CN113456532A - Zero-pore makeup front cream without silicone oil and preparation method thereof - Google Patents
Zero-pore makeup front cream without silicone oil and preparation method thereof Download PDFInfo
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- 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
- A61K8/81—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
- A61K8/8141—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
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- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
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- A61K8/9789—Magnoliopsida [dicotyledons]
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- A61K8/00—Cosmetics or similar toiletry preparations
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- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
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- A61K2800/782—Enzyme inhibitors; Enzyme antagonists
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/80—Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
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Abstract
The invention discloses a zero-pore makeup front cream without silicone oil, which comprises the following components: the invention also provides a preparation method of the pore-free makeup front cream without silicone oil; the invention adopts the water-soluble component of sodium polyacrylate to replace the traditional silicone oil polymer, and is compounded with the extract component with the skin nourishing effect, so that the skin care product can fill pores and wrinkles, does not close the pores, can quickly enhance the absorption of nutrient components by the skin, and has more natural and transparent skin and more durable makeup.
Description
Technical Field
The invention belongs to the technical field of cosmetics, and particularly relates to a zero-pore makeup front cream free of silicone oil and a preparation method thereof.
Background
Most of zero-pore products in the market at present generally contain silicone oil polymer components, and the silicone oil polymer components are used for filling fine lines and pores on the skin and can bring better skin feel; however, the raw materials are not absorbed by the skin, and are easy to adhere to the surface of the skin to form a closed film, so that pores of the skin are not breathable and stuffy, and acne is easily generated. And the effect of the currently used pore-free products is not satisfactory in the aspects of maintaining the durability of makeup, the uniformity of smearing and the like, so that the development of a silicone oil-free pore-free product which can promote the absorption of effective components of skin, make skin natural and transparent and maintain the original characteristics has important significance.
Disclosure of Invention
In order to solve the defects and shortcomings in the prior art, the invention aims to provide the pore-free makeup front cream without silicone oil, which adopts a water-soluble component of sodium polyacrylate to replace the traditional silicone oil polymer and is compounded with an extract component with a skin nourishing effect, so that pores and wrinkles can be filled, the pores are not closed, the skin can quickly absorb nutrient components, and the skin is more natural and transparent and can be more fitted and lasting.
In order to achieve the purpose, the invention adopts the following technical scheme: the pore-free makeup front cream without silicone oil is characterized by comprising the following components: sodium polyacrylate and extract with skin caring effect.
Preferably, the pore-free makeup front cream also comprises the following components: deionized water, 1, 3-propylene glycol, allantoin, sodium hyaluronate, sodium polyglutamate, 1, 2-hexanediol, butanediol, p-hydroxyacetophenone, hexanediol, 1, 2-pentanediol, caprylyl hydroxamic acid, glyceryl caprylate, and a colorant.
Preferably, the extract components having skin-nourishing effect include lactobacillus/eriodictyon fermentation product extract, hydrolyzed rice extract, spent grain water, lactobacillus fermentation lysate, burdock root extract, silybum marianum extract, paeonia radix extract, and gentian root extract.
Preferably, the pore-free makeup front cream comprises the following components in parts by weight: 75-85 parts of deionized water, 5-8 parts of 1, 3-propylene glycol, 2-5 parts of sodium polyacrylate, 1.5-2 parts of lactobacillus/eriodictyon fermentation product extract, 1.5-2 parts of hydrolyzed rice extract, 1.5-2 parts of rice lees water, 0.9-1.2 parts of lactobacillus fermentation lysate, 0.9-1.2 parts of burdock root extract, 0.9-1.2 parts of silybum marianum extract, 0.2-0.8 part of propylene glycol, 0.1-0.4 part of allantoin, 0.05-0.2 part of sodium hyaluronate, 0.05-0.2 part of sodium polyglutamate, 0.1-0.5 part of 1, 2-hexanediol, 0.1-0.3 part of butanediol, 0.05-0.2 part of p-hydroxyacetophenone, 0.08-0.16 part of hexanediol, 0.01-0.04 part of 1, 2-pentanediol, 0.1-025 part of caprylyl hydroxamic acid, 0.01-0.1.01-0.025 part of caprylic acid ester, Radix Paeoniae extract 0.01-0.05 parts, radix Gentianae extract 0.001-0.002 parts, and colorant 0.0006-0.001 parts.
Preferably, the colorant comprises CI 42090 and CI 19140.
The invention also provides a preparation method of the pore-free makeup front cream without silicone oil, which comprises the following steps:
step S1: weighing deionized water, sodium polyacrylate, 1, 3-propylene glycol, allantoin, p-hydroxyacetophenone, sodium hyaluronate and sodium polyglutamate in a 200ML beaker, placing on an electric furnace, stirring, heating to 85 ℃, homogenizing for 3 minutes, preserving heat for 20 minutes, sterilizing, and cooling;
step S2: cooling to 45 deg.C, adding caprylyl hydroximic acid, glyceryl caprylate and 1, 2-hexanediol dispersed with propylene glycol, and stirring to dissolve completely;
step S3: cooling to 40 deg.C, respectively adding lactobacillus/North American eriodictyon fermentation product extract, hydrolyzed rice extract, rice wine lees water, lactobacillus fermentation lysate, Maackia scabra root extract, herba Silybi Mariani extract, butanediol, 1, 2-pentanediol, hexanediol, radix Paeoniae extract, radix Gentianae extract, and colorant, stirring thoroughly, and mixing well;
step S4: cooling to 36 ℃, standing for 24 hours, and inspecting;
step S5: carrying out 50 ℃ heat resistance test for 48h, then carrying out minus 15 ℃ cold resistance test for 48h, recovering the room temperature, observing that the product has no abnormal sample, and judging the product to be qualified;
step S6: and (4) detecting microorganisms (bacteria and mould fungi), and judging the skin cream is qualified to obtain the skin cream without pores.
Preferably, in step S1, the stirring speed is 200 rpm, and the homogenizing speed is 2800 rpm.
Preferably, the stirring speed is 100 rpm in step S2 and step S3.
The effects of the important components of the invention are as follows:
the sodium polyacrylate is an edible additive component, is an unprecedented hydrophilic rheology modifier, and can be used for preparing products with different textures. The water-based product has excellent silicon elastic texture, matte appearance, extremely smooth feeling and powder texture, is easy to paint, has no sticky feeling, and has long-acting refreshing experience. The prepared 'zero pore cream' semi-permeable gel has a frosted appearance, and has optical dispersibility: make the skin look more transparent and elastic. Can better fill various fine lines of the skin, make the skin smooth and flat and more easy to use various makeup products, and enhance the makeup effect and the makeup duration.
The hydrolyzed rice extract is a rice composite fermentation product with anti-aging effect, and its preparation method comprises: inoculating the zymophyte into a fermentation substrate consisting of rice, burdock root, silybum marianum and water for fermentation culture, and then carrying out sterilization treatment to obtain the rice composite fermentation product with the anti-aging effect. The rice composite fermentation product has good anti-aging effect. The composition can be used as skin conditioner in cosmetics, and has mild and non-irritating effects, and can help skin supplement moisture and brighten skin. The rice is a finished product prepared by the working procedures of cleaning, hulling, milling, finishing and the like of the rice, contains nearly 64 percent of nutrient substances in the rice and more than 90 percent of nutrient elements required by a human body, and is a main food for people in most regions of China. The rice can provide abundant nutrients such as vitamins, oryzanol, protein, anthocyanin, etc. The rice has the skin care function, the rice extract is used as the main component (rich in y-oryzanol, rice chaff sterol, procyanidine and other components), has mild and safe properties and strong whitening effect, and can supplement water missing from the skin, so that the skin is smooth and fine and is full of elastic function.
The Lactobacillus/North American eriodictyon fermentation product extract has excellent moisturizing, lubricating and soothing properties, and can be used as a skin feel modifier to make the skin soft and smooth.
The rice wine lees water has promoting effect on the generation of cholesterol and cerebroamide, and is helpful for improving the softness and the moisture of the skin; has effects of activating glutathione reductase, improving skin function by combining with its oxidation resistance, and resisting aging.
The lactobacillus fermentation lysate contains thalli and all active ingredients synthesized in the fermentation process, contains peptidoglycan, teichoic acid, protein, phospholipid, sterol, fatty acid, various enzymes, peptide, amino acid, nucleotide, exopolysaccharide and the like, provides rich nutrition for skin, and has good anti-aging effect.
The extract of Arctium lappa has effect in inhibiting androgen level, and can be used for inhibiting acne and alopecia; has good antioxidant, antiaging, antiinflammatory, and antibacterial effects, and can be used for preventing scytitis; meanwhile, the contraction effect on the collagen fibers shows that the collagen fibers can astringe the skin and shrink pores.
The silybum marianum extract can capture and neutralize free radicals and inhibit the generation of malondialdehyde so as to inhibit saccharification reaction, has strong inoxidizability, and can remove yellow and brighten skin, wherein the inoxidizability is 10 times of that of vitamin E; good inhibition of elastase, and astringent effect on skin pores; the collagen structure in the skin can be kept unchanged, so that the generation of wrinkles is prevented, the smooth feeling and the firmness of the skin are improved, and the wrinkle depth is reduced.
The effective component paeoniflorin of the peony extract has inhibitory effect on some pathogenic bacteria and fungi; the inhibition of elastase, the elimination of free radicals, the inhibition of nitrogen oxide generation, the promotion of cathepsin activity and the like show that the skin-activating anti-aging liquid has the functions of activating skin and resisting aging and has better moisturizing capability.
The gentian root extract has a good activating effect on luciferase, so that the gentian root extract has an effect on atopic dermatitis and allergy, can inhibit stimulation and has an anti-inflammatory effect; the activation of aromatase shows that the aromatase inhibitor has an effect on the local estrogen level of the skin, and has an anti-aging effect on the inhibition and the anti-oxidation of elastase; it has effect in promoting the secretion of epidermal cell cholesterol, which is an important soft component in human sebum and can improve the state of oily rough skin.
The invention has the beneficial effects that:
(1) the invention adopts the water-soluble component of the sodium polyacrylate to replace the traditional silicone polymer, can fill pores and wrinkles, does not seal the pores, enables the skin to quickly enhance the absorption of nutrient components, better covers the pores of the skin, and enables the skin to be more natural and transparent and make up more comfortable and durable.
(2) According to the invention, extracts such as lactobacillus/eriodictyon officinalis fermentation product extract, hydrolyzed rice extract, lactobacillus fermentation lysate, burdock root extract, silybum marianum extract, paeonia lactiflora extract and gentian root extract are added, so that the problems of daily collagen loss, skin sensitivity, dryness, water shortage and the like of the skin can be effectively prevented, and various skin care effects such as water replenishing, moisture retaining, oxidation resistance and the like are achieved.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention is further illustrated by the following examples. It is to be understood that the following examples are only a few, but not all, of the present invention; it should be understood that the embodiments of the present invention are only for illustrating the technical effects of the present invention, and are not intended to limit the scope of the present invention.
The zero-pore makeup front cream without silicone oil in the embodiment of the invention comprises the following components: sodium polyacrylate and extract with skin caring effect.
The pore-free makeup front cream also comprises the following components: deionized water, 1, 3-propylene glycol, allantoin, sodium hyaluronate, sodium polyglutamate, 1, 2-hexanediol, butanediol, p-hydroxyacetophenone, hexanediol, 1, 2-pentanediol, caprylyl hydroxamic acid, glyceryl caprylate, and a colorant.
The extract component with skin caring effect comprises lactobacillus/eriodictyon fermentation product extract, hydrolyzed rice extract, rice wine lees, lactobacillus fermentation lysate, radix Arctii extract, herba Silybi Mariani extract, radix Paeoniae extract and radix Gentianae extract.
The pore-free make-up front cream comprises the following components in parts by weight: 75-85 parts of deionized water, 5-8 parts of 1, 3-propylene glycol, 2-5 parts of sodium polyacrylate, 1.5-2 parts of lactobacillus/eriodictyon fermentation product extract, 1.5-2 parts of hydrolyzed rice extract, 1.5-2 parts of rice lees water, 0.9-1.2 parts of lactobacillus fermentation lysate, 0.9-1.2 parts of burdock root extract, 0.9-1.2 parts of silybum marianum extract, 0.2-0.8 part of propylene glycol, 0.1-0.4 part of allantoin, 0.05-0.2 part of sodium hyaluronate, 0.05-0.2 part of sodium polyglutamate, 0.1-0.5 part of 1, 2-hexanediol, 0.1-0.3 part of butanediol, 0.05-0.2 part of p-hydroxyacetophenone, 0.08-0.16 part of hexanediol, 0.01-0.04 part of 1, 2-pentanediol, 0.1-025 part of caprylyl hydroxamic acid, 0.01-0.1.01-0.025 part of caprylic acid ester, Radix Paeoniae extract 0.01-0.05 parts, radix Gentianae extract 0.001-0.002 parts, and colorant 0.0006-0.001 parts.
The colorants include CI 42090 and CI 19140.
The embodiment of the invention also provides a preparation method of the pore-free makeup front cream without containing silicone oil, which comprises the following steps:
step S1: weighing deionized water, sodium polyacrylate, 1, 3-propylene glycol, allantoin, p-hydroxyacetophenone, sodium hyaluronate and sodium polyglutamate in a 200ML beaker, placing on an electric furnace, stirring, heating to 85 ℃, homogenizing for 3 minutes, preserving heat for 20 minutes, sterilizing, and cooling;
step S2: cooling to 45 deg.C, adding caprylyl hydroximic acid, glyceryl caprylate and 1, 2-hexanediol dispersed with propylene glycol, and stirring to dissolve completely;
step S3: cooling to 40 deg.C, respectively adding lactobacillus/North American eriodictyon fermentation product extract, hydrolyzed rice extract, rice wine lees water, lactobacillus fermentation lysate, Maackia scabra root extract, herba Silybi Mariani extract, butanediol, 1, 2-pentanediol, hexanediol, radix Paeoniae extract, radix Gentianae extract, and colorant, stirring thoroughly, and mixing well;
step S4: cooling to 36 ℃, standing for 24 hours, and inspecting;
step S5: carrying out 50 ℃ heat resistance test for 48h, then carrying out minus 15 ℃ cold resistance test for 48h, recovering the room temperature, observing that the product has no abnormal sample, and judging the product to be qualified;
step S6: and (4) detecting microorganisms (bacteria and mould fungi), and judging the skin cream is qualified to obtain the skin cream without pores.
In the present embodiment, in step S1, the stirring speed is 200 rpm, and the homogenizing speed is 2800 rpm.
In the present embodiment, the stirring speed is 100 rpm in both step S2 and step S3.
The compounded formula components are sequentially put into the preparation method to prepare, so that the product is more stable, and the active substances can better exert the effects of the active substances.
Item detection of the product of the invention:
randomly selecting the zero-pore makeup cream sample prepared by the preparation method, and carrying out inspection and measurement according to the national standard GB/T29665(O/W), wherein the detection result is shown in Table 1:
TABLE 1
As can be seen from Table 1, the zero-pore makeup cream prepared by the invention has no other abnormal appearance, meets the standard requirements, and also meets the standard in the detection of microorganisms (bacteria and mold).
Example 1
The pore-free make-up front cream comprises the following components in parts by weight: the paint comprises the following components in parts by weight: the balance of deionized water, 6 parts of 1, 3-propylene glycol, 3 parts of sodium polyacrylate, 1.5 parts of lactobacillus/eriodictyon fermentation product extract, 1.5 parts of hydrolyzed rice extract, 1.5 parts of rice wine lees water, 0.9 part of lactobacillus fermentation lysate, 0.9 part of burdock wuyue extract, 0.9 part of silybum marianum extract, 0.6 part of propylene glycol, 0.2 part of allantoin, 0.1 part of sodium hyaluronate, 0.1 part of sodium polyglutamate, 0.26 part of 1, 2-hexanediol, 0.16 part of butanediol, 0.1 part of p-hydroxyacetophenone, 0.08 part of hexanediol, 0.04 part of 1, 2-pentanediol, 0.025 part of caprylyl hydroxamic acid, 0.05 part of glyceryl caprylate, 0.04 part of radix paeoniae extract, 0.00175 part of radix gentianae extract and 0.0006 part of colorant.
Example 2
The pore-free make-up front cream comprises the following components in parts by weight: the paint comprises the following components in parts by weight: the balance of deionized water, 6 parts of 1, 3-propylene glycol, 3 parts of sodium polyacrylate, 1.75 parts of lactobacillus/eriodictyon fermentation product extract, 1.75 parts of hydrolyzed rice extract, 1.75 parts of rice stillage, 1.05 parts of lactobacillus fermentation lysate, 1.05 parts of burdock wuyue extract, 1.05 parts of silybum marianum extract, 0.6 part of propylene glycol, 0.2 part of allantoin, 0.1 part of sodium hyaluronate, 0.1 part of sodium polyglutamate, 0.26 part of 1, 2-hexanediol, 0.16 part of butanediol, 0.1 part of p-hydroxyacetophenone, 0.12 part of hexanediol, 0.04 part of 1, 2-pentanediol, 0.0625 part of octanoyl hydroxamic acid, 0.05 part of glycerol caprylate, 0.04 part of paeonia radix extract, 0.00175 part of gentian root extract and 0.0006 part of colorant.
Comparative example
Compared with the example 1, the sodium polyacrylate in the comparative example is changed into the traditional silicone oil polymer, and other components and mixture ratio are not changed.
The product of the invention has the following efficacy verification:
30 volunteers, 10 in each example and comparative example, were randomly selected, used before makeup for one month, the use results are shown in table 2, and the effects are classified into three grades:
concealer, penetrating, lasting effect is obvious: after the cosmetic is used, skin pores are fine, the integral glossiness of the skin is greatly improved, the skin is natural and transparent, and the makeup lasts for a long time.
The concealer, penetrating and lasting effects are general: after the cosmetic is used, skin pores are fine, the whole glossiness of the skin is not obviously improved, the skin is generally transparent, and the makeup durability is general.
Concealer, penetrating, lasting effect change is not obvious: after the cosmetic is used, skin pores are fine and normal, the integral glossiness of the skin is hardly improved, the skin is smooth and has a normal skin permeability and a normal makeup durability.
Table 2 shows the effects of examples 1 to 2 and comparative example 1
From the self-evaluation results of the testers, the finished product provided by the invention has better concealer, penetrating and lasting effects on most of the testers, and no phenomenon of irritability to the testers caused by the product is found. Thus, according to the survey results, it was shown that: the invention can better improve the rough skin pores, wrinkles and the like, enables the skin to be more natural and transparent and enables the makeup to be more appropriate and lasting.
In conclusion, the pore-free make-up cream prepared by the method in the embodiments 1-2 has good concealing and penetrating effects, good ductility and fresh skin feel; in the comparative example, the "sodium polyacrylate" was replaced with "silicone-oil-based polymer", and the corresponding functional effect was reduced.
The embodiments of the present invention are not limited to the above-mentioned embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and they are included in the scope of the present invention.
Claims (8)
1. The zero-pore makeup front cream is free of silicone oil and is characterized in that: comprises the following components: sodium polyacrylate and extract with skin caring effect.
2. The silicone oil-free pore-free makeup front cream according to claim 1, characterized in that: the pore-free makeup front cream also comprises the following components: deionized water, 1, 3-propylene glycol, allantoin, sodium hyaluronate, sodium polyglutamate, 1, 2-hexanediol, butanediol, p-hydroxyacetophenone, hexanediol, 1, 2-pentanediol, caprylyl hydroxamic acid, glyceryl caprylate, and a colorant.
3. The silicone oil-free pore-free makeup front cream according to claim 2, characterized in that: the extract component with skin caring effect comprises lactobacillus/eriodictyon fermentation product extract, hydrolyzed rice extract, rice wine lees, lactobacillus fermentation lysate, radix Arctii extract, herba Silybi Mariani extract, radix Paeoniae extract and radix Gentianae extract.
4. The silicone oil-free pore-free makeup front cream according to claim 3, characterized in that: the pore-free make-up front cream comprises the following components in parts by weight: 75-85 parts of deionized water, 5-8 parts of 1, 3-propylene glycol, 2-5 parts of sodium polyacrylate, 1.5-2 parts of lactobacillus/eriodictyon fermentation product extract, 1.5-2 parts of hydrolyzed rice extract, 1.5-2 parts of rice lees water, 0.9-1.2 parts of lactobacillus fermentation lysate, 0.9-1.2 parts of burdock root extract, 0.9-1.2 parts of silybum marianum extract, 0.2-0.8 part of propylene glycol, 0.1-0.4 part of allantoin, 0.05-0.2 part of sodium hyaluronate, 0.05-0.2 part of sodium polyglutamate, 0.1-0.5 part of 1, 2-hexanediol, 0.1-0.3 part of butanediol, 0.05-0.2 part of p-hydroxyacetophenone, 0.08-0.16 part of hexanediol, 0.01-0.04 part of 1, 2-pentanediol, 0.1-025 part of caprylyl hydroxamic acid, 0.01-0.1.01-0.025 part of caprylic acid ester, Radix Paeoniae extract 0.01-0.05 parts, radix Gentianae extract 0.001-0.002 parts, and colorant 0.0006-0.001 parts.
5. The silicone oil-free pore-free makeup front cream according to claim 4, characterized in that: the colorants include CI 42090 and CI 19140.
6. A method for preparing the pore-free makeup front cream according to any one of claims 1-5, characterized by comprising the following steps:
step S1: weighing deionized water, sodium polyacrylate, 1, 3-propylene glycol, allantoin, p-hydroxyacetophenone, sodium hyaluronate and sodium polyglutamate in a 200ML beaker, placing on an electric furnace, stirring, heating to 85 ℃, homogenizing for 3 minutes, preserving heat for 20 minutes, sterilizing, and cooling;
step S2: cooling to 45 deg.C, adding caprylyl hydroximic acid, glyceryl caprylate and 1, 2-hexanediol dispersed with propylene glycol, and stirring to dissolve completely;
step S3: cooling to 40 deg.C, respectively adding lactobacillus/North American eriodictyon fermentation product extract, hydrolyzed rice extract, rice wine lees water, lactobacillus fermentation lysate, Maackia scabra root extract, herba Silybi Mariani extract, butanediol, 1, 2-pentanediol, hexanediol, radix Paeoniae extract, radix Gentianae extract, and colorant, stirring thoroughly, and mixing well;
step S4: cooling to 36 ℃, standing for 24 hours, and inspecting;
step S5: carrying out 50 ℃ heat resistance test for 48h, then carrying out minus 15 ℃ cold resistance test for 48h, recovering the room temperature, observing that the product has no abnormal sample, and judging the product to be qualified;
step S6: and (4) detecting microorganisms (bacteria and mould fungi), and judging the skin cream is qualified to obtain the skin cream without pores.
7. The method for preparing the pore-free makeup front cream without silicone oil according to claim 6, characterized in that: in step S1, the stirring speed was 200 rpm, and the homogenization speed was 2800 rpm.
8. The method for preparing the pore-free makeup front cream without silicone oil according to claim 6, characterized in that: in both of the steps S2 and S3, the stirring speed was 100 rpm.
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| CN114042021A (en) * | 2021-10-28 | 2022-02-15 | 秦胜军 | Eye-moistening essence and preparation method thereof |
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