A child care skin care essential oil and a preparation method thereof
Patent Information
- Application Number
- CN202610144268.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2026-02-02
- Publication Date
- 2026-09-15
- Estimated Expiration
- 2046-02-02
AI Technical Summary
本发明提供了一种儿童护肤精油及其制备方法,其包含以下重量百分比的单方精油:椰子油35~40%,甜杏仁油1~3%,葡萄柚精油0.1~0.2%,姜黄油0.05~0.15%,黑胡椒精油0.03~0.06%,余量为葡萄籽油。本发明所得护肤精油对于儿童的安全性好,且具有良好的护肤效果。
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Abstract
Description
Technical Field
[0001] This invention belongs to the field of skin care essential oil preparation technology, specifically relating to a children's skin care essential oil and its preparation method. Background Technology
[0002] Children's skin has the following characteristics: 1. Children's skin has a high metabolic rate and is only 1 / 10 the thickness of adult skin. It is relatively delicate and sensitive to environmental factors such as dryness, cold, and humidity, as well as chemical stimuli such as alkaline and acidic substances. Its resistance is also weak. Children's skin is very delicate and requires special care. Improper care can lead to a series of problems and affect children's health. Children's skin loses moisture easily, and the loss of moisture and oil can cause leaks in the skin's natural protective barrier, resulting in a deficiency of both water and oil. This can cause gaps and loosening of the stratum corneum, reducing its ability to resist external stimuli and leading to various skin problems.
[0003] 2. Children's skin accounts for a higher proportion of their body weight, and their skin barrier function is not as perfect as that of adults. Therefore, their skin permeability is higher than that of adults, and their skin absorbs topical skin care products more efficiently.
[0004] 3. Children's skin has not yet fully developed melanosomes and has fewer melanosomes, making them less resistant to ultraviolet rays and more prone to sunburn.
[0005] 4. Because newborns' skin secretes a lot of sebum and their skin is less able to resist external stimuli, insufficient cleaning can easily lead to bacterial infections.
[0006] In general, children's skin has poor resistance to irritants from the external environment and is prone to skin diseases. Therefore, children's skin care products have higher requirements for the safety of raw material sources and should be gentle and free of side effects.
[0007] Many natural skincare products are available on the market now, but besides natural active ingredients, most contain added chemically synthesized products such as surfactants, preservatives, thickeners, moisturizers, and fragrances. These chemically synthesized products are highly irritating to the skin and still pose a threat to children's skin health.
[0008] Essential oils are concentrated substances extracted from plants. When applied to the skin, they offer benefits such as moisturizing, anti-inflammation, anti-oxidation, promoting repair, and regulating oil production. Therefore, using essential oils in children's skincare has great potential. However, because children's skin is delicate, the use of essential oils requires extra caution. High-purity essential oils are highly irritating, and direct application may harm children's skin. While they are usually diluted before use, issues such as high oil content, poor efficacy, and difficulty in meeting the safety requirements for children's skincare (allergic reactions, etc.) still exist. Therefore, selecting essential oil ingredients suitable for children's skincare and optimizing the processing methods are essential.
[0009] Patent CN105616210B discloses a children's sunscreen rose skin care product, which includes a dispersion of N-trans-feruloyl norsylephrine and rose essential oil. In addition to the natural ingredient rose essential oil, it also contains chemically synthesized ingredients such as N-trans-feruloyl norsylephrine, which is highly irritating to children's skin. Summary of the Invention
[0010] In view of the shortcomings of the existing technology, the purpose of this invention is to provide a children's skin care essential oil and its preparation method.
[0011] To achieve the above objectives, the present invention adopts the following technical solution: A children's skin care essential oil contains the following single essential oils by weight percentage: coconut oil 35-40%, sweet almond oil 1-3%, grapefruit essential oil 0.1-0.2%, ginger oil 0.05-0.15%, black pepper essential oil 0.03-0.06%, and the balance being grapeseed oil.
[0012] Preferred, the single essential oils contain the following weight percentages: 38.7% coconut oil, 2% sweet almond oil, 0.15% grapefruit essential oil, 0.1% ginger oil, 0.05% black pepper essential oil, with the balance being grapeseed oil.
[0013] Preferably, the coconut oil or turmeric oil is prepared by the following method: fresh coconut meat or fresh turmeric root is completely immersed in saturated lime water at 5 to 7 times its weight, soaked at room temperature for 20 to 24 hours, taken out and rinsed with running water, drained, pressed to obtain pressed material, treated under ultra-high pressure, steam distilled, the volatile oil is collected, and dehydrated with anhydrous sodium sulfate to obtain the final product.
[0014] Further preferred ultra-high pressure treatment conditions are: 300-400 MPa ultra-high pressure treatment for 6-8 minutes.
[0015] A further preferred method involves mixing the ultra-high pressure treated pressed material with 8 to 10 times its weight of water and then performing steam distillation. The specific method is as follows: heat to boiling, collect the volatile oil, and distill for 2 hours.
[0016] Preferably, the sweet almond oil, black pepper oil, or grape seed oil is prepared by the following method: crushing the ripe sweet almonds, black pepper, or grape seeds to 80-100 mesh, adding 2-3 times the weight of the ripe sweet almonds, black pepper, or grape seeds to a 50-60% ethanol aqueous solution, treating with ultrasonic vibration at 500-600W for 30-40 minutes, supercritical CO2 extraction, standing at room temperature for 8-10 hours, and separating the oil layer to obtain the oil.
[0017] Further preferred supercritical CO2 extraction conditions are: extraction temperature 40-45℃, extraction pressure 28-32MPa, CO2 flow rate 8-12L / h, and the extract is collected every 30 minutes. The extraction ends when no more extract flows out.
[0018] Preferably, the grapefruit essential oil is prepared by the following method: using grapefruit peel as raw material, removing impurities, drying, crushing, steaming, and cold pressing to obtain crude oil I and cake residue, performing subcritical extraction on the cake residue to obtain crude oil II, combining crude oil I and crude oil II, centrifuging to remove insoluble matter, and thus obtaining the final product.
[0019] Further preferred methods include: drying at 50–60°C until the moisture content is ≤4% by weight; crushing and passing through a 50-mesh sieve; steaming at 55–60°C for 40–50 minutes; and subcritical extraction conditions: solvent n-butane, pressure 0.4–0.5 MPa, temperature 30–35°C, time 40–50 minutes, liquid-to-solid ratio 1.4:1, and extraction four times; and rotary evaporation to remove n-butane after subcritical extraction.
[0020] The specific steps of the aforementioned method for preparing a children's skincare essential oil are as follows: (1) First, mix the coconut oil, sweet almond oil, grapefruit essential oil, ginger oil, black pepper essential oil and grapeseed oil in the specified amounts to obtain a mixed essential oil; (2) Then, under the action of a pore-forming agent, thiol-modified chitosan was used to prepare thiol-modified chitosan porous microspheres; then, a portion of the mixed essential oil was loaded onto the thiol-modified chitosan porous microspheres to obtain the loaded material; (3) Finally, the loading material and tyramine-modified β-cyclodextrin are mixed to form an aqueous phase, and the remaining part is mixed with essential oil as an oil phase. The mixture is then mixed to prepare the children's skin care essential oil.
[0021] Preferably, in step (2), the thiol-modified chitosan is prepared by the following method: first, cysteine hydrochloride monohydrate is dissolved in 8-10 times its weight of a 1-2% hydrochloric acid solution; then, N-hydroxysuccinimide and carbodiimide hydrochloride are added, such that the molar ratio of cysteine hydrochloride monohydrate, N-hydroxysuccinimide, and carbodiimide hydrochloride is 1:3-5:2-3; the mixture is stirred and activated at room temperature for 2-3 hours to obtain a mixed solution; then, the chitosan is prepared using a 1-2% hydrochloric acid solution. Prepare a 1-2% (w / w) chitosan solution using 2% hydrochloric acid solution; then add the chitosan solution to the mixture, treat with ultrasonic vibration at 400-500W for 30-40 minutes, adjust the pH to 5-6, and stir the reaction at room temperature for 6-8 hours under nitrogen protection to obtain the reaction solution; add an equal volume of 3-5% (w / w) sodium hydroxide ethanol solution to the reaction solution, mix well, centrifuge to collect the precipitate, wash with water, and dry to obtain the final product; wherein the mass ratio of cysteine hydrochloride monohydrate to chitosan is 1:4-5.
[0022] Preferably, in step (2), the pore-forming agent is sodium bicarbonate or potassium bicarbonate.
[0023] Preferably, in step (2), the specific preparation method of the thiol-modified chitosan porous microspheres is as follows: first, the thiol-modified chitosan is stirred and dispersed in deionized water, then glyceryl monolaurate is added, stirred and emulsified to obtain an emulsion; then the emulsion is stirred and mixed with sodium alginate aqueous solution, a pore-forming agent is added, stirred evenly, vanillin solution is added, stirred and crosslinked reaction is performed, the precipitate is collected by centrifugation, washed, and dried to obtain the microspheres.
[0024] A further preferred embodiment is that the ratio of mercapto-modified chitosan, deionized water, glyceryl monolaurate, sodium alginate aqueous solution, pore-forming agent, and vanillin solution is 1g:90-100mL:8-10g:100-110mL:0.1-0.12g:90-100mL, wherein the mass concentration of sodium alginate aqueous solution is 0.5-1%, and the mass concentration of vanillin solution is 8-10%.
[0025] Further preferred, the stirring emulsification conditions are: stirring emulsification at 8000-10000 r / min for 20-30 minutes; the stirring crosslinking reaction conditions are: stirring crosslinking reaction at 500-700 r / min and 40-45℃ for 3-4 hours.
[0026] Preferably, in step (2), the specific method of loading is as follows: first, the thiol-modified chitosan porous microspheres are ultrasonically dispersed in a portion of the mixed essential oil of equal mass, and then ultrasonically oscillated at 800-1000W for 1-2 hours under a magnetic field of 800-1000Gs to obtain the loaded material.
[0027] Preferably, in step (3), the tyramine-modified β-cyclodextrin is prepared by the following method: β-cyclodextrin is stirred and dispersed in deionized water, pH is adjusted to 8-9, N-hydroxysuccinimide is added, stirred at room temperature for 30-40 minutes, tyramine is added, stirred and mixed, stirred and reacted at 55-60℃ for 4-5 hours, the precipitate is collected by centrifugation, washed with water, and dried to obtain the product; wherein, the mass ratio of β-cyclodextrin, deionized water, N-hydroxysuccinimide and tyramine is 1:8-10:1.2-1.4:0.8-1.
[0028] Preferably, the specific method of step (3) is as follows: first, tyramine-modified β-cyclodextrin is stirred and dissolved in deionized water, then the loading material is added, and ultrasonic oscillation is performed to obtain an aqueous phase; then the remaining mixed essential oil is added to the aqueous phase, and ultrasonic oscillation is performed under pulsed electric field conditions to homogenize it.
[0029] A further preferred embodiment is that the ratio of tyramine-modified β-cyclodextrin, deionized water, loading material, and remaining mixed essential oil is 1g: 12-15mL: 0.2-0.3g: 5-7mL.
[0030] Further preferred, the pulsed electric field conditions are: electric field strength 35-40 kV / cm, frequency 80-100 Hz, pulse width 4-5 μs; the ultrasonic oscillation treatment conditions are: 800-1000 W ultrasonic oscillation treatment for 8-10 minutes.
[0031] Further preferred homogenization conditions are: homogenization at 20-30 MPa for 6-7 minutes.
[0032] Compared with the prior art, the present invention has the following beneficial effects: This invention provides a children's skincare essential oil and its preparation method, comprising the following single essential oils by weight percentage: coconut oil 35-40%, sweet almond oil 1-3%, grapefruit essential oil 0.1-0.2%, ginger oil 0.05-0.15%, black pepper essential oil 0.03-0.06%, and the balance being grapeseed oil. The skincare essential oil obtained by this invention is safe for children and has good skincare effects.
[0033] The essential oils of this invention are extracted using different methods, retaining beneficial components and reducing irritating components. The composition of the essential oils is safe, and the synergistic effect of coconut oil, sweet almond oil, grapefruit essential oil, ginger oil, black pepper essential oil, and grapeseed oil improves skin care effects.
[0034] In the preparation process, coconut oil, sweet almond oil, grapefruit essential oil, ginger oil, black pepper essential oil, and grapeseed oil are first mixed evenly to obtain a mixed essential oil. Then, thiol-modified chitosan is prepared into thiol-modified chitosan porous microspheres under the action of a pore-forming agent. A portion of the mixed essential oil is then loaded onto the thiol-modified chitosan porous microspheres to obtain the loaded material. Finally, the loaded material and tyramine-modified β-cyclodextrin are mixed to form an aqueous phase, and the remaining mixed essential oil is used as the oil phase. The mixture is then used to obtain the final product. Through the preparation method of this invention, the mixed essential oil undergoes graded adsorption or coating treatment, reducing the concentration of the essential oil and minimizing direct contact between the essential oil and the skin, thus reducing skin irritation, ensuring good safety, providing sustained effects, and resulting in good skin care benefits. Detailed Implementation
[0035] The technical solutions of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention.
[0036] Unless otherwise specified, all products in this invention were purchased through market channels.
[0037] Example 1 A children's skin care essential oil contains the following single essential oils by weight percentage: 35% coconut oil, 1% sweet almond oil, 0.1% grapefruit essential oil, 0.05% ginger oil, 0.03% black pepper essential oil, and the balance being grapeseed oil.
[0038] The coconut oil or turmeric oil is prepared by the following method: Fresh coconut meat or fresh turmeric root is completely immersed in saturated lime water (5 times its weight) for 20 hours at room temperature. After soaking, it is rinsed with running water, drained, and pressed to obtain the pressed material. This material is then subjected to ultra-high pressure treatment, steam distillation, and the volatile oil is collected. The oil is then dehydrated using anhydrous sodium sulfate. The ultra-high pressure treatment conditions are: 300 MPa for 6 minutes. The pressed material after ultra-high pressure treatment is mixed with 8 times its weight of water and then subjected to steam distillation. Specifically, the mixture is heated to boiling, the volatile oil is collected, and the distillation time is 2 hours.
[0039] The sweet almond oil, black pepper oil, or grape seed oil is prepared by the following method: mature sweet almonds, black peppercorns, or grape seeds are pulverized to 80 mesh. A 50% ethanol aqueous solution with a volume concentration twice the weight of the mature sweet almonds, black peppercorns, or grape seeds is added. The mixture is subjected to ultrasonic vibration at 500W for 30 minutes, followed by supercritical CO2 extraction. After standing at room temperature for 8 hours, the oil layer is separated. The supercritical CO2 extraction conditions are: extraction temperature 40℃, extraction pressure 28MPa, CO2 flow rate 8L / h. The extract is collected every 30 minutes, and extraction is terminated when no more extract flows out.
[0040] The grapefruit essential oil is prepared by the following method: grapefruit peel is used as raw material, which is cleaned, dried, crushed, steamed, and cold-pressed to obtain crude oil I and cake. The cake is subjected to subcritical extraction to obtain crude oil II. Crude oil I and crude oil II are combined, and insoluble matter is removed by centrifugation to obtain the final product. The drying temperature is 50℃, and the moisture content is dried to ≤4% by weight. The product is crushed and passed through a 50-mesh sieve. The steaming temperature is 55℃, and the steaming time is 40 minutes. The subcritical extraction conditions are: solvent n-butane, pressure 0.4MPa, temperature 30℃, time 40 minutes, liquid-to-solid ratio 1.4:1, and extraction is performed 4 times. After the subcritical extraction, n-butane is removed by rotary evaporation.
[0041] The specific steps of the aforementioned method for preparing a children's skincare essential oil are as follows: (1) First, mix the coconut oil, sweet almond oil, grapefruit essential oil, ginger oil, black pepper essential oil and grapeseed oil in the specified amounts to obtain a mixed essential oil; (2) Then, under the action of a pore-forming agent, thiol-modified chitosan was used to prepare thiol-modified chitosan porous microspheres; then, a portion of the mixed essential oil was loaded onto the thiol-modified chitosan porous microspheres to obtain the loaded material; (3) Finally, the loading material and tyramine-modified β-cyclodextrin are mixed to form an aqueous phase, and the remaining part is mixed with essential oil as an oil phase. The mixture is then mixed to prepare the children's skin care essential oil.
[0042] In step (2), the thiol-modified chitosan is prepared by the following method: first, cysteine hydrochloride monohydrate is stirred and dissolved in 8 times its weight of a 1% hydrochloric acid solution, then N-hydroxysuccinimide and carbodiimide hydrochloride are added, so that the molar ratio of cysteine hydrochloride monohydrate, N-hydroxysuccinimide, and carbodiimide hydrochloride is 1:3:2, and the mixture is stirred and activated at room temperature for 2 hours to obtain a mixed solution; then, chitosan is prepared into a 1% chitosan solution using a 1% hydrochloric acid solution; then, the chitosan solution is added to the mixed solution, ultrasonically oscillated at 400W for 30 minutes, the pH is adjusted to 5, and the reaction is stirred at room temperature for 6 hours under nitrogen protection to obtain a reaction solution; an equal volume of 3% sodium hydroxide ethanol solution is added to the reaction solution, mixed evenly, centrifuged to collect the precipitate, washed with water, and dried to obtain the final product; wherein, the mass ratio of cysteine hydrochloride monohydrate to chitosan is 1:4.
[0043] In step (2), the pore-forming agent is sodium bicarbonate.
[0044] The specific preparation method of the thiol-modified chitosan porous microspheres is as follows: First, thiol-modified chitosan is stirred and dispersed in deionized water, then glyceryl monolaurate is added and stirred to emulsify, resulting in an emulsion; then, the emulsion is stirred and mixed with sodium alginate aqueous solution, a pore-forming agent is added, and the mixture is stirred evenly, then vanillin solution is added, and the mixture is stirred to crosslink. The precipitate is collected by centrifugation, washed, and dried to obtain the final product.
[0045] The ratio of mercapto-modified chitosan, deionized water, glyceryl monolaurate, sodium alginate aqueous solution, porogen, and vanillin solution is 1g:90mL:8g:100mL:0.1g:90mL, wherein the mass concentration of sodium alginate aqueous solution is 0.5% and the mass concentration of vanillin solution is 8%.
[0046] The stirring emulsification conditions were: stirring at 8000 r / min for 20 minutes; the stirring crosslinking reaction conditions were: stirring at 500 r / min and 40℃ for 3 hours.
[0047] In step (2), the specific method of loading is as follows: first, the thiol-modified chitosan porous microspheres are ultrasonically dispersed in a portion of the mixed essential oil of equal mass, and then ultrasonically oscillated at 800W for 1 hour under a magnetic field of 800Gs to obtain the loaded material.
[0048] In step (3), the tyramine-modified β-cyclodextrin is prepared by the following method: β-cyclodextrin is dispersed in deionized water and the pH is adjusted to 8. N-hydroxysuccinimide is added and stirred at room temperature for 30 minutes. Tyramine is added and stirred until well mixed. The mixture is stirred at 55°C for 4 hours. The precipitate is collected by centrifugation, washed with water, and dried to obtain the product. The mass ratio of β-cyclodextrin, deionized water, N-hydroxysuccinimide, and tyramine is 1:8:1.2:0.8.
[0049] The specific method of step (3) is as follows: first, tyramine-modified β-cyclodextrin is stirred and dissolved in deionized water, then the loading material is added, and ultrasonic oscillation is performed to obtain an aqueous phase; then the remaining mixed essential oil is added to the aqueous phase, and ultrasonic oscillation is performed under pulsed electric field conditions to homogenize it.
[0050] The ratio of tyramine-modified β-cyclodextrin, deionized water, loading material, and remaining mixed essential oils was 1g:12mL:0.2g:5mL.
[0051] The pulsed electric field conditions were: electric field strength 35kV / cm, frequency 80Hz, and pulse width 4μs; the ultrasonic oscillation treatment conditions were: 800W ultrasonic oscillation treatment for 8 minutes.
[0052] The homogenization conditions were: homogenization at 20 MPa for 6 minutes.
[0053] Example 2 A children's skin care essential oil contains the following single essential oils by weight percentage: 40% coconut oil, 3% sweet almond oil, 0.2% grapefruit essential oil, 0.15% ginger oil, 0.06% black pepper essential oil, and the balance being grapeseed oil.
[0054] The coconut oil or turmeric oil is prepared by the following method: Fresh coconut meat or fresh turmeric root is completely immersed in saturated lime water (7 times its weight) for 24 hours at room temperature. After soaking, it is rinsed with running water, drained, and pressed to obtain the pressed material. This material is then subjected to ultra-high pressure treatment, steam distillation, and the volatile oil is collected and dehydrated using anhydrous sodium sulfate. The ultra-high pressure treatment conditions are: 400 MPa for 8 minutes. The pressed material after ultra-high pressure treatment is mixed with 10 times its weight of water and then steam distilled. The specific method is: heating to boiling, collecting the volatile oil, and distilling for 2 hours.
[0055] The sweet almond oil, black pepper oil, or grape seed oil is prepared by the following method: mature sweet almonds, black peppercorns, or grape seeds are pulverized to 100 mesh. Three times their weight in a 60% ethanol aqueous solution is added. The mixture is subjected to ultrasonic vibration at 600W for 40 minutes, followed by supercritical CO2 extraction. After standing at room temperature for 10 hours, the oil layer is separated. The supercritical CO2 extraction conditions are: extraction temperature 45℃, extraction pressure 32MPa, CO2 flow rate 12L / h. The extract is collected every 30 minutes, and extraction is terminated when no more extract flows out.
[0056] The grapefruit essential oil is prepared by the following method: grapefruit peel is used as raw material, which is cleaned, dried, crushed, steamed, and cold-pressed to obtain crude oil I and cake. The cake is subjected to subcritical extraction to obtain crude oil II. Crude oil I and crude oil II are combined, and insoluble matter is removed by centrifugation to obtain the final product. The drying temperature is 60℃, and the moisture content is ≤4% by weight. The product is crushed and passed through a 50-mesh sieve. The steaming temperature is 60℃, and the steaming time is 50 minutes. The subcritical extraction conditions are: solvent n-butane, pressure 0.5MPa, temperature 35℃, time 50 minutes, liquid-to-solid ratio 1.4:1, and extraction is performed 4 times. After the subcritical extraction, n-butane is removed by rotary evaporation.
[0057] The specific steps of the aforementioned method for preparing a children's skincare essential oil are as follows: (1) First, mix the coconut oil, sweet almond oil, grapefruit essential oil, ginger oil, black pepper essential oil and grapeseed oil in the specified amounts to obtain a mixed essential oil; (2) Then, under the action of a pore-forming agent, thiol-modified chitosan was used to prepare thiol-modified chitosan porous microspheres; then, a portion of the mixed essential oil was loaded onto the thiol-modified chitosan porous microspheres to obtain the loaded material; (3) Finally, the loading material and tyramine-modified β-cyclodextrin are mixed to form an aqueous phase, and the remaining part is mixed with essential oil as an oil phase. The mixture is then mixed to prepare the children's skin care essential oil.
[0058] In step (2), the thiol-modified chitosan is prepared by the following method: first, cysteine hydrochloride monohydrate is stirred and dissolved in 10 times its weight of a 2% hydrochloric acid solution, then N-hydroxysuccinimide and carbodiimide hydrochloride are added, so that the molar ratio of cysteine hydrochloride monohydrate, N-hydroxysuccinimide, and carbodiimide hydrochloride is 1:5:3, and the mixture is stirred and activated at room temperature for 3 hours to obtain a mixed solution; then, chitosan is prepared into a 2% chitosan solution using a 2% hydrochloric acid solution; then, the chitosan solution is added to the mixed solution, ultrasonically oscillated at 500W for 40 minutes, the pH is adjusted to 6, and the reaction is stirred at room temperature for 8 hours under nitrogen protection to obtain a reaction solution; an equal volume of 5% sodium hydroxide ethanol solution is added to the reaction solution, mixed evenly, centrifuged to collect the precipitate, washed with water, and dried to obtain the final product; wherein, the mass ratio of cysteine hydrochloride monohydrate to chitosan is 1:5.
[0059] In step (2), the pore-forming agent is potassium bicarbonate.
[0060] The specific preparation method of the thiol-modified chitosan porous microspheres is as follows: First, thiol-modified chitosan is stirred and dispersed in deionized water, then glyceryl monolaurate is added and stirred to emulsify, resulting in an emulsion; then, the emulsion is stirred and mixed with sodium alginate aqueous solution, a pore-forming agent is added, and the mixture is stirred evenly, then vanillin solution is added, and the mixture is stirred to crosslink. The precipitate is collected by centrifugation, washed, and dried to obtain the final product.
[0061] The ratio of mercapto-modified chitosan, deionized water, glyceryl monolaurate, sodium alginate aqueous solution, porogen, and vanillin solution is 1g:100mL:10g:110mL:0.12g:100mL, wherein the mass concentration of sodium alginate aqueous solution is 1% and the mass concentration of vanillin solution is 10%.
[0062] The stirring emulsification conditions were: stirring at 10000 r / min for 30 minutes; the stirring crosslinking reaction conditions were: stirring at 700 r / min and 45℃ for 4 hours.
[0063] In step (2), the specific method of loading is as follows: first, the thiol-modified chitosan porous microspheres are ultrasonically dispersed in a portion of the mixed essential oil of equal mass, and then ultrasonically oscillated at 1000W for 2 hours under a magnetic field of 1000Gs to obtain the loaded material.
[0064] In step (3), the tyramine-modified β-cyclodextrin is prepared by the following method: β-cyclodextrin is stirred and dispersed in deionized water, pH is adjusted to 9, N-hydroxysuccinimide is added, stirred at room temperature for 40 minutes, tyramine is added, stirred and mixed, stirred at 60°C for 5 hours, the precipitate is collected by centrifugation, washed with water, and dried to obtain the product; wherein, the mass ratio of β-cyclodextrin, deionized water, N-hydroxysuccinimide and tyramine is 1:10:1.4:1.
[0065] The specific method of step (3) is as follows: first, tyramine-modified β-cyclodextrin is stirred and dissolved in deionized water, then the loading material is added, and ultrasonic oscillation is performed to obtain an aqueous phase; then the remaining mixed essential oil is added to the aqueous phase, and ultrasonic oscillation is performed under pulsed electric field conditions to homogenize it.
[0066] The ratio of tyramine-modified β-cyclodextrin, deionized water, loading material, and remaining mixed essential oils was 1g:15mL:0.3g:7mL.
[0067] The pulsed electric field conditions were: electric field strength 40kV / cm, frequency 100Hz, pulse width 5μs; the ultrasonic oscillation treatment conditions were: 1000W ultrasonic oscillation treatment for 10 minutes.
[0068] The homogenization conditions were: homogenization at 30 MPa for 7 minutes.
[0069] Example 3 A children's skin care essential oil contains the following single essential oils by weight percentage: coconut oil 38.7%, sweet almond oil 2%, grapefruit essential oil 0.15%, ginger oil 0.1%, black pepper essential oil 0.05%, and the balance being grapeseed oil.
[0070] The coconut oil or turmeric oil is prepared by the following method: Fresh coconut meat or fresh turmeric root is completely immersed in saturated lime water (6 times its weight) for 22 hours at room temperature. After soaking, it is rinsed with running water, drained, and pressed to obtain the pressed material. This material is then subjected to ultra-high pressure treatment, steam distillation, and the volatile oil is collected and dehydrated using anhydrous sodium sulfate. The ultra-high pressure treatment conditions are: 400 MPa for 7 minutes. The pressed material after ultra-high pressure treatment is mixed with 9 times its weight of water and then subjected to steam distillation. Specifically, the mixture is heated to boiling, the volatile oil is collected, and the distillation time is 2 hours.
[0071] The sweet almond oil, black pepper oil, or grape seed oil is prepared by the following method: mature sweet almonds, black peppercorns, or grape seeds are pulverized to 90 mesh. A 55% ethanol aqueous solution with a volume concentration twice the weight of the mature sweet almonds, black peppercorns, or grape seeds is added. The mixture is subjected to ultrasonic vibration at 600W for 35 minutes, followed by supercritical CO2 extraction. After standing at room temperature for 9 hours, the oil layer is separated. The supercritical CO2 extraction conditions are: extraction temperature 42℃, extraction pressure 30MPa, CO2 flow rate 10L / h. The extract is collected every 30 minutes, and extraction is terminated when no more extract flows out.
[0072] The grapefruit essential oil is prepared by the following method: grapefruit peel is used as raw material, which is cleaned, dried, crushed, steamed, and cold-pressed to obtain crude oil I and cake. The cake is subjected to subcritical extraction to obtain crude oil II. Crude oil I and crude oil II are combined, and insoluble matter is removed by centrifugation to obtain the final product. The drying temperature is 55℃, and the moisture content is dried to ≤4% by weight. The product is crushed and passed through a 50-mesh sieve. The steaming temperature is 58℃, and the steaming time is 45 minutes. The subcritical extraction conditions are: solvent n-butane, pressure 0.45MPa, temperature 33℃, time 45 minutes, liquid-to-solid ratio 1.4:1, and extraction is performed 4 times. After the subcritical extraction, n-butane is removed by rotary evaporation.
[0073] The specific steps of the aforementioned method for preparing a children's skincare essential oil are as follows: (1) First, mix the coconut oil, sweet almond oil, grapefruit essential oil, ginger oil, black pepper essential oil and grapeseed oil in the specified amounts to obtain a mixed essential oil; (2) Then, under the action of a pore-forming agent, thiol-modified chitosan was used to prepare thiol-modified chitosan porous microspheres; then, a portion of the mixed essential oil was loaded onto the thiol-modified chitosan porous microspheres to obtain the loaded material; (3) Finally, the loading material and tyramine-modified β-cyclodextrin are mixed to form an aqueous phase, and the remaining part is mixed with essential oil as an oil phase. The mixture is then mixed to prepare the children's skin care essential oil.
[0074] In step (2), the thiol-modified chitosan is prepared by the following method: first, cysteine hydrochloride monohydrate is stirred and dissolved in 9 times its weight of a 1.5% hydrochloric acid solution, then N-hydroxysuccinimide and carbodiimide hydrochloride are added, so that the molar ratio of cysteine hydrochloride monohydrate, N-hydroxysuccinimide, and carbodiimide hydrochloride is 1:4:2.5, and the mixture is stirred and activated at room temperature for 2 hours to obtain a mixed solution; then, chitosan is prepared into a 1% chitosan solution using a 2% hydrochloric acid solution; then, the chitosan solution is added to the mixed solution, ultrasonically oscillated at 500W for 35 minutes, the pH is adjusted to 6, and the reaction is stirred at room temperature for 7 hours under nitrogen protection to obtain a reaction solution; an equal volume of 4% sodium hydroxide ethanol solution is added to the reaction solution, mixed evenly, centrifuged to collect the precipitate, washed with water, and dried to obtain the final product; wherein, the mass ratio of cysteine hydrochloride monohydrate to chitosan is 1:4.5.
[0075] In step (2), the pore-forming agent is sodium bicarbonate.
[0076] The specific preparation method of the thiol-modified chitosan porous microspheres is as follows: First, thiol-modified chitosan is stirred and dispersed in deionized water, then glyceryl monolaurate is added and stirred to emulsify, resulting in an emulsion; then, the emulsion is stirred and mixed with sodium alginate aqueous solution, a pore-forming agent is added, and the mixture is stirred evenly, then vanillin solution is added, and the mixture is stirred to crosslink. The precipitate is collected by centrifugation, washed, and dried to obtain the final product.
[0077] The ratio of mercapto-modified chitosan, deionized water, glyceryl monolaurate, sodium alginate aqueous solution, porogen, and vanillin solution is 1g:95mL:9g:105mL:0.11g:95mL, wherein the mass concentration of sodium alginate aqueous solution is 0.8% and the mass concentration of vanillin solution is 9%.
[0078] The stirring emulsification conditions were: stirring emulsification at 9000 r / min for 25 minutes; the stirring crosslinking reaction conditions were: stirring crosslinking reaction at 600 r / min and 42℃ for 3 hours.
[0079] In step (2), the specific method of loading is as follows: first, the thiol-modified chitosan porous microspheres are ultrasonically dispersed in a portion of the mixed essential oil of equal mass, and then ultrasonically oscillated at 900W for 2 hours under a magnetic field of 900Gs to obtain the loaded material.
[0080] In step (3), the tyramine-modified β-cyclodextrin is prepared by the following method: β-cyclodextrin is dispersed in deionized water by stirring, pH is adjusted to 8, N-hydroxysuccinimide is added, stirred at room temperature for 35 minutes, tyramine is added, stirred and mixed, stirred at 57°C for 4 hours, the precipitate is collected by centrifugation, washed with water, and dried to obtain the product; wherein, the mass ratio of β-cyclodextrin, deionized water, N-hydroxysuccinimide and tyramine is 1:9:1.3:0.9.
[0081] The specific method of step (3) is as follows: first, tyramine-modified β-cyclodextrin is stirred and dissolved in deionized water, then the loading material is added, and ultrasonic oscillation is performed to obtain an aqueous phase; then the remaining mixed essential oil is added to the aqueous phase, and ultrasonic oscillation is performed under pulsed electric field conditions to homogenize it.
[0082] The ratio of tyramine-modified β-cyclodextrin, deionized water, loading material, and remaining mixed essential oils was 1g:13mL:0.25g:6mL.
[0083] The pulsed electric field conditions were: electric field strength 38kV / cm, frequency 90Hz, and pulse width 4μs; the ultrasonic oscillation treatment conditions were: 900W ultrasonic oscillation treatment for 9 minutes.
[0084] The homogenization conditions were: homogenization at 25 MPa for 6 minutes.
[0085] Comparative Example 1 Omit the ginger oil; The rest is the same as in Example 1.
[0086] Comparative Example 2 Omit the black pepper oil; The rest is the same as in Example 1.
[0087] Comparative Example 3 A method for preparing a skincare essential oil, the specific steps of which are as follows: (1) First, mix the coconut oil, sweet almond oil, grapefruit essential oil, ginger oil, black pepper essential oil and grapeseed oil in the specified amounts to obtain a mixed essential oil; (2) Then, tyramine-modified β-cyclodextrin is mixed to form an aqueous phase, and the mixed essential oil is used as the oil phase. The mixture is then mixed to prepare the skin care essential oil.
[0088] The specific method of step (2) is as follows: first, tyramine-modified β-cyclodextrin is stirred and dissolved in deionized water, and ultrasonically oscillated to obtain an aqueous phase; then, the mixed essential oil is added to the aqueous phase, and ultrasonically oscillated under pulsed electric field conditions to homogenize it.
[0089] The ratio of tyramine-modified β-cyclodextrin, deionized water, and mixed essential oils was 1g:12mL:5mL.
[0090] The pulsed electric field conditions were: electric field strength 35kV / cm, frequency 80Hz, and pulse width 4μs; the ultrasonic oscillation treatment conditions were: 800W ultrasonic oscillation treatment for 8 minutes.
[0091] The homogenization conditions were: homogenization at 20 MPa for 6 minutes.
[0092] The rest is the same as in Example 1.
[0093] Comparative Example 4 A method for preparing a skincare essential oil, the specific steps of which are as follows: (1) First, mix the coconut oil, sweet almond oil, grapefruit essential oil, ginger oil, black pepper essential oil and grapeseed oil in the specified amounts to obtain a mixed essential oil; (2) Then, under the action of a pore-forming agent, thiol-modified chitosan was used to prepare thiol-modified chitosan porous microspheres; then, a portion of the mixed essential oil was loaded onto the thiol-modified chitosan porous microspheres to obtain the loaded material; (3) Finally, the load material is made into an aqueous phase, and the remaining part is mixed with essential oil as an oil phase. The mixture is then prepared to obtain the skin care essential oil.
[0094] The specific method of step (3) is as follows: first, the load material is stirred and dissolved in deionized water, and ultrasonically oscillated to obtain an aqueous phase; then the remaining mixed essential oil is added to the aqueous phase, and ultrasonically oscillated under pulsed electric field conditions to homogenize it.
[0095] The ratio of deionized water, loading material, and remaining mixed essential oils is 12mL:0.2g:5mL.
[0096] The pulsed electric field conditions were: electric field strength 35kV / cm, frequency 80Hz, and pulse width 4μs; the ultrasonic oscillation treatment conditions were: 800W ultrasonic oscillation treatment for 8 minutes.
[0097] The homogenization conditions were: homogenization at 20 MPa for 6 minutes.
[0098] Comparative Example 5 A method for preparing a skin care essential oil involves mixing coconut oil, sweet almond oil, grapefruit essential oil, ginger oil, black pepper essential oil, and grapeseed oil in the specified amounts until homogeneous.
[0099] Security inspection The safety of the skin care essential oils obtained in Examples 1-3 and Comparative Examples 4 and 5 was investigated. Specifically, 50 healthy children (aged 3-5 years, half boys and half girls, with similar lifestyles and physical conditions) were randomly divided into 5 groups of 10 children each. During the experiment, their daily routines and diets remained normal. Every evening after bathing, they applied the skin care essential oil to the same area on the inner forearm (2cm × 2cm), using 0.03mL of the oil. The application method was to apply evenly and massage clockwise for 3 minutes. The condition of the treated area was assessed after 3 days, and the results are shown in Table 1.
[0100] Table 1. Safety Assessment
[0101] As shown in Table 1, the skin care essential oils obtained in Examples 1-3 do not cause allergic reactions on children's skin and have good safety.
[0102] Comparative Example 4 omitted tyramine-modified β-cyclodextrin, and Comparative Example 5 directly mixed the individual essential oils without further treatment, resulting in a significant decrease in safety. This indicates that the present invention reduces high-dose contact between essential oil components and the skin through the combined effect of thiol-modified chitosan porous microsphere loading and tyramine-modified β-cyclodextrin coating, thus avoiding irritation to children's skin.
[0103] Skincare effect evaluation The skincare effects of the skincare essential oils obtained in Examples 1-3 and Comparative Examples 1-4 were investigated (Comparative Example 5 had poor safety and was not investigated for skincare effects). The specific method was as follows: Seventy healthy children (aged 3-5 years, half male and half female, with similar lifestyles and physical conditions) were randomly divided into 7 groups of 10 children each. During the experiment, their daily routines and diets were normal. Every night after bathing, they applied the skincare essential oil to the same area on the inner forearm (2cm × 2cm), using 0.03mL of the oil. The application method was to apply the oil evenly and massage clockwise for 3 minutes. The skin moisture content of the skincare area was measured using a moisture meter at 0h, 2h, 6h, and 12h after skincare. The increase in skin moisture content at 2h, 6h, and 12h was calculated, and the average value was calculated. The results are shown in Table 2.
[0104] The formula for calculating the increase in skin moisture content is: W = (M1 - M0) / M0 × 100%, where W is the increase in skin moisture content, M1 is the skin moisture content after 2 hours, 6 hours or 12 hours of skin care, and M0 is the skin moisture content after 0 hours of skin care.
[0105] Table 2. Evaluation of Skin Care Effects
[0106] As shown in Table 2, the skin care essential oils obtained in Examples 1 to 3 can still maintain a certain increase in skin moisture content after 12 hours of skin care, indicating that they can provide long-lasting moisturization and have good skin care effects.
[0107] Comparative Example 1 omitted ginger oil, Comparative Example 2 omitted black pepper essential oil, Comparative Example 3 omitted the preparation of the loading material, and Comparative Example 4 omitted tyramine-modified β-cyclodextrin. The skin care effect of all of them was significantly worse. Although the increase in skin moisture content was large at the beginning of Comparative Examples 3 and 4, the increase in skin moisture content was significantly smaller after 6 hours of skin care. This shows that the essential oil formulation of the present invention, the loading of thiol-modified chitosan porous microspheres, and the coating of tyramine-modified β-cyclodextrin work together to improve the skin care effect and long-lasting skin care.
[0108] The present invention has been illustrated through the above embodiments, but the present invention is not limited to the above embodiments, that is, it does not mean that the present invention must rely on the above embodiments to be implemented. Those skilled in the art should understand that any improvements to the present invention, equivalent substitutions of individual raw materials in the product of the present invention, addition of auxiliary components, selection of specific methods, etc., all fall within the protection scope and disclosure scope of the present invention.
Claims
1. A child skin care essential oil characterized in that, The preparation steps are as follows: (1) First, mix the following single essential oils by weight percentage evenly to obtain a mixed essential oil: coconut oil 35-40%, sweet almond oil 1-3%, grapefruit essential oil 0.1-0.2%, ginger oil 0.05-0.15%, black pepper essential oil 0.03-0.06%, and the remainder is grapeseed oil; (2) Then, under the action of a pore-forming agent, thiol-modified chitosan porous microspheres are prepared; then, a portion of the mixed essential oil is loaded onto the thiol-modified chitosan porous microspheres to obtain the loaded material; wherein, the preparation method of the thiol-modified chitosan porous microspheres is as follows: first, thiol-modified chitosan is stirred and dispersed in deionized water, then glyceryl monolaurate is added, stirred and emulsified to obtain an emulsion; then, the emulsion is stirred and mixed with sodium alginate aqueous solution, pore-forming agent sodium bicarbonate or potassium bicarbonate is added, stirred evenly, vanillin solution is added, stirred and crosslinked reaction is performed, centrifuged to obtain the precipitate, washed, dried, and obtained; the loading method is as follows: first, thiol-modified chitosan porous microspheres are ultrasonically dispersed in a portion of the mixed essential oil of equal mass, and under a magnetic field of 800-1000 Gs, ultrasonic oscillation at 800-1000 W for 1-2 hours is performed to obtain the loaded material; (3) Tyramine-modified β-cyclodextrin was dissolved in deionized water by stirring, then the loading material was added, and the mixture was subjected to ultrasonic oscillation to obtain an aqueous phase. The remaining mixed essential oil was then added to the aqueous phase, and the mixture was homogenized by ultrasonic oscillation under a pulsed electric field to prepare the children's skincare essential oil. The ratio of tyramine-modified β-cyclodextrin, deionized water, loading material, and remaining mixed essential oil was 1g:12-15mL:0.2-0.3g:5-7mL. The tyramine-modified β-cyclodextrin was dissolved in deionized water by stirring, then the loading material was added, and the mixture was subjected to ultrasonic oscillation to obtain an aqueous phase. The remaining mixed essential oil was then added to the aqueous phase, and the mixture was subjected to ultrasonic oscillation under a pulsed electric field to obtain the children's skincare essential oil. β-Cyclodextrin is prepared by the following method: β-Cyclodextrin is dispersed in deionized water under stirring, the pH is adjusted to 8-9, N-hydroxysuccinimide is added, and the mixture is stirred at room temperature for 30-40 minutes. Tyramine is then added, and the mixture is stirred and mixed. The mixture is stirred and reacted at 55-60°C for 4-5 hours. The precipitate is collected by centrifugation, washed with water, and dried to obtain the final product. The mass ratio of β-Cyclodextrin, deionized water, N-hydroxysuccinimide, and tyramine is 1:8-10:1.2-1.4:0.8-1.
2. The children's skin care essential oil according to claim 1, characterized in that, It contains the following single essential oils by weight percentage: coconut oil 38.7%, sweet almond oil 2%, grapefruit essential oil 0.15%, ginger oil 0.1%, black pepper essential oil 0.05%, and the balance is grapeseed oil.
3. The children's skin care essential oil according to claim 1, characterized in that, The coconut oil or turmeric oil is prepared by the following method: fresh coconut meat or fresh turmeric root is completely immersed in saturated lime water with a weight of 5 to 7 times its weight, soaked at room temperature for 20 to 24 hours, taken out and rinsed with running water, drained, pressed to obtain pressed material, treated under ultra-high pressure, steam distilled, the volatile oil is collected, and dehydrated with anhydrous sodium sulfate to obtain the final product.
4. The children's skin care essential oil according to claim 1, characterized in that, The sweet almond oil, black pepper essential oil, or grape seed oil is prepared by the following method: crushing the ripe sweet almonds, black pepper fruits, or grape seeds to 80-100 mesh, adding 2-3 times the weight of the ripe sweet almonds, black pepper fruits, or grape seeds in a 50-60% ethanol aqueous solution, treating with ultrasonic vibration at 500-600W for 30-40 minutes, supercritical CO2 extraction, standing at room temperature for 8-10 hours, and separating the oil layer to obtain the oil.
5. The children's skin care essential oil according to claim 1, characterized in that, The grapefruit essential oil is prepared by the following method: grapefruit peel is used as raw material, impurities are removed, dried, crushed, steamed, and cold-pressed to obtain crude oil I and cake. The cake is subjected to subcritical extraction to obtain crude oil II. Crude oil I and crude oil II are combined and centrifuged to remove insoluble matter, thus obtaining the final product.
Citation Information
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