CN112266825A - Compound essential oil, preparation method thereof and application of compound essential oil in whitening and anti-wrinkle cosmetics - Google Patents
Compound essential oil, preparation method thereof and application of compound essential oil in whitening and anti-wrinkle cosmetics Download PDFInfo
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- CN112266825A CN112266825A CN202011182423.1A CN202011182423A CN112266825A CN 112266825 A CN112266825 A CN 112266825A CN 202011182423 A CN202011182423 A CN 202011182423A CN 112266825 A CN112266825 A CN 112266825A
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- oil
- essential oil
- seed oil
- compound essential
- nanocapsule
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- C11B9/00—Essential oils; Perfumes
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- A—HUMAN NECESSITIES
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- A61K8/922—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof of vegetable origin
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- A—HUMAN NECESSITIES
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- A61Q19/00—Preparations for care of the skin
- A61Q19/08—Anti-ageing preparations
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
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Abstract
The invention relates to compound essential oil, a preparation method thereof and application thereof in whitening and anti-wrinkle cosmetics. The compound essential oil is prepared from suaeda salsa seed oil, pepper seed oil, citrus seed oil and szechwan chinaberry fruit oil according to the weight ratio of 3-4: 1-2: 2-3: 5-6, preparing the nanocapsule containing 33% of compound essential oil according to a reverse emulsification method, and adding the nanocapsule into the whitening anti-wrinkle cosmetic according to the proportion of 10-15%. The compound essential oil is a pure natural plant extract, can inhibit tyrosinase activity, is efficient in antioxidation, can effectively reduce volatilization of the essential oil by preparing the compound essential oil into a nanocapsule, can protect active ingredients of the essential oil, is added into cosmetics, is mild and has no toxic or side effect, and can whiten skin and delay senescence after being used for a long time.
Description
Technical Field
The invention relates to compound essential oil, in particular to compound essential oil consisting of suaeda salsa seed oil, pepper seed oil, citrus seed oil and szechwan chinaberry fruit oil, a preparation method of the compound essential oil and application of the compound essential oil in daily cosmetics for whitening and resisting wrinkles.
Background
In the modern society, the living standard and aesthetic standard of people are continuously improved, and people have fair and smooth skin which is advocated by modern women. In recent years, the development of whitening anti-wrinkle cosmetics is becoming active, and in view of the current development situation of the global cosmetics industry, natural active ingredients are obtained from Chinese herbal medicines, so that the natural active ingredients are becoming a new popular trend for the development of the cosmetics industry.
Tyrosinase, also known as polyphenol oxidase, is a copper-containing oxidoreductase of about 75kb, widely present in animals, plants, microorganisms and human bodies, and is a rate-limiting enzyme for melanin synthesis, which directly affects the synthesis of melanin. Meanwhile, it is also related to the occurrence of diseases such as excessive melanin deposition such as freckles, chloasma and the like. Therefore, the real whitening of the skin can be realized by inhibiting the activity of tyrosinase. At present, skin whitening active substances on the market are mainly tyrosinase inhibitors, including arbutin, kojic acid, hydroquinone and the like, but the skin whitening active substances have some defects, such as unstable properties, easy oxidative discoloration, weak efficacy caused by poor percutaneous absorption, certain cytotoxicity, easy skin irritation and the like. Therefore, the development of safer and more effective whitening products is a hot point of research in the field of cosmetics.
Aging is an "oxidation process" of the human body. In the skin, oxidation is usually an influence of radicals. After the skin is oxidized, the human body can generate redundant free radicals. Our usual anti-aging care, namely "anti-oxidation", is to reduce free radicals in the skin mainly by some methods. Therefore, the antioxidant belongs to basic care of skin, is indispensable care, is equivalent to a skin's dart', provides certain protective effect to skin, prevents color cosmetics and ultraviolet rays from influencing the skin, and can delay aging, enable the skin to be in a relatively tight state and prevent wrinkles from generating.
The plant essential oil is a pure natural plant extract, can relieve various skin problems after long-term facial use, can reduce wrinkles, delay skin aging, soften skin, regulate oil secretion of skin, improve the water deficiency state of skin, enable the skin to have luster, sterilize, diminish inflammation, relieve skin and the like; the plant essential oil is a pure natural substance, does not contain other chemical additives such as preservatives and the like, is easy to be absorbed and transformed by the skin, and cannot be deposited on the surface of the skin.
Suaeda glauca is a herbaceous plant of Chenopodiaceae and is one of indication plants of saline-alkali soil. The suaeda salsa is an oil plant with potential application value and mainly grows in saline-alkali wastelands such as seashore, desert and the like and tidal flat lands. The suaeda glauca seeds contain a large amount of fat, the extracted essential oil has extremely high nutritional value, and can reduce blood fat, and the suaeda glauca seeds can also be used as natural edible pigment to be added into feed.
The pepper is a rutaceae plant and is widely distributed in China. The prickly ash seeds contain a large amount of aromatic components and essential oil, and are one of eight traditional seasonings in China. The Chinese prickly ash is used as a traditional Chinese medicine and has the effects of warming the middle-jiao and promoting the circulation of qi, expelling cold, relieving pain and killing insects; treating stomach and abdomen psychroalgia, emesis, diarrhea, schistosome, ascariasis, etc.; can also be used as epidermal anesthetic.
Citrus is a plant of the genus Citrus in the family Rutaceae, China is a world large producing country of citrus, and planting area and yield are the first place in the world. The citrus fruits contain more than 30 health-care substances, have high nutritional value, and can resist tumor, soothe the liver, strengthen the spleen, resolve phlegm, regulate qi and the like; the citrus seed extract has antibacterial effect.
Fructus Toosendan is a dried mature fruit of Meliaceae plant, and is a well-known Chinese medicinal material. The product contains a large amount of volatile oil substances, has high medicinal value, and can be used for treating stagnation of liver-qi, pathogenic fire, chest and hypochondrium, abdominal pain, hernia pain, and abdominal pain due to parasitic infestation.
The plant essential oil has various extraction methods, and different extraction methods can cause the difference of the components, the content, the biological activity and the like of the plant essential oil. The invention also discovers that the compound essential oil has tyrosinase activity inhibiting and antioxidant activities and can be used in whitening cosmetics. However, the plant essential oil as a fat-soluble liquid has volatility, and the storage condition of the essential oil is very harsh, so that the storage condition of the essential oil is limited in practical application; can protect the active components of the essential oil; the stability of the essential oil can be improved; the storage period of the essential oil can be prolonged; can broaden the application range of the essential oil. The compound essential oil nanocapsule can be added into daily cosmetics such as water, milk, face cream, etc.
The inventor finally obtains the compound essential oil with the optimal proportion through a large number of research experiments, and proves the positive effects of the compound essential oil on whitening and wrinkle resistance through rigorous experiments. The invention provides compound essential oil and a nanocapsule prepared from the compound essential oil, which can play a role in whitening and resisting wrinkles when added into cosmetics.
Disclosure of Invention
The first purpose of the invention is to provide the compound essential oil which is simple in extraction method and has the effects of whitening and resisting wrinkles.
The second purpose of the invention is to provide a preparation method of the compound essential oil and the nanocapsules thereof.
The third purpose of the invention is to provide the application of the compound essential oil nanocapsule in the preparation of the whitening anti-wrinkle daily-use cosmetic.
The invention provides compound essential oil which is prepared from suaeda salsa seed oil, pepper seed oil, citrus seed oil and szechwan chinaberry fruit oil in a proportion of 3-4: 1-2: 2-3: 5-6.
The compound essential oil comprises the following components in a ratio of 3:1:2: 5.
Preferably, the preparation method of the suaeda salsa seed oil in the compound essential oil comprises the following steps:
taking suaeda salsa seeds, crushing, sieving, placing in a charging basket of microwave dynamic extraction equipment, adding 60 times of water, soaking for 45min at room temperature, setting the microwave power to 287W, performing microwave radiation for 30min, connecting a volatile oil separator on the microwave extraction equipment, and collecting distilled essential oil to obtain the suaeda salsa seed oil.
The preparation method of the pricklyash seed oil in the compound essential oil comprises the following steps:
pulverizing semen Zanthoxyli, sieving, and placing in supercritical CO2Adding 70% ethanol in an amount which is 2.5 times that of the extraction kettle, soaking for 150min at room temperature, wherein the extraction conditions are as follows: the extraction pressure is 40MPa, the extraction temperature is 40 ℃, the extraction time is 3h, and CO is added2The flow rate was 20 kg/h. Filtering the extractive solution, recovering 70% ethanol with rotary evaporator, and volatilizing to obtain oleum Zanthoxyli Bungeani.
The preparation method of the citrus seed oil in the compound essential oil comprises the following steps:
pulverizing citrus seeds, sieving, and placing in supercritical CO2Adding 3 times of 70% ethanol into an extraction kettle, soaking for 150min at room temperature, wherein the extraction conditions are as follows: the extraction pressure is 35MPa, the extraction temperature is 45 ℃, the extraction time is 3h, and CO is2The flow rate was 25 kg/h. Filtering the extractive solution, recovering 70% ethanol with rotary evaporator, and volatilizing to obtain citrus seed oil.
The preparation method of the chinaberry fruit oil in the compound essential oil comprises the following steps:
pulverizing fructus Toosendan, sieving, placing in round bottom flask, adding 10 times of distilled water, adjusting pH to 4.5 with hydrochloric acid, adding 1% cellulase into container, slightly stirring, placing in water bath, performing enzymolysis at 50 deg.C for 35min, performing steam distillation, installing volatile oil extractor, heating to boil, distilling for 2.5 hr, and collecting distilled essential oil to obtain fructus Toosendan oil.
The invention also provides a preferable preparation method of the compound essential oil, which comprises the following steps:
(1) preparation of suaeda salsa seed oil
Taking suaeda salsa seeds, crushing, sieving, placing in a charging basket of microwave dynamic extraction equipment, adding 60 times of water, soaking for 45min at room temperature, setting the microwave power to 287W, performing microwave radiation for 30min, connecting a volatile oil separator on the microwave extraction equipment, and collecting distilled essential oil to obtain the suaeda salsa seed oil.
(2) Preparation of pricklyash seed oil
Pulverizing semen Zanthoxyli, sieving, and placing in supercritical CO2Adding 70% ethanol 2.5 times the amount of the extract in an extraction kettle, and soaking at room temperature150min, and the extraction conditions are as follows: the extraction pressure is 40MPa, the extraction temperature is 40 ℃, the extraction time is 3h, and CO is added2The flow rate was 20 kg/h. Filtering the extractive solution, recovering 70% ethanol with rotary evaporator, and volatilizing to obtain oleum Zanthoxyli Bungeani.
(3) Preparation of citrus seed oil
Pulverizing citrus seeds, sieving, and placing in supercritical CO2Adding 3 times of 70% ethanol into an extraction kettle, soaking for 150min at room temperature, wherein the extraction conditions are as follows: the extraction pressure is 35MPa, the extraction temperature is 45 ℃, the extraction time is 3h, and CO is2The flow rate was 25 kg/h. Filtering the extractive solution, recovering 70% ethanol with rotary evaporator, and volatilizing to obtain citrus seed oil.
(4) Preparation of Chuanlian chinaberry seed oil
Pulverizing fructus Toosendan, sieving, placing in round bottom flask, adding 10 times of distilled water, adjusting pH to 4.5 with hydrochloric acid, adding 1% cellulase into container, slightly stirring, placing in water bath, performing enzymolysis at 50 deg.C for 35min, performing steam distillation, installing volatile oil extractor, heating to boil, distilling for 2.5 hr, and collecting distilled essential oil to obtain fructus Toosendan oil.
(5) Selecting Suaeda salsa seed oil, pricklyash peel seed oil, citrus seed oil and fructus Toosendan oil according to a certain proportion, and mixing uniformly to obtain the final product.
The compound essential oil for the whitening anti-wrinkle cosmetic is prepared into nanocapsules containing 33% of compound essential oil according to a reverse emulsification method, and the nanocapsules are added into the whitening anti-wrinkle cosmetic according to the proportion of 10-15%.
The whitening anti-wrinkle cosmetic has no special limitation on the selection of the dosage form and the matrix, and can be prepared into whitening anti-wrinkle water, whitening anti-wrinkle milk, whitening anti-wrinkle cream and the like.
The invention also comprises the application of the compound essential oil in the field of whitening and anti-wrinkle cosmetics.
The compound essential oil has the following beneficial effects in the field of whitening and anti-wrinkle cosmetics:
1. the compound essential oil is a pure natural plant extract, has wide raw material sources, no toxic or side effect after long-term use, simple preparation process and enriched effective active ingredients, and is suitable for long-term whitening and wrinkle resistance.
2. The invention originally combines the suaeda salsa seed oil, the pepper seed oil, the citrus seed oil and the szechwan chinaberry fruit oil, and determines the dosage and proportion of the components through a large number of experiments, so that the compound essential oil has obvious synergistic effect. By optimizing the preparation scheme and adopting a reverse emulsification method, the compound essential oil nanocapsule is prepared, so that the volatilization loss of essential oil can be reduced, the active ingredients of the essential oil are protected, and the storage time of the essential oil is prolonged. The compound essential oil nanocapsule is added into cosmetics, is mild and has no toxic or side effect, and can remarkably inhibit tyrosinase activity, remove free radicals, resist oxidation, whiten skin and delay aging after long-term use.
Detailed Description
The technical solution of the present invention will be further described with reference to the following specific examples, but the embodiments of the present invention are not limited thereto.
Example 1 preparation of skin whitening anti-wrinkle series cosmetics
The first step is as follows: preparation of various essential oils
The preparation method of the suaeda salsa seed oil comprises the following steps:
taking suaeda salsa seeds, crushing, sieving, placing in a charging basket of microwave dynamic extraction equipment, adding 60 times of water, soaking for 45min at room temperature, adding 0.1% of cellulase, setting the microwave power to 287W, performing microwave radiation for 30min, connecting a volatile oil separator on the microwave extraction equipment, and collecting distilled essential oil to obtain the suaeda salsa seed oil.
The preparation method of the pricklyash seed oil comprises the following steps:
pulverizing semen Zanthoxyli, sieving, and placing in supercritical CO2Adding 70% ethanol in an amount which is 2.5 times that of the extraction kettle, soaking for 150min at room temperature, wherein the extraction conditions are as follows: the extraction pressure is 40MPa, the extraction temperature is 40 ℃, the extraction time is 3h, and CO is added2The flow rate was 20 kg/h. Filtering the extractive solution, recovering 70% ethanol with rotary evaporator, and volatilizing to obtain oleum Zanthoxyli Bungeani.
The preparation method of the citrus seed oil comprises the following steps:
pulverizing citrus seeds, sieving, and placing in supercritical CO2Adding 70% ethanol 3 times the amount of the extract in an extraction kettle, and soaking at room temperature150min, and the extraction conditions are as follows: the extraction pressure is 35MPa, the extraction temperature is 45 ℃, the extraction time is 3h, and CO is2The flow rate was 25 kg/h. Filtering the extractive solution, recovering 70% ethanol with rotary evaporator, and volatilizing to obtain citrus seed oil.
The preparation method of the szechwan chinaberry fruit oil comprises the following steps:
pulverizing fructus Toosendan, sieving, placing in round bottom flask, adding 10 times of distilled water, adjusting pH to 4.5 with hydrochloric acid, adding 1% cellulase into container, slightly stirring, placing in water bath, performing enzymolysis at 50 deg.C for 35min, performing steam distillation, installing volatile oil extractor, heating to boil, distilling for 2.5 hr, and collecting distilled essential oil to obtain fructus Toosendan oil.
The second step is that: preparing a compound essential oil nanocapsule:
taking 0.1g of acetyl chitosan, placing the acetyl chitosan in a beaker, and adding deionized water to 10mL to obtain an acetyl chitosan solution for later use; taking 10g of sodium alginate, placing the sodium alginate in a beaker, adding 10mL of compound essential oil, carrying out ultrasonic emulsification completely, slowly dropwise adding 0.5mol/LNaOH to adjust the pH value to 7.5 to obtain sodium alginate nanocapsules, washing and centrifuging the sodium alginate nanocapsules, adding the sodium alginate nanocapsules into an acetyl chitosan solution, and carrying out magnetic stirring for 3 hours to obtain the compound essential oil nanocapsules.
The third step: the compound essential oil nanocapsule is added into daily cosmetics to prepare whitening anti-wrinkle moisturizing water, whitening anti-wrinkle milk and whitening anti-wrinkle cream.
The invention provides an application of the compound essential oil nanocapsule in a whitening and anti-wrinkle cosmetic, and preferably the compound essential oil nanocapsule is added in the whitening and anti-wrinkle cosmetic in an amount of 10-15% by mass.
The whitening anti-wrinkle cosmetic has no special limitation on the selection of the formulation and the matrix, and can be prepared into whitening anti-wrinkle moisturizing lotion, whitening anti-wrinkle milk, whitening anti-wrinkle cream and the like.
Preparing whitening anti-wrinkle moisturizing lotion:
the components and contents of the whitening anti-wrinkle moisturizing lotion are shown in table 1.
TABLE 1 whitening anti-wrinkle moisturizing lotion formula
The preparation process comprises the following steps:
adding the compound essential oil nanocapsule into sodium hyaluronate, and uniformly mixing to obtain a mixed material A; and adding the mixed material A and the other components into deionized water, and uniformly mixing to obtain the whitening anti-wrinkle moisturizing lotion.
Preparation of the whitening anti-wrinkle milk:
the components and contents of the whitening anti-wrinkle milk are shown in table 2.
TABLE 2 whitening anti-wrinkle emulsion formula
The preparation process comprises the following steps:
heating vitamin E acetate, methyl paraben, polyethylene glycol (25) spermaceti stearate, glyceryl monostearate, and dimethyl silicone oil as oil phase to 50 deg.C, stirring, and keeping the temperature for 25 min; heating glycerol, carbomer and deionized water as water phase to 50 deg.C, stirring, and keeping the temperature for 25 min; adding the oil phase into an emulsifying pot, maintaining the temperature at 50 deg.C, starting homogenizing and stirring at the stirring speed of 27r/min, pumping the water phase into the emulsifying pot, homogenizing for 5min, and stirring for 20 min; cooling to 35 ℃, adding the compound essential oil nanocapsules, stirring and mixing uniformly, and cooling to room temperature to obtain the whitening anti-wrinkle emulsion.
Preparation of whitening anti-wrinkle cream:
the components and contents of the whitening anti-wrinkle cream are shown in table 3.
TABLE 3 whitening anti-wrinkle cream formula
The preparation process comprises the following steps:
uniformly mixing sodium hyaluronate, glyceryl monostearate and compound essential oil nanocapsules to obtain a mixed material A; placing medical vaseline and glycerol on a water bath kettle, heating to 75 ℃ and dissolving to obtain a mixed material B; and when the temperature of the mixed material B is reduced to 25 ℃, adding the hexadecanol, the propyl p-hydroxybenzoate, the polyacrylamide and the mixed material A, uniformly stirring, adding deionized water, and adjusting the pH value to 5.5-6 to obtain the whitening anti-wrinkle cream.
The following test examples further illustrate that the compound essential oil has the effects of inhibiting tyrosinase activity, removing hydroxyl free radicals and oxygen free radicals and reducing force, can be used for preparing series of cosmetics for whitening and resisting wrinkles, and the trial effect of the series of cosmetics on human bodies.
Test example 1
The tyrosinase inhibition test of the compound essential oil comprises the following steps:
1. materials and methods
1.1 test materials
Suaeda salsa seed oil, pepper seed oil, citrus seed oil and Chinaberry fruit oil are respectively prepared according to the embodiment. Preparing compound essential oil (composition 1, lacking Chinaberry fruit oil) of Suaeda glauca seed oil, pricklyash peel seed oil and citrus seed oil according to the formula proportion; compound essential oil of suaeda salsa seed oil, pepper seed oil and chinaberry seed oil (composition 2, lacking of citrus seed oil); compound essential oil of suaeda glauca seed oil, citrus seed oil and chinaberry seed oil (composition 3, lacking of pepper seed oil); compound essential oil of pricklyash peel seed oil, orange seed oil and chinaberry seed oil (composition 4, lacking suaeda salsa seed oil); the essential oil missing in the composition is replaced by peanut oil with equal proportion. The invention is compounded with essential oil (composition 5); the compound essential oil nanocapsule (composition 6, nanocapsule prepared by composition 5); positive control arbutin.
1.2 test methods
The inhibition effect of samples on tyrosinase activity is measured by a dopa rate oxidation method, samples are added according to table 4, phosphate buffer solution, the samples and tyrosinase are sequentially added into a test tube, water bath is carried out at 35 ℃ for 15min, then tyrosine is added, the mixture is uniformly mixed, reaction is carried out at 35 ℃ for 30min, the mixture is rapidly transferred into a cuvette, and the absorbance value is measured at 475 nm. Each group was assayed 3 times in parallel with arbutin as a positive control.
Calculating the formula: tyrosinase inhibition rate [ (a-B)/a ] x 100%;
wherein A is the absorbance value of the standard control, and B is the absorbance value of the test solution or the positive control.
TABLE 4 reaction solution composition
Note: when the absorbance is measured by a spectrophotometer, the test solution, the standard control and the positive control are respectively zeroed by the negative control 1, the negative control 2 and the negative control 3.
2. Results and analysis
The inhibition of tyrosinase by each composition is shown in table 5.
In comparison with the composition 1, the composition,△P<0.01; in comparison with the composition 2, the present inventors have shown that,▲P<0.01; in comparison with the composition 3, the composition,*P<0.01; in comparison with the composition 4, the composition,θP<0.01; in comparison with the composition No. 5,×P<0.01; compared with the arbutin, the preparation method has the advantages that,#P<0.01。
as shown in Table 5, each composition can inhibit tyrosinase activity and has whitening effect, wherein the tyrosinase inhibition rate of the composition 6 is the highest, and the whitening activity of the composition is higher than that of arbutin. Compared with the compositions 1, 2, 3 and 4, the whitening effect of the composition 5 is obviously improved, which shows that the whitening effect is improved after the combination of the 4 natural plant essential oils, and the effect is reduced if any one of the natural plant essential oils is absent. The composition 5 can be used for preparing nanocapsules, which have tyrosinase inhibition rate significantly higher than that of composition 5, because essential oils in compositions 1-5 are volatile and have short action time, and the nanocapsules prepared by the method can overcome the defect and improve anti-allergy activity.
3. And (4) conclusion: the compound essential oil and the nanocapsule thereof can effectively inhibit the activity of tyrosinase, thereby achieving the effect of whitening.
Test example 2
The hydroxyl radical scavenging activity test of the compound essential oil of the invention comprises:
1. materials and methods
1.1 test materials
Suaeda salsa seed oil, pepper seed oil, citrus seed oil and Chinaberry fruit oil are respectively prepared according to the embodiment. Preparing compound essential oil (composition 1, lacking Chinaberry fruit oil) of Suaeda glauca seed oil, pricklyash peel seed oil and citrus seed oil according to the formula proportion; compound essential oil of suaeda salsa seed oil, pepper seed oil and chinaberry seed oil (composition 2, lacking of citrus seed oil); compound essential oil of suaeda glauca seed oil, citrus seed oil and chinaberry seed oil (composition 3, lacking of pepper seed oil); compound essential oil of pricklyash peel seed oil, orange seed oil and chinaberry seed oil (composition 4, lacking suaeda salsa seed oil); the essential oil missing in the composition is replaced by peanut oil with equal proportion. The invention is compounded with essential oil (composition 5); the compound essential oil nanocapsule (composition 6, nanocapsule prepared from composition 5); positive control vitamin c (vc) in water.
1.2 test methods
Measuring hydroxyl radical scavenging activity by Fenton method, adding sample and ferrous sulfate (FeSO) into test tube according to Table 64) Mixing with salicylic acid, standing at room temperature for 15min, adding hydrogen peroxide (H) into the test tube2O2) Standing at room temperature for 35min after mixing uniformly, and finally measuring the absorbance value at the wavelength of 510nm by using an enzyme-labeling instrument, wherein each group is subjected to parallel measurement for 3 times, and VC is used as a positive control.
Calculating the formula: hydroxyl radical scavenging rate Ao- (Ax-Axo)/Ao × 100%;
wherein Ao is the absorbance value of the blank control, Ax is the absorbance value of the added sample, and Axo is the absorbance value of the added sample without H2O2Aox is the absorbance value of the positive control.
TABLE 6 reaction solution composition
2. Results and analysis
The hydroxyl radical scavenging rate of each composition is shown in table 7.
In comparison with the composition 1, the composition,△P<0.05,△△P<0.01; in comparison with the composition 2, the present inventors have shown that,▲P<0.01; in comparison with the composition 3, the composition,**P<0.05,*P<0.01; in comparison with the composition 4, the composition,θP<0.01; in comparison with the composition No. 5,×P<0.05; in comparison with VC, the comparison is made,#P<0.01。
as can be seen from table 7, each composition had hydroxyl radical scavenging activity, and composition 6 had the highest hydroxyl radical scavenging rate, which was higher than VC powder. Compared with the compositions 1, 2, 3 and 4 respectively, the hydroxyl radical scavenging rate of the composition 5 is obviously improved, which shows that the activity of scavenging hydroxyl radicals is improved after the combination of the 4 natural plant essential oils, and the activity is reduced when any one of the 4 natural plant essential oils is absent. The nanocapsule prepared from composition 5 has significantly higher hydroxyl radical scavenging rate than composition 5, because essential oil in compositions 1-5 is volatile and has short action time, and the prepared nanocapsule can overcome the defect and improve the hydroxyl radical scavenging activity.
3. And (4) conclusion: the compound essential oil and the nanocapsules thereof have high hydroxyl radical scavenging activity, which shows that the compound essential oil has strong oxidation resistance, and can smooth skin and prevent wrinkles after long-term use.
Test example 3
The oxygen free radical scavenging activity test of the compound essential oil of the invention comprises:
1. materials and methods
1.1 test materials
Suaeda salsa seed oil, pepper seed oil, citrus seed oil and Chinaberry fruit oil are respectively prepared according to the embodiment. Preparing compound essential oil (composition 1, lacking Chinaberry fruit oil) of Suaeda glauca seed oil, pricklyash peel seed oil and citrus seed oil according to the formula proportion; compound essential oil of suaeda salsa seed oil, pepper seed oil and chinaberry seed oil (composition 2, lacking of citrus seed oil); compound essential oil of suaeda glauca seed oil, citrus seed oil and chinaberry seed oil (composition 3, lacking of pepper seed oil); compound essential oil of pricklyash peel seed oil, orange seed oil and chinaberry seed oil (composition 4, lacking suaeda salsa seed oil); the essential oil missing in the composition is replaced by peanut oil with equal proportion. The invention is compounded with essential oil (composition 5); the compound essential oil nanocapsule (composition 6, nanocapsule prepared from composition 5); positive control vitamin c (vc) in water.
1.2 test methods
Adopts pyrogallol autoxidation method.
(1) Preparing and measuring pyrogallol solution: adding 2.95mL of Tris-HCl buffer solution into a quartz cuvette, adding about 0.50mL of pyrogallol solution, quickly and uniformly mixing, starting timing, measuring the absorbance value at 325nm, reading the value A once every 30s, stopping reading when 300 seconds, and carrying out parallel measurement for 3 times in each group;
(2) preparation and determination of sample solution: adding 0.50mL of sample solution into a quartz cuvette, sequentially adding 2.90mL of Tris-HCl buffer solution and 0.50mL of pyrogallol solution, quickly and uniformly mixing, starting timing, measuring the absorbance value at 325nm, reading the value A once every 30s, stopping reading when 300 seconds, and carrying out parallel measurement for 3 times in each group;
(3) preparing and measuring a VC solution: adding 0.50mLVC solution into a quartz cuvette, sequentially adding 2.90mLTris-HCl buffer solution and 0.50mL pyrogallol solution, quickly and uniformly mixing, starting timing, measuring the absorbance value at 325nm, reading the A value once every 30s, stopping reading when 300 seconds, and carrying out parallel measurement on each group for 3 times;
calculating the formula: clearance rate ([ Delta ] A)0-△AS)/△A0 x 100%;
In the formula, Delta A0Is the difference in absorbance at 325nm between 300s and 30s for the pyrogallol solution; delta ASIs the difference in absorbance at 325nm between 300s and 30s for the sample solution or VC solution.
2. Results and analysis
The oxygen radical clearance of each composition is shown in table 8.
In comparison with the composition 1, the composition,△P<0.01; in comparison with the composition 2, the present inventors have shown that,▲P<0.01,▲▲P<0.01; in comparison with the composition 3, the composition,*P<0.01; in comparison with the composition 4, the composition,θP<0.01; in comparison with the composition No. 5,×P<0.01; in comparison with VC, the comparison is made,#P<0.01。
from table 7, each composition had oxygen radical scavenging activity, and composition 6 had the highest oxygen radical scavenging rate, comparable to VC. Compared with the compositions 1, 2, 3 and 4 respectively, the oxygen radical clearance rate of the composition 5 is obviously increased, which shows that the activity of the combination of the 4 natural plant essential oils is increased, and the activity of the combination is reduced if any one of the compositions is absent. The composition 5 can be used to prepare nanocapsules, which have higher oxygen free radical scavenging rate than composition 5, because essential oils in compositions 1-5 are volatile and have short action time, and the prepared nanocapsules can overcome the defect and improve oxygen free radical scavenging activity.
3. And (4) conclusion: the compound essential oil and the nanocapsule thereof have high oxygen radical scavenging activity, which shows that the compound essential oil has strong oxidation resistance, and can smooth skin and prevent wrinkles after long-term use.
Test example 4
The reducing power of the compound essential oil is measured and tested as follows:
1. materials and methods
1.1 test materials
Suaeda salsa seed oil, pepper seed oil, citrus seed oil and Chinaberry fruit oil are respectively prepared according to the embodiment. Preparing compound essential oil (composition 1, lacking Chinaberry fruit oil) of Suaeda glauca seed oil, pricklyash peel seed oil and citrus seed oil according to the formula proportion; compound essential oil of suaeda salsa seed oil, pepper seed oil and chinaberry seed oil (composition 2, lacking of citrus seed oil); compound essential oil of suaeda glauca seed oil, citrus seed oil and chinaberry seed oil (composition 3, lacking of pepper seed oil); compound essential oil of pricklyash peel seed oil, orange seed oil and chinaberry seed oil (composition 4, lacking suaeda salsa seed oil); the invention is compounded with essential oil (composition 5); the compound essential oil nanocapsule of the invention (composition 6, nanocapsule prepared from composition 5).
1.2 test methods
The reducing power is measured by adopting a potassium ferricyanide reduction method, a sample, 1 percent of potassium ferricyanide and 1mL of 0.2mol/L phosphate buffer solution are sequentially added into a test tube, the mixture is bathed in water at 50 ℃ for 25min, then the mixture is rapidly cooled, the temperature is reduced to 15 ℃, 10 percent of trichloroacetic acid solution is added, the mixture is evenly mixed and centrifuged, 1mL of supernatant is taken into the test tube, and 1mL of water and 0.4mL of 1 percent of FeCl are added3Standing for 10min at room temperature after uniform mixing, and finally measuring the absorbance value at the wavelength of 700nm by using an enzyme-labeling instrument, wherein each group is measured in parallel for 3 times, and the higher the absorbance is, the stronger the reduction capability is.
2. Results and analysis
The results of the reduction power measurement of each composition are shown in Table 9.
In comparison with the composition 1, the composition,△P<0.01; in comparison with the composition 2, the present inventors have shown that,▲P<0.01; and combinations ofThe comparison of the substance 3 is carried out,*P<0.01; in comparison with the composition 4, the composition,θP<0.01; in comparison with the composition No. 5,×P<0.01。
as can be seen from Table 8, each of the compositions had the highest reducing activity, and composition 6 had the highest reducing activity. The increased reducing activity of composition 5 compared to compositions 1, 2, 3, and 4, respectively, indicates that the activity of the combination of 4 natural plant essential oils is increased and decreased in the absence of any one. The nanocapsule prepared from composition 5 has significantly higher reduction activity than composition 5, because the essential oils in compositions 1-5 are volatile and have short action time, and the nanocapsule prepared from composition 5 can overcome the defect and improve the reduction activity.
3. And (4) conclusion: the compound essential oil and the nanocapsules thereof have high reducing power, which shows that the compound essential oil has strong oxidation resistance, and can smooth skin and prevent wrinkles after long-term use.
Test example 5
Human body efficacy evaluation test of whitening, anti-wrinkle and moisturizing water, milk and cream
1. Test subjects: 20 (5 men, 15 women) volunteers 30-45 years old who were healthy and had no history of cosmetic allergy.
2. The test method comprises the following steps: the skin elasticity, melanin content and moisture content were measured using an MPA580 instrument, the average of the skin elasticity and melanin content of 20 volunteers who did not use the cosmetic of the present invention was used as a blank control, the measurement was performed once a week for 3 weeks, and the results were finally analyzed. 3. Results and analysis
The skin elasticity results are shown in Table 10.
TABLE 10 measurement results of skin elasticity
The melanin content results are shown in table 11.
TABLE 11 melanin content
The moisture content results are shown in Table 12.
TABLE 12 moisture content
From tables 10-12, after the skin whitening, anti-wrinkle and moisturizing lotion, cream and cream are used for 1 week, the elasticity and moisture content of the skin are obviously increased, the melanin content of the skin is obviously reduced, the effect is gradually increased in the using process, after the skin whitening, anti-wrinkle and moisturizing lotion, cream and cream are used for 3 weeks, the elasticity of the skin is increased by 24.66%, the melanin content is reduced by 18.83%, the moisture content is increased by 32.85%, and no local skin allergy, inflammatory reaction and the like are seen, so that the series of cosmetics are safe and effective.
4. And (4) conclusion: the detection result shows that the whitening anti-wrinkle moisturizing lotion, cream and cream have the effects of enhancing skin elasticity, inhibiting melanin and increasing skin water content, can whiten skin, resist wrinkle and delay aging after long-term use, and has no toxic or side effect.
Claims (5)
1. The compound essential oil is characterized by being prepared by combining suaeda salsa seed oil, zanthoxylum bungeanum seed oil, citrus seed oil and szechwan chinaberry fruit oil, wherein the ratio of the suaeda salsa seed oil to the zanthoxylum bungeanum seed oil to the citrus seed oil to the szechwan chinaberry fruit oil is 3-4: 1-2: 2-3: 5-6;
the preparation method of the suaeda salsa seed oil comprises the following steps:
taking suaeda salsa seeds, crushing, sieving, placing in a charging basket of microwave dynamic extraction equipment, adding 60 times of water, soaking for 45min at room temperature, setting the microwave power to 287W, performing microwave radiation for 30min, connecting a volatile oil separator on the microwave extraction equipment, and collecting distilled essential oil to obtain the suaeda salsa seed oil.
The preparation method of the pricklyash seed oil comprises the following steps:
pulverizing semen Zanthoxyli, sieving, and placing in supercritical CO2Adding 70% ethanol in an amount which is 2.5 times that of the extraction kettle, soaking for 150min at room temperature, wherein the extraction conditions are as follows: the extraction pressure is 40MPaThe extraction temperature is 40 ℃, the extraction time is 3h, CO2The flow rate was 20 kg/h. Filtering the extractive solution, recovering 70% ethanol with rotary evaporator, and volatilizing to obtain oleum Zanthoxyli Bungeani.
The preparation method of the citrus seed oil comprises the following steps:
pulverizing citrus seeds, sieving, and placing in supercritical CO2Adding 3 times of 70% ethanol into an extraction kettle, soaking for 150min at room temperature, wherein the extraction conditions are as follows: the extraction pressure is 35MPa, the extraction temperature is 45 ℃, the extraction time is 3h, and CO is2The flow rate was 25 kg/h. Filtering the extractive solution, recovering 70% ethanol with rotary evaporator, and volatilizing to obtain citrus seed oil.
The preparation method of the szechwan chinaberry fruit oil comprises the following steps:
pulverizing fructus Toosendan, sieving, placing in round bottom flask, adding 10 times of distilled water, adjusting pH to 4.5 with hydrochloric acid, adding 1% cellulase into container, slightly stirring, placing in water bath, performing enzymolysis at 50 deg.C for 35min, performing steam distillation, installing volatile oil extractor, heating to boil, distilling for 2.5 hr, and collecting distilled essential oil to obtain fructus Toosendan oil.
The suaeda salsa seed oil, the pepper seed oil, the citrus seed oil and the szechwan chinaberry fruit oil are selected according to the proportion and are uniformly mixed to obtain the compound essential oil.
2. The compound essential oil of claim 1, wherein the ratio of the suaeda salsa seed oil, the pepper seed oil, the citrus seed oil and the chinaberry seed oil is 3:1:2: 5.
3. A nanocapsule containing compound essential oil, which is characterized in that the nanocapsule containing 33% of the compound essential oil is prepared from the compound essential oil according to claim 1 by a reverse emulsification method.
4. The compound essential oil nanocapsule of claim 3, wherein the preparation method of the compound essential oil nanocapsule comprises:
taking 0.1g of acetyl chitosan, placing the acetyl chitosan in a beaker, and adding deionized water to 10mL to obtain an acetyl chitosan solution for later use; taking 10g of sodium alginate, placing the sodium alginate in a beaker, adding 10mL of compound essential oil, carrying out ultrasonic emulsification completely, slowly dropwise adding 0.5mol/LNaOH to adjust the pH value to 7.5 to obtain sodium alginate nanocapsules, washing and centrifuging the sodium alginate nanocapsules, adding the sodium alginate nanocapsules into an acetyl chitosan solution, and carrying out magnetic stirring for 3 hours to obtain the compound essential oil nanocapsules.
5. The application of the compound essential oil nanocapsule is characterized in that the compound essential oil nanocapsule of claim 3 is added into a whitening anti-wrinkle cosmetic according to the mass of the compound essential oil nanocapsule accounting for 10-15% of the mass of the whitening anti-wrinkle cosmetic;
the whitening anti-wrinkle cosmetic prepared from the compound essential oil nanocapsule has no special limitation on the selection of dosage form and matrix, and can be prepared into whitening anti-wrinkle moisturizing lotion, whitening anti-wrinkle milk, whitening anti-wrinkle cream and the like.
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