Eutectic microcapsule wrapping technology and application thereof in cosmetics

Abstract

The invention relates to a eutectic microcapsule wrapping technology and application thereof in cosmetics, and belongs to the technical field of cosmetic production. The wall material of the eutectic microcapsule inclusion comprises at least one of hydrogenated lecithin, caprylic / capric triglyceride, sucrose stearate, PEG-8 caprylic / capric glycerides, PEG-40 hydrogenated castor oil, soya bean lecithin, cyclodextrin, ethyl palmitate and troxerutin. The core material is prepared from at least one of salicylic acid, 4-butylresorcinol, glabridin, a kava extract, cortex magnoliae officinalis total phenols, ginseng oil, ganoderma lucidum spore oil, astaxanthin, coenzyme Q-10, a rosemary extract, ceramide and vitamin E. According to the invention, multiple eutectic coating can be formed, the consumption of the wall material can be reduced, the cost is saved, the wall material and the core material are matched for use, so that the excellent effects of permeation, oxidation resistance, soothing, allergy resistance and skin repair can be achieved, and the utilization rate of active substances is increased.

Description

Technical Field

[0001] The present invention belongs to the technical field of cosmetic production, and in particular relates to a eutectic microcapsule encapsulation technology and its application in cosmetics. Background Art

[0002] As modern consumers’ demands for cosmetics become increasingly diversified and refined, the constant pursuit of innovation and technological excellence to enhance product performance and effects is an eternal theme in the cosmetics industry.

[0003] Traditional cosmetic formulas often face problems such as poor stability of active ingredients, easy inactivation, low transdermal absorption efficiency, and strong irritation. These problems greatly limit the effectiveness of cosmetics and the use experience of consumers. For example, many active ingredients with antioxidant, soothing, repairing, anti-aging and other effects are easily oxidized and decomposed under the influence of external environmental factors (such as light, temperature, and oxygen), thereby losing their activity. In addition, the molecular weight of these active ingredients is large and it is difficult to pass through the skin barrier, resulting in insufficient effective concentration in the skin, affecting the actual effect of the product. In order to solve these problems, researchers have conducted a lot of research and exploration, and microencapsulation technology came into being. Early microencapsulation technology mainly used liposomes, polymer nanoparticles, etc. as carriers, but these technologies have certain limitations in terms of stability, drug loading, and controlled release performance.

[0004] Therefore, a more advanced technology developed on the basis of traditional microencapsulation technology, namely eutectic microencapsulation technology, has been developed. Eutectic refers to a crystal with specific structure and properties formed under specific conditions by two or more substances. In eutectic microencapsulation technology, the active ingredient and the appropriate carrier material form a microcapsule structure through eutectic action. The current eutectic microencapsulation technology still has problems such as incompatibility, and the effects of stability, absorbability, and irritation relief are uneven. It is necessary to select appropriate carrier materials and preparation processes according to different active ingredients and product requirements to achieve simultaneous encapsulation of multiple active ingredients and good synergistic effects. Summary of the invention

[0005] The existing eutectic microcapsule encapsulation technology still has problems such as incompatibility, uneven stability, absorbency, and irritation relief. It is necessary to continuously develop and improve more suitable eutectic microcapsules for different ingredients. The specific technical solution is as follows:

[0006] A eutectic microcapsule encapsulation technology, specifically a eutectic microcapsule encapsulation and / or a preparation method, wherein the mass ratio of the core material to the wall material of the eutectic microcapsule encapsulation is core material: wall material = 100: (3-6); the wall material comprises at least one of hydrogenated lecithin, caprylic / capric triglyceride, sucrose stearate, PEG-8 caprylic / capric glycerides, PEG-40 hydrogenated castor oil, soybean lecithin, cyclodextrin, ethyl palmitate and troxerutin; the core material comprises at least one of salicylic acid, 4-butylresorcinol, glabridin, kava extract, magnolol, ginseng oil, ganoderma lucidum spore oil, astaxanthin, coenzyme Q-10, rosemary extract, ceramide and vitamin E.

[0007] In the above technical solution, the wall material includes ethyl palmitate and troxerutin, and the wall material may also include at least one of hydrogenated lecithin, caprylic / capric triglyceride, sucrose stearate, PEG-8 caprylic / capric glyceride, PEG-40 hydrogenated castor oil, soybean lecithin, and cyclodextrin. The core material includes rosemary extract, ceramide, and vitamin E, and the core material may also include at least one of salicylic acid, 4-butylresorcinol, glabridin, kava extract, magnolol, ginseng oil, ganoderma lucidum spore oil, astaxanthin, and coenzyme Q-10.

[0008] In the above technical solution, the ceramide is at least one of ceramide NP, ceramide NS, ceramide NG, ceramide AS, ceramide EOP and ceramide AP.

[0009] In the above technical solution, the rosemary extract is an extract below 3 kDa obtained by co-enzymatic hydrolysis of rosemary stems and leaves with hemicellulase and pectinase, followed by co-fermentation with Bifidobacterium adolescentis and Clostridium butyricum.

[0010] In the above technical solution, the mass proportion of the ethyl palmitate in the wall material is 50% to 60%; the mass proportion of the troxerutin in the wall material is 10% to 20%.

[0011] In the above technical scheme, the preparation method of the wall material comprises the following steps: dissolving the components of the wall material in an ethanol aqueous solution at 50°C to 60°C, stirring evenly to form a wall material system, and removing ethanol and water by negative pressure distillation to obtain the wall material.

[0012] In the above technical solution, the amount of the ethanol aqueous solution is 15 to 20 times the mass of the wall material; the ethanol volume concentration of the ethanol aqueous solution is 30% to 40%.

[0013] In the above technical solution, the parameters of the negative pressure distillation are: vacuum degree 0.07MPa~0.08MPa, temperature 60℃~70℃.

[0014] In the above technical solution, the mass proportion of the rosemary extract in the core material is 70% to 80%; the mass proportion of the ceramide in the core material is 0.5% to 3%; and the mass proportion of the vitamin E in the core material is 5% to 10%.

[0015] In the above technical scheme, the preparation method of the eutectic microcapsule inclusions comprises the following steps: dispersing the wall material in an ethanol aqueous solution (ethanol concentration of 30-40wt%) to form a dispersion, heating the dispersion to 45°C to 55°C, adding the core material to the dispersion to form a composite liquid, repeatedly filter-filtering the composite liquid through a 0.03μm to 0.05μm filter membrane for 3 to 5 times to obtain a eutectic microcapsule inclusion liquid; freeze-drying the eutectic microcapsule inclusion liquid to obtain a eutectic microcapsule inclusion.

[0016] In the above technical scheme, the preparation method of the rosemary extract comprises the following steps: taking rosemary stems and leaves and crushing them, adding water 8 to 10 times the mass of the rosemary stems and leaves, adjusting the pH to 5.0 to 5.5 with a hydrochloric acid aqueous solution, adding 0.5% to 1.0% of hemicellulase and pectinase by mass of the rosemary stems and leaves respectively, performing enzymolysis at 45°C to 55°C for 2h to 3h, killing the enzymes at high temperature, cooling to room temperature, adjusting the pH to 6.5 to 7.0 with a hydroxide aqueous solution, adding glucose and dipotassium hydrogen phosphate, and then adding 0.3% to 0.5% of Bifidobacterium adolescentis and Clostridium butyricum by mass of the rosemary stems and leaves respectively, performing anaerobic fermentation at 35°C to 40°C for 15h to 20h, sterilizing at high temperature, cooling to room temperature, adding anhydrous ethanol 3 to 4 times the mass of the rosemary stems and leaves, extracting for 1h to 2h, filtering with a 3kDa ultrafiltration membrane to obtain an ultrafiltrate below 3kDa, concentrating, and drying to obtain a rosemary extract.

[0017] In the preparation method of the rosemary extract, the enzymatic activity of the hemicellulase is 50,000 U / g to 100,000 U / g; the enzymatic activity of the pectinase is 50,000 U / g to 100,000 U / g; the amount of glucose added is 1.5% to 2.5% of the mass of the rosemary stems and leaves; the amount of potassium hydrogen phosphate added is 0.1% to 0.3% of the mass of the rosemary stems and leaves; the bacterial activity of the adolescent Bifidobacterium is 5 billion CFU / g to 10 billion CFU / g; the bacterial activity of the butyric Clostridium is 5 billion CFU / g to 10 billion CFU / g; the temperature of the high temperature enzyme inactivation is 85°C to 95°C, and the time is 15min to 25min; the temperature of the high temperature sterilization is 121°C to 125°C, and the time is 15min to 20min; the concentration of the hydrochloric acid aqueous solution is 0.5mol / L to 0.8mol / L; the concentration of the sodium hydroxide aqueous solution is 0.5mol / L to 0.8mol / L. l / L.

[0018] The eutectic microcapsule encapsulation material prepared by the above-mentioned eutectic microcapsule encapsulation technology is used for preparing cosmetics.

[0019] The eutectic microcapsule encapsulation technology provided by the present invention and its application in cosmetics have the following beneficial effects compared with the prior art:

[0020] 1. The core material of the eutectic microcapsule of the present invention includes active ingredients such as rosemary extract, and the wall material contains ethyl palmitate, troxerutin, hydrogenated lecithin and other ingredients. The present invention adopts the selection of wall material and core material to produce eutectic effect and realize eutectic encapsulation; the various components of the wall material and the core material are used in a certain proportion to achieve better eutectic microcapsule encapsulation, which can well enhance the transdermal absorption capacity of the active ingredients and reduce the irritation of the active ingredients. The rosemary extract can achieve good anti-oxidation, soothing and anti-allergic, and skin repair effects.

[0021] 2. Rosemary extract is an extract below 3kDa obtained by co-enzyme hydrolysis of rosemary stems and leaves with hemicellulase and pectinase, followed by co-fermentation with Bifidobacterium adolescentis and Clostridium butyricum. The addition of hydrochloric acid aqueous solution and co-enzyme hydrolysis with hemicellulase and pectinase can promote protein leaching and improve bioavailability. Fermentation with Bifidobacterium adolescentis and Clostridium butyricum can obtain rich functional substances, including active substances such as amino acids and small molecule peptides, which can greatly improve the effects of anti-oxidation, soothing and anti-allergic, and repairing the skin.

[0022] 3. The wall materials such as hydrogenated lecithin, caprylic / capric triglyceride, sucrose stearate, PEG-8 caprylic / capric glycerides, PEG-40 hydrogenated castor oil, soybean lecithin, cyclodextrin, etc. of the present invention are used as coating materials, which have a moisturizing effect, can form a protective film on the skin surface, prevent water loss, and maintain the moisture of the skin; moisturize the skin, help improve the dry and rough condition of the skin, and make the skin smoother and more delicate; enhance the skin barrier function, can repair the damaged skin barrier, and improve the skin's resistance to external stimuli.

[0023] 4. Ceramide (core material) can moisturize and lock in moisture. It has a strong ability to associate with water molecules. It can form a network structure in the stratum corneum of the skin and firmly lock in moisture. It has a good repair effect on damaged skin barriers, enhances the skin's resistance, and reduces the invasion of harmful external substances. It helps to maintain the normal physiological functions of the skin and relieve skin sensitivity, redness and other problems.

[0024] 5. Vitamin E (core material) can effectively remove free radicals, slow down the aging process of the skin, and reduce the formation of wrinkles and spots; it has a certain moisturizing effect, keeping the skin soft and elastic; it helps to accelerate wound healing and has a repairing effect on damaged skin.

[0025] 6. As an oil ingredient, ethyl palmitate can moisturize the skin and make it smooth and soft; in cosmetics, it can adjust the texture and feel of the product, making it easier to apply and absorb.

[0026] 7. Troxerutin can promote blood circulation in the skin, increase the nutrient supply to the skin, and make the skin healthier and more radiant; it has a certain soothing and anti-allergic effect on sensitive skin and relieves skin allergy symptoms.

[0027] The present invention forms a eutectic package with excellent product effect, can effectively reduce the amount of wall material used, save costs, and the wall material and core material are used in combination to achieve excellent penetration, protection, anti-oxidation, soothing and anti-allergic, and skin repair effects, thereby improving the utilization rate of active substances and having good practical value. DETAILED DESCRIPTION

[0028] The present invention is further described below in conjunction with specific implementation cases, but the present invention is not limited to these embodiments.

[0029] Example 1

[0030] A eutectic microcapsule inclusion, wherein the mass ratio of core material to wall material is core material: wall material = 100:4.5; the wall material comprises PEG-40 hydrogenated castor oil, ethyl palmitate, and troxerutin; the core material comprises ceramide, vitamin E, glabridin, and rosemary extract; wherein the ceramide is ceramide NP.

[0031] Among them, the mass proportion of ethyl palmitate in the wall material is 60%, the mass proportion of troxerutin in the wall material is 20%, and the remainder is PEG-40 hydrogenated castor oil.

[0032] Among them, the mass proportion of ceramide in the core material is 3%, the mass proportion of vitamin E in the core material is 10%, the mass proportion of rosemary extract in the core material is 80%, and the balance is glycyrrhizin.

[0033] The preparation method of the wall material comprises the following steps: dissolving the components of the wall material in an ethanol aqueous solution at 55°C, wherein the amount of the ethanol aqueous solution is 18 times the amount of the wall material, the ethanol volume concentration of the ethanol aqueous solution is 35%, stirring evenly to form a wall material system, and removing ethanol and water by negative pressure distillation under vacuum degree of 0.06MPa and temperature of 65°C to obtain the wall material.

[0034] The preparation method of rosemary extract comprises the following steps: crushing rosemary stems and leaves, adding water 9 times the mass of the rosemary stems and leaves, adjusting the pH to 5.2 with a hydrochloric acid aqueous solution with a concentration of 0.6 mol / L, adding hemicellulase and pectinase with a mass of 0.8% of the mass of the rosemary stems and leaves respectively, performing enzymolysis at 50°C for 2.5 hours, inactivating the enzyme at 90°C for 20 minutes, cooling to room temperature, and then adding a hydrochloric acid aqueous solution with a concentration of 0.6 mol / L. l / L of hydroxide aqueous solution to adjust pH6.8, add 2.0% of glucose by weight of rosemary stems and leaves and 0.2% of dipotassium hydrogen phosphate by weight of rosemary stems and leaves, then add 0.4% of Bifidobacterium adolescentis and Clostridium butyricum by weight of rosemary stems and leaves respectively, carry out anaerobic fermentation at 37°C for 18h, sterilize at 122°C for 18min, after cooling to room temperature, add anhydrous ethanol 3.5 times the weight of rosemary stems and leaves, extract for 1.5h, then filter with a 3kDa ultrafiltration membrane to obtain an ultrafiltrate below 3kDa, concentrate, and dry to obtain a rosemary extract.

[0035] The enzymatic activity of the hemicellulase used in this embodiment is 100,000 U / g; the enzymatic activity of the pectinase is 100,000 U / g; the bacterial activity of Bifidobacterium adolescentis is 10 billion CFU / g; the bacterial activity of Clostridium butyricum is 10 billion CFU / g;

[0036] The preparation method of the above-mentioned eutectic microcapsule inclusions includes the following steps: dispersing the wall material in an ethanol aqueous solution (ethanol concentration 35wt%) with a mass 10 times that of the wall material to form a dispersion, heating the dispersion to 50°C, adding the core material to the dispersion to form a composite liquid, repeatedly filter-filtering the composite liquid through a 0.04μm filter membrane 4 times to obtain a eutectic microcapsule inclusion liquid; freeze-drying the eutectic microcapsule inclusion liquid to obtain a eutectic microcapsule inclusion.

[0037] Example 2

[0038] A eutectic microcapsule encapsulation technology, wherein the mass ratio of the core material to the wall material of the eutectic microcapsule is core material: wall material = 100:3; the wall material comprises ethyl palmitate, troxerutin, PEG-8 caprylic / capric glycerides and soy lecithin; the core material comprises rosemary extract, ceramide, vitamin E, salicylic acid and 4-butylresorcinol; wherein the ceramide is ceramide NS and ceramide NG in an equal mass ratio.

[0039] Among them, the mass proportion of ethyl palmitate in the wall material is 58%, the mass proportion of troxerutin in the wall material is 18%, and the remainder is PEG-8 caprylic / capric glycerides and soybean lecithin in equal mass ratios.

[0040] Among them, the mass proportion of rosemary extract in the core material is 75%, the mass proportion of ceramide in the core material is 2%, the mass proportion of vitamin E in the core material is 8%, and the remainder is salicylic acid and 4-butylresorcinol in equal mass proportion.

[0041] The preparation method of the wall material comprises the following steps: dissolving the components of the wall material in an ethanol aqueous solution at 50°C, wherein the amount of the ethanol aqueous solution is 15 times the amount of the wall material, the ethanol volume concentration of the ethanol aqueous solution is 30% to 40%, stirring evenly to form a wall material system, and removing ethanol and water by negative pressure distillation under vacuum degree of 0.05MPa and temperature of 60°C to obtain the wall material.

[0042] The preparation method of rosemary extract comprises the following steps: taking rosemary stems and leaves and crushing them, adding water 8 times the mass of the rosemary stems and leaves, adjusting the pH value to 5.0 with a hydrochloric acid aqueous solution with a concentration of 0.5 mol / L, respectively adding hemicellulase and pectinase with a mass value of 0.5% of the mass of the rosemary stems and leaves, performing enzymolysis at 45 DEG C for 2 hours, performing high temperature enzyme inactivation at 85 DEG C for 15 minutes, adjusting the pH value to 6.5 with a hydroxide aqueous solution with a concentration of 0.5 mol / L after cooling to room temperature, adding glucose with a mass value of 1.5% of the mass of the rosemary stems and leaves and potassium dihydrogen phosphate with a mass value of 0.1% of the mass of the rosemary stems and leaves, then respectively adding bifidobacterium adolescentis and clostridium butyricum with a mass value of 0.3% of the mass of the rosemary stems and leaves, performing anaerobic fermentation at 35 DEG C for 15 hours, performing high temperature sterilization at 121 DEG C for 15 minutes, adding anhydrous ethanol with a mass value of 3 times the mass of the rosemary stems and leaves after cooling to room temperature, extracting for 1 hour, filtering with a 3 kDa ultrafiltration membrane to obtain an ultrafiltrate below 3 kDa, concentrating, and drying to obtain the rosemary extract.

[0043] The enzymatic activity of the hemicellulase used in this embodiment is 50,000 U / g; the enzymatic activity of the pectinase is 50,000 U / g; the bacterial activity of Bifidobacterium adolescentis is 5 billion CFU / g; the bacterial activity of Clostridium butyricum is 5 billion CFU / g;

[0044] The preparation method of the above-mentioned eutectic microcapsule inclusions includes the following steps: dispersing the wall material in an ethanol aqueous solution (ethanol concentration 38wt%) with a mass 10 times that of the wall material to form a dispersion, heating the dispersion to 45°C, adding the core material to the dispersion to form a composite liquid, repeatedly filter-filtering the composite liquid through a 0.03μm filter membrane for 3 times to obtain a eutectic microcapsule inclusion liquid; freeze-drying the eutectic microcapsule inclusion liquid to obtain a eutectic microcapsule inclusion.

[0045] Example 3

[0046] A eutectic microcapsule encapsulation technology, wherein the mass ratio of the core material to the wall material of the eutectic microcapsule encapsulation is core material: wall material = 100:3.5; the wall material comprises ethyl palmitate, troxerutin, hydrogenated lecithin, caprylic / capric triglyceride and sucrose stearate; the core material comprises rosemary extract, ceramide, vitamin E, kava extract, magnolia bark total phenol, ginseng oil and ganoderma lucidum spore oil; wherein the ceramide is ceramide AS, ceramide EOP and ceramide AP in equal mass ratio.

[0047] Among them, the mass proportion of ethyl palmitate in the wall material is 55%, the mass proportion of troxerutin in the wall material is 15%, and the remainder is hydrogenated lecithin, caprylic / capric triglyceride and sucrose stearate in equal mass ratio.

[0048] Among them, the mass proportion of rosemary extract in the core material is 75%, the mass proportion of ceramide in the core material is 1%, the mass proportion of vitamin E in the core material is 6%, and the remainder is kava extract, magnolia bark total phenol, ginseng oil and ganoderma lucidum spore oil in equal mass proportions.

[0049] The preparation method of the wall material comprises the following steps: dissolving the components of the wall material in an ethanol aqueous solution at 60°C, wherein the amount of the ethanol aqueous solution is 20 times the amount of the wall material, the ethanol volume concentration of the ethanol aqueous solution is 30% to 40%, stirring evenly to form a wall material system, and removing ethanol and water by negative pressure distillation under vacuum degree of 0.06MPa and temperature of 70°C to obtain the wall material.

[0050] The preparation method of rosemary extract comprises the following steps: crushing rosemary stems and leaves, adding water 10 times the mass of the rosemary stems and leaves, adjusting the pH to 5.5 with a hydrochloric acid aqueous solution with a concentration of 0.8 mol / L, adding hemicellulase and pectinase with a mass of 1.0% of the mass of the rosemary stems and leaves, respectively, performing enzymolysis at 55°C for 3h, inactivating the enzyme at 95°C for 25min, cooling to room temperature, and then adding a hydrochloric acid aqueous solution with a concentration of 0.8 mol / L. l / L of hydroxide aqueous solution to adjust pH7.0, add 2.5% of glucose by weight of rosemary stems and leaves and 0.3% of dipotassium hydrogen phosphate by weight of rosemary stems and leaves, then add 0.5% of Bifidobacterium adolescentis and Clostridium butyricum by weight of rosemary stems and leaves respectively, perform anaerobic fermentation at 40°C for 20 hours, sterilize at 125°C for 20 minutes, cool to room temperature, add anhydrous ethanol 4 times the weight of rosemary stems and leaves, extract for 2 hours, filter with a 3kDa ultrafiltration membrane, obtain an ultrafiltrate below 3kDa, concentrate, and dry to obtain a rosemary extract.

[0051] The enzymatic activity of the hemicellulase used in this embodiment is 100,000 U / g; the enzymatic activity of the pectinase is 100,000 U / g; the bacterial activity of Bifidobacterium adolescentis is 10 billion CFU / g; the bacterial activity of Clostridium butyricum is 10 billion CFU / g;

[0052] The preparation method of the above-mentioned eutectic microcapsule inclusions includes the following steps: dispersing the wall material in an ethanol aqueous solution (ethanol concentration 33wt%) with a mass 10 times that of the wall material to form a dispersion, heating the dispersion to 55°C, adding the core material to the dispersion to form a composite liquid, repeatedly filter-filtering the composite liquid through a 0.05μm filter membrane for 5 times to obtain a eutectic microcapsule inclusion liquid; freeze-drying the eutectic microcapsule inclusion liquid to obtain a eutectic microcapsule inclusion.

[0053] Example 4

[0054] A eutectic microcapsule encapsulation technology, wherein the mass ratio of the core material to the wall material of the eutectic microcapsule encapsulation is core material: wall material = 100:5; the wall material comprises ethyl palmitate, troxerutin, caprylic / capric triglyceride, sucrose stearate, PEG-40 hydrogenated castor oil, soybean lecithin and cyclodextrin; the core material comprises rosemary extract, ceramide, vitamin E, 4-butylresorcinol, glabridin, ginseng oil, ganoderma lucidum spore oil, astaxanthin and coenzyme Q-10; wherein the ceramides are ceramide NG, ceramide AS, ceramide EOP and ceramide AP in equal mass ratios.

[0055] Among them, the mass proportion of ethyl palmitate in the wall material is 52%, the mass proportion of troxerutin in the wall material is 12%, and the remainder is equal mass proportion of caprylic / capric triglyceride, sucrose stearate, PEG-40 hydrogenated castor oil, soybean lecithin and cyclodextrin.

[0056] Among them, the mass proportion of rosemary extract in the core material is 73%, the mass proportion of ceramide in the core material is 0.8%, the mass proportion of vitamin E in the core material is 6%, and the remainder is 4-butylresorcinol, glycyrrhizin, ginseng oil, ganoderma spore oil, astaxanthin and coenzyme Q-10 in equal mass proportions.

[0057] The preparation method of the wall material comprises the following steps: dissolving the components of the wall material in an ethanol aqueous solution at 50°C, wherein the amount of the ethanol aqueous solution is 20 times the amount of the wall material, the ethanol volume concentration of the ethanol aqueous solution is 30% to 40%, stirring evenly to form a wall material system, and removing ethanol and water by negative pressure distillation under the conditions of a vacuum degree of 0.05MPa and a temperature of 70°C to obtain the wall material.

[0058] The preparation method of rosemary extract comprises the following steps: crushing rosemary stems and leaves, adding water 10 times the mass of the rosemary stems and leaves, adjusting the pH to 5.5 with a hydrochloric acid aqueous solution with a concentration of 0.5 mol / L, adding hemicellulase and pectinase with a mass of 0.5% of the mass of the rosemary stems and leaves respectively, performing enzymolysis at 55°C for 2h, inactivating the enzyme at 95°C for 15min, cooling to room temperature, and then adding a 0.8 mol / L hydrochloric acid aqueous solution with a concentration of 0.8 mol / L. l / L of hydroxide aqueous solution to adjust pH6.5, add 2.5% of glucose by weight of rosemary stems and leaves and 0.1% of dipotassium hydrogen phosphate by weight of rosemary stems and leaves, then add 0.5% of Bifidobacterium adolescentis and Clostridium butyricum by weight of rosemary stems and leaves respectively, perform anaerobic fermentation at 35°C for 20 hours, sterilize at 121°C for 20 minutes, cool to room temperature, add anhydrous ethanol 3 times the weight of rosemary stems and leaves, extract for 2 hours, filter with a 3kDa ultrafiltration membrane, obtain an ultrafiltrate below 3kDa, concentrate, and dry to obtain a rosemary extract.

[0059] The enzymatic activity of the hemicellulase used in this embodiment is 50,000 U / g; the enzymatic activity of the pectinase is 100,000 U / g; the bacterial activity of Bifidobacterium adolescentis is 5 billion CFU / g; the bacterial activity of Clostridium butyricum is 10 billion CFU / g;

[0060] The preparation method of the above-mentioned eutectic microcapsule inclusions includes the following steps: dispersing the wall material in an ethanol aqueous solution (ethanol concentration 30wt%) with a mass 10 times that of the wall material to form a dispersion, heating the dispersion to 45°C, adding the core material to the dispersion to form a composite liquid, repeatedly filter-filtering the composite liquid through a 0.05μm filter membrane for 3 times to obtain a eutectic microcapsule inclusion liquid; freeze-drying the eutectic microcapsule inclusion liquid to obtain a eutectic microcapsule inclusion.

[0061] Example 5

[0062] A eutectic microcapsule encapsulation technology, wherein the mass ratio of the core material to the wall material of the eutectic microcapsule encapsulation is core material: wall material = 100:6; the wall material comprises ethyl palmitate, troxerutin, hydrogenated lecithin, caprylic / capric triglyceride, sucrose stearate, PEG-8 caprylic / capric glycerides, PEG-40 hydrogenated castor oil, soybean lecithin and cyclodextrin; the core material comprises rosemary extract, ceramide, vitamin E, salicylic acid, 4-butylresorcinol, glabridin, kava extract, magnolia bark total phenol, ginseng oil, ganoderma lucidum spore oil, astaxanthin and coenzyme Q-10; wherein the ceramide comprises ceramide NP, ceramide NS, ceramide NG, ceramide AS, ceramide EOP and ceramide AP in equal mass ratio.

[0063] Among them, the mass proportion of ethyl palmitate in the wall material is 50%, the mass proportion of troxerutin in the wall material is 10%, and the remainder is hydrogenated lecithin, caprylic / capric triglyceride, sucrose stearate, PEG-8 caprylic / capric glycerides, PEG-40 hydrogenated castor oil, soybean lecithin and cyclodextrin in equal mass proportions.

[0064] Among them, the mass proportion of rosemary extract in the core material is 70%, the mass proportion of ceramide in the core material is 0.5%, the mass proportion of vitamin E in the core material is 5%, and the remainder is salicylic acid, 4-butylresorcinol, glycyrrhizin, kava extract, magnolia bark total phenol, ginseng oil, ganoderma lucidum spore oil, astaxanthin and coenzyme Q-10 in equal mass proportions.

[0065] The preparation method of the wall material comprises the following steps: dissolving the components of the wall material in an ethanol aqueous solution at 60°C, wherein the amount of the ethanol aqueous solution is 15 times the amount of the wall material, the ethanol volume concentration of the ethanol aqueous solution is 30% to 40%, stirring evenly to form a wall material system, and removing ethanol and water by negative pressure distillation under vacuum degree of 0.06MPa and temperature of 60°C to obtain the wall material.

[0066] The preparation method of rosemary extract comprises the following steps: taking rosemary stems and leaves and crushing them, adding water 8 times the mass of the rosemary stems and leaves, adjusting the pH value to 5.0 with a hydrochloric acid aqueous solution with a concentration of 0.8 mol / L, respectively adding hemicellulase and pectinase in an amount of 1.0% by mass of the rosemary stems and leaves, performing enzymolysis at 45 DEG C for 3 hours, performing high temperature enzyme inactivation at 85 DEG C for 25 minutes, adjusting the pH value to 7.0 with a hydroxide aqueous solution with a concentration of 0.5 mol / L after cooling to room temperature, adding glucose in an amount of 1.5% by mass of the rosemary stems and leaves and potassium dihydrogen phosphate in an amount of 0.3% by mass of the rosemary stems and leaves, respectively adding bifidobacterium adolescentis and clostridium butyricum in an amount of 0.3% by mass of the rosemary stems and leaves, performing anaerobic fermentation at 40 DEG C for 15 hours, performing high temperature sterilization at 125 DEG C for 15 minutes, adding anhydrous ethanol in an amount of 4 times the mass of the rosemary stems and leaves after cooling to room temperature, extracting for 1 hour, filtering with a 3 kDa ultrafiltration membrane to obtain an ultrafiltrate below 3 kDa, concentrating, and drying to obtain the rosemary extract.

[0067] The enzymatic activity of the hemicellulase used in this embodiment is 100,000 U / g; the enzymatic activity of the pectinase is 50,000 U / g; the bacterial activity of Bifidobacterium adolescentis is 10 billion CFU / g; the bacterial activity of Clostridium butyricum is 5 billion CFU / g;

[0068] The preparation method of the above-mentioned eutectic microcapsule inclusions includes the following steps: dispersing the wall material in an ethanol aqueous solution (ethanol concentration 40wt%) with a mass 10 times that of the wall material to form a dispersion, heating the dispersion to 55°C, adding the core material to the dispersion to form a composite liquid, repeatedly filter-filtering the composite liquid through a 0.03μm filter membrane for 5 times to obtain a eutectic microcapsule inclusion liquid; freeze-drying the eutectic microcapsule inclusion liquid to obtain a eutectic microcapsule inclusion.

[0069] Comparative Example 1

[0070] The rosemary extract was not encapsulated in eutectic microencapsulation; other parameters and methods were the same as in Example 1.

[0071] Comparative Example 2

[0072] Ethyl palmitate is not added to the wall material, and ethyl palmitate is replaced by PEG-40 hydrogenated castor oil; other parameters and methods are the same as in Example 1.

[0073] Comparative Example 3

[0074] Troxerutin is not added to the wall material, and PEG-40 hydrogenated castor oil is used instead of troxerutin; other parameters and methods are the same as in Example 1.

[0075] Comparative Example 4

[0076] In the preparation method of rosemary extract, rosemary stems and leaves are crushed, water of 9 times the mass of the rosemary stems and leaves is added, anhydrous ethanol of 3.5 times the mass of the rosemary stems and leaves is added, and the mixture is extracted for 1.5 hours, and then filtered using a 3 kDa ultrafiltration membrane to obtain an ultrafiltrate below 3 kDa, which is concentrated and dried to obtain the rosemary extract. Other parameters and methods are the same as those in Example 1.

[0077] Comparative Example 5

[0078] In the preparation method of rosemary extract, no Bifidobacterium adolescentis added during fermentation; other parameters and methods are the same as those in Example 1.

[0079] Comparative Example 6

[0080] In the preparation method of rosemary extract, Clostridium butyricum is not added during fermentation; other parameters and methods are the same as those in Example 1.

[0081] The product samples of the above-mentioned embodiments and comparative examples were tested for their antioxidant, soothing, anti-allergic and skin repairing effects.

[0082] 1. Antioxidant

[0083] Mouse adherent macrophages were used as test cells. Product sample: purified water = 1:100 to obtain product sample reagent.

[0084] The fluorescent probe DCFH-DA is used to detect reactive oxygen species. DCFH-DA itself has no fluorescence and can freely pass through the cell membrane. After entering the cell, it is hydrolyzed by the esterase in the cell to produce DCFH. However, DCFH cannot penetrate the cell membrane, making it easy for the probe to be loaded into the cell. The reactive oxygen species in the cell can oxidize the non-fluorescent DCFH to produce fluorescent DCF. By detecting the fluorescence of DCF, the level of reactive oxygen species in the cell can be known.

[0085] Blank control sample: dilute DCFH-DA with serum-free culture medium at a ratio of 1:1000 to a final concentration of 10μmol / L to obtain DCFH-DA dilution. After collecting the cells, suspend them in DCFH-DA dilution to a cell concentration of 5 million / mL, and then add purified water equal to the volume of DCFH-DA dilution. Incubate in a cell culture incubator at 37°C for 30 minutes. Invert and mix every 5 minutes to allow the probe and cells to fully contact, and wash the cells three times with serum-free cell culture medium to fully remove the DCF-DA that has not entered the cells. At an excitation wavelength of 488nm and an emission wavelength of 525nm, use a fluorescence microplate reader to detect the intensity of fluorescence, and the value of reactive oxygen species ROS is calculated as R0.

[0086] Example and comparative sample: DCFH-DA was diluted with serum-free culture medium at a ratio of 1:1000 to a final concentration of 10 μmol / L to obtain a DCFH-DA dilution. After the cells were collected, they were suspended in a DCFH-DA dilution solution with a cell concentration of 5 million / mL, and then an equal volume of product sample reagent (corresponding to the product samples of each example and comparative example) of the DCFH-DA dilution solution was added. Incubate in a cell culture incubator at 37°C for 30 minutes. Invert and mix every 5 minutes to allow the probe and cells to fully contact, and wash the cells three times with serum-free cell culture medium to fully remove the DCFH-DA and product samples that have not entered the cells. At an excitation wavelength of 488 nm and an emission wavelength of 525 nm, the intensity of fluorescence was detected using a fluorescence microplate reader, and the reactive oxygen species ROS value was counted as R1.

[0087] The relative improvement rate of ROS was calculated by the formula: R% = (R0-R1) / R0*100%. The test results are shown in Table 1 below.

[0088] Table 1 Antioxidant test results

[0089]

[0090]

[0091] It can be seen from the above results that the eutectic microcapsule packages of Examples 1 to 5 have a good antioxidant effect. It can be seen from the results of Comparative Example 1 that the rosemary extract is not encapsulated with eutectic microcapsules, the permeability is poor, the utilization rate of the rosemary extract is low, the absorption of cells is affected, and the antioxidant effect of cells is reduced. It can be seen from the results of Comparative Example 2 that ethyl palmitate is not added to the components of the wall material, which will reduce the coating effect of the wall material, reduce the permeability, affect the absorption of cells, and reduce the antioxidant effect of cells. It can be seen from the results of Comparative Example 3 that without adding troxerutin, the encapsulation effect is poor, the permeability is poor, the utilization rate of the rosemary extract is low, the absorption of cells is affected, and the antioxidant effect of cells is reduced. It can be seen from the results of Comparative Example 4 that rosemary uses a conventional ethanol aqueous solution extraction method to obtain an extract, and the antioxidant effect is greatly reduced. It can be seen from the results of Comparative Examples 5 and 6 that fermentation does not add Bifidobacterium adolescentis or Clostridium butyricum, which affects the different product components and reduces the antioxidant effect.

[0092] 2. Soothing and anti-allergic

[0093] Hyaluronidase is a participant in type I allergic reactions. Most allergic reactions are type I allergic reactions related to the activity of hyaluronidase in the body. The inhibitory ability of the product sample reagent on hyaluronidase reflects its ability to inhibit type I allergic reactions. The greater the inhibition rate of hyaluronidase, the stronger the anti-allergic activity.

[0094] Take 11.55mL of glacial acetic acid and dissolve it in 1L of distilled water to prepare a 0.2mol / L acetic acid solution; take 16.4g of anhydrous sodium acetate and dissolve it in 1L of distilled water to prepare a 0.2mol / L sodium acetate solution; take 4.8mL of acetic acid solution and 45.2mL of sodium acetate solution, mix them, dilute to 100mL with distilled water, and prepare an acetate buffer solution with a pH of 5.6.

[0095] Using acetate buffer solution as solvent, hyaluronidase was prepared into a 500 U / mL hyaluronidase solution.

[0096] Sodium hyaluronate was prepared into a 0.5 mg / mL sodium hyaluronate solution using acetate buffer solution as solvent.

[0097] The product sample was prepared into a 0.5 mg / mL product sample solution using acetate buffer solution as solvent.

[0098] Acetylacetone solution was prepared using 50 mL of 1.0 mol / L sodium carbonate solution and 3.5 mL of acetylacetone.

[0099] P-DAB color developer: Dissolve 0.8 g of p-dimethylaminobenzaldehyde in 15 mL of concentrated hydrochloric acid and 15 mL of anhydrous ethanol to prepare P-DAB color developer.

[0100] Test tube A: 0.5 mL of product sample solution + 0.5 mL of hyaluronidase solution, incubate at 37°C for 20 min; add 0.1 mL (2.5 mmol / L) CaCl2, incubate at 37°C for 20 min; add 0.5 mL of sodium hyaluronate solution; keep warm at 37°C for 40 min, place at room temperature for 10 min, add 0.5 mL of acetylacetone solution, 0.1 mL of NaOH solution (5 mol / L) and 0.5 mL of distilled water, boil in a water bath for 15 min, immediately cool with ice water for 5 min, add 1 mL of P-DAB colorimetric reagent, shake thoroughly, add 3.5 mL of anhydrous ethanol, place for 30 min, develop color, and measure the OD value at 530 nm, which is calculated as A.

[0101] Test tube B: 0.5 mL of product sample solution + 0.5 mL of hyaluronidase solution, incubate at 37°C for 20 min; add 0.1 mL (2.5 mmol / L) CaCl2, incubate at 37°C for 20 min; add 0.5 mL of acetate buffer solution; keep warm at 37°C for 40 min, place at room temperature for 10 min, add 0.5 mL of acetylacetone solution, 0.1 mL of NaOH solution (5 mol / L) and 0.5 mL of distilled water, boil in a water bath for 15 min, immediately cool with ice water for 5 min, add 1 mL of P-DAB colorimetric reagent, shake thoroughly, add 3.5 mL of anhydrous ethanol, place for 30 min, develop color, and measure the OD value at 530 nm, which is calculated as B.

[0102] C test tube: 0.5mL of distilled water + 0.5mL of acetate buffer solution, incubate at 37℃ for 20min; add 0.1mL (2.5mmol / L) CaCl2, incubate at 37℃ for 20min; add 0.5mL of sodium hyaluronate solution; keep warm at 37℃ for 40min, place at room temperature for 10min, add 0.5mL of acetylacetone solution, 0.1mL of NaOH solution (5mol / L) and 0.5mL of distilled water, boil in a water bath for 15min, immediately cool with ice water for 5min, add 1mL of P-DAB colorimetric reagent, shake thoroughly, add 3.5mL of anhydrous ethanol, place for 30min, develop color, and measure the OD value at 530nm, which is calculated as C.

[0103] D test tube: 0.5 mL of distilled water + 0.5 mL of acetate buffer solution, incubate at 37°C for 20 min; add 0.1 mL (2.5 mmol / L) CaCl2, incubate at 37°C for 20 min; add 0.5 mL of acetate buffer solution; keep warm at 37°C for 40 min, place at room temperature for 10 min, add 0.5 mL of acetylacetone solution, 0.1 mL of NaOH solution (5 mol / L) and 0.5 mL of distilled water, boil in a water bath for 15 min, immediately cool with ice water for 5 min, add 1 mL of P-DAB colorimetric reagent, shake thoroughly, add 3.5 mL of anhydrous ethanol, place for 30 min, develop color, and measure the OD value at 530 nm, which is calculated as D.

[0104] Hyaluronidase inhibition rate (%) = [(CD) - (AB)] / (CD) × 100%; the test results are shown in Table 2 below.

[0105] Table 2 Soothing and anti-allergy test results

[0106]

[0107] It can be seen from the above results that the eutectic microcapsule packages of Examples 1 to 5 have a good hyaluronidase inhibitory effect and can play a good soothing and anti-allergic effect. It can be seen from the results of Comparative Example 1 that in in vitro testing, the rosemary extract is not encapsulated in eutectic microcapsules, ethyl palmitate is not added to the components of the wall material, and troxerutin is not added to the components of the wall material, which has little effect on the in vitro hyaluronidase inhibitory effect. It can be seen from the results of Comparative Example 4 that rosemary is extracted by a conventional ethanol aqueous solution method to obtain an extract, which inhibits hyaluronidase, and the soothing and anti-allergic effect is greatly reduced. It can be seen from the results of Comparative Examples 5 and 6 that no adolescent bifidobacterium or clostridium butyricum is added to the fermentation, which inhibits hyaluronidase, and the soothing and anti-allergic effect is greatly reduced.

[0108] 3. Repair skin

[0109] Product sample: purified water = 1:100 to obtain a product sample reagent, and the mask paper is soaked in the product sample reagent to prepare a mask; 66 female subjects with healthy skin were selected and randomly divided into 10 groups, with 6 subjects in each group; each group used the mask of each comparative example, and applied the mask on the inner side of the forearm for 10 minutes every night for 28 days; after cleansing every night, apply the mask on the face for 10 minutes for 28 days.

[0110] (1) Use TM300 tester to test the transepidermal water loss (TEWL) of the inner side of the forearm before the test, on the 14th day, and on the 28th day; TEWL value decrease rate = (A0-An) / A0×100%; where A0 is the TEWL value before the test, and An is the TEWL value on the nth day. A positive TEWL value decrease rate indicates that the skin barrier has been repaired. The greater the TEWL value decrease rate, the better the skin barrier repair effect. The test results are shown in Table 3 below.

[0111] Table 3 TEWL value reduction rate results (average value)

[0112]

[0113] (2) Use UC22 skin ultrasound tester to test: before the test, on the 14th day, and on the 28th day, the thickness of the skin epidermis D; D value increase rate = (D0-Dn) / D0×100%; where D0 is the thickness of the epidermis before the test, and Dn is the thickness of the epidermis on the nth day. A positive D value increase rate indicates that the skin barrier has been repaired, and the greater the D value increase rate, the better the skin barrier repair effect. The test results are shown in Table 4 below.

[0114] Table 4 D value improvement rate results (average value)

[0115]

[0116] As can be seen from the above results, the eutectic microcapsule packages of Examples 1 to 5 have a good skin repairing effect, thicken the skin, and improve water retention. As can be seen from the results of Comparative Example 1, the rosemary extract is not encapsulated with eutectic microcapsules, the permeability is poor, the utilization rate of the rosemary extract is low, the absorption of cells is affected, and the effect of skin repair is reduced. As can be seen from the results of Comparative Example 2, ethyl palmitate is not added to the components of the wall material, which will reduce the coating effect of the wall material, reduce the permeability, affect the absorption of cells, and reduce the effect of skin repair. As can be seen from the results of Comparative Example 3, troxerutin is not added, the coating effect is poor, the permeability of the microcapsule is poor, the utilization rate of the rosemary extract is low, the absorption of cells is affected, and the effect of skin repair is reduced. As can be seen from the results of Comparative Example 4, rosemary uses a conventional ethanol aqueous solution extraction method to obtain an extract, and its skin repair effect is greatly reduced. As can be seen from the results of Comparative Examples 5 and 6, fermentation does not add Bifidobacterium adolescentis or Clostridium butyricum, which affects the different product components and reduces the effect of skin repair.

Claims

1. A eutectic microencapsulation technology, characterized in that: The mass ratio of the core material to the wall material of the eutectic microcapsule is core material: wall material = 100: (3-6); The wall material comprises at least one of hydrogenated lecithin, caprylic / capric triglyceride, sucrose stearate, PEG-8 caprylic / capric glycerides, PEG-40 hydrogenated castor oil, soybean lecithin, cyclodextrin, ethyl palmitate and troxerutin; The core material comprises at least one of salicylic acid, 4-butylresorcinol, glabridin, kava extract, magnolol, ginseng oil, ganoderma lucidum spore oil, astaxanthin, coenzyme Q-10, rosemary extract, ceramide and vitamin E.

2. The eutectic microencapsulation technology according to claim 1, characterized in that: The ceramide is at least one of ceramide NP, ceramide NS, ceramide NG, ceramide AS, ceramide EOP and ceramide AP.

3. A eutectic microencapsulation technology according to claim 1 or 2, characterized in that: The preparation method of the wall material comprises the following steps: dissolving the components of the wall material in an ethanol aqueous solution at 50° C. to 60° C., stirring evenly to form a wall material system, and removing ethanol and water by negative pressure distillation to obtain the wall material.

4. The eutectic microencapsulation technology according to claim 3, characterized in that: The amount of the ethanol aqueous solution is 15 to 20 times the weight of the wall material; the ethanol volume concentration of the ethanol aqueous solution is 30% to 40%; The parameters of the negative pressure distillation are: vacuum degree 0.07MPa-0.08MPa, temperature 60°C-70°C.

5. The eutectic microencapsulation technology according to claim 3, characterized in that: The preparation method of the eutectic microcapsule inclusions comprises the following steps: dispersing the wall material in an ethanol aqueous solution to form a dispersion liquid, heating the dispersion liquid to 45°C to 55°C, adding the core material to the dispersion liquid to form a composite liquid, repeatedly filtering the composite liquid through a 0.03μm to 0.05μm filter membrane for 3 to 5 times to obtain a eutectic microcapsule inclusion liquid; and freeze-drying the eutectic microcapsule inclusion liquid to obtain the eutectic microcapsule inclusions.

6. The eutectic microencapsulation technology according to claim 3, characterized in that: The rosemary extract is an extract below 3kDa obtained by co-enzymatic hydrolysis of rosemary stems and leaves with hemicellulase and pectinase, followed by co-fermentation with Bifidobacterium adolescentis and Clostridium butyricum; the mass proportion of ethyl palmitate in the wall material is 50% to 60%; and the mass proportion of troxerutin in the wall material is 10% to 20%.

7. The eutectic microencapsulation technology according to claim 1, characterized in that: The mass proportion of the rosemary extract in the core material is 70% to 80%; the mass proportion of the ceramide in the core material is 0.5% to 3%; and the mass proportion of the vitamin E in the core material is 5% to 10%.

8. The eutectic microencapsulation technology according to claim 1, characterized in that: The preparation method of the rosemary extract comprises the following steps: taking rosemary stems and leaves and crushing them, adding water 8 to 10 times the mass of the rosemary stems and leaves, adjusting the pH value to 5.0 to 5.5 by using a hydrochloric acid aqueous solution, respectively adding hemicellulase and pectinase in an amount of 0.5 to 1.0% by mass of the rosemary stems and leaves, performing enzymolysis at 45 to 55° C. for 2 to 3 hours, inactivating the enzymes at high temperature, cooling to room temperature, adjusting the pH value to 6.5 to 7.0 by using a hydroxide aqueous solution, adding glucose and dipotassium hydrogen phosphate, and then respectively adding bifidobacterium adolescentis and clostridium butyricum in an amount of 0.3 to 0.5% by mass of the rosemary stems and leaves, performing anaerobic fermentation at 35 to 40° C. for 15 to 20 hours, performing high temperature sterilization, cooling to room temperature, adding anhydrous ethanol in an amount of 3 to 4 times the mass of the rosemary stems and leaves, extracting for 1 to 2 hours, filtering by using a 3 kDa ultrafiltration membrane to obtain an ultrafiltrate below 3 kDa, concentrating, and drying to obtain the rosemary extract.

9. The eutectic microencapsulation technology according to claim 8, characterized in that: The enzymatic activity of the hemicellulase is 50,000 U / g to 100,000 U / g; the enzymatic activity of the pectinase is 50,000 U / g to 100,000 U / g; the added amount of the glucose is 1.5% to 2.5% of the mass of the rosemary stems and leaves; the added amount of the dipotassium hydrogen phosphate is 0.1% to 0.3% of the mass of the rosemary stems and leaves; the bacterial activity of the adolescent Bifidobacterium is 5 billion CFU / g to 10 billion CFU / g; the bacterial activity of the Clostridium butyricum is 5 billion CFU / g to 10 billion CFU / g; the temperature of the high-temperature enzyme inactivation is 85°C to 95°C, and the time is 15min to 25min; the temperature of the high-temperature sterilization is 121°C to 125°C, and the time is 15min to 20min; the concentration of the hydrochloric acid aqueous solution is 0.5mol / L to 0.8mol / L; the concentration of the sodium hydroxide aqueous solution is 0.5mol / L to 0.8mol / L.

10. A eutectic microcapsule encapsulation material, prepared by the eutectic microcapsule encapsulation technology according to claim 1, characterized in that: The eutectic microcapsule is used for preparing cosmetics.

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