CN115154401B - Anti-inflammatory and soothing emulsion and preparation method thereof - Google Patents
Anti-inflammatory and soothing emulsion and preparation method thereof Download PDFInfo
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- CN115154401B CN115154401B CN202210876983.XA CN202210876983A CN115154401B CN 115154401 B CN115154401 B CN 115154401B CN 202210876983 A CN202210876983 A CN 202210876983A CN 115154401 B CN115154401 B CN 115154401B
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- sodium
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- 239000011734 sodium Substances 0.000 claims abstract description 41
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Classifications
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/73—Polysaccharides
- A61K8/735—Mucopolysaccharides, e.g. hyaluronic acid; Derivatives thereof
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- A—HUMAN NECESSITIES
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- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
- A61K8/04—Dispersions; Emulsions
- A61K8/06—Emulsions
- A61K8/062—Oil-in-water emulsions
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- A—HUMAN NECESSITIES
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- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
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- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
- A61K8/34—Alcohols
- A61K8/345—Alcohols containing more than one hydroxy group
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
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- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
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Abstract
The invention relates to the technical field of cosmetics, and discloses an anti-inflammatory and 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 aqueous phase comprises the following components in percentage by mass: 0.2 to 0.5:10 to 15: 3-8 parts of water, sodium hyaluronate, glycerol and carboxymethyl starch sodium modified polyethylene glycol; the oil phase comprises the following components in percentage by mass of 5-15: 2 to 7:1 to 3:10 to 22 of luteolin, panthenol, honey extract and oil. The invention firstly gives the skin a water-type fresh feel in an oil-in-water type emulsification mode, and then combines the main anti-allergic and anti-inflammatory effects given by water-oil balance and oil phase, thereby avoiding the irritation to the skin, having long-acting moisturizing effect and being safe and reliable for long-term use.
Description
Technical Field
The invention belongs to the technical field of cosmetics, and in particular relates to an anti-inflammatory and soothing emulsion and a preparation method thereof.
Background
Sensitive skin affects the quality of life of people to a large extent. Sensitive skin usually has skin allergy symptoms and discomfort such as redness, itching, dryness, stinging, burning, tightness and the like, and although a specific allergen is difficult to find, the sensitive skin has the common point that the skin barrier is damaged, namely the skin surface loses normal protective function and loss of skin moisture occurs, so that dryness, desquamation or itching of the skin occurs. Meanwhile, allergens such as germs, pollen, chemical substances and the like on the surface of the skin easily pass through damaged skin barriers and enter the interior of the skin, so that skin inflammatory reaction is further initiated. At present, most of the used effective components of cosmetics for treating or relieving skin allergy are anti-inflammatory or anti-irritant chemical agents, but cosmetics taking chemical substances as main raw materials can not meet the demands of people on natural cosmetics with small side effects, and research mainly on plant and traditional Chinese medicine extracts gradually becomes a research hot spot. Moreover, these cosmetics often ignore the repair of skin barrier function, so long-term use of the above products will lead to thinning of epidermis and dermis, impaired skin barrier function, skin atrophy, telangiectasia and other symptoms. In summary, such a vicious circle can cause endless trouble to modern loving women.
For example, chinese patent No. 202010777565.6 discloses an anti-inflammatory acne-removing cosmetic composition and a preparation method thereof, wherein the composition comprises the following components in percentage by weight: 10-15 parts of sorbitan olive oleate, 25-40 parts of glycerol, 60-80 parts of deionized water, 3-5 parts of Hibiscus manihot 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 adding transparent gel matrix obtained by stirring sorbitan olive oleate, glycerol and deionized water as carrier, and adding Hibiscus sabdariffa extract, pollen Pini, dried Bulbus Lilii, semen Ginkgo extract and cistanche tubulosa polysaccharide as effective components into the carrier, and stirring uniformly by stirring device. The cosmetic composition is effective in anti-inflammatory and anti-acne, but does not take into account the repair of skin barrier, and does not achieve an effective soothing effect on skin, which results in impaired skin function and large side effects after long-term use.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention aims to provide the anti-inflammatory and soothing emulsion and the preparation method thereof, and the anti-allergic and anti-inflammatory skin barrier repairing method is combined in an oil-in-water type emulsification mode, so that the skin is effectively relieved, and the safety and the stability are higher.
In order to achieve the aim, the invention provides an anti-inflammatory and 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 aqueous phase comprises the following components in percentage by mass: 0.2 to 0.5:10 to 15: 3-8 parts of water, sodium hyaluronate, glycerol and carboxymethyl starch sodium modified polyethylene glycol; the oil phase comprises the following components in percentage by mass of 5-15: 2 to 7:1 to 3:10 to 22 of luteolin, panthenol, honey extract and oil.
The invention combines the anti-allergic and anti-inflammatory effects with the skin repairing barrier, more importantly, the skin is effectively relaxed, the skin is firstly endowed with water-type refreshing touch in an oil-in-water type emulsification mode, and then the main anti-allergic and anti-inflammatory effects endowed by water-oil balance and oil phase are combined, so that the irritation to the skin is avoided, and the skin is safe and reliable for long-term use. The components such as sodium hyaluronate and glycerol in the water phase can help thicken the stratum corneum, improve the tolerance of the skin, maintain the moisture of the skin and improve the stability of the skin in advance. The cosmetic has the advantages of relieving skin by stabilizing water phase, and relieving by anti-inflammatory and anti-sensitization effects of oil phase, so as to promote skin healing, regeneration, activity and metabolism. Luteolin is a natural plant extract, has anti-inflammatory and antiallergic pharmacological activity of traditional Chinese medicine, and panthenol is also called vitamin B5, and can effectively relieve skin irritation symptoms. 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 by human body, enhance water absorption of horny layer, lock water and restore skin elasticity and softness. The sensitive skin firstly needs to supplement moisture lost by the skin, but the water phase is simply enhanced and cannot effectively preserve moisture, and more importantly, the water-oil balance is maintained.
Further preferably, the oil component includes a mass ratio of 0.5 to 3:2 to 8:0.5 to 2: 1-5 hydrophilic modified wild soybean oil, shea butter, ester oil and ethyl cellulose.
The wild soybean oil, the shea butter and the ester oil in the oil are oil components with high safety, can effectively wrap the anti-inflammatory and anti-allergic components, and have no stimulation to skin. Ethylcellulose has water-insolubility as a backbone material, enabling the oil phase to be stably dispersed in the aqueous phase. In addition, the wild soybean oil is a good humectant and an antioxidant, can be used as an epidermal growth factor, can nourish skin, relieve dryness and roughness, and enable the skin to be durable, smooth and tender and soft in touch. The wild soybean oil is partially grafted and hydrophilically modified to ensure that the oil component and the anti-inflammatory active ingredient have better affinity, can form more stable combination with the water phase, and have better emulsification effect 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 dripping is finished, continuously heating to 70-80 ℃ and stirring for reaction for 5-7 hours, and washing with water and distilling under reduced pressure after the reaction is finished to obtain hydrophilic modified wild soybean oil; the mass ratio of the wild soybean oil to the toluene to the acrylic acid to the benzoyl peroxide to the ethanol is 10: 20-30: 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 proportion of the acrylic acid and balance the hydrophilicity and hydrophobicity, otherwise, the wild soybean oil is unfavorable for forming an oil-in-water type structure, and the refreshing and relieving effects on skin can be poor.
Further preferably, the 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.
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 mixture into an ice-water bath, and dropwise adding acetylsalicylic acid chloride, wherein the mass ratio of the luteolin to the acetylsalicylic acid chloride is 5-15: 8-12; taking out from the ice water bath after the dripping is finished, adding a mixture of panthenol, triethylamine and dichloromethane, stirring and reacting for 30-50 min at 20-30 ℃, adding sodium bicarbonate and honey extract, stirring and mixing for 20-40 min, and performing reduced pressure distillation to obtain a mixture A;
(2) Mixing hydrophilic modified wild soybean oil, shea butter, ester oil and ethyl cellulose to obtain oil component;
(3) And (3) dropwise adding the mixture A into the oil at a dropwise adding speed of 0.5-1 g/min, and obtaining an oil phase after the dropwise adding is finished.
In the preparation of the oil phase, it is most 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. In addition, the luteolin and the panthenol are combined by utilizing the acetylsalicyloyl chloride, so that the relieving effect of the anti-inflammatory component can be improved, the acetylsalicyloyl chloride also has a certain anti-inflammatory effect, and the anti-inflammatory relieving effect can be enhanced by adding the moisturizing effect of the honey extract. However, the rate at which the resulting mixture A is added dropwise to mixture B also affects the dispersive binding effect of the anti-inflammatory component in the oil, and thus the anti-inflammatory soothing effect of the cosmetic.
Further preferably, in the step (1), the ratio of the addition amounts of luteolin, sodium hydroxide and N, N-dimethylformamide is 1g:0.1 to 0.2g:7mL.
Further preferably, in the step (1), the addition amount ratio of the panthenol, the triethylamine, the dichloromethane and the sodium bicarbonate is 1g:0.5 to 0.8g:3mL: 0.2-0.4 g.
Further preferably, the preparation method of the carboxymethyl starch sodium 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 h, wherein the mass ratio of the polyethylene glycol to the sodium carboxymethyl starch is 10:1-4; then adding p-toluenesulfonic acid and glacial acetic acid, and heating to reflux reaction for 3-5 h; and after the reaction is finished, precipitating with cooled anhydrous diethyl ether, and drying to obtain the sodium carboxymethyl starch modified polyethylene glycol.
Polyethylene glycol is a water-soluble component, has good lubricity and moisture retention, is modified by carboxymethyl starch sodium, and has a slow release effect by utilizing the water-soluble expansibility of carboxymethyl starch sodium to resist inflammatory oil phase components, so that the water phase better plays a role in enhancing skin barrier, irritation to skin can be better avoided, and safety is improved.
Further preferably, the ratio of the polyethylene glycol to the water is 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: 30-40: 0.05 to 0.1:0.2 to 0.6.
The invention also provides a preparation method of the anti-inflammatory and soothing emulsion, which comprises the following steps: and (3) 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 adjust the pH to 5.5-6.0 after the adding, homogenizing for 10-20 min at the rotating speed of 7000-8000 r/min, cooling to room temperature, standing and filling to obtain the emulsion.
The oil phase is quickly homogenized and stirred after being dripped into the water phase, so that the anti-inflammatory functional components can be uniformly dispersed, and the emulsion quality is ensured.
Compared with the prior art, the invention has the following advantages: the skin is firstly endowed with water-type refreshing touch in an oil-in-water type emulsification mode, and then the main anti-allergic and anti-inflammatory effects of water-oil balance and oil phase are combined, so that the irritation to the skin is avoided, and the skin is safe and reliable for long-term use; the components such as sodium hyaluronate, glycerol and the like in the water phase can help to thicken the stratum corneum, promote the skin tolerance and repair the skin barrier; the oil phase is wrapped with the anti-inflammatory and anti-allergic active ingredients for targeted alleviation, and the moisturizing factors are still contained in the oil phase, so that the oil phase has long-acting moisturizing effect, can promote skin healing more quickly, and promotes regeneration, activity and metabolism.
Detailed Description
The invention will be further illustrated with reference to specific examples. It should be understood that the detailed description and specific examples are intended for purposes of illustration only and are not intended to limit the scope of the invention. The experimental methods in the following examples are conventional methods unless otherwise specified. The test materials used in the examples described below, unless otherwise specified, are all commercially available products.
Example 1
An anti-inflammatory and soothing emulsion comprises an aqueous 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; adding a mixed solution of 2.2g of sodium carboxymethyl starch, 0.04g of sodium dodecyl sulfate and 8g of ethanol, stirring and mixing for 1h; then 0.012g of p-toluenesulfonic acid and 0.07g of glacial acetic acid are added, and the temperature is raised to reflux reaction for 3.5h; and after the reaction is finished, precipitating with cooled anhydrous diethyl ether, and drying to obtain the sodium carboxymethyl starch modified polyethylene glycol.
(b) The mass ratio is 100:0.3:12:5, mixing water, sodium hyaluronate, glycerol and carboxymethyl starch sodium modified polyethylene glycol, wherein the sodium hyaluronate is micromolecular sodium hyaluronate (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) 10g of luteolin and 1.1g of sodium hydroxide are added to 70mLN, N-dimethylformamide, which is then placed in an ice-water bath, and 9.5g of acetylsalicyloyl chloride is added dropwise; after the dripping is finished, taking out from the ice water bath, adding a mixture of 3g of panthenol, 1.8g of triethylamine and 9mL of dichloromethane, stirring and reacting for 40min at 25 ℃, adding 0.8g of sodium bicarbonate and 2g of honey extract, stirring and mixing for 40min, and performing reduced pressure distillation to obtain a mixture A;
(2) Preparation of hydrophilic modified wild soybean oil: 10g of wild soybean oil is added into 25g of toluene to be mixed, the temperature is raised to 40 ℃, and a mixed solution of 3.3g of acrylic acid, 0.05g of benzoyl peroxide and 8g of ethanol is added dropwise under stirring; after the dripping is finished, continuously heating to 80 ℃ and stirring for reaction for 5.5 hours, and washing with water and distilling under reduced pressure after the reaction is finished to obtain hydrophilic modified wild soybean oil;
(3) The mass ratio is 1.5:5:1:3, mixing the hydrophilic modified wild soybean oil, the shea butter, the isocetyl stearate and the ethyl cellulose to obtain oil component;
(4) The mixture A was added dropwise to 18g of oil at a dropping rate of 0.7g/min while stirring, and an oil phase was obtained after the completion of the addition.
The preparation method of the emulsion comprises the following steps:
and (3) 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 adjust the pH to 5.8 after the addition, homogenizing for 20min at the rotating speed of 7500r/min, cooling to room temperature, standing, and filling to obtain the emulsion.
Example 2
An anti-inflammatory and 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; adding a mixed solution of 2.2g of sodium carboxymethyl starch, 0.04g of sodium dodecyl sulfate and 8g of ethanol, stirring and mixing for 1h; then 0.012g of p-toluenesulfonic acid and 0.07g of glacial acetic acid are added, and the temperature is raised to reflux reaction for 3.5h; and after the reaction is finished, precipitating with cooled anhydrous diethyl ether, and drying to obtain the sodium carboxymethyl starch modified polyethylene glycol.
(b) The mass ratio is 100:0.3:12:5, mixing water, sodium hyaluronate, glycerol and carboxymethyl starch sodium modified polyethylene glycol, wherein the sodium hyaluronate is micromolecular sodium hyaluronate (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) 10g of luteolin and 1.1g of sodium hydroxide are added to 70mLN, N-dimethylformamide, which is then placed in an ice-water bath, and 9.5g of acetylsalicyloyl chloride is added dropwise; after the dripping is finished, taking out from the ice water bath, adding a mixture of 3g of panthenol, 1.8g of triethylamine and 9mL of dichloromethane, stirring and reacting for 40min at 25 ℃, adding 0.8g of sodium bicarbonate and 2g of honey extract, stirring and mixing for 40min, and performing reduced pressure distillation to obtain a mixture A;
(2) Preparation of hydrophilic modified wild soybean oil: 10g of wild soybean oil is added into 25g of toluene to be mixed, the temperature is raised to 45 ℃, and a mixed solution of 4g of acrylic acid, 0.08g of benzoyl peroxide and 8g of ethanol is added dropwise under the stirring condition; after the dripping is finished, continuously heating to 80 ℃ and stirring for reaction for 6.5 hours, and washing with water and distilling under reduced pressure after the reaction is finished to obtain hydrophilic modified wild soybean oil;
(3) The mass ratio is 2:5:1.5:3, mixing the hydrophilic modified wild soybean oil, the shea butter, the isocetyl stearate and the ethyl cellulose to obtain oil component;
(4) The mixture A was added dropwise to 18g of oil at a dropping rate of 0.5g/min while stirring, and an oil phase was obtained after the completion of the addition.
The preparation method of the emulsion comprises the following steps:
and (3) 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 700r/min, adding a pH regulator to adjust the pH to 5.8 after the addition, homogenizing for 20min at the rotating speed of 7500r/min, cooling to room temperature, standing, and filling to obtain the emulsion.
Example 3
An anti-inflammatory and soothing emulsion comprises an aqueous 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 average molecular weight of 2000 into 120mL of water, and uniformly mixing; adding a mixed solution of 2g of sodium carboxymethyl starch, 0.04g of sodium dodecyl sulfate and 8g of ethanol, stirring and mixing for 2h; then adding 0.01g of p-toluenesulfonic acid and 0.1g of glacial acetic acid, and heating to reflux for 4.5h; and after the reaction is finished, precipitating with cooled anhydrous diethyl ether, and drying to obtain the sodium carboxymethyl starch modified polyethylene glycol.
(b) The mass ratio is 100:0.3:14:6, mixing water, sodium hyaluronate, glycerol and carboxymethyl starch sodium modified polyethylene glycol, wherein the sodium hyaluronate is micromolecular sodium hyaluronate (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) 10g of luteolin and 1.1g of sodium hydroxide are added to 70mLN, N-dimethylformamide, which is then placed in an ice-water bath, and 9.5g of acetylsalicyloyl chloride is added dropwise; after the dripping is finished, taking out from the ice water bath, adding a mixture of 3g of panthenol, 1.8g of triethylamine and 9mL of dichloromethane, stirring and reacting for 40min at 25 ℃, adding 0.8g of sodium bicarbonate and 2g of honey extract, stirring and mixing for 40min, and performing reduced pressure distillation to obtain a mixture A;
(2) Preparation of hydrophilic modified wild soybean oil: 10g of wild soybean oil is added into 25g of toluene to be mixed, the temperature is raised to 40 ℃, and a mixed solution of 3.3g of acrylic acid, 0.05g of benzoyl peroxide and 8g of ethanol is added dropwise under stirring; after the dripping is finished, continuously heating to 80 ℃ and stirring for reaction for 5.5 hours, and washing with water and distilling under reduced pressure after the reaction is finished to obtain hydrophilic modified wild soybean oil;
(3) The mass ratio is 1.5:5:1:3, mixing the hydrophilic modified wild soybean oil, the shea butter, the isocetyl stearate and the ethyl cellulose to obtain oil component;
(4) The mixture A was added dropwise to 18g of oil at a dropping rate of 0.7g/min while stirring, and an oil phase was obtained after the completion of the addition.
The preparation method of the emulsion comprises the following steps:
and (3) 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 adjust the pH to 5.9 after the addition, homogenizing for 20min at the rotating speed of 7500r/min, cooling to room temperature, standing, and filling to obtain the emulsion.
Comparative example 1
Luteolin is not added into the emulsion, and the rest components and the preparation method are the same as those of the example 1.
An anti-inflammatory and soothing emulsion comprises an aqueous 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; adding a mixed solution of 2.2g of sodium carboxymethyl starch, 0.04g of sodium dodecyl sulfate and 8g of ethanol, stirring and mixing for 1h; then 0.012g of p-toluenesulfonic acid and 0.07g of glacial acetic acid are added, and the temperature is raised to reflux reaction for 3.5h; and after the reaction is finished, precipitating with cooled anhydrous diethyl ether, and drying to obtain the sodium carboxymethyl starch modified polyethylene glycol.
(b) The mass ratio is 100:0.3:12:5, mixing water, sodium hyaluronate, glycerol and carboxymethyl starch sodium modified polyethylene glycol, wherein the sodium hyaluronate is micromolecular sodium hyaluronate (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) 1.1g of sodium hydroxide was added to 70mLN, N-dimethylformamide, which was then placed in an ice-water bath, and 9.5g of acetylsalicyl chloride was added dropwise; after the dripping is finished, taking out from the ice water bath, adding a mixture of 3g of panthenol, 1.8g of triethylamine and 9mL of dichloromethane, stirring and reacting for 40min at 25 ℃, adding 0.8g of sodium bicarbonate and 2g of honey extract, stirring and mixing for 40min, and performing reduced pressure distillation to obtain a mixture A;
(2) Preparation of hydrophilic modified wild soybean oil: 10g of wild soybean oil is added into 25g of toluene to be mixed, the temperature is raised to 40 ℃, and a mixed solution of 3.3g of acrylic acid, 0.05g of benzoyl peroxide and 8g of ethanol is added dropwise under stirring; after the dripping is finished, continuously heating to 80 ℃ and stirring for reaction for 5.5 hours, and washing with water and distilling under reduced pressure after the reaction is finished to obtain hydrophilic modified wild soybean oil;
(3) The mass ratio is 1.5:5:1:3, mixing the hydrophilic modified wild soybean oil, the shea butter, the isocetyl stearate and the ethyl cellulose to obtain oil component;
(4) The mixture A was added dropwise to 18g of oil at a dropping rate of 0.7g/min while stirring, and an oil phase was obtained after the completion of the addition.
The preparation method of the emulsion comprises the following steps:
and (3) 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 adjust the pH to 5.8 after the addition, homogenizing for 20min at the rotating speed of 7500r/min, cooling to room temperature, standing, and filling to obtain the emulsion.
Comparative example 2
Each component of the mixture A in the emulsion is prepared by direct mixing, and the rest components and the preparation method are the same as in the example 1.
An anti-inflammatory and soothing emulsion comprises an aqueous 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; adding a mixed solution of 2.2g of sodium carboxymethyl starch, 0.04g of sodium dodecyl sulfate and 8g of ethanol, stirring and mixing for 1h; then 0.012g of p-toluenesulfonic acid and 0.07g of glacial acetic acid are added, and the temperature is raised to reflux reaction for 3.5h; and after the reaction is finished, precipitating with cooled anhydrous diethyl ether, and drying to obtain the sodium carboxymethyl starch modified polyethylene glycol.
(b) The mass ratio is 100:0.3:12:5, mixing water, sodium hyaluronate, glycerol and carboxymethyl starch sodium modified polyethylene glycol, wherein the sodium hyaluronate is micromolecular sodium hyaluronate (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) Mixing 10g of luteolin, 3g of panthenol and 2g of honey extract for 60min to obtain a mixture A;
(2) Preparation of hydrophilic modified wild soybean oil: 10g of wild soybean oil is added into 25g of toluene to be mixed, the temperature is raised to 40 ℃, and a mixed solution of 3.3g of acrylic acid, 0.05g of benzoyl peroxide and 8g of ethanol is added dropwise under stirring; after the dripping is finished, continuously heating to 80 ℃ and stirring for reaction for 5.5 hours, and washing with water and distilling under reduced pressure after the reaction is finished to obtain hydrophilic modified wild soybean oil;
(3) The mass ratio is 1.5:5:1:3, mixing the hydrophilic modified wild soybean oil, the shea butter, the isocetyl stearate and the ethyl cellulose to obtain oil component;
(4) The mixture A was added dropwise to 18g of oil at a dropping rate of 0.7g/min while stirring, and an oil phase was obtained after the completion of the addition.
The preparation method of the emulsion comprises the following steps:
and (3) 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 adjust the pH to 5.8 after the addition, homogenizing for 20min at the rotating speed of 7500r/min, 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 other components and preparation method were the same as in example 1.
An anti-inflammatory and soothing emulsion comprises an aqueous 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; adding a mixed solution of 2.2g of sodium carboxymethyl starch, 0.04g of sodium dodecyl sulfate and 8g of ethanol, stirring and mixing for 1h; then 0.012g of p-toluenesulfonic acid and 0.07g of glacial acetic acid are added, and the temperature is raised to reflux reaction for 3.5h; and after the reaction is finished, precipitating with cooled anhydrous diethyl ether, and drying to obtain the sodium carboxymethyl starch modified polyethylene glycol.
(b) The mass ratio is 100:0.3:12:5, mixing water, sodium hyaluronate, glycerol and carboxymethyl starch sodium modified polyethylene glycol, wherein the sodium hyaluronate is micromolecular sodium hyaluronate (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) 10g of luteolin and 1.1g of sodium hydroxide are added to 70mLN, N-dimethylformamide, which is then placed in an ice-water bath, and 9.5g of acetylsalicyloyl chloride is added dropwise; after the dripping is finished, taking out from the ice water bath, adding a mixture of 3g of panthenol, 1.8g of triethylamine and 9mL of dichloromethane, stirring and reacting for 40min at 25 ℃, adding 0.8g of sodium bicarbonate and 2g of honey extract, stirring and mixing for 40min, and performing reduced pressure distillation to obtain a mixture A;
(2) The mass ratio is 1.5:5:1:3, mixing the wild soybean oil, the shea butter, the isocetyl stearate and the ethyl cellulose to obtain oil component;
(3) The mixture A was added dropwise to 18g of oil at a dropping rate of 0.7g/min while stirring, and an oil phase was obtained after the completion of the addition.
The preparation method of the emulsion comprises the following steps:
and (3) 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 adjust the pH to 5.8 after the addition, homogenizing for 20min at the rotating speed of 7500r/min, cooling to room temperature, standing, and filling to obtain the emulsion.
Comparative example 4
The polyethylene glycol in the emulsion was not modified by sodium carboxymethyl starch, and the rest of the components and the preparation method were the same as in example 1.
An anti-inflammatory and soothing emulsion comprises an aqueous 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:
the mass ratio is 100:0.3:12:5, mixing water, sodium hyaluronate, glycerol and polyethylene glycol, wherein the sodium hyaluronate is micromolecular sodium hyaluronate (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) 10g of luteolin and 1.1g of sodium hydroxide are added to 70mLN, N-dimethylformamide, which is then placed in an ice-water bath, and 9.5g of acetylsalicyloyl chloride is added dropwise; after the dripping is finished, taking out from the ice water bath, adding a mixture of 3g of panthenol, 1.8g of triethylamine and 9mL of dichloromethane, stirring and reacting for 40min at 25 ℃, adding 0.8g of sodium bicarbonate and 2g of honey extract, stirring and mixing for 40min, and performing reduced pressure distillation to obtain a mixture A;
(2) Preparation of hydrophilic modified wild soybean oil: 10g of wild soybean oil is added into 25g of toluene to be mixed, the temperature is raised to 40 ℃, and a mixed solution of 3.3g of acrylic acid, 0.05g of benzoyl peroxide and 8g of ethanol is added dropwise under stirring; after the dripping is finished, continuously heating to 80 ℃ and stirring for reaction for 5.5 hours, and washing with water and distilling under reduced pressure after the reaction is finished to obtain hydrophilic modified wild soybean oil;
(3) The mass ratio is 1.5:5:1:3, mixing the hydrophilic modified wild soybean oil, the shea butter, the isocetyl stearate and the ethyl cellulose to obtain oil component;
(4) The mixture A was added dropwise to 18g of oil at a dropping rate of 0.7g/min while stirring, and an oil phase was obtained after the completion of the addition.
The preparation method of the emulsion comprises the following steps:
and (3) 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 adjust the pH to 5.8 after the addition, homogenizing for 20min at the rotating speed of 7500r/min, cooling to room temperature, standing, and filling to obtain the emulsion.
The anti-inflammatory and soothing effects of the emulsion are tested:
1. test object: the emulsions of examples 1-3 and comparative examples 1-4 were used in 30 subjects (aged between 20 and 55 years), respectively, and the skin of the subjects showed mainly cutaneous pruritus, red blood streaks, and was sensitive to skin and frequently developed allergic reactions.
2. The test method comprises the following steps: after the face of the subject is cleaned by the daily facial cleanser, a proper amount of emulsion is smeared on the sensitive area of the skin, and the skin is used for 2 treatment courses once in the morning and evening, and the subject is subjected to 2 treatment course experiments.
3. Judgment standard: the effect is shown: the allergic phenomena such as skin itch, skin damage, red blood streak and the like disappear; the method is effective: the allergic phenomena such as skin itch, skin damage, red blood streak and the like are relieved; invalidation: the allergic phenomena such as skin itch, skin damage, red blood streak and the like have no obvious change. In addition, the subjects scored the skin feel of the lotion (specifically, feel of freshness, no sticky feel and irritation, feel of soft and silky skin after use, etc.) according to the use effect, and scored in order according to the likeness: 5 points are very liked, 4 points are preferred, 3 points are generally less preferred, 2 points are less preferred, 1 point is less preferred, and 5 points are the highest satisfaction value.
TABLE 1
Therefore, the emulsion combines the functions of anti-inflammatory and desensitizing with repairing skin barrier, so that the skin can be effectively relaxed, the skin irritation is avoided, and the emulsion is safe and reliable for long-term use. In addition, the moisturizing agent has long-acting moisturizing effect, can promote skin healing more quickly, promote regeneration, activity and metabolism, and endow the skin with fresh and soft feeling. The absence of luteolin, the main anti-inflammatory active ingredient, in comparative example 1, resulted in reduced efficacy of the emulsion. While comparative examples 2-4 all show the importance of each component and the addition mode in the invention, the oil-in-water emulsion structure is formed, the water-oil slow balance is achieved, the stability and long-acting efficacy of the emulsion are stronger, and the emulsion can also give better skin feel experience to the skin.
The above examples of the present invention are merely illustrative of the present invention and are not intended to limit the embodiments of the present invention. Other variations and modifications of the present invention will be apparent to those of ordinary skill in the art in light of the foregoing description. Not all embodiments are exhaustive. Obvious changes and modifications which are extended by the technical proposal of the invention are still within the protection scope of the invention.
Claims (6)
1. The anti-inflammatory and soothing emulsion is characterized by being 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 aqueous phase comprises the following components in percentage by mass: 0.2 to 0.5: 10-15: 3-8 parts of water, sodium hyaluronate, glycerol and carboxymethyl starch sodium modified polyethylene glycol; the oil phase comprises the following components in percentage by mass: 2-7: 1-3: 10-22 parts of luteolin, panthenol, a honey extract and oil; the oil comprises the following components in percentage by mass of 0.5-3: 2-8: 0.5-2: 1-5 parts of hydrophilically modified wild soybean oil, shea butter, ester oil and ethyl cellulose;
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 dripping is finished, continuously heating to 70-80 ℃ and stirring for reacting for 5-7 hours, and washing with water and distilling under reduced pressure after the reaction is finished to obtain hydrophilic modified wild soybean oil; the mass ratio of the wild soybean oil to the toluene to the acrylic acid to the benzoyl peroxide to the ethanol is 10: 20-30: 1-4: 0.05-0.1: 5-10;
the preparation method of the oil phase comprises the following steps:
(1) Adding luteolin and sodium hydroxide into N, N-dimethylformamide, then placing the mixture in an ice-water bath, and dropwise adding acetylsalicylic acid chloride, wherein the mass ratio of the luteolin to the acetylsalicylic acid chloride is 5-15: 8-12 parts; taking out from the ice water bath after the dripping is finished, adding a mixture of panthenol, triethylamine and dichloromethane, stirring and reacting for 30-50 min at 20-30 ℃, adding sodium bicarbonate and honey extract, stirring and mixing for 20-40 min, and performing reduced pressure distillation to obtain a mixture A;
(2) Mixing hydrophilic modified wild soybean oil, shea butter, ester oil and ethyl cellulose to obtain oil component;
(3) Dripping the mixture A into oil at a dripping speed of 0.5-1 g/min, and obtaining an oil phase after the dripping is finished;
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 10:1-4; then adding p-toluenesulfonic acid and glacial acetic acid, and heating to reflux for 3-5 h; and after the reaction is finished, precipitating with cooled anhydrous diethyl ether, and drying to obtain the sodium carboxymethyl starch modified polyethylene glycol.
2. The anti-inflammatory soothing emulsion of claim 1 wherein the ester oil is one or more of isopropyl myristate, cetyl caprylate, octyl dodecyl myristate, isopropyl palmitate, butyl stearate, isocetyl stearate, diisostearyl malate, sorbitan olive oleate, cetyl palmitate, sorbitan olive oleate.
3. The anti-inflammatory soothing emulsion of claim 1 wherein in step (1), the ratio of the added amounts of luteolin, sodium hydroxide, N-dimethylformamide is 1g: 0.1-0.2 g:7mL.
4. The anti-inflammatory soothing emulsion of claim 1, wherein in step (1), the addition amount ratio of panthenol, triethylamine, dichloromethane, sodium bicarbonate is 1g: 0.5-0.8 g:3mL: 0.2-0.4 g.
5. The anti-inflammatory soothing emulsion of claim 1 wherein the polyethylene glycol and water are added in an amount 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: 30-40: 0.05-0.1: 0.2 to 0.6.
6. A method of preparing an emulsion according to any one of claims 1 to 5, comprising the steps of: and (3) 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 adjust the pH to 5.5-6.0 after the adding, homogenizing for 10-20 min at the rotating speed of 7000-8000 r/min, cooling to room temperature, standing, and filling to obtain the emulsion.
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| 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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| 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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