CN115154401A - Anti-inflammatory soothing emulsion and preparation method thereof - Google Patents
Anti-inflammatory soothing emulsion and preparation method thereof Download PDFInfo
- Publication number
- CN115154401A CN115154401A CN202210876983.XA CN202210876983A CN115154401A CN 115154401 A CN115154401 A CN 115154401A CN 202210876983 A CN202210876983 A CN 202210876983A CN 115154401 A CN115154401 A CN 115154401A
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Abstract
The invention relates to the technical field of cosmetics, and discloses an anti-inflammatory soothing emulsion and a preparation method thereof, wherein the emulsion is an oil-in-water type emulsified cosmetic and comprises a water phase and an oil phase, and the oil phase accounts for 12-16% of the total mass of the emulsion; the water phase comprises 100:0.2 to 0.5:10 to 15: 3-8 parts of water, sodium hyaluronate, glycerol and sodium carboxymethyl starch modified polyethylene glycol; the oil phase comprises the following components in a mass ratio of 5-15: 2 to 7:1 to 3: 10-22 of luteolin, panthenol, honey extract and oil component. The skin moisturizing cream is characterized in that the skin is firstly endowed with water type refreshing feeling by an oil-in-water type emulsification mode, and then the main anti-allergy and anti-inflammation effects of water-oil balance and oil phase are combined, so that the skin moisturizing cream has a long-acting moisturizing effect and is safe and reliable to use for a long time.
Description
Technical Field
The invention belongs to the technical field of cosmetics, and particularly relates to an anti-inflammatory soothing emulsion and a preparation method thereof.
Background
Sensitive skin affects the quality of life of people to a great extent. Sensitive skin usually has skin allergy symptoms and discomfort such as skin redness, itching, dryness, stabbing pain, burning, tightness and the like, and although a specific allergen is difficult to find, the common thing is that the skin barrier is damaged, namely the skin surface loses normal protective function and loses skin moisture, so that the skin is dry, desquamation or pruritus. Meanwhile, allergens such as germs, pollen, chemicals and the like on the surface of the skin easily enter the interior of the skin through the damaged skin barrier, thereby further triggering the skin inflammatory reaction. At present, most of the effective components used in cosmetics for treating or relieving skin allergy are chemical reagents with anti-inflammation or anti-irritation functions, but cosmetics using chemical substances as main raw materials cannot meet the requirements of people on natural cosmetics with small side effects, and researches mainly using plant and traditional Chinese medicine extracts are gradually hot. Moreover, these cosmetics often neglect to repair the skin barrier function, and thus the long-term use of the above products results in thinning of the epidermis and dermis, impaired skin barrier function, skin atrophy, telangiectasia and the like. In conclusion, such a vicious circle can bring endless troubles to modern beauty-conscious women.
For example, the chinese invention patent CN202010777565.6 discloses an anti-inflammatory acne-removing cosmetic composition and a preparation method thereof, which comprises the following components in percentage by weight: 10-15 parts of sorbitan olivate, 25-40 parts of glycerol, 60-80 parts of deionized water, 3-5 parts of Hibiscus mutabilis extract, 1-3 parts of pollen pini, 1-2 parts of dried lily and 8-13 parts of cistanche tubulosa polysaccharide; the preparation method comprises stirring sorbitan olivine oleate, glycerol and deionized water to obtain transparent gel matrix as carrier, adding Hibiscus Mutabilis extract, pollen Pini, dried Bulbus Lilii, semen Ginkgo extract and cistanche tubulosa polysaccharide as effective components into the carrier, and stirring with stirring device. The cosmetic composition can effectively resist inflammation and remove acnes, but the repair of skin barriers is not considered, the effective soothing effect on the skin is not achieved, the skin function is damaged, and the cosmetic composition has larger side effects after long-term use.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide the anti-inflammatory soothing emulsion and the preparation method thereof.
In order to achieve the aim, the invention provides an anti-inflammatory soothing emulsion which is an oil-in-water type emulsified cosmetic and comprises a water phase and an oil phase, wherein the oil phase accounts for 12-16% of the total mass of the emulsion; the water phase comprises 100:0.2 to 0.5: 10-15: 3-8 parts of water, sodium hyaluronate, glycerol and sodium carboxymethyl starch modified polyethylene glycol; the oil phase comprises the following components in a mass ratio of 5-15: 2 to 7:1 to 3: 10-22 of luteolin, panthenol, honey extract and oil component.
The invention combines anti-allergy and anti-inflammation with skin barrier repair, more importantly, the skin is effectively relieved, the skin is firstly endowed with water type fresh touch by an oil-in-water type emulsification mode, and then the main anti-allergy and anti-inflammation effects endowed by water-oil balance and an oil phase are combined, so that the stimulation effect on the skin is avoided, and the long-term use is safe and reliable. The components such as sodium hyaluronate and glycerin in the water phase can help to thicken the horny layer, improve the tolerance of the skin, maintain the moisture of the skin and improve the stability of the skin firstly. The cosmetic firstly relieves the skin by virtue of the stabilizing effect of the water phase, and then performs targeted relief by utilizing the anti-inflammatory and anti-allergy effects of the oil phase, so that the cosmetic can quickly promote the healing of the skin and promote the regeneration, activity and metabolism. Luteolin is a natural plant extract, has pharmacological activities of anti-inflammatory and anti-allergic traditional Chinese medicines, is also called vitamin B5, and can effectively relieve skin irritation. The honey extract is rich in amino acids, oligosaccharides, organic acids, vitamins, calcium, magnesium, sodium, potassium and other minerals, and can supplement natural moisturizing factors lost from human body, enhance water absorption of stratum corneum, lock water, and restore skin elasticity and softness. Sensitive skin firstly needs to supplement water loss of skin, but the water phase cannot be effectively moisturized only by enhancing, more importantly, the water-oil balance is maintained.
More preferably, the oil component includes, by mass, 0.5 to 3:2 to 8:0.5 to 2: 1-5 of hydrophilic modified wild soybean oil, shea butter, ester oil and ethyl cellulose.
The oil components including wild soybean oil, shea butter and ester oil are high in safety, can effectively wrap anti-inflammatory and anti-allergy components, and have no irritation to skin. Ethylcellulose has water insolubility and serves as a framework material, so that the oil phase can be stably dispersed in the water phase. In addition, the wild soybean oil is a good humectant and antioxidant, can be used as a growth factor of epidermis, and can nourish skin, relieve dryness and roughness, make skin smooth and tender for a long time, and make skin soft. The wild soybean oil is partially grafted and hydrophilically modified, so that the affinity between the oil component and the anti-inflammatory active ingredient is better, the wild soybean oil can be stably combined with a water phase, and the emulsification effect of the oil-in-water type cosmetic is better when the oil-in-water type cosmetic is used.
Further preferably, the preparation method of the hydrophilic modified wild soybean oil comprises the following steps: adding wild soybean oil into toluene, mixing, heating to 40-50 ℃, and dropwise adding a mixed solution of acrylic acid, benzoyl peroxide and ethanol under the stirring condition; after the dropwise addition is finished, continuously heating to 70-80 ℃, stirring and reacting for 5-7 h, and after the reaction is finished, washing with water and carrying out reduced pressure distillation to obtain hydrophilic modified wild soybean oil; the weight ratio of the wild soybean oil to the toluene to the acrylic acid to the benzoyl peroxide to the ethanol is 10:20 to 30:1 to 4:0.05 to 0.1:5 to 10.
The wild soybean oil contains abundant unsaturated fatty acid, can be subjected to graft hydrophilic modification with acrylic acid, but needs to control the graft modification ratio of the acrylic acid to balance hydrophilicity and hydrophobicity, otherwise is not beneficial to forming an oil-in-water structure, and has poor refreshing and relieving effects on skin.
Further preferably, the ester oil is one or more of isopropyl myristate, cetyl octanoate, octyl dodecyl myristate, isopropyl palmitate, butyl stearate, isocetyl stearate, diisostearyl malate, sorbitan olive oleate, cetyl palmitate, sorbitan olive oleate.
Further preferably, the preparation method of the oil phase comprises the following steps:
(1) Adding luteolin and sodium hydroxide into N, N-dimethylformamide, then placing the N, N-dimethylformamide into an ice water bath, and dropwise adding acetylsalicyloyl chloride, wherein the mass ratio of luteolin to acetylsalicyloyl chloride is (5-15): 8 to 12; after the dropwise addition, taking out the mixture from the ice water bath, adding a mixture of panthenol, triethylamine and dichloromethane, stirring and reacting at 20-30 ℃ for 30-50 min, then adding sodium bicarbonate and honey extract, stirring and mixing for 20-40 min, and then carrying out reduced pressure distillation to obtain a mixture A;
(2) Mixing the hydrophilic modified wild soybean oil, shea butter, ester oil and ethyl cellulose to obtain oil component;
(3) And dropwise adding the mixture A into the oil component at a dropping speed of 0.5-1 g/min, and obtaining an oil phase after dropwise adding.
During the preparation of the oil phase, it is important to control the order of addition of the ingredients so as to form a structure that locks the anti-inflammatory ingredient into the oil phase. Moreover, the combination of luteolin and panthenol with acetylsalicyloyl chloride can improve the relieving effect of the anti-inflammatory component, and the acetylsalicyloyl chloride also has certain anti-inflammatory effect and can enhance the anti-inflammatory relieving effect by the moisturizing effect of the honey extract. However, the speed of adding the mixture A dropwise into the mixture B also affects the dispersion and combination effect of the anti-inflammatory component in the oil component, and further affects the anti-inflammatory and soothing effect of the cosmetic.
More preferably, in the step (1), the ratio of the addition amounts of luteolin, sodium hydroxide and N, N-dimethylformamide is 1g: 0.1-0.2 g:7mL.
More preferably, in step (1), the ratio of the amounts of panthenol, triethylamine, dichloromethane, and sodium hydrogen carbonate added is 1g: 0.5-0.8 g:3mL of: 0.2 to 0.4g.
Further preferably, the preparation method of the sodium carboxymethyl starch modified polyethylene glycol comprises the following steps: adding polyethylene glycol with the molecular weight of 1000-2000 into water, uniformly mixing, adding a mixed solution of sodium carboxymethyl starch, sodium dodecyl sulfate and ethanol, and stirring and mixing for 1-2 hours, wherein the mass ratio of the polyethylene glycol to the sodium carboxymethyl starch is 10; then adding p-toluenesulfonic acid and glacial acetic acid, and heating to reflux reaction for 3-5 h; after the reaction is finished, precipitating by using cooled anhydrous ether, and drying to obtain the sodium carboxymethyl starch modified polyethylene glycol.
The polyethylene glycol is a water-soluble component, has good lubricity and moisture retention, is modified by the sodium carboxymethyl starch, and has a slow release effect on the anti-inflammatory oil phase component by utilizing the water-soluble expansibility of the sodium carboxymethyl starch, so that the water phase can better play a role in enhancing the skin barrier, the stimulation to the skin can be better avoided, and the safety is improved.
Further preferably, the ratio of the addition amount of the polyethylene glycol to the water is 1g: 10-12 mL; the mass ratio of the sodium carboxymethyl starch, the sodium dodecyl sulfate, the ethanol, the p-toluenesulfonic acid and the glacial acetic acid is 10:0.1 to 0.3:30 to 40:0.05 to 0.1:0.2 to 0.6.
The invention also provides a preparation method of the anti-inflammatory soothing emulsion, which comprises the following steps: respectively and uniformly mixing the water phase and the oil phase, adding the water phase into a high-speed stirrer, adding the oil phase at the rotating speed of 500-700 r/min, adding a pH regulator to regulate the pH to 5.5-6.0 after the addition is finished, homogenizing at the rotating speed of 7000-8000 r/min for 10-20 min, cooling to room temperature, standing, and filling to obtain the emulsion.
The oil phase is dripped into the water phase and then is quickly homogenized and stirred, so that the anti-inflammatory functional components can be uniformly dispersed, and the quality of the emulsion is ensured.
Compared with the prior art, the invention has the following advantages: the skin is endowed with water type refreshing feeling through an oil-in-water emulsification mode, and then the main anti-allergy and anti-inflammation effects endowed by water-oil balance and an oil phase are combined, so that the stimulation effect on the skin is avoided, and the long-term use is safe and reliable; the components such as sodium hyaluronate and glycerin in the water phase can help to thicken the horny layer, improve the skin tolerance and repair the skin barrier; the oil phase wraps the anti-inflammatory and anti-allergy effective components with oil for targeted relief, and the oil phase still contains moisturizing factors, so that the oil phase has a long-acting moisturizing effect, can promote skin healing more quickly, and promotes regeneration, activity and metabolism.
Detailed Description
The invention is further illustrated with reference to specific examples. It should be understood that the specific embodiments described herein are illustrative only and are not limiting upon the scope of the invention. The experimental procedures in the following examples are conventional unless otherwise specified. The test materials used in the following examples are all commercially available products unless otherwise specified.
Example 1
An anti-inflammatory soothing emulsion comprises a water phase and an oil phase, wherein the oil phase accounts for 14% of the total mass of the emulsion.
The preparation method of the water phase comprises the following steps:
(a) Preparing sodium carboxymethyl starch modified polyethylene glycol: adding 10g of polyethylene glycol with the average molecular weight of 1400 into 110mL of water, and uniformly mixing; then adding a mixed solution of 2.2g of sodium carboxymethyl starch, 0.04g of sodium dodecyl sulfate and 8g of ethanol, and stirring and mixing for 1 hour; then adding 0.012g of p-toluenesulfonic acid and 0.07g of glacial acetic acid, and heating to reflux reaction for 3.5h; after the reaction is finished, precipitating by using cooled anhydrous ether, and drying to obtain the sodium carboxymethyl starch modified polyethylene glycol.
(b) And (2) mixing the following components in percentage by mass as 100:0.3:12:5, mixing the water, the sodium hyaluronate, the glycerol and the sodium carboxymethyl starch modified polyethylene glycol, wherein the sodium hyaluronate is small-molecule sodium hyaluronate (the molecular weight is 20-40 ten thousand daltons), and uniformly mixing to obtain a water phase.
The preparation method of the oil phase comprises the following steps:
(1) Adding 10g of luteolin and 1.1g of sodium hydroxide into 70mLN and N-dimethylformamide, placing the mixture into an ice water bath, and dropwise adding 9.5g of acetylsalicyloyl chloride; after the dropwise addition, taking out the mixture from the ice-water bath, adding a mixture of 3g of panthenol, 1.8g of triethylamine and 9mL of dichloromethane, stirring the mixture at 25 ℃ for 40min for reaction, adding 0.8g of sodium bicarbonate and 2g of honey extract, stirring the mixture for 40min, and then carrying out reduced pressure distillation to obtain a mixture A;
(2) Preparing hydrophilic modified wild soybean oil: adding 10g of wild soybean oil into 25g of toluene, mixing, heating to 40 ℃, and dropwise adding a mixed solution of 3.3g of acrylic acid, 0.05g of benzoyl peroxide and 8g of ethanol under the stirring condition; after the dropwise addition is finished, continuously heating to 80 ℃, stirring and reacting for 5.5 hours, and after the reaction is finished, washing with water and distilling under reduced pressure to obtain hydrophilic modified wild soybean oil;
(3) Mixing the components in a mass ratio of 1.5:5:1:3, mixing the hydrophilic modified wild soybean oil, shea butter, isocetyl stearate and ethyl cellulose to obtain oil;
(4) Dropwise adding the mixture A into 18g of oil component at a dropwise adding speed of 0.7g/min, stirring while dropwise adding, and obtaining an oil phase after dropwise adding.
The preparation method of the emulsion comprises the following steps:
respectively and uniformly mixing the water phase and the oil phase, adding the water phase into a high-speed stirrer, adding the oil phase at the rotating speed of 600r/min, adding a pH regulator to regulate the pH to 5.8 after the addition is finished, homogenizing at the rotating speed of 7500r/min for 20min, cooling to room temperature, standing, and filling to obtain the emulsion.
Example 2
An anti-inflammatory soothing emulsion comprises a water phase and an oil phase, wherein the oil phase accounts for 16% of the total mass of the emulsion.
The preparation method of the water phase comprises the following steps:
(a) Preparing sodium carboxymethyl starch modified polyethylene glycol: adding 10g of polyethylene glycol with the average molecular weight of 1400 into 110mL of water, and uniformly mixing; then adding a mixed solution of 2.2g of sodium carboxymethyl starch, 0.04g of sodium dodecyl sulfate and 8g of ethanol, and stirring and mixing for 1 hour; then adding 0.012g of p-toluenesulfonic acid and 0.07g of glacial acetic acid, and heating to reflux reaction for 3.5h; after the reaction is finished, precipitating by using cooled anhydrous ether, and drying to obtain the sodium carboxymethyl starch modified polyethylene glycol.
(b) And (2) mixing the following components in percentage by mass as 100:0.3:12:5, mixing the water, the sodium hyaluronate, the glycerol and the sodium carboxymethyl starch modified polyethylene glycol, wherein the used sodium hyaluronate is small-molecule sodium hyaluronate (the molecular weight is 20-40 ten thousand daltons), and uniformly mixing to obtain a water phase.
The preparation method of the oil phase comprises the following steps:
(1) Adding 10g of luteolin and 1.1g of sodium hydroxide into 70mLN and N-dimethylformamide, placing the mixture into an ice water bath, and dropwise adding 9.5g of acetylsalicyloyl chloride; after the dropwise addition, taking out the mixture from the ice-water bath, adding a mixture of 3g of panthenol, 1.8g of triethylamine and 9mL of dichloromethane, stirring the mixture at 25 ℃ for 40min for reaction, adding 0.8g of sodium bicarbonate and 2g of honey extract, stirring the mixture for 40min, and then carrying out reduced pressure distillation to obtain a mixture A;
(2) Preparing hydrophilic modified wild soybean oil: adding 10g of wild soybean oil into 25g of toluene, mixing, heating to 45 ℃, and dropwise adding a mixed solution of 4g of acrylic acid, 0.08g of benzoyl peroxide and 8g of ethanol under the condition of stirring; after the dropwise addition is finished, continuously heating to 80 ℃, stirring and reacting for 6.5 hours, and after the reaction is finished, washing with water and distilling under reduced pressure to obtain hydrophilic modified wild soybean oil;
(3) Mixing the components in a mass ratio of 2:5:1.5:3, mixing the hydrophilic modified wild soybean oil, shea butter, isocetyl stearate and ethyl cellulose to obtain oil;
(4) Dropwise adding the mixture A into 18g of oil component at a dropwise adding speed of 0.5g/min, stirring while dropwise adding, and obtaining an oil phase after dropwise adding.
The preparation method of the emulsion comprises the following steps:
respectively mixing the water phase and the oil phase uniformly, adding the water phase into a high-speed stirrer, adding the oil phase at the rotating speed of 700r/min, adding a pH regulator to regulate the pH to 5.8 after the addition is finished, homogenizing at the rotating speed of 7500r/min for 20min, cooling to room temperature, standing, and filling to obtain the emulsion.
Example 3
An anti-inflammatory soothing emulsion comprises a water phase and an oil phase, wherein the oil phase accounts for 14% of the total mass of the emulsion.
The preparation method of the water phase comprises the following steps:
(a) Preparing sodium carboxymethyl starch modified polyethylene glycol: adding 10g of polyethylene glycol with the average molecular weight of 2000 into 120mL of water, and uniformly mixing; then adding a mixed solution of 2g of sodium carboxymethyl starch, 0.04g of sodium dodecyl sulfate and 8g of ethanol, and stirring and mixing for 2 hours; then adding 0.01g of p-toluenesulfonic acid and 0.1g of glacial acetic acid, and heating to reflux reaction for 4.5h; after the reaction is finished, precipitating by using cooled anhydrous ether, and drying to obtain the sodium carboxymethyl starch modified polyethylene glycol.
(b) And (2) mixing the following components in percentage by mass as 100:0.3:14:6, mixing the water, the sodium hyaluronate, the glycerol and the sodium carboxymethyl starch modified polyethylene glycol, wherein the used sodium hyaluronate is small-molecule sodium hyaluronate (the molecular weight is 20-40 ten thousand daltons), and uniformly mixing to obtain a water phase.
The preparation method of the oil phase comprises the following steps:
(1) Adding 10g of luteolin and 1.1g of sodium hydroxide into 70mLN and N-dimethylformamide, placing the mixture into an ice water bath, and dropwise adding 9.5g of acetylsalicyloyl chloride; after the dropwise addition, taking out the mixture from the ice-water bath, adding a mixture of 3g of panthenol, 1.8g of triethylamine and 9mL of dichloromethane, stirring the mixture at 25 ℃ for 40min for reaction, adding 0.8g of sodium bicarbonate and 2g of honey extract, stirring the mixture for 40min, and then carrying out reduced pressure distillation to obtain a mixture A;
(2) Preparing hydrophilic modified wild soybean oil: adding 10g of wild soybean oil into 25g of toluene, mixing, heating to 40 ℃, and dropwise adding a mixed solution of 3.3g of acrylic acid, 0.05g of benzoyl peroxide and 8g of ethanol under the stirring condition; after the dropwise addition is finished, continuously heating to 80 ℃, stirring and reacting for 5.5 hours, and after the reaction is finished, washing with water and distilling under reduced pressure to obtain hydrophilic modified wild soybean oil;
(3) Mixing the components in a mass ratio of 1.5:5:1:3, mixing the hydrophilic modified wild soybean oil, shea butter, isocetyl stearate and ethyl cellulose to obtain oil;
(4) And dropwise adding the mixture A into 18g of oil component at a dropwise adding speed of 0.7g/min while stirring, and obtaining an oil phase after dropwise adding.
The preparation method of the emulsion comprises the following steps:
respectively and uniformly mixing the water phase and the oil phase, adding the water phase into a high-speed stirrer, adding the oil phase at the rotating speed of 600r/min, adding a pH regulator to regulate the pH to 5.9 after the addition is finished, homogenizing at the rotating speed of 7500r/min for 20min, cooling to room temperature, standing, and filling to obtain the emulsion.
Comparative example 1
Luteolin was not added to the emulsion, and the remaining ingredients and preparation method were the same as in example 1.
An anti-inflammatory soothing emulsion comprises a water phase and an oil phase, wherein the oil phase accounts for 14% of the total mass of the emulsion.
The preparation method of the water phase comprises the following steps:
(a) Preparing sodium carboxymethyl starch modified polyethylene glycol: adding 10g of polyethylene glycol with the average molecular weight of 1400 into 110mL of water, and uniformly mixing; then adding a mixed solution of 2.2g of sodium carboxymethyl starch, 0.04g of sodium dodecyl sulfate and 8g of ethanol, and stirring and mixing for 1 hour; then adding 0.012g of p-toluenesulfonic acid and 0.07g of glacial acetic acid, and heating to reflux reaction for 3.5h; after the reaction is finished, precipitating by using cooled anhydrous ether, and drying to obtain the sodium carboxymethyl starch modified polyethylene glycol.
(b) And (2) mixing the following components in percentage by mass as 100:0.3:12:5, mixing the water, the sodium hyaluronate, the glycerol and the sodium carboxymethyl starch modified polyethylene glycol, wherein the sodium hyaluronate is small-molecule sodium hyaluronate (the molecular weight is 20-40 ten thousand daltons), and uniformly mixing to obtain a water phase.
The preparation method of the oil phase comprises the following steps:
(1) Adding 1.1g of sodium hydroxide into 70mLN and N-dimethylformamide, then placing the mixture into an ice water bath, and dropwise adding 9.5g of acetylsalicyloyl chloride; after the dropwise addition, taking out the mixture from the ice-water bath, adding a mixture of 3g of panthenol, 1.8g of triethylamine and 9mL of dichloromethane, stirring the mixture at 25 ℃ for 40min for reaction, adding 0.8g of sodium bicarbonate and 2g of honey extract, stirring the mixture for 40min, and then carrying out reduced pressure distillation to obtain a mixture A;
(2) Preparing hydrophilic modified wild soybean oil: adding 10g of wild soybean oil into 25g of toluene, mixing, heating to 40 ℃, and dropwise adding a mixed solution of 3.3g of acrylic acid, 0.05g of benzoyl peroxide and 8g of ethanol under the stirring condition; after the dropwise addition is finished, continuously heating to 80 ℃, stirring and reacting for 5.5 hours, and after the reaction is finished, washing with water and distilling under reduced pressure to obtain hydrophilic modified wild soybean oil;
(3) Mixing the components in a mass ratio of 1.5:5:1:3, mixing the hydrophilic modified wild soybean oil, shea butter, isocetyl stearate and ethyl cellulose to obtain oil;
(4) Dropwise adding the mixture A into 18g of oil component at a dropwise adding speed of 0.7g/min, stirring while dropwise adding, and obtaining an oil phase after dropwise adding.
The preparation method of the emulsion comprises the following steps:
respectively mixing the water phase and the oil phase uniformly, adding the water phase into a high-speed stirrer, adding the oil phase at the rotating speed of 600r/min, adding a pH regulator to regulate the pH to 5.8 after the addition is finished, homogenizing at the rotating speed of 7500r/min for 20min, cooling to room temperature, standing, and filling to obtain the emulsion.
Comparative example 2
The components of mixture a in the emulsion were prepared by direct mixing, the remaining components and the preparation method were the same as in example 1.
An anti-inflammatory soothing emulsion comprises a water phase and an oil phase, wherein the oil phase accounts for 14% of the total mass of the emulsion.
The preparation method of the water phase comprises the following steps:
(a) Preparing sodium carboxymethyl starch modified polyethylene glycol: adding 10g of polyethylene glycol with the average molecular weight of 1400 into 110mL of water, and uniformly mixing; then adding a mixed solution of 2.2g of sodium carboxymethyl starch, 0.04g of sodium dodecyl sulfate and 8g of ethanol, and stirring and mixing for 1 hour; then adding 0.012g of p-toluenesulfonic acid and 0.07g of glacial acetic acid, and heating to reflux reaction for 3.5h; after the reaction is finished, precipitating by using cooled anhydrous ether, and drying to obtain the sodium carboxymethyl starch modified polyethylene glycol.
(b) And (2) mixing the following components in percentage by mass as 100:0.3:12:5, mixing the water, the sodium hyaluronate, the glycerol and the sodium carboxymethyl starch modified polyethylene glycol, wherein the sodium hyaluronate is small-molecule sodium hyaluronate (the molecular weight is 20-40 ten thousand daltons), and uniformly mixing to obtain a water phase.
The preparation method of the oil phase comprises the following steps:
(1) Stirring 10g luteolin, 3g panthenol and 2g Mel extract for 60min to obtain mixture A;
(2) Preparing hydrophilic modified wild soybean oil: adding 10g of wild soybean oil into 25g of toluene, mixing, heating to 40 ℃, and dropwise adding a mixed solution of 3.3g of acrylic acid, 0.05g of benzoyl peroxide and 8g of ethanol under the stirring condition; after the dropwise addition is finished, continuously heating to 80 ℃, stirring and reacting for 5.5 hours, and after the reaction is finished, washing with water and distilling under reduced pressure to obtain hydrophilic modified wild soybean oil;
(3) Mixing the components in a mass ratio of 1.5:5:1:3, mixing the hydrophilic modified wild soybean oil, shea butter, isocetyl stearate and ethyl cellulose to obtain oil;
(4) Dropwise adding the mixture A into 18g of oil component at a dropwise adding speed of 0.7g/min, stirring while dropwise adding, and obtaining an oil phase after dropwise adding.
The preparation method of the emulsion comprises the following steps:
respectively mixing the water phase and the oil phase uniformly, adding the water phase into a high-speed stirrer, adding the oil phase at the rotating speed of 600r/min, adding a pH regulator to regulate the pH to 5.8 after the addition is finished, homogenizing at the rotating speed of 7500r/min for 20min, cooling to room temperature, standing, and filling to obtain the emulsion.
Comparative example 3
The wild soybean oil in the emulsion was not hydrophilically modified, and the remaining components and preparation method were the same as in example 1.
An anti-inflammatory soothing emulsion comprises a water phase and an oil phase, wherein the oil phase accounts for 14% of the total mass of the emulsion.
The preparation method of the water phase comprises the following steps:
(a) Preparing sodium carboxymethyl starch modified polyethylene glycol: adding 10g of polyethylene glycol with the average molecular weight of 1400 into 110mL of water, and uniformly mixing; then adding a mixed solution of 2.2g of sodium carboxymethyl starch, 0.04g of sodium dodecyl sulfate and 8g of ethanol, and stirring and mixing for 1 hour; then adding 0.012g of p-toluenesulfonic acid and 0.07g of glacial acetic acid, and heating to reflux reaction for 3.5h; after the reaction is finished, precipitating by using cooled anhydrous ether, and drying to obtain the sodium carboxymethyl starch modified polyethylene glycol.
(b) And (2) mixing the following components in percentage by mass as 100:0.3:12:5, mixing the water, the sodium hyaluronate, the glycerol and the sodium carboxymethyl starch modified polyethylene glycol, wherein the sodium hyaluronate is small-molecule sodium hyaluronate (the molecular weight is 20-40 ten thousand daltons), and uniformly mixing to obtain a water phase.
The preparation method of the oil phase comprises the following steps:
(1) Adding 10g of luteolin and 1.1g of sodium hydroxide into 70mLN and N-dimethylformamide, placing the mixture into an ice water bath, and dropwise adding 9.5g of acetylsalicyloyl chloride; after the dropwise addition, taking out the mixture from the ice-water bath, adding a mixture of 3g of panthenol, 1.8g of triethylamine and 9mL of dichloromethane, stirring the mixture at 25 ℃ for 40min for reaction, adding 0.8g of sodium bicarbonate and 2g of honey extract, stirring the mixture for 40min, and then carrying out reduced pressure distillation to obtain a mixture A;
(2) Mixing the components in a mass ratio of 1.5:5:1:3, mixing the wild soybean oil, the shea butter, the isocetyl stearate and the ethyl cellulose to obtain oil;
(3) Dropwise adding the mixture A into 18g of oil component at a dropwise adding speed of 0.7g/min, stirring while dropwise adding, and obtaining an oil phase after dropwise adding.
The preparation method of the emulsion comprises the following steps:
respectively mixing the water phase and the oil phase uniformly, adding the water phase into a high-speed stirrer, adding the oil phase at the rotating speed of 600r/min, adding a pH regulator to regulate the pH to 5.8 after the addition is finished, homogenizing at the rotating speed of 7500r/min for 20min, cooling to room temperature, standing, and filling to obtain the emulsion.
Comparative example 4
The polyethylene glycol in the emulsion was not modified with sodium carboxymethyl starch, and the remaining components and preparation method were the same as in example 1.
An anti-inflammatory soothing emulsion comprises a water phase and an oil phase, wherein the oil phase accounts for 14% of the total mass of the emulsion.
The preparation method of the water phase comprises the following steps:
and (2) mixing the following components in percentage by mass as 100:0.3:12:5, mixing the water, the sodium hyaluronate, the glycerol and the polyethylene glycol, wherein the sodium hyaluronate is small molecular sodium hyaluronate (the molecular weight is 20-40 ten thousand daltons), and uniformly mixing to obtain a water phase.
The preparation method of the oil phase comprises the following steps:
(1) Adding 10g of luteolin and 1.1g of sodium hydroxide into 70mLN and N-dimethylformamide, placing the mixture into an ice water bath, and dropwise adding 9.5g of acetylsalicyloyl chloride; after the dropwise addition, taking out the mixture from the ice-water bath, adding a mixture of 3g of panthenol, 1.8g of triethylamine and 9mL of dichloromethane, stirring the mixture at 25 ℃ for 40min for reaction, adding 0.8g of sodium bicarbonate and 2g of honey extract, stirring the mixture for 40min, and then carrying out reduced pressure distillation to obtain a mixture A;
(2) Preparing hydrophilic modified wild soybean oil: adding 10g of wild soybean oil into 25g of toluene, mixing, heating to 40 ℃, and dropwise adding a mixed solution of 3.3g of acrylic acid, 0.05g of benzoyl peroxide and 8g of ethanol under the stirring condition; after the dropwise addition is finished, continuously heating to 80 ℃, stirring and reacting for 5.5 hours, and after the reaction is finished, washing with water and distilling under reduced pressure to obtain hydrophilic modified wild soybean oil;
(3) Mixing the components in a mass ratio of 1.5:5:1:3, mixing the hydrophilic modified wild soybean oil, shea butter, isocetyl stearate and ethyl cellulose to obtain oil;
(4) Dropwise adding the mixture A into 18g of oil component at a dropwise adding speed of 0.7g/min, stirring while dropwise adding, and obtaining an oil phase after dropwise adding.
The preparation method of the emulsion comprises the following steps:
respectively mixing the water phase and the oil phase uniformly, adding the water phase into a high-speed stirrer, adding the oil phase at the rotating speed of 600r/min, adding a pH regulator to regulate the pH to 5.8 after the addition is finished, homogenizing at the rotating speed of 7500r/min for 20min, cooling to room temperature, standing, and filling to obtain the emulsion.
The anti-inflammatory and relieving effect of the emulsion is tested as follows:
1. test subjects: the emulsions of examples 1 to 3 and comparative examples 1 to 4 were applied to 30 subjects (aged 20 to 55 years) respectively, and the clinical manifestations of the skin of the subjects were mainly skin pruritus, redness, sensitive skin and frequent allergic reactions.
2. The test method comprises the following steps: after the testee cleans the face with the facial cleanser every day, a proper amount of lotion is coated on the sensitive area of the skin, the lotion is applied once in the morning and at night, 2 weeks are 1 course of treatment, and the testee performs 2 course of treatment tests.
3. And (4) judging the standard: the effect is shown: skin itch, skin damage, red blood streak and other allergic phenomena disappear; the method has the following advantages: the allergic phenomena of skin itch, skin damage, red blood streak and the like are reduced; and (4) invalidation: the allergic phenomena of skin itch, skin lesions, red blood streak and the like have no obvious change. In addition, the subjects rated the skin feel (specifically, fresh, non-sticky and non-irritating feel, and soft and smooth skin after use) of the lotion according to the effect of use, and rated the skin feel in order of preference: scores of 5 are very much preferred, scores of 4 are preferred, scores of 3 are general, scores of 2 are less preferred, scores of 1 are not preferred, and scores of 5 are the highest satisfaction.
TABLE 1
Therefore, the emulsion disclosed by the invention combines anti-inflammatory and desensitization with skin barrier repair, so that the skin is effectively relieved, the skin irritation is avoided, and the emulsion is safe and reliable to use for a long time. Moreover, the skin moisturizing cream has a long-acting moisturizing effect, can promote skin healing more quickly, promotes regeneration, activity and metabolism, and gives fresh and soft touch to the skin. Comparative example 1, in which luteolin, a main anti-inflammatory active ingredient, was not added, resulted in a decrease in the efficacy of the emulsion. The comparative examples 2 to 4 show the importance of the components and the addition mode in the invention, are beneficial to forming an oil-in-water type emulsified structure, achieve the water-oil slow balance, have stronger stability and long-acting efficacy of the emulsion, and can also provide better skin feeling experience for the skin.
The above examples of the present invention are merely examples for illustrating the present invention and are not intended to limit the embodiments of the present invention. Variations and modifications in other variations will occur to those skilled in the art upon reading the foregoing description. Not all embodiments are exhaustive. All obvious changes and modifications of the present invention are within the scope of the present invention.
Claims (10)
1. The anti-inflammatory soothing emulsion is characterized by being an oil-in-water type emulsified cosmetic and comprising a water phase and an oil phase, wherein the oil phase accounts for 12-16% of the total mass of the emulsion; the water phase comprises the following components in a mass ratio of 100:0.2 to 0.5:10 to 15: 3-8 parts of water, sodium hyaluronate, glycerol and sodium carboxymethyl starch modified polyethylene glycol; the oil phase comprises the following components in a mass ratio of 5-15: 2 to 7:1 to 3: 10-22 of luteolin, panthenol, honey extract and oil component.
2. The anti-inflammatory soothing emulsion of claim 1 wherein said oil component comprises, by mass, from 0.5 to 3:2 to 8:0.5 to 2: 1-5 of hydrophilic modified wild soybean oil, shea butter, ester oil and ethyl cellulose.
3. The anti-inflammatory soothing emulsion of claim 2 wherein said hydrophilically modified wild soybean oil is prepared by a process comprising the steps of: adding wild soybean oil into toluene, mixing, heating to 40-50 ℃, and dropwise adding a mixed solution of acrylic acid, benzoyl peroxide and ethanol under the stirring condition; after the dropwise addition is finished, continuously heating to 70-80 ℃, stirring and reacting for 5-7 h, and after the reaction is finished, washing with water and carrying out reduced pressure distillation to obtain hydrophilic modified wild soybean oil; the weight ratio of the wild soybean oil to the toluene to the acrylic acid to the benzoyl peroxide to the ethanol is 10:20 to 30:1 to 4:0.05 to 0.1:5 to 10.
4. An anti-inflammatory soothing emulsion according to claim 1 wherein said ester oil is one or more of isopropyl myristate, cetyl octanoate, octyldodecyl myristate, isopropyl palmitate, butyl stearate, isocetyl stearate, diisostearyl malate, sorbitan olive oleate, cetyl palmitate, sorbitan olive oleate.
5. An anti-inflammatory soothing emulsion according to claim 2 or 3 wherein said oil phase is prepared by a process comprising the steps of:
(1) Adding luteolin and sodium hydroxide into N, N-dimethylformamide, then placing the N, N-dimethylformamide into an ice water bath, and dropwise adding acetylsalicyloyl chloride, wherein the mass ratio of luteolin to acetylsalicyloyl chloride is (5-15): 8 to 12; after the dropwise addition, taking out the mixture from the ice water bath, adding a mixture of panthenol, triethylamine and dichloromethane, stirring and reacting at 20-30 ℃ for 30-50 min, then adding sodium bicarbonate and honey extract, stirring and mixing for 20-40 min, and then carrying out reduced pressure distillation to obtain a mixture A;
(2) Mixing the hydrophilic modified wild soybean oil, shea butter, ester oil and ethyl cellulose to obtain oil component;
(3) And dropwise adding the mixture A into the oil component at a dropping speed of 0.5-1 g/min, and obtaining an oil phase after the dropwise adding is finished.
6. The anti-inflammatory soothing emulsion of claim 5 wherein in step (1) the ratio of the amounts of luteolin, sodium hydroxide, and N, N-dimethylformamide added is 1g: 0.1-0.2 g:7mL.
7. The anti-inflammatory soothing emulsion of claim 5 wherein in step (1) the ratio of the amounts of panthenol, triethylamine, methylene chloride and sodium bicarbonate added is 1g: 0.5-0.8 g:3mL of: 0.2 to 0.4g.
8. The anti-inflammatory soothing emulsion of claim 1 wherein said sodium carboxymethyl starch modified polyethylene glycol is prepared by a process comprising the steps of: adding polyethylene glycol with the molecular weight of 1000-2000 into water, uniformly mixing, adding a mixed solution of sodium carboxymethyl starch, sodium dodecyl sulfate and ethanol, and stirring and mixing for 1-2 hours, wherein the mass ratio of the polyethylene glycol to the sodium carboxymethyl starch is 10; then adding p-toluenesulfonic acid and glacial acetic acid, and heating to reflux reaction for 3-5 h; after the reaction is finished, precipitating by using cooled anhydrous ether, and drying to obtain the sodium carboxymethyl starch modified polyethylene glycol.
9. The anti-inflammatory, soothing emulsion of claim 8 wherein said polyethylene glycol and water are added in a ratio of 1g: 10-12 mL; the mass ratio of the sodium carboxymethyl starch to the sodium dodecyl sulfate to the ethanol to the p-toluenesulfonic acid to the glacial acetic acid is 10:0.1 to 0.3:30 to 40:0.05 to 0.1:0.2 to 0.6.
10. A process for the preparation of an emulsion according to any one of claims 1 to 9, comprising the steps of: respectively and uniformly mixing the water phase and the oil phase, adding the water phase into a high-speed stirrer, adding the oil phase at the rotating speed of 500-700 r/min, adding a pH regulator to regulate the pH to 5.5-6.0 after the addition is finished, homogenizing at the rotating speed of 7000-8000 r/min for 10-20 min, cooling to room temperature, standing, and filling to obtain the emulsion.
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| US20120201774A1 (en) * | 2009-10-22 | 2012-08-09 | Matthias Schweinsberg | Composition for Shaping Keratin Fibres Containing Starches Modified with Propylene Oxide |
| CN104311750A (en) * | 2014-11-06 | 2015-01-28 | 佛山市三水鲸鲨化工有限公司 | Styrene modified alkyd resin, preparation method thereof and alkyd resin paint |
| CN111149710A (en) * | 2018-11-07 | 2020-05-15 | 林聪� | Diatomite-based cat litter capable of agglomerating, deodorizing, resisting and inhibiting bacteria and being flushed away by closestool and manufacturing method thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20120201774A1 (en) * | 2009-10-22 | 2012-08-09 | Matthias Schweinsberg | Composition for Shaping Keratin Fibres Containing Starches Modified with Propylene Oxide |
| CN104311750A (en) * | 2014-11-06 | 2015-01-28 | 佛山市三水鲸鲨化工有限公司 | Styrene modified alkyd resin, preparation method thereof and alkyd resin paint |
| CN111149710A (en) * | 2018-11-07 | 2020-05-15 | 林聪� | Diatomite-based cat litter capable of agglomerating, deodorizing, resisting and inhibiting bacteria and being flushed away by closestool and manufacturing method thereof |
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