Disclosure of Invention
In order to overcome the technical defects, the invention develops a steady-state delivery system of the compound essential oil functional core ball and a preparation method and application of the essential liquid thereof, and successfully solves the problem of unstable application pain points.
The steady-state delivery system of the composite freeze-dried efficacy core ball has excellent spherical appearance, smooth ball surface, excellent dissolution and dispersion and more than 90% of porosity, and when the steady-state delivery system is dispersed into essence oil, the essence oil rapidly fills the pores of the efficacy core ball to obtain the composite essence oil efficacy core ball.
Firstly, innovatively developing a steady-state delivery system of an unstable small-molecule active ingredient, a biosynthesis active macromolecule, a permeation enhancer molecule, a functional small molecule and essential oil composite essential oil functional core ball, wherein the small-molecule active ingredient, the active macromolecule, the permeation enhancer molecule and the functional small molecule form an orderly stable nano assembly steady-state structure system through intermolecular multiple interactions, and the stability and compatibility problems of the small-molecule active ingredient are solved;
Secondly, developing skin care essential oil, and when the functional core balls are dispersed in the essential oil, rapidly filling the pores of the functional core balls by the essential oil to obtain composite essential oil functional core balls, so that the stability of active ingredients, the mechanical strength of the functional core balls and the shelf stability are further improved;
Thirdly, permeation promoter molecules such as phloretin, cyclodextrin, menthol and the like can further improve the transdermal absorptivity of small molecules, fourthly, developing a solvent, mixing the solvent with essential oil functional core balls, and gently shaking and uniformly mixing to obtain the freshly prepared functional skin care essential emulsion;
Finally, a full-flow low-temperature production and processing technology based on liquid nitrogen quick freezing is developed, the activity of small molecular active ingredients is ensured not to be affected by the technology, and the high-quality production of the functional core balls is ensured.
The steady-state delivery system of the compound essential oil functional core ball comprises an unstable micromolecule active ingredient, a biosynthesis active macromolecule, a permeation enhancer molecule, a functional micromolecule and essential oil.
In the steady-state delivery system of the compound essential oil functional core ball, the micromolecular active ingredients, the active macromolecules, the permeation promoter molecules and the functional micromolecules form an orderly and stable nanometer assembly steady-state structure system through intermolecular multiple interactions, and the problems of application pain points such as stability, compatibility and absorbability of the micromolecular active ingredients are successfully solved.
Further, in the above technical scheme, the unstable small molecule active ingredient comprises one or more of active ingredients such as ergothioneine, glutathione, anthocyanin, blue copper peptide, vitamin C (hereinafter referred to as Vc), ethyl bis iminomethyl elm guaiacol manganese chloride (hereinafter referred to as EUK 134) and the like.
Further, in the above technical scheme, the content of the unstable small molecule active ingredient (the content of the invention refers to the weight content and the same applies below) is 0.1% -70%, more suitable content is 1% -30%, and more suitable content is 5% -20%;
In the steady-state delivery system of the compound essential oil functional core ball, the biosynthesis active macromolecules are used for constructing a skeleton of the functional core ball, so that the mechanical stability of the functional core ball is improved.
Further, in the above technical scheme, the biosynthesis active macromolecule comprises one or more of fermentation polysaccharide, fermentation protein, recombinant collagen, recombinant type III collagen, recombinant type XII collagen, recombinant fibronectin, yeast protein, polyglutamic acid, pullulan, yeast polysaccharide, yeast beta-glucan, sodium hyaluronate, xanthan gum, gellan gum, DNA sodium (PDRN polydeoxyribonucleotide), fermentation ganoderan and the like.
Further, in the above technical scheme, the molecular weight range of the bio-fermentation synthesized active macromolecule is 1000-2000000, more suitable for the molecular weight range of 3000-1200000, and more suitable for the molecular weight range of 10000-800000.
In the steady-state delivery system of the compound essential oil functional core ball, the permeation enhancer molecules can further improve the transdermal absorption efficiency of the small molecule active ingredients.
Further, in the technical scheme, the permeation enhancer molecules comprise one or more of phloretin, menthol, hydroxypropyl beta cyclodextrin, methyl beta cyclodextrin, butanediol and the like.
In the steady-state delivery system of the compound essential oil functional core ball, the functional small molecules can further enrich or improve the skin care effect of the functional core ball.
Further, in the above technical scheme, the functional small molecule comprises one or more active ingredients of madecassoside, asiaticoside, theanine, nidus Collocaliae acid, arbutin, nicotinamide, tranexamic acid, ectoine, vc glucoside, catechin, trehalose, nonapeptide-1, snake venom peptide, conoid peptide, acetyl hexapeptide-8, mannitol and the like.
In the steady-state delivery system of the compound essential oil functional core ball, the functional core ball is dispersed in the essential oil, so that the stability of the active ingredients, the mechanical strength of the functional core ball and the shelf stability are further improved.
Further, in the technical scheme, the essential oil comprises one or more of coco oil-caprylate/caprate, isohexadecane, isododecane, jojoba seed oil, squalane, fermented peony seed oil, fermented merry-go-round oil, fermented rice bran oil, fermented grape seed oil, fermented vegetable oil, semen cassiae Luo Shuangzi lipid, corn germ oil, tocopheryl acetate, rapeseed oil, macadamia nut seed oil, isononyl isononanoate, ethylhexyl palmitate, caprylic/capric triglyceride, white pool flower seed oil, sunflower seed oil, rosebush oil, hydrogenated polyisobutene, polydimethylsiloxane, lavender essential oil, tea tree essential oil, plant essential oil, essence and the like.
Further, in the above technical scheme, the mass ratio of the unstable small molecule active ingredient, the biosynthesis active macromolecule and the permeation enhancer molecule to the functional small molecule is 1:0.1-10:0.05-5:0.1-10:1000-10000, and the more suitable ratio range is 1:0.5-5:0.1-1:0.5-5:100-1000.
Further, in the technical scheme, the particle size of the compound essential oil functional core ball ranges from 0.1 mm to 15mm, more suitably ranges from 0.5 mm to 8mm, and more suitably ranges from 1 mm to 5mm.
The invention also provides a production process of the steady-state delivery system of the compound essential oil functional core ball, which is based on the whole-flow low-temperature processing of liquid nitrogen quick freezing, and ensures that the activity of the micromolecular active ingredients is not influenced by the process. The production process of the steady-state delivery system of the compound essential oil efficacy core ball comprises the following steps of firstly preparing the compound freeze-dried efficacy core ball, and then rapidly filling pores of the efficacy core ball with essential oil when the efficacy core ball is dispersed in the essential oil to obtain the compound essential oil efficacy core ball.
The invention relates to a production process of a steady-state delivery system of a compound essential oil functional core ball, which comprises the following specific steps:
A. Uniformly mixing an unstable micromolecular active raw material and a biosynthesis active macromolecule, adding purified water, and stirring for dissolution to obtain a clear and transparent solution;
B. adding permeation enhancer molecules and functional small molecules into the solution in the stirring process, and stirring until various components are completely dissolved to obtain a target solution;
C. The target solution is dripped into a heat-preservation liquid nitrogen barrel, and nitrogen is required to be introduced into the target solution for protection during dripping, so that the oxidation loss of active ingredients is avoided;
D. And (3) freeze-drying the small ice balls formed by freezing with liquid nitrogen to obtain the composite freeze-drying effect core balls.
E. And dispersing the efficacy core balls into essential oil, and rapidly filling the pores of the efficacy core balls by the essential oil to obtain the steady-state delivery system of the compound essential oil efficacy core balls.
Further, in the above technical solution, in the step C, a dropping device capable of controlling a speed and a droplet size, including but not limited to a peristaltic pump, an injection pump, a flow pump, and the like, is used.
Further, in the technical scheme, the essential oil in the step E is prepared by respectively weighing different grease components, sequentially placing the grease components into a container, and uniformly stirring until the grease components are clear and transparent, thus obtaining the (skin care) essential oil.
The invention also provides a preparation method of the functional skin care essence, which comprises the following steps of mixing the solvent with the steady-state delivery system of the essential oil functional core ball, and mixing the solvent and the essential oil functional core ball uniformly by shaking to obtain the freshly prepared functional skin care essence.
Further, in the above technical solution, the solvent liquid of the present invention includes water, a humectant and/or an emulsifier. The solvent liquid is prepared through weighing humectant component and emulsifier component, adding purified water, and stirring to obtain the solvent liquid.
Further, in the technical scheme, the humectant comprises one or more of xylitol-based glucoside, dehydrated xylitol, tremella polysaccharide, betaine, sodium hyaluronate, xanthan gum, hydroxyethyl cellulose, butanediol, pentanediol, hexanediol, p-hydroxyacetophenone, glycerol, beta-glucan, polyglycerol-10, glycereth-26, chondrus crispus, glycosyl trehalose, hydrogenated starch hydrolysate and the like.
Further, in the above technical scheme, the emulsifier comprises tween-20 (polysorbate-20), tween 80, laureth-4, PEG-40 hydrogenated castor oil, wild soybean seed extract, cocoyl glucoside, PEG stearate, and the like.
Detailed Description
Example 1 preparation of ergothioneine Complex essential oil efficacy core ball steady-state delivery System No. I
A. Weighing 0.3g of ergothioneine, 0.6g of recombinant type III collagen, 0.45g of pram polysaccharide and 0.75g of yeast beta glucan respectively, putting into a beaker, and uniformly mixing;
B. adding 27.9g of purified water, heating and stirring until the active ingredients are completely dissolved;
C. The peristaltic pump drops the solution into a heat-insulating liquid nitrogen barrel dropwise, wherein the size of the drop is about 50mg, and the drop is frozen at a high speed to obtain small ice balls;
D. Transferring small ice balls formed by freezing liquid nitrogen into a freeze dryer, and freeze-drying for 40 hours, wherein the cold trap temperature of the freeze dryer is controlled to be about 70 ℃ (the left and right refer to the deviation of 3 ℃ up and down, the same applies below), and the final temperature of a drying cavity is controlled to be about 30 ℃, so that a steady-state delivery system of the ergothioneine composite freeze-drying efficacy core ball is obtained and is marked as A1;
E. 39.5g of hydrogenated polyisobutene, 35g of coco-caprylate/caprate, 7.0g of fermented peony seed oil, 9.0g of isohexadecane, 5.0g of squalane, 3.0g of maize germ oil, 1.0g of acrylic acid (ester) copolymer and 0.5g of damascus rose flower oil are respectively weighed, placed into a beaker, and then stirred and mixed uniformly to obtain essential oil;
F. Taking a certain amount of freeze-dried efficacy core balls, placing the freeze-dried efficacy core balls into a container such as a penicillin bottle, a glass bottle, a plastic bottle and the like, and then adding a certain amount of essential oil to obtain a steady-state delivery system I of the compound essential oil efficacy core balls, which is marked as B1.
Example 2 preparation of ergothioneine Complex essential oil efficacy core ball steady-state delivery System No. II
A. weighing 0.3g of ergothioneine, 0.48g of recombinant type III collagen, 0.45g of pramipexole, 0.54g of yeast beta glucan, 0.3g of trehalose and 0.06g of ectoin respectively, and putting into a beaker for uniform mixing;
B. adding 27.87g of purified water, heating and stirring until the active ingredients are completely dissolved;
C. The peristaltic pump drops the solution into a heat-insulating liquid nitrogen barrel dropwise, wherein the size of the drop is about 50mg, and the drop is frozen at a high speed to obtain small ice balls;
D. transferring small ice balls formed by freezing liquid nitrogen into a freeze dryer, freeze drying for 40h, controlling the cold trap temperature of the freeze dryer at about-70 ℃ and the final temperature of a drying cavity at about 30 ℃, and obtaining a steady-state delivery system of the ergothioneine composite freeze-drying efficacy core balls, which is marked as A2;
E. 39.5g of hydrogenated polyisobutene, 35g of coco-caprylate/caprate, 7.0g of fermented peony seed oil, 9.0g of isohexadecane, 5.0g of squalane, 3.0g of maize germ oil, 1.0g of acrylic acid (ester) copolymer and 0.5g of damascus rose flower oil are respectively weighed, placed into a beaker, and then stirred and mixed uniformly to obtain essential oil;
F. Taking a certain amount of freeze-dried efficacy core balls, placing the freeze-dried efficacy core balls into a container such as a penicillin bottle, a glass bottle, a plastic bottle and the like, and then adding a certain amount of essential oil to obtain a steady-state delivery system II of the compound essential oil efficacy core balls, which is marked as B2.
Example 3 preparation of ergothioneine Complex essential oil efficacy core ball steady-state delivery System No. III
A. Weighing 0.3g of ergothioneine, 0.48g of recombinant type III collagen, 0.45g of pullulan, 0.54g of yeast beta glucan, 0.3g of trehalose, 0.03g of nonapeptide-1, 0.06g of ectoin, 0.03g of phloretin and 0.18g of methyl beta cyclodextrin respectively, putting into a beaker, and uniformly mixing;
B. Adding 27.66g of purified water, heating and stirring until the active ingredients are completely dissolved;
C. The peristaltic pump drops the solution into a heat-insulating liquid nitrogen barrel dropwise, wherein the size of the drop is about 50mg, and the drop is frozen at a high speed to obtain small ice balls;
D. Transferring small ice balls formed by freezing liquid nitrogen into a freeze dryer, freeze drying for 40h, controlling the cold trap temperature of the freeze dryer at about-70 ℃ and the final temperature of a drying cavity at about 30 ℃, and obtaining a steady-state delivery system of the ergothioneine composite freeze-drying efficacy core balls, which is marked as A3;
E. 39.5g of hydrogenated polyisobutene, 35g of coco-caprylate/caprate, 7.0g of fermented peony seed oil, 9.0g of isohexadecane, 5.0g of squalane, 3.0g of maize germ oil, 1.0g of acrylic acid (ester) copolymer and 0.5g of damascus rose flower oil are respectively weighed, placed into a beaker, and then stirred and mixed uniformly to obtain essential oil;
F. Taking a certain amount of freeze-dried efficacy core balls, placing the freeze-dried efficacy core balls into a container such as a penicillin bottle, a glass bottle, a plastic bottle and the like, and then adding a certain amount of essential oil to obtain a steady-state delivery system III of the compound essential oil efficacy core balls, which is marked as B3.
Example 4 preparation of glutathione composite essential oil efficacy core ball steady state delivery System IV
A. Weighing 0.24g of glutathione, 0.36g of recombinant XVII type collagen, 0.48g of zymosan, 0.36g of sodium hyaluronate, 0.3g of madecassoside, 0.06g of acetyl hexapeptide-8, 0.12g of DNA sodium and 0.18g of mannitol respectively, putting into a beaker, and uniformly mixing;
B. 27.96g of purified water is added and stirred until the active ingredients are completely dissolved;
C. The peristaltic pump drops the solution into a heat-insulating liquid nitrogen barrel dropwise, wherein the size of the drop is about 40mg, and the drop is frozen at a high speed to obtain small ice balls;
D. transferring small ice balls formed by freezing liquid nitrogen into a freeze dryer, freeze drying for 40h, controlling the cold trap temperature of the freeze dryer at about-70 ℃ and the final temperature of a drying cavity at about 30 ℃, and obtaining a steady-state delivery system of the ergothioneine composite freeze-drying efficacy core balls, which is marked as A4;
E. Respectively weighing 41g of jojoba seed oil, 22g of isododecane, 9g of fermented mervine fruit oil, 8g of fermented rice bran oil, 8g of tocopheryl acetate, 11g of sunflower seed oil and 1.0 of tea tree essential oil, putting into a beaker, and then stirring and mixing uniformly to obtain essential oil;
F. Taking a certain amount of freeze-dried efficacy core balls, placing the freeze-dried efficacy core balls into a container such as a penicillin bottle, a glass bottle, a plastic bottle and the like, and then adding a certain amount of essential oil to obtain a steady-state delivery system IV of the compound essential oil efficacy core balls, which is marked as B4.
Example 5 preparation of glutathione composite essential oil efficacy core ball steady state delivery System No. V
A. Weighing 0.24g of glutathione, 0.36g of recombinant XVII type collagen, 0.48g of zymosan, 0.36g of sodium hyaluronate, 0.3g of madecassoside, 0.01g of conoid peptide, 0.12g of DNA sodium, 0.18g of mannitol, 0.06g of menthol and 0.15g of hydroxypropyl beta cyclodextrin respectively, putting into a beaker, and mixing uniformly;
B. Adding 27.75g of purified water, and stirring until the active ingredients are completely dissolved;
C. The peristaltic pump drops the solution into a heat-insulating liquid nitrogen barrel dropwise, wherein the size of the drop is about 40mg, and the drop is frozen at a high speed to obtain small ice balls;
D. Transferring small ice balls formed by freezing liquid nitrogen into a freeze dryer, freeze drying for 40h, controlling the cold trap temperature of the freeze dryer at about-70 ℃ and the final temperature of a drying cavity at about 30 ℃, and obtaining a steady-state delivery system of the ergothioneine composite freeze-drying efficacy core balls, which is marked as A5;
E. Respectively weighing 41g of jojoba seed oil, 22g of isododecane, 9g of fermented mervine fruit oil, 8g of fermented rice bran oil, 8g of tocopheryl acetate, 11g of sunflower seed oil and 1.0 of tea tree essential oil, putting into a beaker, and then stirring and mixing uniformly to obtain essential oil;
F. Taking a certain amount of freeze-dried functional core balls, placing the core balls into a container such as a penicillin bottle, a glass bottle, a plastic bottle and the like, and then adding a certain amount of essential oil to obtain a compound essential oil functional core ball V number which is marked as B5.
Example 6 preparation of anthocyanin-Vc composite essential oil efficacy core ball Steady State delivery System VI
A. Weighing 0.09g anthocyanin, 0.54g recombinant fibronectin, 0.15g xanthan gum, 0.45g polyglutamic acid, 0.3g asiaticoside, 0.42g vitamin C (Vc), 0.15gVc g glucoside and 0.3g theanine respectively, putting into a beaker, and uniformly mixing;
B. Adding 27.75g of purified water, and stirring until the active ingredients are completely dissolved;
C. Dropwise adding the solution into a heat-insulating liquid nitrogen barrel by a peristaltic pump, wherein the size of the liquid drop is about 40mg, and freezing at a high speed to obtain a small ice ball;
D. Transferring small ice balls formed by freezing liquid nitrogen into a freeze dryer, freeze drying for 40h, controlling the cold trap temperature of the freeze dryer at about-70 ℃ and the final temperature of a drying cavity at about 30 ℃, and obtaining a steady-state delivery system of the ergothioneine composite freeze-drying efficacy core balls, which is marked as A6;
E. Respectively weighing 33g of fermented grape seed oil, 32g of ethylhexyl palmitate, 8g of Chinese buckeye Luo Shuangzi fat, 9g of rapeseed oil, 12g of macadamia nut seed oil, 5g of squalane and 1.0g of essence, putting into a beaker, and then stirring and mixing uniformly to obtain essential oil;
F. taking a certain amount of freeze-dried efficacy core balls, placing the freeze-dried efficacy core balls into a container such as a penicillin bottle, a glass bottle, a plastic bottle and the like, and then adding a certain amount of essential oil to obtain a steady-state delivery system VI number of the compound essential oil efficacy core balls, which is marked as B6.
Example 7 preparation of anthocyanin-Vc composite essential oil efficacy core ball Steady State delivery System VII No
A. Weighing 0.09g anthocyanin, 0.54g recombinant fibronectin, 0.15g xanthan gum, 0.45g polyglutamic acid, 0.3g asiaticoside, 0.42g vitamin C, 0.15g Vc glucoside, 0.3g theanine, 0.03g butanediol and 0.03g phloretin respectively, and putting into a beaker for uniform mixing;
B. Adding 27.69g of purified water, and stirring until the active ingredients are completely dissolved;
C. The peristaltic pump drops the solution into a heat-insulating liquid nitrogen barrel dropwise, wherein the size of the drop is about 40mg, and the drop is frozen at a high speed to obtain small ice balls;
D. Transferring small ice balls formed by freezing liquid nitrogen into a freeze dryer, freeze drying for 40h, controlling the cold trap temperature of the freeze dryer at about-70 ℃ and the final temperature of a drying cavity at about 30 ℃, and obtaining a steady-state delivery system of the ergothioneine composite freeze-drying efficacy core balls, which is marked as A7;
E. Respectively weighing 33g of fermented grape seed oil, 32g of ethylhexyl palmitate, 8g of Chinese buckeye Luo Shuangzi fat, 9g of rapeseed oil, 12g of macadamia nut seed oil, 5g of squalane and 1.0g of essence, putting into a beaker, and then stirring and mixing uniformly to obtain essential oil;
F. Taking a certain amount of freeze-dried efficacy core balls, placing the freeze-dried efficacy core balls into a container such as a penicillin bottle, a glass bottle, a plastic bottle and the like, and then adding a certain amount of essential oil to obtain a stable delivery system VII of the compound essential oil efficacy core balls, which is marked as B7.
Example 8 preparation of EUK134 Complex essential oil efficacy core ball Steady State delivery System VIII
A. weighing 0.09g of EUK134, 0.48g of yeast protein, 0.3g of recombinant collagen, 0.24g of gellan gum, 0.18g of fermented ganoderan, 0.45g of nidus Collocaliae acid, 0.09g of snake venom peptide and 0.12g of arbutin respectively, putting into a beaker, and uniformly mixing;
B. Adding 28.14g of purified water, and stirring until the active ingredients are completely dissolved;
C. The peristaltic pump drops the solution into a heat-insulating liquid nitrogen barrel dropwise, wherein the size of the drop is about 40mg, and the drop is frozen at a high speed to obtain small ice balls;
D. Transferring small ice balls formed by freezing liquid nitrogen into a freeze dryer, freeze drying for 40h, controlling the cold trap temperature of the freeze dryer at about-70 ℃ and the final temperature of a drying cavity at about 30 ℃, and obtaining a steady-state delivery system of the ergothioneine composite freeze-drying efficacy core balls, which is marked as A8;
E. Respectively weighing 22g isononyl isononanoate, 37g caprylic/capric triglyceride, 5g Chinese buckeye Luo Shuangzi fat, 20g white pond flower seed oil, 5g polydimethylsiloxane, 10g fermented grape seed oil and 1.0g lavender essential oil, putting into a beaker, and then stirring and mixing uniformly to obtain essential oil;
F. Taking a certain amount of freeze-dried efficacy core balls, placing the freeze-dried efficacy core balls into a container such as a penicillin bottle, a glass bottle, a plastic bottle and the like, and then adding a certain amount of essential oil to obtain a steady-state delivery system VIII of the compound essential oil efficacy core balls, which is marked as B8.
Example 9 preparation of EUK134 Complex essential oil efficacy core ball Steady State delivery System IX
A. Weighing 0.09g of EUK134, 0.48g of yeast protein, 0.3g of recombinant collagen, 0.24g of gellan gum, 0.18g of fermented ganoderan, 0.45g of nidus Collocaliae acid, 0.12g of arbutin, 0.03g of phloretin, 0.18g of hydroxypropyl beta cyclodextrin and 0.03g of butanediol respectively, putting into a beaker, and uniformly mixing;
B. Adding 27.9g of purified water, and stirring until the active ingredients are completely dissolved;
C. The peristaltic pump drops the solution into a heat-insulating liquid nitrogen barrel dropwise, wherein the size of the drop is about 40mg, and the drop is frozen at a high speed to obtain small ice balls;
D. transferring small ice balls formed by freezing liquid nitrogen into a freeze dryer, freeze drying for 40h, controlling the cold trap temperature of the freeze dryer at about-70 ℃ and the final temperature of a drying cavity at about 30 ℃, and obtaining a steady-state delivery system of the ergothioneine composite freeze-drying efficacy core balls, which is marked as A9;
E. Respectively weighing 22g isononyl isononanoate, 37g caprylic/capric triglyceride, 5g Chinese buckeye Luo Shuangzi fat, 20g white pond flower seed oil, 5g polydimethylsiloxane, 10g fermented grape seed oil and 1.0g lavender essential oil, putting into a beaker, and then stirring and mixing uniformly to obtain essential oil;
F. Taking a certain amount of freeze-dried efficacy core balls, placing the freeze-dried efficacy core balls into a container such as a penicillin bottle, a glass bottle, a plastic bottle and the like, and then adding a certain amount of essential oil to obtain a steady-state delivery system IX of the compound essential oil efficacy core balls, which is marked as B9.
Example 10 preparation of blue copper peptide composite essential oil efficacy core ball steady-state delivery System No. X
A. weighing 0.24g of blue copper peptide, 0.36g of recombinant type III collagen, 0.6g of yeast beta glucan, 0.45g of sodium hyaluronate, 0.18g of nicotinamide, 0.09g of ectoin, 0.09g of Vc ethyl ether, 0.45g of hydroxypropyl beta cyclodextrin and 0.06g of phloretin respectively, putting into a beaker, and uniformly mixing;
B. adding 27.48g of purified water, and stirring until the active ingredients are completely dissolved;
C. The peristaltic pump drops the solution into a heat-insulating liquid nitrogen barrel dropwise, wherein the size of the drop is about 40mg, and the drop is frozen at a high speed to obtain small ice balls;
D. Transferring small ice balls formed by freezing liquid nitrogen into a freeze dryer, freeze drying for 40h, controlling the cold trap temperature of the freeze dryer at about-70 ℃ and the final temperature of a drying cavity at about 30 ℃, and obtaining a steady-state delivery system of the ergothioneine composite freeze-drying efficacy core balls, which is marked as A10;
E. Respectively weighing 22g isononyl isononanoate, 37g caprylic/capric triglyceride, 5g Chinese buckeye Luo Shuangzi fat, 20g white pond flower seed oil, 5g polydimethylsiloxane, 10g fermented grape seed oil and 1.0g lavender essential oil, putting into a beaker, and then stirring and mixing uniformly to obtain essential oil;
F. taking a certain amount of freeze-dried efficacy core balls, placing the freeze-dried efficacy core balls into a container such as a penicillin bottle, a glass bottle, a plastic bottle and the like, and then adding a certain amount of essential oil to obtain a steady-state delivery system X of the compound essential oil efficacy core balls, which is marked as B10.
Example 11 preparation of blue copper peptide composite essential oil efficacy core ball steady state delivery System XI
A. Weighing 0.15g of blue copper peptide, 0.06g of nicotinamide, 0.3g of recombinant fibronectin, 0.36g of pullulan, 0.3g of sodium hyaluronate, 0.27g of theanine, 0.15g of trehalose and 0.03g of butanediol respectively, and putting into a beaker to be uniformly mixed;
B. adding 27.69g of purified water, and stirring until the active ingredients are completely dissolved;
C. The peristaltic pump drops the solution into a heat-insulating liquid nitrogen barrel dropwise, wherein the size of the drop is about 40mg, and the drop is frozen at a high speed to obtain small ice balls;
D. Transferring small ice balls formed by freezing liquid nitrogen into a freeze dryer, freeze drying for 40h, controlling the cold trap temperature of the freeze dryer at about-70 ℃ and the final temperature of a drying cavity at about 30 ℃, and obtaining the ergothioneine composite freeze-drying effect core balls, which are marked as A11;
E. Respectively weighing 22g isononyl isononanoate, 37g caprylic/capric triglyceride, 5g Chinese buckeye Luo Shuangzi fat, 20g white pond flower seed oil, 5g polydimethylsiloxane, 10g fermented grape seed oil and 1.0g lavender essential oil, putting into a beaker, and then stirring and mixing uniformly to obtain essential oil;
F. Taking a certain amount of freeze-dried efficacy core balls, placing the freeze-dried efficacy core balls into a container such as a penicillin bottle, a glass bottle, a plastic bottle and the like, and then adding a certain amount of essential oil to obtain a stable delivery system XI of the compound essential oil efficacy core balls, which is marked as B11.
Test example 1 composite lyophilized efficacy pellet steady-state delivery system and appearance of composite essential oil efficacy pellet steady-state delivery system
And shooting by a camera, characterizing the appearance and morphology diagram of the steady-state delivery system of the composite freeze-dried efficacy core ball and the steady-state delivery system of the composite essential oil efficacy core ball, and carrying out comparative analysis.
1) The steady-state delivery system series of the ergothioneine compound essential oil functional core balls can be seen from A1, A2 and A3 in figure 1, and after freeze drying, the steady-state delivery system of the white ergothioneine compound freeze-dried functional core balls, namely the mesitylene, can be obtained in the examples 1-3, and most of the balls are good balls, and the surface is smooth. The surface of the small ball is provided with a few cracks, which are mainly caused by uneven internal stress during freezing, and the subsequent use is not affected. The 3 samples were not significantly different from each other in appearance. After the essential oil is added, the essential oil rapidly fills the pores of the freeze-dried core ball, the steady-state delivery systems B1, B2 and B3 of the composite essential oil functional core ball are obtained, the appearance of a perfect spherical structure is kept intact, and the structural stability of the functional core ball and the shelf life stability of an active substance are also obviously improved.
2) Glutathione composite essential oil efficacy pellet steady state delivery System series A4 and A5 in FIG. 2 are glutathione composite freeze-dried efficacy pellets steady state delivery System from examples 4 and 5. In the samples A4 and A5, the white pellets have good sphericity and a smooth surface. The surface of the small ball is provided with a few cracks, which are mainly caused by uneven internal stress during freezing, and the subsequent use is not affected. After the essential oil is added, the functional core balls B4 and B5 of the composite essential oil are obtained, the appearance of a perfect spherical structure is kept intact, and the structural stability of the functional core balls and the shelf life stability of active substances are also obviously improved.
3) Fig. 3 is an anthocyanin-Vc complex lyophilized efficacy pellet steady state delivery system from examples 6 and 7. In the samples A6 and A7, most of the rose balls have good sphericity and have smoother surfaces. The surface of the small ball is provided with a few cracks, which are mainly caused by uneven internal stress during freezing, and the subsequent use is not affected. After the essential oil is added, the composite essential oil functional core balls B6 and B7 are obtained, the color of the core balls becomes brighter, the appearance of a perfect spherical structure is kept intact, and the structural stability of the functional core balls and the shelf life stability of active substances are also obviously improved.
4) EUK134 composite essential oil efficacy core ball steady state delivery system fig. 4 is EUK composite lyophilized efficacy core ball steady state delivery system from examples 8 and 9. In the samples A8 and A9, the yellow pellets have good sphericity and a smooth surface. The surface of the small ball is provided with a few cracks, which are mainly caused by uneven internal stress during freezing, and the subsequent use is not affected. After the essential oil is added, the composite essential oil functional core balls B8 and B9 are obtained, the color of the core balls becomes brighter, the appearance of a perfect spherical structure is kept intact, and the structural stability of the functional core balls and the shelf life stability of active substances are also obviously improved.
5) Figure 5 is a steady state delivery system of blue copper peptide complex essential oil efficacy core spheres from examples 10 and 11. In the samples A10 and A11, most of the blue pellets have good sphericity and a smooth surface. The surface of the small ball is provided with a few cracks, which are mainly caused by uneven internal stress during freezing, and the subsequent use is not affected. After the essential oil is added, the steady-state delivery systems B10 and B11 of the compound essential oil functional core balls are obtained, the color of the core balls becomes brighter, the appearance of a perfect spherical structure is kept intact, and the structural stability of the functional core balls and the shelf life stability of active substances are also obviously improved.
Test example 2 appearance of an essential emulsion of a composite essential oil efficacy core ball steady state delivery system
Based on the composite essential oil functional core ball, fresh essence emulsion can be prepared, namely the composite essential oil functional core ball steady-state delivery system essence emulsion can be prepared, and the application cases are detailed. The composite efficacy-based core ball essence emulsion was characterized by photographing with a camera and performing comparative analysis (fig. 6).
As can be seen from fig. 6, C2, C3, C4, C5, C6 and C7 are milk cap type essential emulsions. This is mainly due to the addition of emulsifier components such as tween 20, laureth-4 and PEG-40 hydrogenated castor oil, etc. to the vehicle. When the essence emulsion is prepared by shaking, the steady-state delivery system of the efficacy core ball is dissolved in the solvent liquid, and meanwhile, the essence oil is emulsified to form fine emulsion drops. After a period of time, the emulsion drops float upwards, and the milk cover type functional core ball essence emulsion can be obtained. In contrast, C8, C9, C10 and C11 are bilayer clear essences, mainly because no emulsifier is added to the vehicle. Although the essential oil becomes fine emulsion droplets when shaking up to prepare the essential emulsion, stable emulsion cannot be formed due to no emulsifying agent, and after a period of time, oil-water two phases are separated to obtain the double-layer transparent essential liquid. The double-layer transparent essence does not affect the use of consumers, but is easier to form a protective layer on the surface of skin when being smeared for use.
Detection example 3 scanning electron microscope image
FIG. 7 is a scanning electron microscope image of four samples A3, A5, A7 and A9. The efficacy core ball steady-state delivery system was gently broken off and then observed with a scanning electron microscope. As can be seen from the figure, the interior of the pellets is a uniform layered structure with uniformly distributed micro-scale channels between layers. When liquid nitrogen is frozen at a high speed, active substances dissolved in water are quickly separated out to form tiny crystal grains, and then when ice crystals are sublimated in freeze drying, water vapor forms micron-sized water vapor channels, and meanwhile, the tiny active substance crystal grains are connected into a piece to form a layered structure. Since liquid nitrogen freezes very rapidly, the microstructure of the whole pellet is very uniform. The active layer is very thin, substantially less than 1 micron, which ensures that the active is very soluble when water is re-added.
Test example 4 stability
The stability of active ingredients such as ergothioneine, glutathione, anthocyanin, blue copper peptide, vitamin C, EUK and the like is poor, and particularly in an aqueous formula system, the active ingredients are extremely easy to oxidize, complex or decompose, so that the biological activity is lost.
With reference to cosmetic stability evaluation, stability of the composite freeze-dried efficacy core ball steady-state delivery system and the composite essential oil efficacy core ball steady-state delivery system is evaluated through a 45 ℃ acceleration experiment and compared with control essence. Aiming at the stable state delivery system of the composite freeze-drying efficacy core ball and the stable state delivery system of the composite essential oil efficacy core ball, an acceleration experiment is firstly carried out, and then a solution with a certain concentration is prepared for detection and analysis. Different aging times were tested with the initial concentration of the target active ingredient being 100% and the retained concentration of the target active ingredient being a percentage of the initial concentration. The results are shown in the following table.
A. Series of samples of steady-state delivery system of ergothioneine composite efficacy core ball
As can be seen from Table 1, the content or concentration of ergothioneine in the ergothioneine concentrate was reduced by about 10% after 28 days of acceleration experiments. The change of the ergothioneine in the three ergothioneine composite freeze-dried efficacy core spheres is very small and is reduced by less than 1 percent (about 0.8 percent). This demonstrates that the stability of ergothioneine is greatly improved in the composite freeze-dried efficacy core spheres. In the steady-state delivery system of the ergothioneine compound essential oil efficacy core ball, the content of the ergothioneine is almost unchanged, and is reduced by about 0.1 percent, which is about one eighth of the reduction of the freeze-dried efficacy core ball. The essential oil is added into the freeze-dried functional core ball, so that the essential oil can further block the influence of oxygen and even illumination on the ergothioneine, and the stability of the ergothioneine is further improved.
TABLE 1 stability of ergothioneine Complex efficacy core ball steady state delivery System series products
B. glutathione composite efficacy core ball steady-state delivery system series samples
As can be seen from Table 2, the stability of glutathione is relatively poor, about 99% of glutathione in the control essence is oxidized and degraded after 1 day of accelerated experiments, the content is only about 0.3% of the original content, and the glutathione cannot be detected after 7 days. The glutathione in the steady-state delivery system of the two glutathione composite freeze-dried efficacy pellets is very small, and the glutathione is reduced by less than 2 percent (about 1.9 percent) after 28 days. This demonstrates that glutathione stability is greatly improved in a composite freeze-dried efficacy core ball steady-state delivery system. In the steady-state delivery system of the glutathione composite essential oil efficacy core ball, the content change of the glutathione is smaller, the reduction is about 0.9 percent, and the reduction of the glutathione content of the glutathione composite essential oil efficacy core ball is less than half of that of the freeze-drying efficacy core ball. This shows that the essential oil is added into the stable delivery system of the freeze-dried efficacy core ball, and can further block the influence of oxygen and even light on glutathione, thereby further improving the stability of the glutathione.
TABLE 2 stability of glutathione composite efficacy core ball series products
C. anthocyanin-Vc composite efficacy core ball steady-state delivery system series samples
As can be seen from Table 3, the anthocyanin stability is relatively poor, about 99% of glutathione in the control essence is oxidized and degraded after 1 day of accelerated experiment, the content is only about 1% of the original content, and the glutathione is not detected after 7 days. The change of anthocyanin in the steady-state delivery system of the two anthocyanin-Vc composite freeze-dried efficacy pellets is very small, and the anthocyanin is reduced by less than 2 percent (about 1.7 percent) after 28 days. This indicates that the stability of anthocyanin is greatly improved in the complex lyophilized efficacy core ball steady-state delivery system. In the stable state delivery system of the anthocyanin-Vc compound essential oil efficacy core ball, the content change of the anthocyanin is smaller, and the content of the anthocyanin is reduced by about 0.7 percent and is less than half of the reduction of the stable state delivery system of the freeze-drying efficacy core ball. This demonstrates that the addition of essential oils to the lyophilized efficacy pellet steady-state delivery system can further block the effects of oxygen and even light on anthocyanin, further improving its stability.
TABLE 3 anthocyanin stability in the series of products of the anthocyanin-Vc composite efficacy core ball steady-state delivery System
Also, as can be seen from table 4, after 1 day of the accelerated experiment, more than 99% of vitamin C in the control essence was oxidized and degraded, and the content was only about 1% of the original content, and after 7 days, it was not detected at all. The change of Vc in a steady-state delivery system of the two anthocyanin-Vc composite freeze-dried efficacy core spheres is very small, and the Vc is reduced by less than 2 percent (about 1.9 percent) after 28 days. This indicates that the stability of Vc is greatly improved in the composite freeze-dried efficacy core ball steady-state delivery system. In the anthocyanin-Vc compound essential oil efficacy core ball, the Vc content is less in change, and is reduced by about 0.65 percent, which is about one third of the reduction of the steady-state delivery system of the freeze-drying efficacy core ball. This demonstrates that the essential oil is added into the steady-state delivery system of the freeze-dried functional core spheres, and can further block the influence of oxygen and even illumination on Vc, thereby further improving the stability of the essential oil.
TABLE 4 Vc stability in anthocyanin-Vc composite efficacy core ball steady-state delivery System series products
D. EUK134 composite efficacy core ball steady state delivery System series samples
As can be seen from Table 5, after 28 days of accelerated experiments, the EUK content or concentration in EUK134,134 essence is reduced by about 13%. The EUK134 in the steady-state delivery system of the two EUK and 134 composite lyophilized efficacy pellets is very little changed and drops by about 1%. This indicates that EUK134,134 stability is greatly improved in the composite freeze-dried efficacy core ball steady state delivery system. In the EUK and 134 compound essential oil efficacy pellet steady-state delivery system, the EUK and 134 content is almost unchanged, and the reduction is about 0.3 percent, which is about one third of the reduction of the lyophilized efficacy pellet steady-state delivery system. This indicates that the addition of essential oil to the lyophilized efficacy pellet steady state delivery system can further block the oxygen and even light effects on EUK134,134, further improving its storage stability.
TABLE 5 EUK stability of a series of products of a composite efficacy core ball steady state delivery system
F. blue copper peptide composite efficacy core ball steady-state delivery system series samples
As can be seen from Table 6, the content or concentration of the blue copper peptide in the blue copper peptide essence is reduced by about 17% after the 28-day acceleration experiment. The change of the blue copper peptide in the steady-state delivery system of the two blue copper peptide composite freeze-drying efficacy core spheres is very small, and the decrease is about 0.9%. This indicates that the stability of the blue copper peptide is greatly improved in the steady-state delivery system of the composite freeze-dried efficacy core sphere. In the EUK and 134 compound essential oil efficacy pellet steady-state delivery system, the EUK and 134 content is almost unchanged, and the reduction is about 0.2 percent, which is about one quarter of the reduction of the lyophilized efficacy pellet steady-state delivery system. This shows that the essential oil is added into the stable delivery system of the freeze-dried efficacy core sphere, and can further block the influence of oxygen and light on the blue copper peptide, thereby further improving the storage stability of the blue copper peptide.
TABLE 6 stability of blue copper peptide composite efficacy core ball steady state delivery System series products
Test example 5 transdermal absorption
For the application cases of steady-state delivery systems of compound essential oil efficacy core balls with different active ingredients, corresponding control essences are selected, and are subjected to systemic transdermal experimental efficacy evaluation and comparison, wherein the evaluation method refers to the chemical skin absorption in-vitro test method, and the evaluation results are as follows:
TABLE 7 active ingredient composite essential oil efficacy core ball and transdermal test evaluation data of control essential
For the ergothioneine series application examples 1-3, it can be seen from Table 7 that the transdermal effect of the steady-state delivery system essence emulsion II of the core ball of the ergothioneine composite efficacy is significantly better than that of the ergothioneine control essence, and the transdermal amount of the ergothioneine composite efficacy core ball is approximately 3 times that of the control essence. And the steady-state delivery system essence emulsion III of the ergothioneine composite efficacy core ball added with the penetration enhancer has better transdermal effect, and the transdermal quantity of 24 hours is more than 4 times of that of a control essence.
For glutathione series application examples 4-6, only 1h and 4h transdermal effects were tested, as glutathione is very unstable and subject to oxidative deterioration. As can be seen from table 7, the glutathione composite efficacy core ball steady-state delivery system essence emulsion IV transdermal effect is significantly better than the glutathione control essence, with a 4h transdermal amount of about 2 times that of the control essence. And the glutathione composite efficacy core ball steady-state delivery system essence emulsion V added with the penetration enhancer has better transdermal effect, and the transdermal quantity of 4 hours is about 3 times that of the control essence.
For anthocyanin-Vc series application examples 7-9, also because of poor stability of anthocyanin and Vc, only 1h and 4h transdermal effects are detected. As can be seen from table 7, the stable delivery system essence emulsion VI of the anthocyanin-Vc composite efficacy core ball has a significantly better transdermal effect than the anthocyanin-Vc control essence, the 4h transdermal amount of anthocyanin is about 2.5 times that of the control essence, and the 4h transdermal amount of Vc is about 2 times that of the control essence. The permeation enhancer is added into the stable delivery system essence emulsion VII of the composite efficacy core ball, the transdermal effect is better, the transdermal quantity of anthocyanin 4h is about 4 times of that of the control essence, and the transdermal quantity of Vc 4h is about 3 times of that of the control essence.
For EUK-134 series application examples 10-12, as can be seen from table 7, the transdermal effect of EUK-134 composite efficacy core ball steady-state delivery system essence emulsion VIII is significantly better than EUK control essence, and the 24-hour transdermal amount is approximately 2 times that of the control essence. And the permeation enhancer EUK and the compound efficacy core ball steady-state delivery system essence emulsion IX are added, so that the transdermal effect is better, and the transdermal quantity for 24 hours is about 3 times that of the control essence.
Aiming at application examples 13-15 of blue copper peptide series, active ingredients of a penetration enhancer are added into a steady-state delivery system of two blue copper peptide composite efficacy core spheres. As can be seen from table 7, the steady-state delivery system essence emulsions X and XI of the blue copper peptide composite efficacy core ball have significantly better transdermal effects than the blue copper peptide control essence, and the 24-hour transdermal amounts are about 4 times that of the control essence.
Application example 1 ergothioneine control essence
(1) 86.6G of purified water, 5.0g of butanediol, 0.80g of carrageenan and 0.40g of raspberry ketone are sequentially weighed, placed into a container, heated at 40 ℃ and stirred for uniform dissolution;
(2) After stirring and cooling, sequentially adding 5.0g of rose damascus (ROSA damascana) floral water, 2.0g of 1, 2-pentanediol and 0.20g of ergothioneine, stirring uniformly, and discharging to obtain ergothioneine control essence for subsequent evaluation.
Application example 2 ergothioneine Complex efficacy core ball steady-state delivery System essence emulsion II
(1) Weighing 1.0g of ergothioneine compound essential oil efficacy core ball steady-state delivery system B (wherein, 0.95g of essential oil and 0.05g of A2 efficacy core ball) and placing into a penicillin bottle;
(2) Preparing a solvent liquid of the beauty ball:
91.5g of purified water, 2.0g of butanediol, 0.5g of tremella polysaccharide, 0.2g of glyceroglucoside, 0.2g of carrageenan, 0.5g of PEG-40 hydrogenated castor oil, 1.0g of tween-20, 0.5g of p-hydroxyacetophenone, 1.0g of 1, 2-hexanediol, 0.5g of 1, 2-pentanediol and 2.1g of damascus rose water are sequentially weighed and put into a container, heated and stirred at 40 ℃ to be dissolved uniformly, stirred and cooled, and then discharged to obtain the medium liquid of the metacore ball.
(3) 3ML of the metacentric sphere solvent is added into a steady-state delivery system B2 penicillin bottle filled with 1.0g of compound essential oil;
(4) And (3) gently shaking, wherein the steady-state delivery system of the composite freeze-dried functional core ball can be dissolved in a solvent, and meanwhile, the solvent is used for emulsifying essential oil to obtain an essential emulsion. After the composition is placed for 5min, the essence emulsion part floats upwards, and the milk-capped ergothioneine composite efficacy core ball steady-state delivery system essence emulsion II (see the essence emulsion in figure 6 and C2) is obtained for subsequent evaluation and use.
Application example 3 steady-state delivery system essence emulsion III of ergothioneine composite efficacy core sphere
(1) Weighing 1.0g of ergothioneine compound essential oil efficacy core ball steady-state delivery system B (wherein, 0.95g of essential oil and 0.05g of A3 efficacy core ball) and placing into a penicillin bottle;
(2) Preparing a solvent liquid of the beauty ball:
91.5g of purified water, 2.0g of butanediol, 0.5g of tremella polysaccharide, 0.2g of glyceroglucoside, 0.2g of carrageenan, 0.5g of PEG-40 hydrogenated castor oil, 1.0g of tween-20, 0.5g of p-hydroxyacetophenone, 1.0g of 1, 2-hexanediol, 0.5g of 1, 2-pentanediol and 2.1g of damascus rose water are sequentially weighed and put into a container, heated and stirred at 40 ℃ to be dissolved uniformly, stirred and cooled, and then discharged to obtain the medium liquid of the metacore ball.
(3) Adding 3mL of the metacentric sphere solvent into a steady-state delivery system B3 penicillin bottle filled with 1.0g of compound essential oil;
(4) And (3) gently shaking, wherein the steady-state delivery system of the composite freeze-dried functional core ball can be dissolved in a solvent, and meanwhile, the solvent is used for emulsifying essential oil to obtain an essential emulsion. After the composition is placed for 5min, the essence emulsion part floats upwards, and the milk-capped ergothioneine composite efficacy core ball steady-state delivery system essence emulsion III (see the essence emulsion in figure 6 and C3) is obtained for subsequent evaluation and use.
Application example 4 glutathione control essence
(1) 86.6G of purified water, 5.0g of butanediol, 0.80g of carrageenan and 0.40g of raspberry ketone are sequentially weighed, placed into a container, heated at 40 ℃ and stirred for uniform dissolution;
(2) After stirring and cooling, sequentially adding 5.0g of rose damascus (ROSA damascana) floral water, 2.0g of 1, 2-pentanediol and 0.20g of glutathione, stirring for about 10 minutes to obtain a uniform solution, and discharging to obtain glutathione control essence for subsequent evaluation.
Application example 5 glutathione composite efficacy core ball steady-state delivery system essence emulsion IV
(1) Weighing 1.0g of glutathione composite essential oil efficacy core ball steady-state delivery system B (wherein, essential oil is 0.95g and A4 efficacy core ball is 0.05 g) and placing into a penicillin bottle;
(2) Preparing a solvent liquid of the beauty ball:
94.5g of purified water, 1.8g of butanediol, 0.5g of wild soybean seed extract, 0.5g of cocoyl glucoside, 0.8g of PEG stearate, 0.3g of hydroxyethyl cellulose, 0.1g of hydrogenated starch hydrolysate, 0.5g of p-hydroxyacetophenone and 1.0g of 1, 2-pentanediol are sequentially weighed and put into a container, heated and stirred at 40 ℃ for uniform dissolution, stirred and cooled, and then discharged to obtain the solvent liquid of the metaballs.
(3) 3ML of the metacentric sphere solvent is added into a steady-state delivery system B4 penicillin bottle filled with 1.0g of compound essential oil;
(4) And (3) gently shaking, wherein the steady-state delivery system of the composite freeze-dried functional core ball can be dissolved in a solvent, and meanwhile, the solvent is used for emulsifying essential oil to obtain an essential emulsion. After the mixture is placed for 5min, the essence emulsion part floats upwards, and the milk cap type glutathione composite effect core ball essence emulsion IV (see the essence emulsion in figure 6 and C4) is obtained and is used for subsequent evaluation.
Application example 6 glutathione composite efficacy core ball steady-state delivery system essence emulsion V
(1) Weighing glutathione composite essential oil efficacy core ball steady-state delivery system B5.0 g (wherein: essential oil 0.95g, A5 efficacy core ball 0.05 g) and placing into a penicillin bottle;
(2) Preparing a solvent liquid of the beauty ball:
94.5g of purified water, 1.8g of butanediol, 0.5g of wild soybean seed extract, 0.5g of cocoyl glucoside, 0.8g of PEG stearate, 0.3g of hydroxyethyl cellulose, 0.1g of hydrogenated starch hydrolysate, 0.5g of p-hydroxyacetophenone and 1.0g of 1, 2-pentanediol are sequentially weighed and put into a container, heated and stirred at 40 ℃ for uniform dissolution, stirred and cooled, and then discharged to obtain the solvent liquid of the metaballs.
(3) 3ML of the metacentric sphere solvent is added into a steady-state delivery system B5 penicillin bottle filled with 1.0g of compound essential oil;
(4) And (3) gently shaking, wherein the steady-state delivery system of the composite freeze-dried functional core ball can be dissolved in a solvent, and meanwhile, the solvent is used for emulsifying essential oil to obtain an essential emulsion. After the mixture is placed for 5min, the essence emulsion part floats upwards, and the milk cap type glutathione composite efficacy core ball steady-state delivery system essence emulsion V (see the essence emulsion in figure 6 and C5) is obtained and is used for subsequent evaluation.
Application example 7 anthocyanin-Vc control essence
(1) 86.4G of purified water, 5.0g of butanediol, 0.80g of carrageenan and 0.40g of raspberry ketone are sequentially weighed, placed into a container, heated at 40 ℃ and stirred for uniform dissolution;
(2) After stirring and cooling, 5.0g of rose damascus (ROSA damascana) flower water, 2.0g of 1, 2-pentanediol, 0.10g of anthocyanin and 0.30g of vitamin C are sequentially added, and stirring is carried out for about 10 minutes to obtain a uniform solution, namely, the uniform solution is discharged for subsequent evaluation and use.
Application example 8 anthocyanin-Vc composite efficacy core ball steady-state delivery System essence emulsion VI
(1) Weighing 1.0g of anthocyanin-Vc composite essential oil efficacy core ball steady-state delivery system B6 (wherein 0.95g of essential oil and 0.05g of A6 efficacy core ball) and placing into a penicillin bottle;
(2) Preparing a solvent liquid of the beauty ball:
93.0g of purified water, 1.5g of Tween 80, 0.7g of laureth-4, 0.5g of xylitol-based glucoside, 0.6g of dehydrated xylitol, 0.5g of sodium hyaluronate, 10.6 g of polyglycerol-10, 0.8g of p-hydroxyacetophenone and 0.8g of hexanediol are sequentially weighed and put into a container, heated at 40 ℃ and stirred uniformly for dissolution, stirred and cooled, and then discharged to obtain the solvent liquid of the metaballs.
(3) 3ML of the metacentric sphere solvent is added into a steady-state delivery system B6 penicillin bottle filled with 1.0g of compound essential oil;
(4) And (3) gently shaking, wherein the steady-state delivery system of the composite freeze-dried functional core ball can be dissolved in a solvent, and meanwhile, the solvent is used for emulsifying essential oil to obtain an essential emulsion. After the mixture is placed for 5min, the essence emulsion part floats upwards, and the milk cap anthocyanin-Vc composite efficacy core ball steady-state delivery system essence emulsion VI (see the essence emulsion in figure 6 and C6) is obtained and is used for subsequent evaluation.
Application example 9 anthocyanin-Vc composite efficacy core ball steady-state delivery system essence emulsion VII
(1) Weighing 1.0g of anthocyanin-Vc composite essential oil efficacy core ball steady-state delivery system B (wherein 0.95g of essential oil and 0.05g of A7 efficacy core ball) and placing into a penicillin bottle;
(2) Preparing a solvent liquid of the beauty ball:
93.0g of purified water, 1.5g of Tween 80, 0.7g of laureth-4, 0.5g of xylitol-based glucoside, 0.6g of dehydrated xylitol, 0.5g of sodium hyaluronate, 10.6 g of polyglycerol-10, 0.8g of p-hydroxyacetophenone and 0.8g of hexanediol are sequentially weighed and put into a container, heated at 40 ℃ and stirred uniformly for dissolution, stirred and cooled, and then discharged to obtain the solvent liquid of the metaballs.
(3) 3ML of the metacentric sphere solvent is added into a penicillin bottle filled with 1.0g of compound essential oil efficacy core sphere steady-state delivery system B7 by a liquid-transferring gun;
(4) And (3) gently shaking, wherein the steady-state delivery system of the composite freeze-dried functional core ball can be dissolved in a solvent, and meanwhile, the solvent is used for emulsifying essential oil to obtain an essential emulsion. After the mixture is placed for 5min, the essence emulsion part floats upwards, and the milk cap anthocyanin-Vc composite efficacy core ball steady-state delivery system essence emulsion VII (see the essence emulsion in figure 6 and C7) is obtained and is used for subsequent evaluation.
Application example 10 EUK134 control essence
(1) 86.7G of purified water, 5.0g of butanediol, 0.80g of carrageenan and 0.40g of raspberry ketone are sequentially weighed, placed into a container, heated at 40 ℃ and stirred for uniform dissolution;
(2) After stirring and cooling, 5.0g of rose damascus (ROSA damascana) flower water, 2.0g of 1, 2-pentanediol and 0.10g of EUK134 are sequentially added, and stirring is carried out for about 20 minutes to obtain a uniform solution, namely, the uniform solution is discharged for subsequent evaluation.
Application example 11 EUK134 composite efficacy core ball steady-state delivery System essence emulsion VIII
(1) The EUK-134 composite essential oil efficacy core ball steady-state delivery system B8.0 g (wherein, essential oil is 0.95g and A8 efficacy core ball is 0.05 g) is weighed and put into a penicillin bottle;
(2) Preparing a solvent liquid of the beauty ball:
94.5g of purified water, 2.0g of butanediol, 1.5g of xylitol, 0.6g of betaine, 0.5g of xanthan gum, 0.4g of glycereth-26, 2.0g of beta-glucan, 0.3g of glycosyl trehalose, 0.6g of p-hydroxyacetophenone and 1.0g of hexanediol are sequentially weighed and put into a container, heated and stirred at 40 ℃ to be dissolved uniformly, stirred and cooled, and then discharged to obtain the solvent liquid of the metaballs.
(3) 3ML of the metacentric sphere solvent is added into a penicillin bottle filled with 1.0g of compound essential oil efficacy core sphere steady-state delivery system B8 by a liquid-transferring gun;
(4) And (3) gently shaking, wherein the steady-state delivery system of the composite freeze-dried functional core ball can be dissolved in a solvent, and meanwhile, the solvent is used for emulsifying essential oil to obtain an essential emulsion. After 5min, the essence emulsion part floats upwards to obtain the double-layer transparent EUK-134 composite efficacy core ball steady-state delivery system essence emulsion VIII (see the essence emulsion in figure 6, C8) for subsequent evaluation and use.
Application example 12 EUK134 composite efficacy core ball steady-state delivery System essence emulsion IX
(1) EUK134 composite essential oil efficacy core ball steady-state delivery system B9.0 g (wherein: essential oil 0.95g, A9 efficacy core ball 0.05 g) is weighed and put into a penicillin bottle;
(2) Preparing a solvent liquid of the beauty ball:
94.5g of purified water, 2.0g of butanediol, 1.5g of xylitol, 0.6g of betaine, 0.5g of xanthan gum, 0.4g of glycereth-26, 2.0g of beta-glucan, 0.3g of glycosyl trehalose, 0.6g of p-hydroxyacetophenone and 1.0g of hexanediol are sequentially weighed and put into a container, heated and stirred at 40 ℃ to be dissolved uniformly, stirred and cooled, and then discharged to obtain the solvent liquid of the metaballs.
(3) 3ML of the metacentric sphere solvent is added into a penicillin bottle filled with 1.0g of compound essential oil efficacy core sphere steady-state delivery system B9 by a liquid-transferring gun;
(4) And (3) gently shaking, wherein the steady-state delivery system of the composite freeze-dried functional core ball can be dissolved in a solvent, and meanwhile, the solvent is used for emulsifying essential oil to obtain an essential emulsion. After 5min, the essence emulsion partially floats, and the double-layer transparent EUK-134 composite efficacy core ball steady-state delivery system essence emulsion IX (see figure 6 essence emulsion, C9) can be obtained for subsequent evaluation and use.
Application example 13 blue copper peptide control essence
(1) 86.6G of purified water, 5.0g of butanediol, 0.80g of carrageenan and 0.40g of raspberry ketone are sequentially weighed, placed into a container, heated at 40 ℃ and stirred for uniform dissolution;
(2) After stirring and cooling, 5.0g of rose damascus (ROSA damascana) flower water, 2.0g of 1, 2-pentanediol and 0.20g of blue copper peptide are sequentially added, and the mixture is stirred for about 10 minutes to obtain a uniform solution, namely, the uniform solution is discharged for subsequent evaluation.
Application example 14 blue copper peptide composite efficacy core ball steady-state delivery system essence emulsion X
(1) Weighing 1.0g of blue copper peptide composite essential oil efficacy core ball steady-state delivery system B (wherein, 0.95g of essential oil and 0.05g of A10 efficacy core ball) and placing into a penicillin bottle;
(2) Preparing a solvent liquid of the beauty ball:
91.1g of purified water, 2.0g of butanediol, 1.2g of xylitol, 2.0g of glycerol, 0.5g of sodium hyaluronate, 1.0g of beta-glucan, 0.5g of glycosyl trehalose, 0.7g of p-hydroxyacetophenone and 1.0g of pentanediol are sequentially weighed and put into a container, heated and stirred at 40 ℃ to be dissolved uniformly, stirred and cooled, and then discharged to obtain the solvent liquid of the metaballs.
(3) 3ML of the metacentric sphere solvent is added into a steady-state delivery system B10 penicillin bottle filled with 1.0g of compound essential oil;
(4) And (3) gently shaking, wherein the steady-state delivery system of the composite freeze-dried functional core ball can be dissolved in a solvent, and meanwhile, the solvent is used for emulsifying essential oil to obtain an essential emulsion. After the solution is placed for 5min, the essence emulsion part floats upwards, and the double-layer transparent blue copper peptide composite efficacy core ball steady-state delivery system essence emulsion X (see the essence emulsion in figure 6 and C10) is obtained for subsequent evaluation and use.
Application example 15 blue copper peptide composite efficacy core ball steady-state delivery system essence emulsion XI
(1) Weighing 1.0g of blue copper peptide composite essential oil efficacy core ball steady-state delivery system B (wherein, 0.95g of essential oil and 0.05g of A11 efficacy core ball) and placing into a penicillin bottle;
(2) Preparing a solvent liquid of the beauty ball:
91.1g of purified water, 2.0g of butanediol, 1.2g of xylitol, 2.0g of glycerol, 0.5g of sodium hyaluronate, 1.0g of beta-glucan, 0.5g of glycosyl trehalose, 0.7g of p-hydroxyacetophenone and 1.0g of pentanediol are sequentially weighed and put into a container, heated and stirred at 40 ℃ to be dissolved uniformly, stirred and cooled, and then discharged to obtain the solvent liquid of the metaballs.
(3) 3ML of the metacentric sphere solvent is added into a steady-state delivery system B11 penicillin bottle filled with 1.0g of compound essential oil;
(4) And (3) gently shaking, wherein the steady-state delivery system of the composite freeze-dried functional core ball can be dissolved in a solvent, and meanwhile, the solvent is used for emulsifying essential oil to obtain an essential emulsion. After the solution is placed for 5min, the essence emulsion part floats upwards, and the double-layer transparent blue copper peptide composite efficacy core ball steady-state delivery system essence emulsion XI (see the essence emulsion in figure 6, C11) can be obtained for subsequent evaluation and use.
The foregoing embodiments illustrate the basic principles, principal features and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the above-described embodiments, and that the above-described embodiments and descriptions are merely illustrative of the principles of the present invention, and various changes and modifications may be made without departing from the scope of the principles of the invention, which are defined in the appended claims.