An eye cream with anti-wrinkle effect and a preparation method thereof
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-12-05
- Publication Date
- 2026-08-11
AI Technical Summary
[0051](1)本发明提供的一种抗皱眼霜,选用中草药组合物为核心抗皱成分,搭配使用搭配抗衰功效成分阿拉伯茉莉和单子山楂花提取物、乙酰基四肽-11、乙酰基四肽-9,能够多维度发挥最佳的抗皱功效,制得的眼霜稳定性好,刺激性小,抗皱功效佳。
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Figure CN117618317B_ABST
Abstract
Description
Technical Field
[0001] This invention belongs to the field of cosmetic technology, specifically relating to an eye cream with anti-wrinkle effects and its preparation method. Background Technology
[0002] Skin wrinkles are lines of wrinkle formation on the skin caused by degenerative changes in the morphology and structure of dermal collagen fibers, elastic fibers, and matrix, as well as by a reduction in subcutaneous fat and loss of skin moisture, resulting from the long-term, repetitive traction of limb joints and local subcutaneous muscles. Traditional Chinese medicine does not have a corresponding disease name for wrinkles; based on their clinical characteristics and manifestations, they can be categorized under terms such as "anti-aging and wrinkle removal," "reducing wrinkles," and "anti-aging and preventing aging."
[0003] Modern medicine believes that wrinkles are mainly the result of natural skin aging and photoaging, and are related to multiple factors. With age, the natural moisturizing factors in the stratum corneum of the epidermis decrease, the skin's hydration capacity declines, leading to reduced moisture in skin cells, cell shrinkage, aging, and the appearance of fine wrinkles. Under the influence of various factors, the number of dermal fibroblasts decreases, the ratio of collagen types reverses, and elastic fibers in the papillary and reticular layers of the dermis decrease and degenerate. Disordered arrangement of collagen and elastic fibers leads to wrinkle formation. With age, the volume of subcutaneous fat cells decreases, and adipose tissue gradually atrophies, causing the fibrous trabeculae in the lower reticular layer of the dermis and fascia to lose support, resulting in skin laxity. Combined with the effects of gravity, this causes the loose skin to sag, forming wrinkles. Furthermore, facial wrinkles are also related to facial expression muscles. These muscles attach to the skin, and when they contract, wrinkles appear at right angles to the contraction, increasing in number and depth with age.
[0004] In the prior art, there have been some reports on wrinkle removal. For example, patent document CN102641228A provides an anti-wrinkle eye cream with Rhodiola rosea root extract, black tea extract, Coix seed extract, and Lonicera japonica flower extract as the main active ingredients. Its anti-wrinkle efficacy is only 90%, which needs further improvement. Patent document CN103479552A provides a gold-containing anti-wrinkle eye cream, which is expensive, and the long-term safety of the gold element needs further verification. Patent document CN112704712A discloses a traditional Chinese medicine composition for eye care, which selects traditional Chinese medicine materials such as Ligusticum chuanxiong, Poria cocos, Atractylodes macrocephala, Bletilla striata, Ampelopsis japonica, artificial bezoar, pearl, and borneol. Through reasonable formulation, the resulting additive has good antioxidant, whitening, and blood-activating effects. This traditional Chinese medicine additive has multiple effects, but its anti-wrinkle effect on the eyes is insufficient.
[0005] Therefore, it is proposed that an eye cream with anti-wrinkle effect and its preparation method be described in this invention. Summary of the Invention
[0006] To address the aforementioned technical problems, the present invention aims to provide an eye cream with anti-wrinkle effects and its preparation method, which selects active ingredients from traditional Chinese medicine, combines them with other functional ingredients, has low irritation, and achieves highly effective anti-wrinkle effects.
[0007] To achieve the above objectives, the present invention adopts the following technical solution:
[0008] In a first aspect, the present invention provides an eye cream with anti-wrinkle effects, comprising, by weight, the following raw materials:
[0009]
[0010] As a further preferred embodiment of the technical solution of the present invention, the herbal extract is prepared from 100-200 parts of ginseng, 100-200 parts of kudzu root, 50-150 parts of Solomon's seal, 10-100 parts of poria cocos, 10-100 parts of angelica sinensis, 1-5 parts of pearl, 0.1-3 parts of artificial bezoar, and 0.1-3 parts of borneol.
[0011] In the above technical solution, the herbal composition of the present invention is composed of eight medicinal materials: ginseng, kudzu root, poria cocos, polygonatum odoratum, angelica sinensis, pearl, artificial bezoar, and borneol. This formula emphasizes invigorating qi, nourishing yin, and moistening dryness. Ginseng and kudzu root are the principal herbs, which have the effects of promoting body fluid production and nourishing blood. Poria cocos, angelica sinensis, and polygonatum odoratum are the assistant herbs, which have the effects of dredging qi and blood, nourishing yin and moistening dryness, and promoting body fluid production and quenching thirst. Borneol is the adjuvant herb, which opens the orifices, disperses stagnant heat, reduces swelling and relieves pain. Pearl and artificial bezoar are the guiding herbs, which have the effect of harmonizing the various herbs, in line with the basic principles of traditional Chinese medicine for the prevention and treatment of wrinkles.
[0012] The above technical solution uses core Chinese herbal anti-wrinkle ingredients, combined with jasmine flower extract, hawthorn flower extract, acetyl tetrapeptide-11, and acetyl tetrapeptide-9, which can exert the best anti-wrinkle effect from multiple dimensions.
[0013] The above technical solution utilizes the synergistic and complementary active effects of two white flower extracts, Arabian jasmine and hawthorn flower, with a standardized flavonoid content exceeding 800ppm. This three-in-one eye care ingredient can effectively improve eye microcirculation, reduce protein glycation, improve dark circles, lift the upper eyelids, improve eye wrinkles, restore skin firmness, and brighten the eyes.
[0014] In the above technical solution, acetyl tetrapeptide-11 and acetyl tetrapeptide-9 work synergistically to increase the synthesis of multiligand polysaccharide-1 and collagen XVII in reconstructed skin and keratinocytes, respectively, thereby improving the density and structure of extracellular collagen fibers in 3D bioprinted skin. The two peptides can promote the synthesis of key dermal and epidermal components. Acetyl tetrapeptide-9 and acetyl tetrapeptide-11 work synergistically to address skin aging problems from multiple angles, quickly and visibly reducing wrinkles and firming the skin, providing three-dimensional anti-aging.
[0015] As a more preferred technical solution of the present invention, the herbal extract is prepared from 120-180 parts of ginseng, 120-180 parts of kudzu root, 80-120 parts of Solomon's seal, 40-60 parts of poria cocos, 40-60 parts of angelica sinensis, 2-4 parts of pearl, 0.5-2 parts of artificial bezoar, and 0.5-2 parts of borneol.
[0016] As the preferred technical solution of the present invention, the herbal extract is prepared from 160 parts ginseng, 140 parts kudzu root, 100 parts Solomon's seal, 50 parts Poria cocos, 50 parts Angelica sinensis, 3 parts pearl, 1 part artificial bezoar, and 1 part borneol.
[0017] As a further preferred embodiment of the technical solution of the present invention, the preparation of the herbal extract includes the following steps:
[0018] (1) Take ginseng, kudzu root, poria cocos, polygonatum odoratum and angelica sinensis by weight, put them in a steam explosion machine for steam explosion treatment, and then depressurize to obtain depressurized material;
[0019] (2) The pressure relief material obtained in step (1) is subjected to countercurrent extraction to obtain filtrate and filter residue;
[0020] (3) Add water to the filter residue obtained in step (2) and treat it under ultrasound, then filter to obtain filter residue liquid;
[0021] (4) Take the filtrate obtained in step (2) and the residue obtained in step (3) and mix them together. Then add ethanol for alcohol precipitation, let stand and filter. Recover the ethanol from the filtrate under reduced pressure until there is no alcohol taste. Then continue to concentrate under reduced pressure to obtain concentrated Chinese herbal medicine.
[0022] (5) Dissolve artificial bezoar and borneol in a solvent, then add pearl and the concentrated Chinese herbal medicine solution obtained in step (4) in sequence, and finally add solvent and deionized water to mix well. After filtration, the product is obtained.
[0023] As a further preferred embodiment of the technical solution of the present invention, in step (1), saturated steam is used for steam explosion and the steam is treated at 1.1-1.2 MPa for 1-3 minutes;
[0024] In step (2), the countercurrent extraction temperature is 20-25℃, the countercurrent extraction time is 10-30 min, and the countercurrent extraction solvent is an aqueous solution containing 1-1.2 g / L Tween 80;
[0025] In step (3), the ultrasonic treatment power is 80-120W, the ultrasonic treatment time is 0.5-5h, and the mass ratio of filter residue to water is 1:8-15.
[0026] In step (4), the ethanol concentration of the alcohol precipitation is 50-70 wt%; the concentration is carried out under reduced pressure to a relative density of 1.15-1.25;
[0027] In step (5), the solvent is one or more of butanediol, 1,3-propanediol, or glycerol; filtration is performed sequentially using 1.0 μm and 0.60 μm microporous filter membranes made of titanium rods. Preferably, the solvent is 1,3-propanediol, because 1,3-propanediol has good safety and moisturizing properties, and it has excellent solubility for the herbal medicines of this invention.
[0028] As a further preferred embodiment of the technical solution of the present invention, the excipients of the eye cream are selected from one or more of polyols, moisturizers, emollients, emulsifiers, thickeners, antioxidants, metal ion chelating agents, preservatives, pH adjusters, antioxidants, and deionized water, by weight.
[0029] As a further preferred embodiment of the technical solution of the present invention, the emollient is selected from one or more of the following: shea butter, phytosterol isostearate, hydrogenated polydecene, isononyl isononanoate, polydimethylsiloxane, squalane, cetearyl alcohol, isohexadecane, and cyclopentamethoxysiloxane. Preferably, the emollient is shea butter, polydimethylsiloxane, or squalane.
[0030] The emulsifier is selected from one or more of sodium stearoyl glutamate, cetearyl oleate, cetearyl palmitate, sorbitan oleate, and PEG-100 stearate.
[0031] The preservative is selected from one or more of phenoxyethanol, ethylhexylglycerin, chlorphenesin, methylparaben, p-hydroxyacetophenone, propylparaben, 1,2-hexanediol, and sorbitan octanoate.
[0032] The chelating agent is selected from one or more of disodium EDTA, EDTA, and tetrasodium EDTA.
[0033] The polyol is selected from one or more of glycerol, propylene glycol, butylene glycol, sorbitol, dipropylene glycol, 1,3-propanediol, pentanediol, and hexanediol.
[0034] The antioxidant is selected from one or more of butylated hydroxytoluene, butylated hydroxyanisole, and tocopheryl acetate.
[0035] The thickener is selected from one or two of hydroxyethyl acrylate / sodium acryloyl dimethyl taurate copolymer and sorbitan isostearate.
[0036] Secondly, the present invention also provides a method for preparing the above-mentioned eye cream, comprising the following steps:
[0037] (1) Add the thickener to the first polyol and stir well to obtain mixture 1 for later use;
[0038] (2) Add purified water to the emulsification tank, then add the first part of emulsifier, sodium hyaluronate, the second part of polyol, the first part of preservative, and chelating agent. Slowly heat to 79-83°C, keep warm and stir until the material is completely dissolved to obtain mixture 2.
[0039] (3) Add the emollient, the second part of the emulsifier and the antioxidant to the reaction vessel in sequence, heat to 80-85°C while stirring, mix evenly until completely dissolved, and obtain mixture 3;
[0040] (4) The mixture 3 obtained in step (3) is filtered into the emulsification tank of step (2), kept at 79-83°C, then vacuum homogenized and stirred until the material is evenly dispersed to obtain mixture 4.
[0041] (5) Add the mixture 1 obtained in step (1) to the mixture 4 obtained in step (4), perform vacuum homogenization and keep stirring until the material is uniform, then cool down to 40-50℃ to obtain mixture 5.
[0042] (6) Add the Chinese herbal medicine extract, jasmine flower extract, hawthorn flower extract, acetyl tetrapeptide-11, and acetyl tetrapeptide-9 to the mixture 5 obtained in step (5), and after vacuum homogenization, keep stirring until the mixture is uniform to obtain mixture 6.
[0043] (7) Add the second part of the preservative to the mixture 6 obtained in step (6), homogenize under vacuum and keep stirring until the mixture is uniform, then cool down and stop stirring to obtain the eye cream.
[0044] As a further preferred embodiment of the technical solution of the present invention, in step (2) of the above preparation method, the stirring speed is 30-50 rpm.
[0045] In step (3), the stirring speed is 600-900 rpm;
[0046] In step (4), the vacuum homogenization speed is 2000-2500 rpm and the time is 8-12 min; the stirring speed is 30-50 rpm.
[0047] In step (5), the vacuum homogenization speed is 2000-2500 rpm, the time is 8-12 min, and the stirring speed is 30-50 rpm;
[0048] In step (6), the vacuum homogenization speed is 1500-2000 rpm and the time is 3-5 min; the stirring speed is 30-50 rpm and the stirring time is 8-10 min.
[0049] In step (7), the vacuum homogenization speed is 1500-2000 rpm, the time is 1-2 min, the stirring time is not less than 15 min, and the temperature is reduced to below 40℃.
[0050] Compared with the prior art, the present invention has the following beneficial effects:
[0051] (1) The present invention provides an anti-wrinkle eye cream, which uses a combination of traditional Chinese medicine as the core anti-wrinkle ingredients, and combines it with anti-aging ingredients such as Arabian jasmine and hawthorn flower extract, acetyl tetrapeptide-11 and acetyl tetrapeptide-9. It can exert the best anti-wrinkle effect in multiple dimensions. The resulting eye cream has good stability, low irritation and good anti-wrinkle effect.
[0052] (2) The present invention provides a method for preparing an anti-wrinkle eye cream with a simple process flow, which is easy to scale up the production of eye cream products.
[0053] (3) The herbal composition used in the anti-wrinkle eye cream provided by the present invention is prepared by combining eight herbal materials. Ginseng, kudzu root, poria cocos, polygonatum odoratum and angelica sinensis are specifically selected. From the perspective of traditional Chinese medicine prevention and treatment of wrinkles, the focus is on tonifying qi, nourishing yin and moisturizing dryness. Artificial bezoar and pearl are added to further enhance the skin beautifying and antioxidant effects of the product. Borneol is added to promote the transdermal absorption of other active ingredients, which greatly improves the skin tightening and anti-aging effects of the product. At the same time, the herbal composition has excellent DPPH free radical scavenging, hydroxyl free radical scavenging and superoxide anion scavenging effects, and also has a good inhibitory effect on skin photoaging, with significant anti-wrinkle effect.
[0054] (4) The present invention provides an anti-wrinkle eye cream. Regarding the preparation method of the herbal composition, the present invention abandons the traditional water extraction and alcohol precipitation process and makes targeted optimizations. Specifically: the present invention first performs steam explosion treatment on ginseng, kudzu root, poria cocos, polygonatum odoratum and angelica sinensis to break cell tissues, which facilitates the subsequent countercurrent immersion to improve the efficiency of extracting effective ingredients. At the same time, the countercurrent immersion uses water solvent containing Tween 80 as the extraction solvent, which is safe and non-toxic. Compared with traditional water solvents, the anti-wrinkle effect of the herbal composition obtained is more significant because the addition of Tween 80 helps to reduce interfacial tension and facilitates the extraction and dissolution of ingredients. For the treatment of filter residue, ultrasonic-assisted water extraction is further adopted to minimize the loss of effective ingredients. Finally, alcohol precipitation is performed to obtain the herbal extract. In the process of adding artificial bezoar, borneol and pearl, the applicant also optimized the solvent, that is, using 1,3-propanediol, which has better solubility. Attached Figure Description
[0055] Figure 1 The image shows the anti-wrinkle effect on the skin around the eyes of the subjects in the example group (VISIA-CR Standard 2 light source mode photo).
[0056] Figure 2 This image shows the anti-wrinkle effect on the skin around the eyes of the subjects in the comparative group (VISIA-CR Standard 2 light source mode photo). Detailed Implementation
[0057] The technical solutions of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention.
[0058] Unless otherwise specified, in all embodiments and comparative examples of this invention, the raw materials and medicinal herbs were obtained through market channels. Specifically, the pearl in the herbal composition was added in the form of pearl extract; acetyl tetrapeptide-11 and acetyl tetrapeptide-9 were added in the form of a compound, the trade name of which is... BASF products; Jasmine flower extract and Hawthorn flower extract were added in the form of a compound under the trade name EYE FECTIVE (purchased from Guangzhou Nuoran Biotechnology Co., Ltd.); Phenoxyethanol / Ethylhexylglycerin was traded as euxyl PE 9010; Hydroxyethyl acrylate / Sodium acryloyl dimethyl taurate copolymer / Sorbitan isostearate was traded as SEPINOV WEO; Cetearyl oleate / Sorbitan oleate was traded as Olivem 1000; Cetyl palmitate was traded as Olivax LC.
[0059] Meanwhile, the equipment used in this invention, such as steam explosion and countercurrent extraction, are all commercially available equipment.
[0060] Example 1
[0061] A traditional Chinese medicine composition with anti-wrinkle effects is made from the following raw materials by weight:
[0062]
[0063] In this embodiment, a method for preparing the above-mentioned traditional Chinese medicine composition is also provided, comprising the following steps:
[0064] (1) Take ginseng, kudzu root, poria cocos, polygonatum odoratum and angelica sinensis by weight, place them in a steam explosion machine and steam explosion at 1.15 MPa for 2 minutes with saturated steam, then depressurize to obtain depressurized material;
[0065] (2) The pressure relief material obtained in step (1) is subjected to countercurrent extraction at 20°C for 1 hour to obtain filtrate and filter residue; the solvent used for countercurrent extraction is an aqueous solution containing 1.1 g / L Tween 80.
[0066] (3) According to the mass ratio of filter residue to water of 1:10, add water to the filter residue obtained in step (2) and ultrasonically treat it at a power of 100W for 0.5h, and filter to obtain filter residue liquid.
[0067] (4) Take the filtrate obtained in step (2) and the residue obtained in step (3) and mix them together. Then add ethanol to the concentration of 70wt% for alcohol precipitation. Let it stand and filter. Recover the ethanol from the filtrate under reduced pressure until there is no alcohol taste. Then continue to concentrate under reduced pressure to 1.2 (about 60℃) to obtain the concentrated Chinese herbal medicine.
[0068] (5) Dissolve artificial bezoar and borneol in 0.8L of 1,3-propanediol, then add pearl extract (equivalent to 3g of pearl) and the concentrated Chinese herbal medicine solution obtained in step (4) in sequence. Finally, add 4L of 1,3-propanediol and deionized water and mix well. After filtering with titanium rods and 1.0μm and 0.60μm microporous filter membranes in sequence, the Chinese herbal medicine extract is obtained.
[0069] Example 2
[0070] An anti-wrinkle eye cream, by weight, is prepared from the following ingredients:
[0071]
[0072] The herbal extract in phase D was prepared in Example 1.
[0073] In this embodiment, a method for preparing the eye cream is also provided, comprising the following steps:
[0074] (1) Add the hydroxyethyl acrylate / sodium acryloyl dimethyl taurate copolymer / sorbitan isostearate in phase C to butanediol, stir evenly to obtain mixture 1, and set aside;
[0075] (2) Add the purified water in phase A to the emulsification tank, then add sodium stearoyl glutamate, sodium hyaluronate, 1,3-propanediol, 1,2-hexanediol and disodium EDTA. Slowly heat to 80°C and stir (40 rpm) until the material is completely dissolved to obtain mixture 2.
[0076] (3) Add polydimethylsiloxane, squalane, cetyl palmitate, cetearyl oleate / sorbitan oleate, PEG-100 stearate, shea butter and tocopheryl acetate from phase B to the reaction vessel in sequence, heat to 80°C under stirring (800 rpm), mix evenly until completely dissolved to obtain mixture 3;
[0077] (4) The mixture 3 obtained in step (3) is filtered into the emulsification tank of step (2), kept at 80°C, then vacuum homogenized (2000 rpm, 10 min) and stirred (50 rpm) until the material is evenly dispersed to obtain mixture 4.
[0078] (5) Add the mixture 1 obtained in step (1) to the mixture 4 obtained in step (4), vacuum homogenize (2200 rpm, 10 min), and then keep stirring (50 rpm) until the material is uniform. Then cool down to 45°C to obtain mixture 5.
[0079] (6) After filtering the active ingredients in phase D through a 200-mesh sieve, add them to the mixture 5 obtained in step (5), vacuum homogenize (1800 rpm, 5 min), and then keep stirring (50 rpm, 8 min) until the material is uniform to obtain mixture 6.
[0080] (7) Add the phenoxyethanol / ethylhexylglycerin in phase E to the mixture 6 obtained in step (6), homogenize under vacuum for 2 minutes, and then keep stirring for more than 15 minutes until the mixture is uniform. Then cool down to below 40°C and stop stirring to obtain the eye cream.
[0081] Example 3
[0082] An anti-wrinkle eye cream, by weight, is prepared from the following ingredients:
[0083]
[0084]
[0085] The herbal extract in phase D was prepared in Example 1.
[0086] In this embodiment, a method for preparing the eye cream is also provided, comprising the following steps:
[0087] (1) Add the hydroxyethyl acrylate / sodium acryloyl dimethyl taurate copolymer / sorbitan isostearate in phase C to butanediol, stir evenly to obtain mixture 1, and set aside;
[0088] (2) Add the purified water in phase A to the emulsification tank, then add sodium stearoyl glutamate, sodium hyaluronate, 1,3-propanediol, 1,2-hexanediol and disodium EDTA. Slowly heat to 80°C and stir (40 rpm) until the material is completely dissolved to obtain mixture 2.
[0089] (3) Add polydimethylsiloxane, squalane, cetyl palmitate, cetearyl oleate / sorbitan oleate, PEG-100 stearate, shea butter and tocopheryl acetate from phase B to the reaction vessel in sequence, heat to 80°C under stirring (800 rpm), mix evenly until completely dissolved to obtain mixture 3;
[0090] (4) The mixture 3 obtained in step (3) is filtered into the emulsification tank of step (2), kept at 80°C, then vacuum homogenized (2000 rpm, 10 min) and stirred (50 rpm) until the material is evenly dispersed to obtain mixture 4.
[0091] (5) Add the mixture 1 obtained in step (1) to the mixture 4 obtained in step (4), vacuum homogenize (2200 rpm, 10 min), and then keep stirring (50 rpm) until the material is uniform. Then cool down to 45°C to obtain mixture 5.
[0092] (6) After filtering the active ingredients in phase D through a 200-mesh sieve, add them to the mixture 5 obtained in step (5), vacuum homogenize (1800 rpm, 5 min), and then keep stirring (50 rpm, 8 min) until the material is uniform to obtain mixture 6.
[0093] (7) Add the phenoxyethanol / ethylhexylglycerin in phase E to the mixture 6 obtained in step (6), homogenize under vacuum for 2 minutes, and then keep stirring for more than 15 minutes until the mixture is uniform. Then cool down to below 40°C and stop stirring to obtain the eye cream.
[0094] Example 4
[0095] An anti-wrinkle eye cream, by weight, is prepared from the following ingredients:
[0096]
[0097]
[0098] The herbal extract in phase D was prepared in Example 1.
[0099] In this embodiment, a method for preparing the eye cream is also provided, comprising the following steps:
[0100] (1) Add the hydroxyethyl acrylate / sodium acryloyl dimethyl taurate copolymer / sorbitan isostearate in phase C to butanediol, stir evenly to obtain mixture 1, and set aside;
[0101] (2) Add the purified water in phase A to the emulsification tank, then add sodium stearoyl glutamate, sodium hyaluronate, 1,3-propanediol, 1,2-hexanediol and disodium EDTA. Slowly heat to 80°C and stir (40 rpm) until the material is completely dissolved to obtain mixture 2.
[0102] (3) Add polydimethylsiloxane, squalane, cetyl palmitate, cetearyl oleate / sorbitan oleate, PEG-100 stearate, shea butter and tocopheryl acetate from phase B to the reaction vessel in sequence, heat to 80°C under stirring (800 rpm), mix evenly until completely dissolved to obtain mixture 3;
[0103] (4) The mixture 3 obtained in step (3) is filtered into the emulsification tank of step (2), kept at 80°C, then vacuum homogenized (2000 rpm, 10 min) and stirred (50 rpm) until the material is evenly dispersed to obtain mixture 4.
[0104] (5) Add the mixture 1 obtained in step (1) to the mixture 4 obtained in step (4), vacuum homogenize (2200 rpm, 10 min), and then keep stirring (50 rpm) until the material is uniform. Then cool down to 45°C to obtain mixture 5.
[0105] (6) After filtering the active ingredients in phase D through a 200-mesh sieve, add them to the mixture 5 obtained in step (5), vacuum homogenize (1800 rpm, 5 min), and then keep stirring (50 rpm, 8 min) until the material is uniform to obtain mixture 6.
[0106] (7) Add the phenoxyethanol / ethylhexylglycerin in phase E to the mixture 6 obtained in step (6), homogenize under vacuum for 2 minutes, and then keep stirring for more than 15 minutes until the mixture is uniform. Then cool down to below 40°C and stop stirring to obtain the eye cream.
[0107] Comparative Example 1
[0108] A traditional Chinese medicine composition with anti-wrinkle effects is made from the following raw materials by weight:
[0109]
[0110] This comparative example also provides a method for preparing the above-mentioned traditional Chinese medicine composition, comprising the following steps:
[0111] (1) Take ginseng, angelica, poria, polygonatum and angelica by weight, place them in a steam explosion machine and steam explosion at 1.15 MPa for 2 minutes with saturated steam, then depressurize to obtain depressurized material;
[0112] (2) The pressure relief material obtained in step (1) is subjected to countercurrent extraction at 20°C for 1 hour to obtain filtrate and filter residue; the solvent used for countercurrent extraction is an aqueous solution containing 1.1 g / L Tween 80.
[0113] (3) According to the mass ratio of filter residue to water of 1:10, add water to the filter residue obtained in step (2) and ultrasonically treat it at a power of 100W for 0.5h, and filter to obtain filter residue liquid.
[0114] (4) Take the filtrate obtained in step (2) and the residue obtained in step (3) and mix them together. Then add ethanol to the concentration of 70wt% for alcohol precipitation. Let it stand and filter. Recover the ethanol from the filtrate under reduced pressure until there is no alcohol taste. Then continue to concentrate under reduced pressure to 1.2 (about 60℃) to obtain the concentrated Chinese herbal medicine.
[0115] (5) Dissolve artificial bezoar and borneol in 0.8L of 1,3-propanediol, then add the concentrated Chinese herbal medicine solution obtained in step (4), and finally add 4L of 1,3-propanediol and deionized water and mix well. After filtering with 1.0μm and 0.60μm microporous membrane titanium rods, the Chinese herbal medicine extract is obtained.
[0116] Compared with Example 1, in Comparative Example 1, kudzu root was replaced with angelica root, and the use of pearl extract was omitted.
[0117] Comparative Example 2
[0118] A traditional Chinese medicine composition with anti-wrinkle effects is made from the following raw materials by weight:
[0119]
[0120]
[0121] This comparative example also provides a method for preparing the above-mentioned traditional Chinese medicine composition, comprising the following steps:
[0122] (1) Take ginseng, kudzu root, poria cocos, polygonatum odoratum, angelica sinensis and bletilla striata by weight, place them in a steam explosion machine and steam explosion at 1.15 MPa for 2 minutes with saturated steam, then depressurize to obtain depressurized material;
[0123] (2) The pressure relief material obtained in step (1) is subjected to countercurrent extraction at 20°C for 1 hour to obtain filtrate and filter residue; the solvent used for countercurrent extraction is an aqueous solution containing 1.1 g / L Tween 80.
[0124] (3) According to the mass ratio of filter residue to water of 1:10, add water to the filter residue obtained in step (2) and ultrasonically treat it at a power of 100W for 0.5h, and filter to obtain filter residue liquid.
[0125] (4) Take the filtrate obtained in step (2) and the residue obtained in step (3) and mix them together. Then add ethanol to the concentration of 70wt% for alcohol precipitation. Let it stand and filter. Recover the ethanol from the filtrate under reduced pressure until there is no alcohol taste. Then continue to concentrate under reduced pressure to 1.2 (about 60℃) to obtain the concentrated Chinese herbal medicine.
[0126] (5) Dissolve borneol in 0.8L of 1,3-propanediol, then add pearl extract (equivalent to 3g of pearl) and the concentrated Chinese herbal medicine obtained in step (4) in sequence. Finally, add 4L of 1,3-propanediol and deionized water and mix well. Filter the solution through titanium rods with 1.0μm and 0.60μm microporous membranes in sequence to obtain the Chinese herbal medicine extract.
[0127] Compared with Example 1, Comparative Example 2 omitted the use of artificial bezoar and added 50g of Bletilla striata.
[0128] Comparative Example 3
[0129] A traditional Chinese medicine composition with anti-wrinkle effects is made from the following raw materials by weight:
[0130]
[0131]
[0132] This comparative example also provides a method for preparing the above-mentioned traditional Chinese medicine composition, comprising the following steps:
[0133] (1) Take ginseng, kudzu root, Solomon's seal, poria cocos and angelica sinensis, add water and decoct three times, each time for 1.5 hours, add 10 times the amount of water each time, filter the decoction, combine the filtrates, and concentrate under reduced pressure to a relative density of 1.06 (60℃) to obtain a clear herbal extract.
[0134] (2) Add ethanol to make the ethanol concentration reach 70wt%, seal, refrigerate and stand for 24 hours, filter, and recover ethanol from the filtrate under reduced pressure until there is no alcohol taste. Continue to concentrate the medicinal solution to a relative density of 1.2 (60℃) to obtain a concentrated Chinese herbal medicine solution.
[0135] (3) Take artificial bezoar and borneol, add 0.8L of 1,3-propanediol and heat until dissolved, add pearl extract (equivalent to 3g of pearl), then add 4L of 1,3-propanediol and deionized water, and mix the resulting mixed solution with the concentrated Chinese herbal medicine solution.
[0136] (4) Install the transfer pump in advance, turn on the transfer pump to filter the above solution through 1.0μm and 0.60μm microporous filter membrane titanium rods into stainless steel barrels, and the solution is obtained.
[0137] In this comparative example, the herbal composition was treated using the traditional water extraction and alcohol precipitation method.
[0138] Comparative Example 4
[0139] A traditional Chinese medicine composition with anti-wrinkle effects is made from the following raw materials by weight:
[0140]
[0141] This comparative example also provides a method for preparing the above-mentioned traditional Chinese medicine composition, comprising the following steps:
[0142] (1) Take ginseng, kudzu root, poria cocos, polygonatum odoratum and angelica sinensis by weight, place them in a steam explosion machine and steam explosion at 1.15 MPa for 2 minutes with saturated steam, then depressurize to obtain depressurized material;
[0143] (2) The pressure relief material obtained in step (1) is subjected to countercurrent extraction at 20°C for 1 hour to obtain filtrate and filter residue; the solvent used for countercurrent extraction is an aqueous solution.
[0144] (3) According to the mass ratio of filter residue to water of 1:10, add water to the filter residue obtained in step (2) and ultrasonically treat it at a power of 100W for 0.5h, and filter to obtain filter residue liquid.
[0145] (4) Take the filtrate obtained in step (2) and the residue obtained in step (3) and mix them together. Then add ethanol to the concentration of 70wt% for alcohol precipitation. Let it stand and filter. Recover the ethanol from the filtrate under reduced pressure until there is no alcohol taste. Then continue to concentrate under reduced pressure to 1.2 (about 60℃) to obtain the concentrated Chinese herbal medicine.
[0146] (5) Dissolve artificial bezoar and borneol in 0.8L of 1,3-propanediol, then add pearl extract (equivalent to 3g of pearl) and the concentrated Chinese herbal medicine solution obtained in step (4) in sequence. Finally, add 4L of 1,3-propanediol and deionized water and mix well. After filtering with titanium rods and 1.0μm and 0.60μm microporous filter membranes in sequence, the Chinese herbal medicine extract is obtained.
[0147] In this comparative example, countercurrent extraction was performed using water, without Tween 80.
[0148] Comparative Example 5
[0149] Compared with Example 2, the only difference is that no herbal extracts are added to component D; all other components and preparation methods are the same.
[0150] Experimental Example 1
[0151] The anti-wrinkle effects of the herbal extracts prepared in Example 1 and Comparative Examples 1-4 were observed using biochemical methods to scavenge DPPH free radicals, hydroxyl radicals, and superoxide anions. The products prepared in Example 1 were designated as experimental group a, and the products prepared in Comparative Examples 1-4 were designated as experimental groups b, c, d, and e, respectively.
[0152] 1. Experimental reagents
[0153] The nitrogen free radical (DPPH) scavenging ability kit (batch number 20221130) was purchased from Shanghai Congyi Biotechnology Co., Ltd.; the hydroxyl free radical scavenging rate detection kit (Feton colorimetric method, batch number N18HR201184) was purchased from Shanghai Yuanye Biotechnology Co., Ltd.; and the superoxide anion scavenging ability test kit (micro method, batch number N579966W) was purchased from Shanghai Enzyme-Linked Biotechnology Co., Ltd.
[0154] 2. Experimental Methods
[0155] 2.1 DPPH free radical scavenging
[0156] The experiment was divided into a blank control group (solvent control, 50% ethanol) and experimental groups a–e. 100 μL of each sample was pipetted into a 96-well plate, 100 μL of DPPH solution was added, and the mixture was stirred and kept at room temperature in the dark for 30 min. The absorbance (A) was measured at 517 nm. The absorbance of the blank control group was set as A0, the absorbance of each sample with DPPH solution was set as the test sample (A1), and the absorbance of each sample with sample dilution was set as the control sample (A2). Therefore, the sample absorbance is A(A1-A2). The clearance rate was calculated using the formula: Clearance rate (%) = (A0 – A) / A0 × 100.
[0157] 2,2-hydroxyl radical scavenging
[0158] The experiment was divided into a blank control group (solvent control, double-distilled water) and experimental groups a to g. The experimental procedures were strictly followed according to the kit instructions, and the absorbance (A) was measured at 536 nm. Absorbance values were set for the blank tube (A0), undamaged tube (A1), damaged tube (A2), control tube (A3), and test tube (A4). The clearance rate was calculated using the formula: Clearance rate (%) = [(A4 - A3) - (A2 - A0)] / (A1 - A2) × 100.
[0159] 2.3 Superoxide anion scavenging
[0160] The experiment was divided into a blank control group (solvent control, double-distilled water) and experimental groups a to e. The experimental procedures were strictly followed according to the kit instructions, and the absorbance (A) was measured at 530 nm. The absorbance value of the blank tube (A0) was set, and the absorbance value of the measured tube (A) was also set. The clearance rate was calculated using the formula: Clearance rate (%) = (A0 - A) / A0 × 100.
[0161] 3. Experimental Results
[0162] 3.1 Effect on DPPH free radical scavenging rate
[0163] The results of DPPH free radical scavenging ability show that the DPPH free radical scavenging rate of the products prepared in the examples is ≥90%, and the product prepared in Example 1 reaches the maximum DPPH free radical scavenging rate (96.24±2.69)%, with a better anti-wrinkle effect. In contrast, the DPPH free radical scavenging rates of Comparative Examples 1-4 are relatively low, and the anti-wrinkle effect is insufficient.
[0164] Table 1 shows the effect of DPPH free radical scavenging rate. n=9)
[0165] Experimental group a 96.24±2.69 Experimental group b 81.47±1.02 Experimental group c 75.53±0.81 experimental group d 79.38±2.11 Experimental group e 85.29±1.98
[0166] 3.2 Effect on hydroxyl radical scavenging rate
[0167] The results of the hydroxyl radical scavenging ability showed that the hydroxyl radical scavenging rate of the products prepared in the examples was ≥85%, and the product prepared in Example 1 achieved the maximum hydroxyl radical scavenging rate (90.50±5.89)%, with a better anti-wrinkle effect. In contrast, the hydroxyl radical scavenging rates of Comparative Examples 1-4 were relatively low, and the anti-wrinkle effect was insufficient.
[0168] Table 2 shows the effect on hydroxyl radical scavenging rate. n=9)
[0169] Experimental group a 90.50±5.89 Experimental group b 66.40±5.89 Experimental group c 51.54±6.21 experimental group d 74.87±4.41 Experimental group e 81.64±5.65
[0170] 3.3 Effect on superoxide anion scavenging rate
[0171] The results of superoxide anion scavenging ability show that the superoxide anion free radical scavenging rate of the products prepared in the examples is ≥85%, and the product prepared in Example 1 reaches the maximum superoxide anion free radical scavenging rate (91.12±1.97)%, with a better anti-wrinkle effect. However, the superoxide anion free radical scavenging rates of Comparative Examples 1-4 are relatively low, and the anti-wrinkle effect is insufficient.
[0172] Table 3 shows the effect on superoxide anion scavenging rate. n=9)
[0173] Experimental group a 91.12±1.97 Experimental group b 73.25±2.22 Experimental group c 65.67±4.32 experimental group d 76.81±2.56 Experimental group e 82.98±3.54
[0174] Experimental Example 2: Human Efficacy Evaluation Trial
[0175] This invention uses the VISIR-CR facial imaging system to test and evaluate the area of crow's feet wrinkles in the eye creams prepared in Example 2 and Comparative Example 5. The instruments, testing methods, and test results are as follows:
[0176] Measuring instruments: VISIA-CR facial imaging tester (CANFIELD, USA), image processing enhancement and analysis system Plus Chinese Version 7.0.1.
[0177] Measurement requirements: Acquire images once (front 0°, left 37°, right 37°), and analyze the images once.
[0178] Testing Method: Thirty subjects aged 30-60 years with fine lines around the eyes were randomly selected and divided into two groups of 15 each: an example group and a comparative group. The test samples from Example 2 and Comparative Example 5 were applied evenly to the skin around the eyes of each subject for 10-15 minutes, gently massaging until absorbed. The samples were used twice daily, morning and evening. During the entire testing period, subjects were prohibited from prolonged sun exposure, outdoor sports, travel, etc., and were not allowed to use cosmetics or medications with similar effects to the product. Subjects were also not allowed to change their daily skincare routines during the testing period.
[0179] Statistical method: Each subject was tested three times, and the average value was taken. SPSS software was then used for statistical analysis. Lower values indicated smaller wrinkle areas within the test region. Unit: mm 2 .
[0180] Test results: See Table 4. The comparison of anti-wrinkle effects on the skin around the eyes of one subject in the example group is shown in Table 4. Figure 1 The comparison of the anti-wrinkle effect on the skin around the eyes of one subject in the control group is shown in the figure. Figure 2 .
[0181] Table 4. Results of eyelid wrinkle area test before and after product use (X±S, n=15)
[0182] Example 2 7.57±4.22 6.85±4.69* 6.12±4.16** Comparative Example 5 7.65±4.51 7.39±4.98 6.88±4.24*
[0183] (Compared with before product use, *P<0.05, **P<0.01)
[0184] As shown in Table 4, after 14 days of using the product from the example, the area of crow's feet wrinkles decreased by 9.5%, showing a highly significant reduction (p<0.05). After 28 days of using the product from the example, the area of crow's feet wrinkles decreased by 19.2%, showing a highly significant reduction (p<0.01). Figure 1 The comparison shows that the present invention has a significant effect on improving wrinkles. After 28 days of use, the wrinkles around the eyes of the subjects basically disappeared. The product of the present invention has a good anti-wrinkle effect and takes effect quickly. After 14 days of use of the comparative product, there was no significant difference in the area of wrinkles at the corners of the eyes, and the improvement of wrinkles around the eyes was not obvious. Therefore, it can be seen that the anti-wrinkle effect of the product of the present invention is far superior to that of the comparative product.
[0185] Experiment 4: Self-assessment results
[0186] A questionnaire survey was used to conduct subjective self-evaluation of the 30 participants in Experiment 3. The evaluation criteria for the improvement of eye wrinkles were specifically divided into four categories: no improvement or minimal improvement, mild improvement, moderate improvement, and significant or complete improvement. Significant effect = moderate improvement + significant or complete improvement; effective = mild improvement + moderate improvement + significant or complete improvement.
[0187] Table 5. Effects of the trial products on improving eye wrinkles in the example group.
[0188]
[0189]
[0190] Table 6. Effects of the product on improving eye wrinkles in the comparative control group.
[0191]
[0192] The improvement effects on eye wrinkles after 14 days and 28 days of use are shown in Tables 5-6. As can be seen from the tables, the eye cream prepared in this embodiment of the invention is fast-acting, with an effectiveness rate of 86.7% after 14 days and as high as 100% after 28 days, and no allergic reactions or discomfort were observed. The herbal composition of this invention has a highly significant effect on improving eye wrinkles, excellent anti-wrinkle effect, and is non-irritating.
[0193] The applicant declares that the technical solution of this invention is illustrated through the above embodiments, but this invention is not limited to the above embodiments, that is, it does not mean that this invention must rely on the above embodiments to be implemented. Those skilled in the art should understand that any improvements to this invention, equivalent substitutions of individual raw materials in the product of this invention, additions of auxiliary components, and selection of specific methods, all fall within the protection scope and disclosure scope of this invention.
Claims
1. An eye cream with anti-wrinkle effects, characterized in that, By weight, it contains the following raw materials: 1-5 parts of herbal extract, 0.01-2 parts of acetyl tetrapeptide-11, 0.01-2 parts of acetyl tetrapeptide-9, 0.01-2 parts of jasmine extract, 0.01-2 parts of hawthorn flower extract, and 0.05-1 part of sodium hyaluronate. The herbal extract is prepared from 100-200 parts ginseng, 100-200 parts kudzu root, 50-150 parts Solomon's seal, 10-100 parts Poria cocos, 10-100 parts Angelica sinensis, 1-5 parts pearl, 0.1-3 parts artificial bezoar, and 0.1-3 parts borneol. The preparation of the herbal extract includes the following steps: (1) Take ginseng, kudzu root, poria cocos, polygonatum odoratum and angelica sinensis by weight, put them in a steam explosion machine for steam explosion treatment, and then depressurize to obtain depressurized material; (2) The pressure relief material obtained in step (1) is subjected to countercurrent extraction to obtain filtrate and filter residue; wherein, the countercurrent extraction solvent is an aqueous solution containing 1~1.2g / L Tween 80; (3) Add water to the filter residue obtained in step (2) and treat it under ultrasound, then filter to obtain filter residue liquid; (4) Take the filtrate obtained in step (2) and the residue obtained in step (3) and mix them together. Then add ethanol for alcohol precipitation, let stand and filter. Recover the ethanol from the filtrate under reduced pressure until there is no alcohol taste. Then continue to concentrate under reduced pressure to obtain concentrated Chinese herbal medicine. (5) Dissolve artificial bezoar and borneol in a solvent, then add pearl and the concentrated Chinese herbal medicine solution obtained in step (4) in sequence, and finally add solvent and deionized water to mix well. After filtration, the product is obtained.
2. An eye cream with anti-wrinkle effects according to claim 1, characterized in that, The raw materials for preparing the eye cream also include excipients; by weight, the excipients are selected from one or more of polyols, moisturizers, emollients, emulsifiers, thickeners, antioxidants, chelating agents, preservatives, pH adjusters, antioxidants, and deionized water.
3. An eye cream with anti-wrinkle effects according to claim 1, characterized in that, In step (1), saturated steam is used for steam explosion and the steam is treated at 1.1~1.2MPa for 1~3min.
4. An eye cream with anti-wrinkle effects according to claim 1, characterized in that, In step (2), the countercurrent extraction temperature is 20~25℃ and the countercurrent extraction time is 10~30min.
5. An eye cream with anti-wrinkle effects according to claim 1, characterized in that, In step (3), the ultrasonic treatment power is 80~120W, the ultrasonic treatment time is 0.5~5h, and the mass ratio of filter residue to water is 1:8~15; In step (4), the ethanol concentration of the alcohol precipitation is 50~70wt%; it is concentrated under reduced pressure to a relative density of 1.15~1.25; In step (5), the solvent is one or more of butanediol, 1,3-propanediol or glycerol; the filtration is carried out using 1.0µm and 0.60µm microporous filter membrane titanium rods in sequence.
6. An eye cream with anti-wrinkle effects according to claim 2, characterized in that, The emollient is selected from one or more of the following: shea butter, phytosterol isostearate, hydrogenated polydecene, isononyl isononanoate, polydimethylsiloxane, squalane, cetearyl alcohol, isohexadecane, and cyclopentamethoxysiloxane. The emulsifier is selected from one or more of sodium stearoyl glutamate, cetearyl oleate, cetearyl palmitate, sorbitan oleate, and PEG-100 stearate; The preservative is selected from one or more of phenoxyethanol, ethylhexylglycerin, chlorphenesin, methylparaben, p-hydroxyacetophenone, propylparaben, 1,2-hexanediol, and sorbitan octanoate; The chelating agent is selected from one or more of disodium EDTA, EDTA, and tetrasodium EDTA. The polyol is selected from one or more of glycerol, propylene glycol, butylene glycol, sorbitol, dipropylene glycol, 1,3-propanediol, pentanediol, and hexanediol; The antioxidant is selected from one or more of butylated hydroxytoluene, butylated hydroxyanisole, and tocopheryl acetate. The thickener is selected from one or two of hydroxyethyl acrylate / sodium acryloyl dimethyl taurate copolymer and sorbitan isostearate.
7. A method for preparing the eye cream according to any one of claims 1 to 6, characterized in that, Includes the following steps: (1) Add the thickener to the first polyol and stir well to obtain mixture 1, which is ready for use; (2) Add purified water to the emulsification tank, then add the first part of emulsifier, sodium hyaluronate, the second part of polyol, the first part of preservative, and chelating agent. Slowly heat to 79-83°C, keep warm and stir until the material is completely dissolved to obtain mixture 2. (3) Add the emollient, the second part of the emulsifier and the antioxidant to the reaction vessel in sequence, heat to 80-85°C while stirring, mix evenly until completely dissolved, and obtain mixture 3; (4) The mixture 3 obtained in step (3) is filtered into the emulsification tank of step (2), kept at 79-83°C, then vacuum homogenized and stirred until the material is evenly dispersed to obtain mixture 4. (5) Add the mixture 1 obtained in step (1) to the mixture 4 obtained in step (4), perform vacuum homogenization and keep stirring until the material is uniform, then cool down to 40-50℃ to obtain mixture 5; (6) Add the Chinese herbal medicine extract, jasmine flower extract, hawthorn flower extract, acetyl tetrapeptide-11, and acetyl tetrapeptide-9 to the mixture 5 obtained in step (5), and after vacuum homogenization, keep stirring until the mixture is uniform to obtain mixture 6. (7) Add the second part of the preservative to the mixture 6 obtained in step (6), homogenize under vacuum and keep stirring until the mixture is uniform, then cool down and stop stirring to obtain the eye cream.
8. The preparation method according to claim 7, characterized in that, In step (2), the stirring speed for heat preservation is 30~50 rpm; In step (3), the stirring speed is 600~900 rpm; In step (4), the vacuum homogenization speed is 2000~2500 rpm, the time is 8~12 min; the stirring speed is 30~50 rpm; In step (5), the vacuum homogenization speed is 2000~2500 rpm, the time is 8~12 min; the stirring speed is 30~50 rpm; In step (6), the vacuum homogenization speed is 1500~2000 rpm and the time is 3~5 min; the stirring speed is 30~50 rpm and the stirring time is 8~10 min. In step (7), the vacuum homogenization speed is 1500~2000 rpm, the time is 1~2 min, the stirring time is not less than 15 min, and the temperature is reduced to below 40℃.
Citation Information
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