0272] An acne-removing product is prepared according to the formula table in Table 13, and the preparation method is as follows:
[0273] Step 1: Pre-mix phase A2 and stir to disperse evenly.
[0274] Step 2: Add the pure water in phase A1 to the homogenizer, turn on the homogenizer, add the pre-dispersed phase A2, and homogenize at medium speed for 30-60 seconds. Then add the remaining raw materials in phase A1 in turn, stir and heat to 80-85℃, and homogenize at medium speed for 1-2 minutes until there are no gel particles. After keeping warm for 30 minutes, stir and cool down.
[0275] Step 3: After the temperature drops to 45°C, add phases B and C in sequence, and stir evenly to obtain an acne-removing product; the formula is shown in Table 13;
[0276] Table 13 Basic acne-removing product formula
[0277]
[0278] The applicant declares that the present invention illustrates the process method of the present invention through the above-mentioned embodiments, but the present invention is not limited to the above-mentioned process steps, and it does not mean that the present invention must rely on the above-mentioned process steps to be implemented. Those skilled in the art should understand that any improvement of the present invention, equivalent replacement of the raw materials selected by the present invention, addition of auxiliary components, selection of specific methods, etc., all fall within the protection scope and disclosure scope of the present invention.
Claims
1. An anti-acne composition, characterized in that: It includes the following components by weight: 0.1-10 parts of Panax notoginseng extract; 0.1-10 parts of Phellodendron chinense bark extract; 0.5-15 parts of Sophora flavescens root extract; 0.1-10 parts of lotus seed extract; The preparation method of the Panax notoginseng extract is as follows: crush the Panax notoginseng raw material into powder, add 45-60wt% ethanol for extraction, filter after extraction, purify the filtrate using an HP-20 macroporous resin column, and then concentrate the Panax notoginseng extract to complete dryness to obtain the Panax notoginseng extract; The preparation method of the Huangpi tree bark extract comprises: crushing the Huangpi tree bark into powder, then adding ethanol with a concentration of 70 to 90 wt % and continuously refluxing and extracting until it is colorless, centrifuging the filtrate after the extraction is completed, concentrating the filtrate to remove ethanol, and vacuum drying and drying to a powder state to obtain the Huangpi tree bark extract; The preparation method of the Sophora flavescens root extract comprises: crushing the Sophora flavescens root raw material into powder, adding ethanol with a concentration of 70 to 90 wt% for extraction, filtering after the extraction is completed, purifying and decolorizing the filtrate using a neutral alumina column, and then concentrating the Sophora flavescens root extract to complete dryness to obtain the Sophora flavescens root extract; The preparation method of the lotus seed extract comprises the following steps: crushing the lotus seed raw material into powder, adding pure water to perform heating extraction, centrifuging after the extraction is completed, and then concentrating the lotus seed extract until it is completely dry to obtain the lotus seed extract.
2. The anti-acne composition according to claim 1, characterized in that: Also includes bitter orange flower extract and / or dandelion extract; The preparation method of the bitter orange flower extract comprises: crushing the bitter orange flower into powder, then adding ethanol with a concentration of 70 to 90 wt % and continuously refluxing and extracting until it becomes colorless, centrifuging the filtrate after the extraction is completed, concentrating the filtrate to remove ethanol, and vacuum drying and drying to a powder state to obtain the bitter orange flower extract; The preparation method of the dandelion extract is as follows: crushing the dandelion raw material into powder, adding pure water to perform heating reflux extraction, centrifuging after the extraction is completed, and then concentrating the dandelion extract into an extract, adding water to suspend the extract, purifying it with a polyamide resin column, and then decompressing and concentrating the eluate to complete dryness to obtain the dandelion extract.
3. The anti-acne composition according to claim 2, characterized in that: The bitter orange flower extract is used in an amount of 0.1 to 10 parts and / or the dandelion extract is used in an amount of 0.1 to 10 parts.
4. The anti-acne composition according to claim 3, characterized in that: It includes the following components by weight: 0.5-5 parts of Panax notoginseng extract; 0.5-5 parts of Phellodendron chinense bark extract; 1-10 parts of Sophora flavescens root extract; 0.5-5 parts of lotus seed extract; 0.5-5 parts of bitter orange flower extract; 0.5-5 parts of dandelion extract.
5. Use of the anti-acne composition according to any one of claims 1 to 4 in preparing cosmetics.
6. An acne-removing product, characterized in that: Contains the anti-acne composition according to any one of claims 1 to 4.
7. The acne-removing product according to claim 6, characterized in that: The content of the anti-acne composition is 0.1-30wt%.
Citation Information
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