Water-oil two-phase microbead essence and preparation method thereof

Abstract

The invention discloses a water-oil two-phase microbead essence and a preparation method thereof, and relates to the technical field of cosmetics. Comprising the following raw materials in percentage by weight: 2wt%-5wt% of plant polysaccharide, 0.005 wt%-0.015 wt% of meso-tetramethyl-meso-tetra-p-aminophenyl calix [4] pyrrole, 0.5 wt%-1wt% of hyaluronic acid, 0.3 wt%-1wt% of fish collagen peptide, 0.1 wt%-3wt% of other plant extracts, 8wt%-15wt% of glycerol, 0.1 wt%-0.3 wt% of plant germ oil, 1wt%-4wt% of other vegetable fat, 0.1 wt%-0.3 wt% of hydroxypropyl beta-cyclodextrin, 0.3 wt%-0.5 wt% of ceramide and the balance of water. And the balance of deionized water. The water-oil two-phase microbead essence is high in stability, small in skin irritation and remarkable in whitening, moisturizing, anti-wrinkle and sunscreen effects.

Description

Technical Field

[0001] The invention relates to the technical field of cosmetics, and in particular to a water-oil two-phase micro-bead essence and a preparation method thereof. Background Art

[0002] Essence is a high-concentration skin care product, usually used in skin care. Its efficacy can help improve skin texture, reduce fine lines, wrinkles and spots, and provide the skin with the necessary nutrition and moisturizing. As a more representative dosage form of essence, water-oil two-phase micro-bead essence continues to be a popular cosmetic among consumers due to its novel appearance, high-end visual experience, good use experience, and good transdermal effect.

[0003] The existing water-oil two-phase micro-bead essence has low water-oil mixing stability and is prone to stratification problems; it contains a large amount of surfactants and co-surfactants, which cause certain damage to the stratum corneum of the skin, and has poor efficacy. Long-term use will make the skin sensitive due to excessive stimulation. In addition, the water-oil two-phase micro-bead essence on the market has more or less technical defects such as insufficient whitening and moisturizing effects, and the sun protection and anti-wrinkle effects need to be further improved.

[0004] In order to solve the above problems, the Chinese invention patent with the authorization announcement number CN111249184B discloses a transparent micro-bead essence containing both water-soluble and fat-soluble anti-wrinkle polypeptides. The product contains the following substances in percentage by mass: 0.5% to 5.0% of vegetable oil, 0.0001% to 0.1% of fat-soluble anti-wrinkle polypeptide, 0.0001% to 0.9% of water-soluble anti-wrinkle polypeptide, 0.15% to 0.3% of aqueous thickener, 0% to 0.3% of pH adjuster, 2.0% to 15.0% of moisturizer, and the balance is deionized water. The micro-bead essence of the invention dissolves the fat-soluble anti-wrinkle polypeptide in vegetable oil and suspends it evenly and stably in the form of oil droplets in the transparent aqueous essence. It does not contain emulsifiers, solubilizers and synthetic silicone oil components, and the micro-beads are not wrapped in a shell, which effectively solves the technical problem that fat-soluble biological polypeptides cannot be directly added to transparent aqueous essences because they are insoluble in water. The micro-bead essence of the invention has a transparent and beautiful appearance, a clear texture, and a refreshing and moisturizing feeling on the skin. At the same time, the fat-soluble anti-wrinkle peptides and water-soluble anti-wrinkle peptides are reasonably matched to synergistically enhance the effect, and have better anti-wrinkle effects. However, the whitening and sunscreen functions of the essence need to be further improved, and the irritation to the skin needs to be further reduced. Summary of the invention

[0005] The purpose of the present invention is to overcome the deficiencies of the prior art and provide a water-oil two-phase micro-bead essence with high stability, little skin irritation, and significant whitening, moisturizing, anti-wrinkle and sunscreen effects and a preparation method thereof.

[0006] To achieve the above-mentioned purpose, the technical scheme adopted by the present invention is: a water-oil two-phase micro-bead essence, which comprises the following raw materials by weight percentage: 2wt%-5wt% of plant polysaccharides, 0.005wt%-0.015wt% of meso-tetramethyl-meso-tetra-p-aminophenyl cup [4] pyrrole, 0.5wt%-1wt% of hyaluronic acid, 0.3wt%-1wt% of fish collagen peptide, 0.1wt%-3wt% of other plant extracts, 8wt%-15wt% of glycerol, 0.1wt%-0.3wt% of plant germ oil, 1wt%-4wt% of other plant oils and fats, 0.1wt%-0.3wt% of hydroxypropyl β-cyclodextrin, 0.3wt%-0.5wt% of ceramide, and the balance is deionized water.

[0007] Preferably, the plant polysaccharide is at least one of Flammulina velutipes polysaccharide, Tremella fuciformis polysaccharide and Coriolus versicolor polysaccharide.

[0008] Preferably, the preparation method of the meso-tetramethyl-meso-tetraaminophenylcalix[4]pyrrole is described in: Guo Yong, Shao Shijun, He Lijun, et al. Synthesis and Characterization of Meso-tetramethyl-meso-tetraaminophenylcalix[4]pyrrole [J]. Chemical Reagents, 2002(6):344-345.

[0009] Preferably, the average molecular weight of the fish collagen peptide is 1000-2000 Daltons.

[0010] Preferably, the other plant extracts are extracted from the following plant raw materials by weight: 4-6 parts of citrus, 3-5 parts of melon flowers, 5-8 parts of bamboo orchid, 4-6 parts of tea, 5-8 parts of Sophora japonica, 6-10 parts of Poria cocos, 3-6 parts of bamboo shavings, 5-8 parts of ginseng flowers, 4-6 parts of jasmine, 1-3 parts of rice flour, 5-8 parts of Evodia rutaecarpa, 3-6 parts of aloe vera, 6-10 parts of Centella asiatica, 1-3 parts of magnolia, 2-4 parts of raspberry, 5-8 parts of asparagus, 3-5 parts of almond, 3-5 parts of cloves, and 2-4 parts of azalea roots.

[0011] Preferably, the method for extracting the other plant extracts comprises the following steps:

[0012] Step S1, uniformly mixing the plant raw materials of other plant extracts to obtain a mixed material, adding water and boiling for 1-3 hours, filtering and collecting the water extract and filter residue;

[0013] Step S2, extracting the filter residue with ethanol, and collecting the alcohol extract by filtering;

[0014] Step S3, combining the above two extracts, concentrating under reduced pressure to recover ethanol and water, and obtaining other plant extracts.

[0015] Preferably, in step S1, the mass ratio of the mixed material to water is 1:(5-8); and the decoction temperature is 95-98°C.

[0016] Preferably, the mass ratio of the filter residue to ethanol in step S2 is 1:(6-8).

[0017] Preferably, the extraction in step S2 is a heating reflux extraction, which is performed three times, each time for 1-2 hours, and the three extracts are combined and allowed to stand.

[0018] Preferably, the plant germ oil is at least one of wheat germ oil, rice germ oil and corn germ oil.

[0019] Preferably, the other vegetable oils are any one or more of wormwood oil, tamanu oil, grape seed oil, and olive oil.

[0020] Preferably, the water-oil two-phase micro-bead essence further includes: 0.003wt%-0.01wt% of a functional copolymer; the functional copolymer includes structural units introduced by the following monomers: 3-[N,N-dimethyl-[2-(2-methylprop-2-enoyloxy)ethyl]ammonium]propane-1-sulfonic acid inner salt, N-trihydroxymethylmethylacrylamide, and single-terminated vinyl silicone oil.

[0021] Preferably, the single-ended vinyl silicone oil is CX-352M single-ended vinyl silicone oil, provided by Guangdong Chensi New Material Technology Co., Ltd.

[0022] Preferably, the preparation method of the functional copolymer comprises the following steps: adding 3-[N,N-dimethyl-[2-(2-methylprop-2-enoyloxy)ethyl]ammonium]propane-1-sulfonic acid inner salt, N-trihydroxymethyl methacrylamide, single-end vinyl silicone oil, and an initiator to a high boiling point solvent, stirring and reacting at 60-70° C. in an inert gas atmosphere for 3-5 hours, then removing the solvent by rotary evaporation, dissolving the obtained crude product in water, taking the supernatant and placing it in a dialysis bag, dialyzing it in deionized water for 20-30 hours, and then rotary evaporating the solution in the dialysis bag to remove water to obtain a functional copolymer.

[0023] Preferably, the mass ratio of the 3-[N,N-dimethyl-[2-(2-methylprop-2-enoyloxy)ethyl]ammonium]propane-1-sulfonic acid inner salt, N-trimethylolmethyl acrylamide, single-terminated vinyl silicone oil, initiator, and high boiling point solvent is 1:(1-3):0.3:(0.03-0.05):(9-15).

[0024] Preferably, the initiator is azobisisobutyronitrile; the high boiling point solvent is at least one of N,N-dimethylformamide, N-methylpyrrolidone, and dimethyl sulfoxide; and the inert gas is any one of nitrogen, helium, neon, and argon.

[0025] Another object of the present invention is to provide a method for preparing the water-oil two-phase micro-bead essence, comprising the following steps: adding plant polysaccharides, hyaluronic acid, fish collagen peptides, other plant extracts, hydroxypropyl β-cyclodextrin, and functional copolymers into deionized water, and mixing them evenly to obtain a water phase; uniformly dispersing meso-tetramethyl-meso-tetra-aminophenylcalix[4]pyrrole, plant germ oil, other plant oils and fats, and ceramide in glycerol to obtain an oil phase; and uniformly dispersing the oil phase in the form of oil droplets in the water phase to prepare the water-oil two-phase micro-bead essence.

[0026] Due to the application of the above technical solution, the present invention has the following beneficial effects:

[0027] (1) The method for preparing the water-oil two-phase micro-bead essence disclosed in the present invention has a simple and safe process, low dependence on equipment and labor intensity, small impact on the environment, high preparation efficiency and finished product qualification rate, is suitable for continuous large-scale production, and has high promotion and application value.

[0028] (2) The water-oil two-phase micro-bead essence disclosed in the present invention comprises the following raw materials by weight percentage: 2wt%-5wt% of plant polysaccharide, 0.005wt%-0.015wt% of meso-tetramethyl-meso-tetra-p-aminophenyl cup [4] pyrrole, 0.5wt%-1wt% of hyaluronic acid, 0.3wt%-1wt% of fish collagen peptide, 0.1wt%-3wt% of other plant extracts, 8wt%-15wt% of glycerol, 0.1wt%-0.3wt% of plant germ oil, 1wt%-4wt% of other plant oils and fats, 0.1wt%-0.3wt% of hydroxypropyl β-cyclodextrin, 0.3wt%-0.5wt% of ceramide, and the balance is deionized water. Through the mutual coordination and joint action of the raw materials, the water-oil two-phase micro-bead essence has high stability, little skin irritation, and significant whitening, moisturizing, anti-wrinkle and sunscreen effects.

[0029] (3) The water-oil two-phase micro-bead essence disclosed in the present invention further comprises: 0.003wt%-0.01wt% of a functional copolymer; the other plant extracts are extracted from the following plant raw materials in parts by weight: 4-6 parts of citrus, 3-5 parts of melon flowers, 5-8 parts of bamboo orchid, 4-6 parts of tea leaves, 5-8 parts of Sophora japonica flowers, 6-10 parts of Poria cocos, 3-6 parts of bamboo shavings, 5-8 parts of ginseng flowers, 4-6 parts of jasmine flowers, 1-3 parts of rice flour, 5-8 parts of Evodia rutaecarpa, 3-6 parts of aloe vera, 6-10 parts of Centella asiatica, 1-3 parts of magnolia, 2-4 parts of raspberry, 5-8 parts of asparagus, 3-5 parts of almonds, 3-5 parts of cloves, and 2-4 parts of azalea roots. Through the reasonable selection of the types and amounts of these raw materials, they can be better compatible with each other and with other raw materials, giving the product strong penetration, which can penetrate deep into the skin epidermis and have a good nourishing effect on the skin. Long-term use can make the skin whiter and firmer; the use of functional copolymers can make the microbeads in the essence more evenly dispersed, making the essence more stable and improving the moisturizing effect; in combination with other raw materials, it can also better fill the gaps between keratinocytes, repair the skin barrier, and improve skin quality. DETAILED DESCRIPTION

[0030] The following description is used to disclose the present invention so that those skilled in the art can implement the present invention. The preferred embodiments described below are only examples, and those skilled in the art may think of other obvious variations.

[0031] Example 1

[0032] A water-oil two-phase micro-bead essence comprises the following raw materials, measured by weight percentage: 2wt% of plant polysaccharide, 0.005wt% of meso-tetramethyl-meso-tetra-p-aminophenyl cup [4] pyrrole, 0.5wt% of hyaluronic acid, 0.3wt% of fish collagen peptide, 0.5wt% of other plant extracts, 8wt% of glycerol, 0.1wt% of plant germ oil, 1wt% of other plant oils and fats, 0.1wt% of hydroxypropyl β-cyclodextrin, 0.3wt% of ceramide, and the balance is deionized water.

[0033] The plant polysaccharide is Flammulina velutipes polysaccharide; the preparation method of Meso-tetramethyl-meso-tetraaminophenylcalix[4]pyrrole, see: Guo Yong, Shao Shijun, He Lijun, et al. Synthesis and Characterization of Meso-tetramethyl-meso-tetraaminophenylcalix[4]pyrrole[J]. Chemical Reagents, 2002(6):344-345; the average molecular weight of the fish collagen peptide is 1000 Daltons.

[0034] The other plant extracts are extracted from the following plant raw materials in parts by weight: 4 parts of citrus, 3 parts of melon flowers, 5 parts of bamboo orchid, 4 parts of tea, 5 parts of Sophora japonica flowers, 6 parts of Poria cocos, 3 parts of bamboo shavings, 5 parts of ginseng flowers, 4 parts of jasmine flowers, 1 part of rice flour, 5 parts of Evodia rutaecarpa, 3 parts of aloe vera, 6 parts of Centella asiatica, 1 part of magnolia, 2 parts of raspberry, 5 parts of asparagus, 3 parts of almonds, 3 parts of cloves, and 2 parts of azalea roots.

[0035] The method for extracting the other plant extracts comprises the following steps:

[0036] Step S1, mixing the plant raw materials of other plant extracts evenly to obtain a mixed material, adding water and boiling for 1 hour, filtering and collecting the water extract and filter residue;

[0037] Step S2, extracting the filter residue with ethanol, and collecting the alcohol extract by filtering;

[0038] Step S3, combining the above two extracts, concentrating under reduced pressure to recover ethanol and water, and obtaining other plant extracts.

[0039] The mass ratio of the mixed material to water in step S1 is 1:5; the decoction temperature is 95°C; the mass ratio of the filter residue to ethanol in step S2 is 1:6; the extraction in step S2 is heating reflux extraction, the extraction is performed 3 times, each time for 1 hour, and the 3 extracts are combined and allowed to stand.

[0040] The plant germ oil is wheat germ oil; the other plant oil is wormwood oil.

[0041] A method for preparing the water-oil two-phase micro-bead essence comprises the following steps: adding plant polysaccharides, hyaluronic acid, fish collagen peptides, other plant extracts, and hydroxypropyl β-cyclodextrin into deionized water, and mixing them evenly to obtain a water phase; uniformly dispersing meso-tetramethyl-meso-tetra-p-aminophenylcalix[4]pyrrole, plant germ oil, other plant oils and fats, and ceramide in glycerol to obtain an oil phase; and uniformly dispersing the oil phase in the form of oil droplets in the water phase to prepare the water-oil two-phase micro-bead essence.

[0042] Example 2

[0043] A water-oil two-phase micro-bead essence comprises the following raw materials, measured by weight percentage: 3wt% of plant polysaccharide, 0.007wt% of meso-tetramethyl-meso-tetra-p-aminophenyl cup [4] pyrrole, 0.6wt% of hyaluronic acid, 0.5wt% of fish collagen peptide, 1wt% of other plant extracts, 10wt% of glycerol, 0.15wt% of plant germ oil, 2wt% of other plant oils and fats, 0.15wt% of hydroxypropyl β-cyclodextrin, 0.35wt% of ceramide, and the balance is deionized water.

[0044] The plant polysaccharide is Tremella polysaccharide; the preparation method of Meso-tetramethyl-meso-tetraaminophenylcalix[4]pyrrole, see: Guo Yong, Shao Shijun, He Lijun, et al. Synthesis and Characterization of Meso-tetramethyl-meso-tetraaminophenylcalix[4]pyrrole[J]. Chemical Reagents, 2002(6):344-345; the average molecular weight of the fish collagen peptide is 1200 Daltons.

[0045] The other plant extracts are extracted from the following plant raw materials in parts by weight: 4.5 parts of citrus, 3.5 parts of melon flower, 6 parts of bamboo orchid, 4.5 parts of tea, 6 parts of Sophora japonica flower, 7 parts of Poria cocos, 4 parts of bamboo shavings, 6 parts of ginseng flower, 4.5 parts of jasmine, 1.5 parts of rice flour, 6 parts of Evodia rutaecarpa, 4 parts of aloe vera, 7 parts of Centella asiatica, 1.5 parts of magnolia, 2.5 parts of raspberry, 6 parts of asparagus, 3.5 parts of almond, 3.5 parts of clove, and 2.5 parts of azalea root.

[0046] The method for extracting the other plant extracts comprises the following steps:

[0047] Step S1, mixing the plant raw materials of other plant extracts evenly to obtain a mixed material, adding water and boiling for 1.5 hours, filtering and collecting the water extract and filter residue;

[0048] Step S2, extracting the filter residue with ethanol, and collecting the alcohol extract by filtering;

[0049] Step S3, combining the above two extracts, concentrating under reduced pressure to recover ethanol and water, and obtaining other plant extracts.

[0050] The mass ratio of the mixed material to water in step S1 is 1:6; the decoction temperature is 96°C; the mass ratio of the filter residue to ethanol in step S2 is 1:6.5; the extraction in step S2 is heating reflux extraction, the extraction is performed 3 times, each time for 1.2 hours, and the 3 extracts are combined and allowed to stand.

[0051] The plant germ oil is rice germ oil; the other plant oil is tamanu oil.

[0052] The water-oil two-phase micro-bead essence also includes: 0.003wt% of functional copolymer; the functional copolymer includes structural units introduced by the following monomers: 3-[N,N-dimethyl-[2-(2-methylprop-2-enoyloxy)ethyl]ammonium]propane-1-sulfonic acid inner salt, N-trihydroxymethylmethylacrylamide, single-ended vinyl silicone oil; the single-ended vinyl silicone oil is CX-352M single-ended vinyl silicone oil, provided by Guangdong Chensi New Material Technology Co., Ltd.

[0053] The preparation method of the functional copolymer comprises the following steps: adding 3-[N,N-dimethyl-[2-(2-methylprop-2-enoyloxy)ethyl]ammonium]propane-1-sulfonic acid inner salt, N-trihydroxymethyl methacrylamide, single-end vinyl silicone oil and an initiator to a high boiling point solvent, stirring and reacting at 60° C. for 3 hours in an inert gas atmosphere, then removing the solvent by rotary evaporation, dissolving the obtained crude product in water, taking the supernatant and placing it in a dialysis bag, and dialyzing it in deionized water for 20 hours. Then, the solution in the dialysis bag is evaporated to remove water to obtain a functional copolymer; the mass ratio of the 3-[N,N-dimethyl-[2-(2-methylprop-2-enoyloxy)ethyl]ammonium]propane-1-sulfonic acid inner salt, N-trihydroxymethyl methacrylamide, single-terminated vinyl silicone oil, initiator, and high boiling point solvent is 1:1:0.3:0.03:9; the initiator is azobisisobutyronitrile; the high boiling point solvent is N,N-dimethylformamide; and the inert gas is nitrogen. The M of the obtained functional copolymer is measured by GPC test. n =12310 g / mol, M W / M n =1.275; through elemental analysis and weight change calculation, the mass ratio of the structural units introduced by 3-[N,N-dimethyl-[2-(2-methylprop-2-enoyloxy)ethyl]ammonium]propane-1-sulfonic acid inner salt, N-trimethylolmethyl acrylamide, and single-end vinyl silicone oil in the functional copolymer is 0.99:0.98:0.3.

[0054] A method for preparing the water-oil two-phase micro-bead essence comprises the following steps: adding plant polysaccharides, hyaluronic acid, fish collagen peptides, other plant extracts, hydroxypropyl β-cyclodextrin, and functional copolymers into deionized water, and mixing them evenly to obtain a water phase; uniformly dispersing meso-tetramethyl-meso-tetra-p-aminophenylcalix[4]pyrrole, plant germ oil, other plant oils and fats, and ceramide in glycerol to obtain an oil phase; and uniformly dispersing the oil phase in the form of oil beads in the water phase to prepare the water-oil two-phase micro-bead essence.

[0055] Example 3

[0056] A water-oil two-phase micro-bead essence comprises the following raw materials, measured by weight percentage: 3.5wt% of plant polysaccharides, 0.01wt% of meso-tetramethyl-meso-tetra-p-aminophenyl cup [4] pyrrole, 0.75wt% of hyaluronic acid, 0.6wt% of fish collagen peptide, 1.5wt% of other plant extracts, 12wt% of glycerol, 0.2wt% of plant germ oil, 2.5wt% of other plant oils and fats, 0.2wt% of hydroxypropyl β-cyclodextrin, 0.4wt% of ceramide, and the balance is deionized water.

[0057] The plant polysaccharide is Coriolus versicolor polysaccharide; the preparation method of Meso-tetramethyl-meso-tetraaminophenylcalix[4]pyrrole, see: Guo Yong, Shao Shijun, He Lijun, et al. Synthesis and Characterization of Meso-tetramethyl-meso-tetraaminophenylcalix[4]pyrrole[J]. Chemical Reagents, 2002(6):344-345; the average molecular weight of the fish collagen peptide is 1500 Daltons.

[0058] The other plant extracts are extracted from the following plant raw materials in parts by weight: 5 parts of citrus, 4 parts of melon flower, 6.5 parts of bamboo orchid, 5 parts of tea, 6.5 parts of Sophora japonica flower, 8 parts of Poria cocos, 4.5 parts of bamboo shavings, 6.5 parts of ginseng flower, 5 parts of jasmine, 2 parts of rice flour, 6.5 parts of Evodia rutaecarpa, 4.5 parts of aloe vera, 8 parts of Centella asiatica, 2 parts of magnolia, 3 parts of raspberry, 6.5 parts of asparagus, 4 parts of almond, 4 parts of clove, and 3 parts of azalea root.

[0059] The method for extracting the other plant extracts comprises the following steps:

[0060] Step S1, mixing the plant raw materials of other plant extracts evenly to obtain a mixed material, adding water and boiling for 2 hours, filtering and collecting the water extract and filter residue;

[0061] Step S2, extracting the filter residue with ethanol, and collecting the alcohol extract by filtering;

[0062] Step S3, combining the above two extracts, concentrating under reduced pressure to recover ethanol and water, and obtaining other plant extracts.

[0063] The mass ratio of the mixed material to water in step S1 is 1:6.5; the decoction temperature is 97° C.; the mass ratio of the filter residue to ethanol in step S2 is 1:7; the extraction in step S2 is heating reflux extraction, the extraction is performed 3 times, each time for 1.5 hours, and the 3 extracts are combined and allowed to stand.

[0064] The plant germ oil is corn germ oil; the other plant oil is grape seed oil.

[0065] The water-oil two-phase micro-bead essence also includes: 0.006wt% of functional copolymer; the functional copolymer includes structural units introduced by the following monomers: 3-[N,N-dimethyl-[2-(2-methylprop-2-enoyloxy)ethyl]ammonium]propane-1-sulfonic acid inner salt, N-trihydroxymethylmethylacrylamide, single-ended vinyl silicone oil; the single-ended vinyl silicone oil is CX-352M single-ended vinyl silicone oil, provided by Guangdong Chensi New Material Technology Co., Ltd.

[0066] The preparation method of the functional copolymer comprises the following steps: adding 3-[N,N-dimethyl-[2-(2-methylprop-2-enoyloxy)ethyl]ammonium]propane-1-sulfonic acid inner salt, N-trihydroxymethyl methacrylamide, single-end vinyl silicone oil and an initiator to a high boiling point solvent, stirring and reacting at 65°C for 4 hours in an inert gas atmosphere, then removing the solvent by rotary evaporation, dissolving the obtained crude product in water, taking the supernatant and placing it in a dialysis bag, and dialyzing it in deionized water for 25 hours. Then, the solution in the dialysis bag is rotary evaporated to remove water to obtain a functional copolymer; the mass ratio of the 3-[N,N-dimethyl-[2-(2-methylprop-2-enoyloxy)ethyl]ammonium]propane-1-sulfonic acid inner salt, N-trihydroxymethyl methacrylamide, single-terminated vinyl silicone oil, initiator, and high boiling point solvent is 1:2:0.3:0.04:12; the initiator is azobisisobutyronitrile; the high boiling point solvent is N-methylpyrrolidone; and the inert gas is helium.

[0067] A method for preparing the water-oil two-phase micro-bead essence comprises the following steps: adding plant polysaccharides, hyaluronic acid, fish collagen peptides, other plant extracts, hydroxypropyl β-cyclodextrin, and functional copolymers into deionized water, and mixing them evenly to obtain a water phase; uniformly dispersing meso-tetramethyl-meso-tetra-p-aminophenylcalix[4]pyrrole, plant germ oil, other plant oils and fats, and ceramide in glycerol to obtain an oil phase; and uniformly dispersing the oil phase in the form of oil beads in the water phase to prepare the water-oil two-phase micro-bead essence.

[0068] Example 4

[0069] A water-oil two-phase micro-bead essence comprises the following raw materials, measured by weight percentage: 4.5wt% of plant polysaccharides, 0.013wt% of meso-tetramethyl-meso-tetra-p-aminophenyl cup [4] pyrrole, 0.9wt% of hyaluronic acid, 0.9wt% of fish collagen peptide, 2.5wt% of other plant extracts, 14wt% of glycerol, 0.25wt% of plant germ oil, 3.5wt% of other plant oils and fats, 0.25wt% of hydroxypropyl β-cyclodextrin, 0.45wt% of ceramide, and the balance is deionized water.

[0070] The plant polysaccharide is a mixture of Flammulina velutipes polysaccharide, Tremella fuciformis polysaccharide and Versicolor coriolus polysaccharide in a mass ratio of 1:2:3; the preparation method of Meso-tetramethyl-meso-tetraaminophenylcalix[4]pyrrole, see: Guo Yong, Shao Shijun, He Lijun, et al. Synthesis and Characterization of Meso-tetramethyl-meso-tetraaminophenylcalix[4]pyrrole[J]. Chemical Reagents, 2002(6):344-345; the average molecular weight of the fish collagen peptide is 1800 Daltons.

[0071] The other plant extracts are extracted from the following plant raw materials in parts by weight: 5.5 parts of citrus, 4.5 parts of melon flower, 7.5 parts of bamboo orchid, 5.5 parts of tea, 7.5 parts of Sophora japonica flower, 9.5 parts of Poria cocos, 5.5 parts of bamboo shavings, 7.5 parts of ginseng flower, 5.5 parts of jasmine, 2.5 parts of rice flour, 7.5 parts of Evodia rutaecarpa, 5.5 parts of aloe vera, 9.5 parts of Centella asiatica, 2.5 parts of magnolia, 3.5 parts of raspberry, 7.5 parts of asparagus, 4.5 parts of almond, 4.5 parts of clove, and 3.5 parts of azalea root.

[0072] The method for extracting the other plant extracts comprises the following steps:

[0073] Step S1, mixing the plant raw materials of other plant extracts evenly to obtain a mixed material, adding water and boiling for 2.5 hours, filtering and collecting the water extract and filter residue;

[0074] Step S2, extracting the filter residue with ethanol, and collecting the alcohol extract by filtering;

[0075] Step S3, combining the above two extracts, concentrating under reduced pressure to recover ethanol and water, and obtaining other plant extracts.

[0076] The mass ratio of the mixed material to water in step S1 is 1:7.5; the decoction temperature is 97° C.; the mass ratio of the filter residue to ethanol in step S2 is 1:7.5; the extraction in step S2 is heating reflux extraction, the extraction is performed 3 times, each time for 1.8 hours, and the 3 extracts are combined and allowed to stand.

[0077] The plant germ oil is a mixture of wheat germ oil, rice germ oil and corn germ oil in a mass ratio of 1:2:1; the other plant oils are a mixture of wormwood oil, tamanu oil, grape seed oil and olive oil in a mass ratio of 1:2:2:3.

[0078] The water-oil two-phase micro-bead essence also includes: 0.008wt% of a functional copolymer; the functional copolymer includes structural units introduced by the following monomers: 3-[N,N-dimethyl-[2-(2-methylprop-2-enoyloxy)ethyl]ammonium]propane-1-sulfonic acid inner salt, N-trihydroxymethylmethylacrylamide, and single-ended vinyl silicone oil; the single-ended vinyl silicone oil is CX-352M single-ended vinyl silicone oil, provided by Guangdong Chensi New Materials Technology Co., Ltd.

[0079] The preparation method of the functional copolymer comprises the following steps: adding 3-[N,N-dimethyl-[2-(2-methylprop-2-enoyloxy)ethyl]ammonium]propane-1-sulfonic acid inner salt, N-trihydroxymethyl methacrylamide, single-end vinyl silicone oil and an initiator to a high boiling point solvent, stirring and reacting at 68°C in an inert gas atmosphere for 4.5 hours, then removing the solvent by rotary evaporation, dissolving the obtained crude product in water, taking the supernatant and placing it in a dialysis bag, dialysing it in deionized water for 28 hours, and then The solution in the dialysis bag is then rotary evaporated to remove water to obtain a functional copolymer; the mass ratio of the 3-[N,N-dimethyl-[2-(2-methylprop-2-enoyloxy)ethyl]ammonium]propane-1-sulfonic acid inner salt, N-trihydroxymethyl methacrylamide, single-terminated vinyl silicone oil, initiator, and high boiling point solvent is 1:2.5:0.3:0.045:14; the initiator is azobisisobutyronitrile; the high boiling point solvent is N,N-dimethylformamide; and the inert gas is argon.

[0080] A method for preparing the water-oil two-phase micro-bead essence comprises the following steps: adding plant polysaccharides, hyaluronic acid, fish collagen peptides, other plant extracts, hydroxypropyl β-cyclodextrin, and functional copolymers into deionized water, and mixing them evenly to obtain a water phase; uniformly dispersing meso-tetramethyl-meso-tetra-p-aminophenylcalix[4]pyrrole, plant germ oil, other plant oils and fats, and ceramide in glycerol to obtain an oil phase; and uniformly dispersing the oil phase in the form of oil beads in the water phase to prepare the water-oil two-phase micro-bead essence.

[0081] Example 5

[0082] A water-oil two-phase micro-bead essence comprises the following raw materials, measured by weight percentage: 5wt% of plant polysaccharide, 0.015wt% of meso-tetramethyl-meso-tetra-p-aminophenyl cup [4] pyrrole, 1wt% of hyaluronic acid, 1wt% of fish collagen peptide, 3wt% of other plant extracts, 15wt% of glycerol, 0.3wt% of plant germ oil, 4wt% of other plant oils and fats, 0.3wt% of hydroxypropyl β-cyclodextrin, 0.5wt% of ceramide, and the balance is deionized water.

[0083] The plant polysaccharide is Flammulina velutipes polysaccharide; the preparation method of Meso-tetramethyl-meso-tetraaminophenylcalix[4]pyrrole, see: Guo Yong, Shao Shijun, He Lijun, et al. Synthesis and Characterization of Meso-tetramethyl-meso-tetraaminophenylcalix[4]pyrrole[J]. Chemical Reagents, 2002(6):344-345; the average molecular weight of the fish collagen peptide is 2000 Daltons.

[0084] The other plant extracts are extracted from the following plant raw materials in parts by weight: 6 parts of citrus, 5 parts of melon flowers, 8 parts of bamboo orchid, 6 parts of tea, 8 parts of Sophora japonica flowers, 10 parts of Poria cocos, 6 parts of bamboo shavings, 8 parts of ginseng flowers, 6 parts of jasmine flowers, 3 parts of rice flour, 8 parts of Evodia rutaecarpa, 6 parts of aloe vera, 10 parts of Centella asiatica, 3 parts of magnolia, 4 parts of raspberry, 8 parts of asparagus, 5 parts of almond, 5 parts of cloves, and 4 parts of azalea roots.

[0085] The method for extracting the other plant extracts comprises the following steps:

[0086] Step S1, mixing the plant raw materials of other plant extracts evenly to obtain a mixed material, adding water and boiling for 3 hours, filtering and collecting the water extract and filter residue;

[0087] Step S2, extracting the filter residue with ethanol, and collecting the alcohol extract by filtering;

[0088] Step S3, combining the above two extracts, concentrating under reduced pressure to recover ethanol and water, and obtaining other plant extracts.

[0089] The mass ratio of the mixed material to water in step S1 is 1:8; the decoction temperature is 98°C; the mass ratio of the filter residue to ethanol in step S2 is 1:8; the extraction in step S2 is heating reflux extraction, the extraction is performed 3 times, each time for 2 hours, and the 3 extracts are combined and allowed to stand.

[0090] The plant germ oil is wheat germ oil; the other plant oil is olive oil.

[0091] The water-oil two-phase micro-bead essence also includes: 0.01wt% of a functional copolymer; the functional copolymer includes structural units introduced by the following monomers: 3-[N,N-dimethyl-[2-(2-methylprop-2-enoyloxy)ethyl]ammonium]propane-1-sulfonic acid inner salt, N-trihydroxymethylmethylacrylamide, and single-ended vinyl silicone oil; the single-ended vinyl silicone oil is CX-352M single-ended vinyl silicone oil, provided by Guangdong Chensi New Materials Technology Co., Ltd.

[0092] The preparation method of the functional copolymer comprises the following steps: adding 3-[N,N-dimethyl-[2-(2-methylprop-2-enoyloxy)ethyl]ammonium]propane-1-sulfonic acid inner salt, N-trihydroxymethyl methacrylamide, single-end vinyl silicone oil and an initiator to a high boiling point solvent, stirring and reacting at 70°C for 5 hours in an inert gas atmosphere, then removing the solvent by rotary evaporation, dissolving the obtained crude product in water, taking the supernatant and placing it in a dialysis bag, and dialyzing it in deionized water for 30 hours. Then, the solution in the dialysis bag is rotary evaporated to remove water to obtain a functional copolymer; the mass ratio of the 3-[N,N-dimethyl-[2-(2-methylprop-2-enoyloxy)ethyl]ammonium]propane-1-sulfonic acid inner salt, N-trihydroxymethyl methacrylamide, single-terminated vinyl silicone oil, initiator, and high boiling point solvent is 1:3:0.3:0.05:15; the initiator is azobisisobutyronitrile; the high boiling point solvent is N-methylpyrrolidone; and the inert gas is argon.

[0093] A method for preparing the water-oil two-phase micro-bead essence comprises the following steps: adding plant polysaccharides, hyaluronic acid, fish collagen peptides, other plant extracts, hydroxypropyl β-cyclodextrin, and functional copolymers into deionized water, and mixing them evenly to obtain a water phase; uniformly dispersing meso-tetramethyl-meso-tetra-p-aminophenylcalix[4]pyrrole, plant germ oil, other plant oils and fats, and ceramide in glycerol to obtain an oil phase; and uniformly dispersing the oil phase in the form of oil beads in the water phase to prepare the water-oil two-phase micro-bead essence.

[0094] Comparative Example 1

[0095] A water-oil two-phase micro-bead essence and a preparation method thereof are basically the same as those in Example 1, except that meso-tetramethyl-meso-tetra-p-aminophenylcalix[4]pyrrole and hydroxypropyl β-cyclodextrin are not added.

[0096] Comparative Example 2

[0097] A water-oil two-phase micro-bead essence and a preparation method thereof are basically the same as those in Example 1, except that no other plant extracts and plant germ oil are added.

[0098] In order to further illustrate the beneficial technical effects of the water-oil two-phase micro-bead essence involved in each embodiment of the present invention, relevant performance tests were conducted on the water-oil two-phase micro-bead essence involved in Examples 1-5 and Comparative Examples 1-2. The test results are shown in Table 1. The test method is as follows:

[0099] (1) Sunscreen test: The test is conducted using the method for determining the sun protection factor (SPF value) of sunscreen cosmetics in Chapter 8 of the 2015 edition of the Technical Specifications for Safety of Cosmetics, which states the human efficacy evaluation test method.

[0100] (2) Skin improvement: 210 volunteers aged 35 to 60 who met the test conditions were selected and randomly divided into 7 groups, corresponding to the products of Examples 1-5 and Comparative Examples 1-2, respectively. After cleansing their faces in the morning and evening, about 0.5 g / time of the test product was evenly applied to the face and around the eyes, and gently massaged until absorbed. After 28 days, the moisture retention was tested using a skin moisture tester Corneometer CM825 (CK Company, Germany); the wrinkle reduction effect was tested using a human skin rapid optical imaging system (PRIMOS, Germany); Sa: average wrinkle depth; skin elasticity was tested using a skin elasticity tester MPA580 (Courage+Khazaka Company, Germany), and the test data was the average value of 30 subjects in each group. The sensitivity to stimulation, comfort and whitening effect were scored on a scale of 1-10 points. The higher the score, the better the evaluation. The average value of each group of volunteers was calculated; among them, the higher the score of irritation, the less irritation and the better the effect.

[0101] Table 1

[0102]

[0103] As can be seen from Table 1, the water-oil two-phase micro-bead essence involved in the embodiment of the present invention has more significant whitening, moisturizing, anti-wrinkle and sun protection effects than the comparative example product, and has less skin irritation; the combined use of meso-tetramethyl-meso-tetra-p-aminophenylcalix[4]pyrrole, hydroxypropyl β-cyclodextrin, other plant extracts and plant germ oil is beneficial to improving the above properties.

[0104] Each product was placed at room temperature for 6 months, and the essence after placement was observed. The microbeads of each product were uniform in size, complete in shape, and not aggregated, which confirmed that the water-oil two-phase microbead essence involved in each example of the present invention had high stability.

[0105] The above embodiments are only for illustrating the technical concept and features of the present invention, and their purpose is to enable people familiar with this technology to understand the contents of the present invention and implement them accordingly. They cannot be used to limit the protection scope of the present invention. All equivalent changes or modifications made according to the spirit of the present invention should be included in the protection scope of the present invention.

Claims

1. A water-oil two-phase micro-bead essence, characterized in that: The invention comprises the following raw materials by weight percentage: 2wt%-5wt% of plant polysaccharides, 0.005wt%-0.015wt% of meso-tetramethyl-meso-tetra-p-aminophenyl cup [4] pyrrole, 0.5wt%-1wt% of hyaluronic acid, 0.3wt%-1wt% of fish collagen peptide, 0.1wt%-3wt% of other plant extracts, 8wt%-15wt% of glycerol, 0.1wt%-0.3wt% of plant germ oil, 1wt%-4wt% of other plant oils and fats, 0.1wt%-0.3wt% of hydroxypropyl β-cyclodextrin, 0.3wt%-0.5wt% of ceramide, and the balance is deionized water.

2. The water-oil two-phase micro-bead essence according to claim 1, characterized in that: The plant polysaccharide is at least one of Flammulina velutipes polysaccharide, Tremella fuciformis polysaccharide and Coriolus versicolor polysaccharide.

3. The water-oil two-phase micro-bead essence according to claim 1, characterized in that: The average molecular weight of the fish collagen peptide is 1000-2000 Daltons.

4. The water-oil two-phase micro-bead essence according to claim 1, characterized in that: The other plant extracts are extracted from the following plant raw materials in parts by weight: 4-6 parts of citrus, 3-5 parts of melon flowers, 5-8 parts of bamboo orchid, 4-6 parts of tea, 5-8 parts of Sophora japonica flowers, 6-10 parts of Poria cocos, 3-6 parts of bamboo shavings, 5-8 parts of ginseng flowers, 4-6 parts of jasmine flowers, 1-3 parts of rice flour, 5-8 parts of Evodia rutaecarpa, 3-6 parts of aloe vera, 6-10 parts of Centella asiatica, 1-3 parts of magnolia, 2-4 parts of raspberry, 5-8 parts of asparagus, 3-5 parts of almonds, 3-5 parts of cloves, and 2-4 parts of azalea roots.

5. The water-oil two-phase micro-bead essence according to claim 4, characterized in that: The method for extracting the other plant extracts comprises the following steps: Step S1, uniformly mixing the plant raw materials of other plant extracts to obtain a mixed material, adding water and boiling for 1-3 hours, filtering and collecting the water extract and filter residue; Step S2, extracting the filter residue with ethanol, and collecting the alcohol extract by filtering; Step S3, combining the above two extracts, concentrating under reduced pressure to recover ethanol and water, and obtaining other plant extracts.

6. The water-oil two-phase micro-bead essence according to claim 5, characterized in that: The mass ratio of the mixed material to water in step S1 is 1:(5-8); the decoction temperature is 95-98°C; the mass ratio of the filter residue to ethanol in step S2 is 1:(6-8); the extraction in step S2 is heating reflux extraction, the extraction is performed 3 times, each time for 1-2 hours, and the 3 extracts are combined and allowed to stand.

7. The water-oil two-phase micro-bead essence according to claim 1, characterized in that: The plant germ oil is at least one of wheat germ oil, rice germ oil and corn germ oil; the other plant oils are any one or more of wormwood oil, tamanu oil, grape seed oil and olive oil.

8. The water-oil two-phase micro-bead essence according to claim 1, characterized in that: The water-oil two-phase micro-bead essence also includes: 0.003wt%-0.01wt% of a functional copolymer; the functional copolymer includes a structural unit introduced by the following monomers: 3-[N,N-dimethyl-[2-(2-methylprop-2-enoyloxy)ethyl]ammonium]propane-1-sulfonic acid inner salt, N-trihydroxymethylmethylacrylamide, and single-terminal vinyl silicone oil; the single-terminal vinyl silicone oil is CX-352M single-terminal vinyl silicone oil.

9. The water-oil two-phase micro-bead essence according to claim 1, characterized in that: The preparation method of the functional copolymer comprises the following steps: adding 3-[N,N-dimethyl-[2-(2-methylprop-2-enoyloxy)ethyl]ammonium]propane-1-sulfonic acid inner salt, N-trihydroxymethyl methacrylamide, single-end vinyl silicone oil and an initiator to a high boiling point solvent, stirring and reacting at 60-70°C for 3-5 hours in an inert gas atmosphere, then removing the solvent by rotary evaporation, dissolving the obtained crude product in water, taking the supernatant and placing it in a dialysis bag, dialyzing it in deionized water for 20-30 hours, and then removing water by rotary evaporation of the solution in the dialysis bag to obtain the functional copolymer. The mass ratio of the 3-[N,N-dimethyl-[2-(2-methylprop-2-enoyloxy)ethyl]ammonium]propane-1-sulfonic acid inner salt, N-trihydroxymethylmethyl acrylamide, single-terminated vinyl silicone oil, initiator, and high boiling point solvent is 1:(1-3):0.3:(0.03-0.05):(9-15); the initiator is azobisisobutyronitrile; the high boiling point solvent is at least one of N,N-dimethylformamide, N-methylpyrrolidone, and dimethyl sulfoxide; the inert gas is any one of nitrogen, helium, neon, and argon.

10. A method for preparing the water-oil two-phase micro-bead essence according to any one of claims 8 to 9, characterized in that: The method comprises the following steps: adding plant polysaccharides, hyaluronic acid, fish collagen peptides, other plant extracts, hydroxypropyl beta-cyclodextrin and functional copolymers into deionized water and mixing them evenly to obtain a water phase; uniformly dispersing meso-tetramethyl-meso-tetra-p-aminophenyl cup [4] pyrrole, plant germ oil, other plant oils and fats and ceramide in glycerol to obtain an oil phase; and uniformly dispersing the oil phase in the form of oil droplets in the water phase to prepare a water-oil two-phase micro-bead essence.

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