Preparation method of whitening, freckle-removing and anti-wrinkle essence oil
Through the use of modified β-cyclodextrin and complex antioxidants, the problems of poor extraction of various plant essential oils and poor stability of antioxidants have been solved, and the multi-effect integration and efficient extraction of whitening, freckle removal and anti-wrinkle essence oils have been achieved.
Patent Information
- Application Number
- CN202411283894.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-09-13
- Publication Date
- 2024-12-13
- Estimated Expiration
- Not applicable · inactive patent
AI Technical Summary
The prior art is not good when extracting a variety of plant essential oils, resulting in poor inclusion of β-cyclodextrin, which leads to poor in the extraction of essential oils. Traditional antioxidants such as vitamin C and vitamin E have poor stability or high cost, which affects the skin care effect. .
Using modified β-cyclodextrin and composite antioxidants, essential oil is extracted through water-grinding pressing and reduced pressure distillation technology, and dipropyl thiodiacetate is combined with vitamin E to enhance the antioxidant and stability of the essence oil.
It improves the extraction efficiency and antioxidant properties of essential oils, ensures the whitening, anti-wrinkle and moisturizing effects of essence oils, while reducing viscosity and improving the comfort and stability of the product.
Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of skin care products, and particularly relates to a method for preparing a whitening, freckle-removing and anti-wrinkle essence oil. Background Art
[0002] Essence oil is a pure oil-based skin care product, which is mainly composed of plant oils, natural essential oils, antioxidants, etc. in a certain proportion. It can replenish oil for the skin, nourish the skin, moisturize and prevent dryness. Although oil-based skin care products have a long history of application in ancient and modern times, they are gradually fading out of the market because traditional moisturizing oils are generally greasy and heavy, and have a poor skin feel. In recent years, the concept of using oil to nourish the skin has become more and more popular. Essence oils with a light and moisturizing feel, combined with water and lotion skin care, are favored by people due to their excellent skin care effects. Essence oils have also become a popular skin care product category.
[0003] At present, the main methods for extracting natural essential oils include steam distillation, solvent extraction, and supercritical CO2 extraction. Steam distillation can only produce essential oils with high aromatic components. It cannot produce essential oils for plant materials without aromatic components or with low aromatic components. In addition, the structure of aromatic compounds may be destroyed during the distillation process, thereby affecting the quality of the essential oils. Solvent extraction requires the use of a large amount of organic solvents, which may cause pollution and harm to the environment and human body. Supercritical CO2 extraction has the advantages of environmental protection, high efficiency, and safety. This method does not require the use of organic solvents, can be carried out at a lower temperature, and better retains the nutrients and aroma of the essential oils. However, supercritical CO2 extraction requires the use of high-pressure equipment, which has high pressure resistance requirements for the equipment and is costly, which is not economical for large-scale production.
[0004] Microcapsule aqueous two-phase extraction technology is a technology with few process steps, environmental protection, low energy consumption and production costs, and can be mass-produced. Before extracting essential oils, the essential oil components must generally be precipitated from the plant principles. Generally, ethanol solution is added to precipitate the essential oil components, but the use of ethanol for precipitation requires multiple extractions on the one hand, and ethanol is also an organic solvent and will have an impact on the human body on the other hand. Another method is to precipitate the essential oil components in the plant raw materials through water grinding and pressing, but this method has the problem of incomplete pressing, and some essential oil components will not be precipitated, resulting in poor extraction effect.
[0005] Currently, there are many literatures on the extraction of plant essential oils by microencapsulation aqueous two-phase extraction, but generally they are used to extract a single essential oil. When extracting multiple plant raw materials, conventional β-cyclodextrin cannot effectively encapsulate multiple essential oil components due to its own structure, thereby affecting the extraction effect of plant essential oils. Therefore, β-cyclodextrin needs to be modified to solve this problem. Summary of the invention
[0006] The purpose of the present invention is to provide a method for preparing a whitening, freckle-removing and anti-wrinkle essential oil.
[0007] In order to solve the above technical problems, the technical solution adopted by the present invention comprises the following steps: A whitening, freckle-removing and anti-wrinkle essential oil comprising the following components in parts by weight: 2-3 parts of isononyl isononanoate, 0.1-0.3 parts of cyclopentasiloxane, 30-32 parts of jojoba seed oil, 0.2-0.4 parts of ascorbyl tetraisopalmitate, 12-14 parts of caprylic / capric triglyceride, 0.6-0.8 parts of bisabolol, 48-50 parts of compound plant essential oils, and 0.3-0.5 parts of compound antioxidants. The specific preparation steps are: First, add isononyl isononanoate, cyclopentasiloxane, ascorbyl tetraisopalmitate, caprylic / capric triglyceride and bisabolol into jojoba seed oil, stir evenly, then continue to add compound plant essential oil and compound antioxidant, and continue to stir until evenly mixed.
[0008] Wherein, the preparation steps of the composite plant essential oil are: (1) Mandarin orange peel, lemon peel, poppy flower, bergamot peel, rose flower, myrrh resin, and ylang-ylang flower are prepared in a mass ratio of 3-5:5-7:4-6:2-3:4-5:3-4:6-8, washed with clean water and dried to obtain a mixture a, then the mixture a and a water-grinding accelerator are subjected to water-grinding and squeezing treatment at 36-40° C. for 60-70 min in a mass ratio of 1:0.7-0.8, and the filtrate a is obtained after filtering and removing the filter residue; (2) Add 16% to 20% by weight of enhanced β-cyclodextrin and 10% to 14% by weight of anhydrous sodium sulfate to the filtrate a, stir for 15 to 25 minutes until uniform, and then stand to separate the polymer phase and dry it. Then add 95% by volume ethanol solution and continue stirring for 70 to 80 minutes. After stirring, filter to obtain filtrate b. Wash and dry the dextrin and then recycle it. (3) The filtrate b is subjected to reduced pressure distillation at 0.004-0.006 MPa and 28-30° C. until no liquid is evaporated to obtain the composite plant essential oil.
[0009] The water-grinding accelerator is specifically prepared by uniformly mixing sodium diethylhexyl sulfosuccinate, rosin glycidyl ethanolamine and deionized water in a mass ratio of 0.06-0.08:0.03-0.05:1.
[0010] Wherein, the preparation method of enhanced β-cyclodextrin is: (1) β-cyclodextrin and anhydrous citric acid are weighed in a molar ratio of 1:1.2~1.4, and 0.1 mol / L sodium dihydrogen phosphate solution is added in an amount of 2~3 times the total mass. The system is then heated to 95~100°C and stirred at a speed of 300~400 r / min for 40~50 min. The reactants are then placed in an environment of 125~135°C and continue to react until the product is solid. The solid is washed twice with deionized water and anhydrous ethanol respectively, and then dried to obtain product a; (2) 1-2 parts by mass of chitosan are immersed in a 0.06-0.08 mol / L sulfuric acid solution until it is completely dissolved, and then 2-4 parts of product a are added, the system is heated to 120-130°C and stirred for reaction for 150-160 min, and then quickly cooled to room temperature, 1 mol / L sodium hydroxide solution is added to the system until no precipitation is produced, and the obtained precipitate is washed twice with deionized water and anhydrous ethanol respectively, and dried to obtain product b; (3) Product b is immersed in a 0.06-0.08 mol / L sulfuric acid solution, heated to 40°C and stirred until it is completely dissolved, then 0.6-0.7 times the mass of product b of 1,2-epoxypropyldimethyldodecylammonium chloride is added to the system, the temperature is continued to be raised to 58-60°C, and the reaction is stirred at a speed of 150-250 r / min for 23.5-24.5 h. After the reaction is completed, the solid is washed twice with deionized water and anhydrous ethanol respectively, and then dried to obtain enhanced β-cyclodextrin.
[0011] The composite antioxidant is specifically prepared by uniformly mixing dipropyl thiodiacetate and vitamin E in a mass ratio of 0.6-0.8:1.
[0012] The beneficial effects of the present invention are: (1) The present invention adopts plant essential oils of specific components and compound auxiliary ingredients. The prepared essential oil has the characteristics of whitening, anti-wrinkle and moisturizing, which can keep the skin color white, translucent, young and fair. The water grinding promoter is used to promote the water grinding and pressing effect of plant raw materials, thereby increasing the precipitation of essential oil components. By modifying β-cyclodextrin, the inclusion effect of β-cyclodextrin in extracting various plant essential oils is effectively enhanced, thereby enhancing the separation and extraction effect of essential oil components. Finally, by compounding a specific antioxidant, the antioxidant property of the essential oil product is effectively enhanced, thereby ensuring its skin care effect. (2) The present invention enhances the extraction effect of essential oil components by adding a water milling promoter in the water milling and squeezing treatment step. Compared with conventional penetrants such as sodium dodecyl sulfate, sodium diethyl sulfosuccinate has excellent permeability, as well as excellent wettability, dispersibility and defoaming properties. On the one hand, it can accelerate the wetting of plant raw materials by water, and on the other hand, it can also enhance the dispersibility of essential oil components in water, further promoting the precipitation of essential oil components in the raw materials. At the same time, its defoaming property can reduce bubbles, thereby ensuring the stability of the extraction process. In addition, sodium diethyl sulfosuccinate is highly safe and has little harm to the human body. (3) Rosin glycidyl ethanolamine is also a surfactant with excellent penetration effect. Compared with conventional penetrants such as sodium dodecylbenzene sulfonate, rosin glycidyl ethanolamine also has excellent dispersibility, wettability and low foaming properties, and has a synergistic effect with sodium diethylhexyl sulfosuccinate; (4) The present invention enhances the inclusion effect of β-cyclodextrin on essential oils by modifying the β-cyclodextrin. Compared with other modifiers such as propylene oxide, 1,2-epoxypropyldimethyldodecylammonium chloride can enhance the water solubility of β-cyclodextrin and increase the amount and type of essential oils included in it, so that β-cyclodextrin can extract more essential oils. 1,2-epoxypropyldimethyldodecylammonium chloride can also improve the interaction between β-cyclodextrin and essential oils, thereby providing inclusion stability and efficiency. In addition, since 1,2-epoxypropyldimethyldodecylammonium chloride has a bactericidal effect, it can avoid the negative impact of bacteria and microorganisms on essential oils during the extraction process. (5) Commonly used antioxidants in essential oils include vitamin C, vitamin E and ergothioneine. Among them, vitamin C and vitamin E have poor stability. When the essential oil is used, their antioxidant effect may be greatly reduced, thereby affecting the effect of protecting the essential oil components. At the same time, it also has negative effects such as irritation to the skin when the concentration is high. Ergothioneine has excellent antioxidant effect, but it also has the problem of high cost. The present invention enhances the antioxidant property of the essential oil by adding a composite antioxidant. Compared with conventional antioxidants such as vitamin C, dipropyl thiodiacetate has antioxidant properties and is more stable than vitamin C, which can better play its role in protecting the essential oil components. At the same time, it has a synergistic effect with vitamin E, which can enhance the antioxidant property and the stability of vitamin E. Dipropyl thiodiacetate is not hygroscopic and will not absorb moisture in the air when the essential oil is used, resulting in a decrease in the efficacy and stability of the essential oil. Dipropyl thiodiacetate has a low viscosity and a certain volatility, which can reduce the stickiness of the essential oil and make the essential oil more refreshing to use. DETAILED DESCRIPTION
[0013] The present invention will be further described in detail below in conjunction with the embodiments. Example 1
[0014] The water-grinding accelerator is obtained by uniformly mixing sodium diethylhexyl sulfosuccinate, rosin glycidyl ethanolamine and deionized water in a mass ratio of 0.07:0.04:1.
[0015] Tangerine peel, lemon peel, poppy flower, bergamot peel, rose, myrrh resin and ylang-ylang flower are prepared in a mass ratio of 4:6:5:2.5:4.5:3.5:7, washed with clean water and dried to obtain a mixture a, then the mixture a and a water-grinding accelerator are water-milled and squeezed at 38°C for 65 minutes in a mass ratio of 1:0.75, and the filter residue is removed by filtering to obtain a filtrate a. Example 2
[0016] The water-grinding accelerator is obtained by uniformly mixing sodium diisooctyl sulfosuccinate, rosin glycidyl ethanolamine and deionized water in a mass ratio of 0.06:0.05:1.
[0017] Tangerine peel, lemon peel, poppy flower, bergamot peel, rose, myrrh resin and ylang-ylang flower are prepared in a mass ratio of 3:7:4:3:4:4:6, washed with clean water and dried to obtain a mixture a, then the mixture a and a water-grinding accelerator are water-milled and squeezed at 36°C for 70 minutes in a mass ratio of 1:0.7, and the filter residue is removed by filtering to obtain a filtrate a. Example 3
[0018] The water-grinding accelerator is obtained by uniformly mixing sodium diisooctyl sulfosuccinate, rosin glycidyl ethanolamine and deionized water in a mass ratio of 0.08:0.03:1.
[0019] Tangerine peel, lemon peel, poppy flower, bergamot peel, rose, myrrh resin and ylang-ylang flower are prepared in a mass ratio of 5:5:6:2:5:3:8, washed with clean water and dried to obtain a mixture a, then the mixture a and a water-grinding accelerator are water-milled and squeezed at 40°C for 60 minutes in a mass ratio of 1:0.8, and the filter residue is removed by filtering to obtain a filtrate a. Example 4
[0020] Sodium dodecyl sulfate, rosin glycidyl ethanolamine and deionized water were uniformly mixed in a mass ratio of 0.07:0.04:1 to obtain a water-grinding accelerator.
[0021] The rest is the same as in Example 1. Example 5
[0022] The water-grinding accelerator is obtained by uniformly mixing sodium dioctyl sulfosuccinate, sodium dodecylbenzene sulfonate and deionized water in a mass ratio of 0.07:0.04:1.
[0023] The rest is the same as in Example 1. Example 6
[0024] Tangerine peel, lemon peel, poppy flower, bergamot peel, rose, myrrh resin and ylang-ylang flower are prepared in a mass ratio of 4:6:5:2.5:4.5:3.5:7, washed with clean water and dried to obtain a mixture a, then the mixture a and a water-grinding accelerator are water-milled and squeezed at 38°C for 65 minutes in a mass ratio of 1:0.4, and the filter residue is removed by filtering to obtain a filtrate a.
[0025] The rest is the same as in Example 1. Example 7
[0026] Tangerine peel, lemon peel, poppy flower, bergamot peel, rose, myrrh resin and ylang-ylang flower are prepared in a mass ratio of 4:6:5:2.5:4.5:3.5:7, washed with clean water and dried to obtain a mixture a, then the mixture a and a water-grinding accelerator are water-milled and squeezed at 25°C for 65 minutes in a mass ratio of 1:0.75, and the filter residue is removed by filtering to obtain a filtrate a.
[0027] The rest is the same as in Example 1. Example 8
[0028] Tangerine peel, lemon peel, poppy flower, bergamot peel, rose, myrrh resin and ylang-ylang flower are prepared in a mass ratio of 4:6:5:2.5:4.5:3.5:7, washed with clean water and dried to obtain a mixture a, then the mixture a and a water-grinding accelerator are water-milled and squeezed at 38°C for 40 minutes in a mass ratio of 1:0.75, and the filter residue is removed by filtering to obtain a filtrate a.
[0029] The rest is the same as in Example 1.
[0030] Test 1: The contents of limonene, linalool and linalool in the filtrates of Examples 1 to 8 were determined by gas chromatography-mass spectrometry, and the precipitation rate of limonene was calculated by the formula a=m1 / M1, wherein a is the precipitation rate of limonene, m1 is the mass of limonene, and M1 is the mass of lemon peel; b=m2 / M2, wherein b is the precipitation rate of linalool, m2 is the mass of linalool, and M2 is the mass of myrrh resin; c=m3 / M3, wherein c is the precipitation rate of linalool, m3 is the mass of linalool, and M3 is the mass of ylang-ylang flower; the specific data are shown in Table 1.
[0031] Table 1 Analysis and extraction rate data of some essential oil groups in Examples 1 to 8 Implementation items a(%) b(%) c(%) Example 1 0.914 0.752 0.458 Example 2 0.898 0.734 0.447 Example 3 0.905 0.743 0.452 Example 4 0.754 0.601 0.339 Example 5 0.772 0.631 0.350 Example 6 0.815 0.667 0.392 Example 7 0.868 0.704 0.425 Example 8 0.852 0.699 0.417 It can be seen from Table 1 that the analysis rate of the essential oil components in Examples 1 to 3 is the highest; the reason why the analysis rate of the essential oil components in Example 4 is significantly reduced may be that after sodium dodecyl sulfate is replaced with sodium sulfosuccinate diethyl ester, the penetration, wetting and dispersion properties of sodium dodecyl sulfate are not as good as those of sodium dodecyl sulfate, and sodium dodecyl sulfate has the properties of a foaming agent, which will produce bubbles and affect the stability of the essential oil component analysis process, thereby affecting the analysis rate of the essential oil components; the reason why the analysis rate of the essential oil components in Example 5 is significantly reduced may be that after rosin glycidyl ethanolamine is replaced with sodium dodecylbenzene sulfonate, the sodium dodecylbenzene sulfonate The permeability and wettability are not as good as those of rosin glycidyl ethanolamine, and sodium dodecylbenzene sulfonate also has the properties of a foaming agent, which will affect the stability of the essential oil component precipitation process, thereby affecting the essential oil component precipitation rate; the reason why the essential oil component precipitation rate of Example 6 is not as good as that of Example 1 may be that the amount of water-milling accelerator used is relatively small, thereby affecting the essential oil component precipitation rate; the reason why the essential oil component precipitation rate of Example 7 is not as good as that of Example 1 may be that the temperature during water-milling and pressing is lower, thereby affecting the precipitation of essential oil components; the reason why the essential oil component precipitation rate of Example 8 is not as good as that of Example 1 may be that the water-milling and pressing treatment time is relatively short, and some essential oil components have not been precipitated.
[0032] The filtrate a obtained in Example 1 was further used in Examples 9 to 14 to prepare composite plant essential oils. Example 9
[0033] β-cyclodextrin and anhydrous citric acid were weighed in a molar ratio of 1:1.3, and 0.1 mol / L sodium dihydrogen phosphate solution was added in an amount 2.5 times the total mass thereof. The system was then heated to 98°C and stirred at 350 r / min for 45 min. The reactants were then placed in an environment of 130°C and continued to react until the product was solid. The solid was washed twice with deionized water and anhydrous ethanol, respectively, and dried to obtain product a after washing. 1.5 parts by mass of chitosan were immersed in a 0.07 mol / L sulfuric acid solution until completely dissolved, and then 3 parts of product a were added, the system was heated to 125°C and stirred for reaction for 155 minutes, and then quickly cooled to room temperature, 1 mol / L sodium hydroxide solution was added to the system until no precipitation was produced, and the obtained precipitate was washed twice with deionized water and anhydrous ethanol respectively, and dried to obtain product b; The product b was immersed in a 0.07 mol / L sulfuric acid solution, heated to 40°C and stirred until it was completely dissolved, and then 0.65 times the mass of the product b 1,2-epoxypropyldimethyldodecylammonium chloride was added to the system, and the temperature was continued to rise to 59°C. The reaction was stirred at a speed of 200 r / min for 24 hours. After the reaction was completed, the solid was washed twice with deionized water and anhydrous ethanol respectively, and then dried after washing to obtain enhanced β-cyclodextrin.
[0034] Add 18% by weight of enhanced β-cyclodextrin and 12% by weight of anhydrous sodium sulfate to the filtrate a, stir for 20 minutes until uniform, and then stand for stratification, separate the polymer phase and dry it, then add 95% by volume ethanol solution, continue stirring for 75 minutes, and filter after stirring to obtain filtrate b, wash and dry the dextrin and then recycle it; The filtrate b is subjected to reduced pressure distillation at 0.005 MPa and 29° C. until no liquid is evaporated to obtain the composite plant essential oil. Example 10
[0035] β-cyclodextrin and anhydrous citric acid were weighed in a molar ratio of 1:1.2, and a 0.1 mol / L sodium dihydrogen phosphate solution of 3 times the total mass was added, and then the system was heated to 100°C and stirred at a speed of 300 r / min for 40 minutes, and then the reactants were placed in an environment of 125°C to continue the reaction until the product was solid, and the obtained solid was washed twice with deionized water and anhydrous ethanol respectively, and dried after washing to obtain product a; Immerse 1 part of chitosan in 0.06 mol / L sulfuric acid solution until it is completely dissolved, then add 4 parts of product a, heat the system to 120°C and stir to react for 160 minutes, then quickly cool to room temperature, add 1 mol / L sodium hydroxide solution to the system until no precipitation is produced, wash the obtained precipitate twice with deionized water and anhydrous ethanol respectively, and dry to obtain product b; The product b was immersed in a 0.08 mol / L sulfuric acid solution, heated to 40°C and stirred until it was completely dissolved, and then 0.7 times the mass of the product b 1,2-epoxypropyldimethyldodecylammonium chloride was added to the system, and the temperature was continued to rise to 60°C. The reaction was stirred at a speed of 150 r / min for 23.5 hours. After the reaction was completed, the solid was washed twice with deionized water and anhydrous ethanol respectively, and then dried after washing to obtain enhanced β-cyclodextrin.
[0036] Add 16% by weight of enhanced β-cyclodextrin and 14% by weight of anhydrous sodium sulfate to the filtrate a, stir for 15 minutes until uniform, and then stand for stratification, separate the polymer phase and dry it, then add 95% by volume ethanol solution, continue stirring for 80 minutes, and filter after stirring to obtain filtrate b, wash and dry the dextrin and then recycle it; The filtrate b is subjected to reduced pressure distillation at 0.004 MPa and 30° C. until no liquid is evaporated to obtain the composite plant essential oil. Embodiment 11
[0037] β-cyclodextrin and anhydrous citric acid were weighed in a molar ratio of 1:1.4, and a 0.1 mol / L sodium dihydrogen phosphate solution twice the total mass was added, and then the system was heated to 95°C and stirred at a speed of 400 r / min for 50 min, and then the reactants were placed in an environment of 135°C to continue the reaction until the product was solid, and the obtained solid was washed twice with deionized water and anhydrous ethanol respectively, and dried after washing to obtain product a; 1-2 parts by mass of chitosan were immersed in a 0.08 mol / L sulfuric acid solution until completely dissolved, and then 2 parts of product a were added, the system was heated to 130°C and stirred for reaction for 150 minutes, and then quickly cooled to room temperature, 1 mol / L sodium hydroxide solution was added to the system until no precipitation was produced, and the obtained precipitate was washed twice with deionized water and anhydrous ethanol respectively, and dried to obtain product b; The product b was immersed in a 0.06 mol / L sulfuric acid solution, heated to 40°C and stirred until it was completely dissolved, and then 0.6 times the mass of the product b 1,2-epoxypropyldimethyldodecylammonium chloride was added to the system, and the temperature was continued to rise to 58°C. The reaction was stirred at a speed of 250 r / min for 24.5 hours. After the reaction was completed, the solid was washed twice with deionized water and anhydrous ethanol respectively, and then dried after washing to obtain enhanced β-cyclodextrin.
[0038] Add 20% by weight of enhanced β-cyclodextrin and 10% by weight of anhydrous sodium sulfate to the filtrate a, stir for 25 minutes until uniform, and then stand for stratification, separate the polymer phase and dry it, then add 95% by volume ethanol solution, continue stirring for 70 minutes, and filter after stirring to obtain filtrate b, wash and dry the dextrin and then recycle it; The filtrate b is subjected to reduced pressure distillation at 0.006 MPa and 28° C. until no liquid is evaporated to obtain the composite plant essential oil. Example 12
[0039] β-cyclodextrin and anhydrous citric acid were weighed in a molar ratio of 1:1.3, and 0.1 mol / L sodium dihydrogen phosphate solution was added in an amount 2.5 times the total mass thereof. The system was then heated to 98°C and stirred at 350 r / min for 45 min. The reactants were then placed in an environment of 130°C and continued to react until the product was solid. The solid was washed twice with deionized water and anhydrous ethanol, respectively, and dried to obtain product a after washing. 1.5 parts by mass of chitosan were immersed in a 0.07 mol / L sulfuric acid solution until completely dissolved, and then 3 parts of product a were added, the system was heated to 125°C and stirred for reaction for 155 minutes, and then quickly cooled to room temperature, 1 mol / L sodium hydroxide solution was added to the system until no precipitation was produced, and the obtained precipitate was washed twice with deionized water and anhydrous ethanol respectively, and dried to obtain product b; The product b was immersed in a 0.07 mol / L sulfuric acid solution, heated to 40°C and stirred until it was completely dissolved. Then, 0.65 times the mass of the product b propylene oxide was added to the system, and the temperature was continued to rise to 59°C. The reaction was stirred at a speed of 200 r / min for 24 hours. After the reaction was completed, the solid was washed twice with deionized water and anhydrous ethanol respectively, and then dried after washing to obtain enhanced β-cyclodextrin.
[0040] The rest is the same as Example 9. Embodiment 13
[0041] β-cyclodextrin and anhydrous citric acid were weighed in a molar ratio of 1:1.3, and deionized water 2.5 times of the total mass was added, and then the system was heated to 98°C and stirred at a speed of 350 r / min for 45 minutes, and then the reactants were placed in an environment of 130°C to continue the reaction until the product was solid, and the obtained solid was washed twice with deionized water and anhydrous ethanol respectively, and dried after washing to obtain product a; 1.5 parts by mass of chitosan were immersed in a 0.07 mol / L sulfuric acid solution until completely dissolved, and then 3 parts of product a were added, the system was heated to 125°C and stirred for reaction for 155 minutes, and then quickly cooled to room temperature, 1 mol / L sodium hydroxide solution was added to the system until no precipitation was produced, and the obtained precipitate was washed twice with deionized water and anhydrous ethanol respectively, and dried to obtain product b; The product b was immersed in a 0.07 mol / L sulfuric acid solution, heated to 40°C and stirred until it was completely dissolved, and then 0.65 times the mass of the product b 1,2-epoxypropyldimethyldodecylammonium chloride was added to the system, and the temperature was continued to rise to 59°C. The reaction was stirred at a speed of 200 r / min for 24 hours. After the reaction was completed, the solid was washed twice with deionized water and anhydrous ethanol respectively, and then dried after washing to obtain enhanced β-cyclodextrin.
[0042] The rest is the same as Example 9. Embodiment 14
[0043] β-cyclodextrin and anhydrous citric acid were weighed in a molar ratio of 1:1.3, and 0.1 mol / L sodium dihydrogen phosphate solution was added in an amount 2.5 times the total mass thereof. The system was then heated to 98°C and stirred at 350 r / min for 45 min. The reactants were then placed in an environment of 130°C and continued to react until the product was solid. The solid was washed twice with deionized water and anhydrous ethanol, respectively, and dried to obtain product a after washing. 1.5 parts by mass of chitosan were immersed in a 0.07 mol / L sulfuric acid solution until completely dissolved, and then 3 parts of product a were added, the system was heated to 125°C and stirred for reaction for 155 minutes, and then naturally cooled to room temperature, 1 mol / L sodium hydroxide solution was added to the system until no precipitation was produced, and the obtained precipitate was washed twice with deionized water and anhydrous ethanol respectively, and dried to obtain product b; The product b was immersed in a 0.07 mol / L sulfuric acid solution, heated to 40°C and stirred until it was completely dissolved, and then 0.65 times the mass of the product b 1,2-epoxypropyldimethyldodecylammonium chloride was added to the system, and the temperature was continued to rise to 59°C. The reaction was stirred at a speed of 200 r / min for 24 hours. After the reaction was completed, the solid was washed twice with deionized water and anhydrous ethanol respectively, and then dried after washing to obtain enhanced β-cyclodextrin.
[0044] The rest is the same as Example 9. Embodiment 15
[0045] β-cyclodextrin and anhydrous citric acid were weighed in a molar ratio of 1:1.3, and 0.1 mol / L sodium dihydrogen phosphate solution was added in an amount 2.5 times the total mass thereof. The system was then heated to 98°C and stirred at 350 r / min for 45 min. The reactants were then placed in an environment of 130°C and continued to react until the product was solid. The solid was washed twice with deionized water and anhydrous ethanol, respectively, and dried to obtain product a after washing. 1.5 parts by mass of chitosan were immersed in a 0.07 mol / L sulfuric acid solution until completely dissolved, and then 3 parts of product a were added, the system was heated to 125°C and stirred for reaction for 155 minutes, and then quickly cooled to room temperature, 1 mol / L sodium hydroxide solution was added to the system until no precipitation was produced, and the obtained precipitate was washed twice with deionized water and anhydrous ethanol respectively, and dried to obtain product b; The product b was immersed in a 0.07 mol / L sulfuric acid solution, heated to 40°C and stirred until it was completely dissolved, and then 0.40 times the mass of the product b of 1,2-epoxypropyldimethyldodecylammonium chloride was added to the system, and the temperature was continued to rise to 59°C. The reaction was stirred at a speed of 200 r / min for 24 hours. After the reaction was completed, the solid was washed twice with deionized water and anhydrous ethanol respectively, and then dried after washing to obtain enhanced β-cyclodextrin.
[0046] The rest is the same as Example 9.
[0047] Test 2: The solubility A of the enhanced β-cyclodextrin prepared in Examples 9 to 15 at 25° C. was measured; the mass M4 of the filtrate a before separation of the essential oil component was measured respectively, and the mass m4 of the composite plant essential oil was measured at the same time, and the essential oil separation rate was calculated according to the formula d=m4 / M4; the specific data are shown in Table 2.
[0048] Table 2 Implementation items A (g / L) d(%) Example 9 62.7 8.26 Example 10 61.5 8.11 Embodiment 11 61.9 8.15 Example 12 28.6 4.85 Embodiment 13 32.4 5.54 Embodiment 14 55.7 7.20 Embodiment 15 48.8 6.73 It can be seen from Table 2 that the enhanced β-cyclodextrin prepared in Examples 9 to 11 has the best water solubility and the best effect of extracting composite plant essential oil; the reason why the data of Example 12 is not as good as that of Example 9 may be that after 1,2-epoxypropyldimethyldodecylammonium chloride is replaced by ethylene oxide, on the one hand, ethylene oxide does not have the properties of a surfactant, and on the other hand, the molecular structure of ethylene oxide is not as complex as that of 1,2-epoxypropyldimethyldodecylammonium chloride, so its modification effect on β-cyclodextrin is not as good as that of 1,2-epoxypropyldimethyldodecylammonium chloride, which in turn affects the water solubility and inclusion function of β-cyclodextrin; the reason why the data of Example 13 is not as good as that of Example 9 may be that After the sodium dihydrogen phosphate solution was replaced with deionized water, there was no sodium dihydrogen phosphate as a catalyst to promote the reaction between β-cyclodextrin and citric acid, which reduced the degree of reaction and affected the subsequent modification reaction, resulting in poor modification effect of β-cyclodextrin; the reason why the data in Example 14 was not as good as that in Example 9 may be that the cooling method after the reaction of product a with chitosan was natural cooling, which increased the crystallinity of cyclodextrin, reduced the water solubility of cyclodextrin and affected the subsequent modification reaction; the reason why the data in Example 15 was not as good as that in Example 9 may be that the amount of 1,2-epoxypropyldimethyldodecylammonium chloride used was less, so the modification effect was also a little worse, affecting the water solubility and inclusion function of cyclodextrin.
[0049] The composite plant essential oil prepared in Example 9 was further used in Examples 16 to 20 to prepare whitening, freckle-removing and anti-wrinkle essential oil. Example 16
[0050] The composite antioxidant is obtained by uniformly mixing dipropyl thiodiacetate and vitamin E in a mass ratio of 0.7:1.
[0051] First, add 2.5 parts of isononyl isononanoate, 0.2 parts of cyclopentasiloxane, 0.3 parts of ascorbyl tetraisopalmitate, 13 parts of caprylic / capric triglyceride and 0.7 parts of bisabolol to 31 parts of jojoba seed oil, stir evenly, then continue to add 49 parts of compound plant essential oil and 0.4 parts of compound antioxidant, continue to stir until evenly mixed to obtain the whitening, anti-freckle and anti-wrinkle essence oil. Embodiment 17
[0052] The composite antioxidant is obtained by uniformly mixing dipropyl thiodiacetate and vitamin E in a mass ratio of 0.6:1.
[0053] First, add 3 parts of isononyl isononanoate, 0.1 parts of cyclopentasiloxane, 0.4 parts of ascorbyl tetraisopalmitate, 12 parts of caprylic / capric triglyceride and 0.6 parts of bisabolol to 32 parts of jojoba seed oil, stir evenly, then continue to add 48 parts of compound plant essential oil and 0.3 parts of compound antioxidant, continue to stir until evenly mixed to obtain the whitening, anti-freckle and anti-wrinkle essence oil. Embodiment 18
[0054] The composite antioxidant is obtained by uniformly mixing dipropyl thiodiacetate and vitamin E in a mass ratio of 0.8:1.
[0055] First, add 3 parts of isononyl isononanoate, 0.3 parts of cyclopentasiloxane, 0.2 parts of ascorbyl tetraisopalmitate, 14 parts of caprylic / capric triglyceride and 0.8 parts of bisabolol to 30 parts of jojoba seed oil, stir evenly, then continue to add 50 parts of compound plant essential oil and 0.5 parts of compound antioxidant, continue to stir until evenly mixed to obtain the whitening, anti-freckle and anti-wrinkle essence oil. Embodiment 19
[0056] The composite antioxidant is obtained by uniformly mixing vitamin C and vitamin E in a mass ratio of 0.7:1.
[0057] The rest is the same as Example 16. Embodiment 20
[0058] Add 2.5 parts of isononyl isononanoate, 0.2 parts of cyclopentasiloxane, 0.3 parts of ascorbyl tetraisopalmitate, 13 parts of caprylic / capric triglyceride, 0.7 parts of bisabolol, 49 parts of compound plant essential oil and 0.4 parts of compound antioxidant to 31 parts of jojoba seed oil, stir evenly to obtain whitening, freckle-removing and anti-wrinkle essential oil.
[0059] The rest is the same as Example 16.
[0060] Test 3: The DPPH free radical method was used to test the antioxidant properties of the whitening, anti-freckle and anti-wrinkle essence oils prepared in Examples 16 to 20 on the first day and the 80th day after opening. The DPPH free radical scavenging rate on the first day was recorded as e, and the DPPH free radical scavenging rate on the 40th day was recorded as f. At the same time, the viscosity at 20°C was measured and recorded as g. The specific data are shown in Table 3.
[0061] Table 3 Performance data of whitening and anti-freckle anti-wrinkle essence oil of Example 16 to Example 20 Implementation items e(%) f(%) g (mPa.s) Example 16 74.6 74.0 142 Embodiment 17 72.8 72.3 151 Embodiment 18 73.5 72.8 147 Embodiment 19 59.3 55.1 206 Embodiment 20 65.1 63.8 165 It can be seen from Table 3 that the whitening, freckle-removing and anti-wrinkle essence oils prepared in Examples 16 to 18 have the best antioxidant properties and the lowest viscosity; Example 19 has worse antioxidant properties and poorer stability than Example 16, and its viscosity is also higher. The reason may be that dipropyl thiodiacetate is replaced by vitamin C. On the one hand, there is no synergistic effect between vitamin C and vitamin E, and on the other hand, the stability of vitamin C is also worse, so its antioxidant properties will weaken over time. At the same time, vitamin C is solid and has no effect on regulating viscosity; the reason why the data of Example 20 is not as good as that of Example 16 may be that the components of the essence oil are not added step by step. When adding in one step, some components are mixed unevenly, which not only affects the effect of the antioxidant components, but also has a certain impact on the viscosity of the essence oil due to the uneven mixing of the components.
Claims
1. A whitening, freckle-removing and anti-wrinkle essential oil, characterized in that: Contains the following components by mass: 2-3 parts of isononyl isononanoate, 0.1-0.3 parts of cyclopentasiloxane, 30-32 parts of jojoba seed oil, 0.2-0.4 parts of ascorbyl tetraisopalmitate, 12-14 parts of caprylic / capric triglyceride, 0.6-0.8 parts of bisabolol, 48-50 parts of compound plant essential oils, and 0.3-0.5 parts of compound antioxidants. The specific preparation steps are: First, add isonyl isononanoate, cyclopentasiloxane, ascorbyl tetraisopalmitate, caprylic / capric triglyceride and bisabolol into jojoba seed oil, stir evenly, then continue to add compound plant essential oil and compound antioxidant, and continue to stir until evenly mixed.
2. The whitening, freckle-removing and anti-wrinkle essential oil according to claim 1, characterized in that: The preparation steps of the composite plant essential oil are: (1) Mandarin orange peel, lemon peel, poppy flower, bergamot peel, rose flower, myrrh resin, and ylang-ylang flower are prepared in a mass ratio of 3-5:5-7:4-6:2-3:4-5:3-4:6-8, washed with clean water and dried to obtain a mixture a, then the mixture a and a water-grinding accelerator are subjected to water-grinding and squeezing treatment at 36-40° C. for 60-70 min in a mass ratio of 1:0.7-0.8, and the filtrate a is obtained after filtering and removing the filter residue; (2) Add 16% to 20% by weight of enhanced β-cyclodextrin and 10% to 14% by weight of anhydrous sodium sulfate to the filtrate a, stir for 15 to 25 minutes until uniform, and then stand to separate the polymer phase and dry it. Then add 95% by volume ethanol solution and continue stirring for 70 to 80 minutes. After stirring, filter to obtain filtrate b. Wash and dry the dextrin and then recycle it. (3) The filtrate b is subjected to reduced pressure distillation at 0.004-0.006 MPa and 28-30° C. until no liquid is evaporated to obtain the composite plant essential oil.
3. A whitening, freckle-removing and anti-wrinkle essential oil as claimed in claim 2, characterized in that: The water grinding accelerator is specifically prepared by uniformly mixing sodium dioctyl sulfosuccinate, rosin glycidyl ethanolamine and deionized water in a mass ratio of 0.06-0.08:0.03-0.05:
1.
4. The whitening, freckle-removing and anti-wrinkle essential oil according to claim 2, characterized in that: The preparation method of enhanced β-cyclodextrin is as follows: (1) β-cyclodextrin and anhydrous citric acid are weighed in a molar ratio of 1:1.2~1.4, and 0.1 mol / L sodium dihydrogen phosphate solution is added in an amount of 2~3 times the total mass. The system is then heated to 95~100°C and stirred at a speed of 300~400 r / min for 40~50 min. The reactants are then placed in an environment of 125~135°C and continue to react until the product is solid. The solid is washed twice with deionized water and anhydrous ethanol respectively, and then dried to obtain product a; (2) 1-2 parts by mass of chitosan are immersed in a 0.06-0.08 mol / L sulfuric acid solution until it is completely dissolved, and then 2-4 parts of product a are added, the system is heated to 120-130°C and stirred for reaction for 150-160 min, and then quickly cooled to room temperature, 1 mol / L sodium hydroxide solution is added to the system until no precipitation is produced, and the obtained precipitate is washed twice with deionized water and anhydrous ethanol respectively, and dried to obtain product b; (3) Product b is immersed in a 0.06-0.08 mol / L sulfuric acid solution, heated to 40°C and stirred until it is completely dissolved, then 0.6-0.7 times the mass of product b of 1,2-epoxypropyldimethyldodecylammonium chloride is added to the system, the temperature is continued to be raised to 58-60°C, and the reaction is stirred at a speed of 150-250 r / min for 23.5-24.5 h. After the reaction is completed, the solid is washed twice with deionized water and anhydrous ethanol respectively, and then dried to obtain enhanced β-cyclodextrin.
5. The whitening, freckle-removing and anti-wrinkle essential oil according to claim 1, characterized in that: The composite antioxidant is specifically prepared by uniformly mixing dipropyl thiodiacetate and vitamin E in a mass ratio of 0.6-0.8:1.
