CN110721097A - Water-in-oil frost and preparation method and application thereof - Google Patents

Water-in-oil frost and preparation method and application thereof Download PDF

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CN110721097A
CN110721097A CN201911075737.9A CN201911075737A CN110721097A CN 110721097 A CN110721097 A CN 110721097A CN 201911075737 A CN201911075737 A CN 201911075737A CN 110721097 A CN110721097 A CN 110721097A
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water
oil
frost
cream
stirring
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CN110721097B (en
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郭潇潇
李楚忠
赵冰怡
胡根华
吴知情
胡兴国
胡根润
龚盛昭
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Guangzhou Huanya Cosmetic Science and Technology Co Ltd
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Guangzhou Huanya Cosmetic Science and Technology Co Ltd
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/84Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions otherwise than those involving only carbon-carbon unsaturated bonds
    • A61K8/89Polysiloxanes
    • A61K8/891Polysiloxanes saturated, e.g. dimethicone, phenyl trimethicone, C24-C28 methicone or stearyl dimethicone
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/02Cosmetics or similar toiletry preparations characterised by special physical form
    • A61K8/04Dispersions; Emulsions
    • A61K8/06Emulsions
    • A61K8/064Water-in-oil emulsions, e.g. Water-in-silicone emulsions
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/26Aluminium; Compounds thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/34Alcohols
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin

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Abstract

The invention provides a water-in-oil frost, a preparation method and application thereof, wherein the water-in-oil frost comprises the following components in percentage by weight according to 100% of the total mass: 13-18% of oil phase raw material, 2-4% of emulsifier, 3-5% of suspending agent, 18-28% of humectant and the balance of water; the oil phase raw materials comprise a fat-liquoring emollient and silicone oil with the viscosity of less than 10 cst. The invention combines the raw materials together according to a certain mass ratio for the first time to obtain the frost with semitransparent appearance, moisturizing, good stability and good use feeling. The preparation method of the water-in-oil frost disclosed by the invention has the advantages that the system does not need to be heated, the operation process is simple, and the time and energy cost can be effectively reduced.

Description

Water-in-oil frost and preparation method and application thereof
Technical Field
The invention relates to the technical field of cosmetics, in particular to a water-in-oil frost, a preparation method and application thereof.
Background
In summer, the skin is greatly lost due to comfortable air-conditioned room; the dry lack of water of skin is long-lived in autumn and winter that calms the rain, only relies on O/W type (oil in water type) cream temporary rapid water supplement far away not enough, and forms the lipid membrane on the skin surface after W/O type (water in oil type) cream is paintd, effectively reduces the percutaneous water loss rate of skin, and the lock water is moist, the persistence is good, must be the optimal choice.
The emulsion is a carrier for the most preferable delivery of active ingredients, and a W/O type cosmetic in which an oil phase is an external phase and an aqueous phase is an internal phase can effectively spread oil-soluble active ingredients, for example, emollient oil, oil-soluble drugs, ultraviolet absorbers, etc. on the skin, and thus is a suitable formulation for cosmetics, which is superior to the oil-in-water type. However, W/O emulsion systems also have some disadvantages: high oil phase is needed, and a refreshing formula is not easy to prepare; the skin feel is poor, and is generally sticky and heavy compared with the O/W type; the stability of the formula is greatly influenced by temperature change, and the difficulty of formula design and production process regulation is high. Therefore, W/O emulsion is difficult to gain the favor of consumers, and the development of the W/O emulsion in the market is greatly limited.
CN106726713A discloses a translucent moisturizing cream, which comprises polyhydric alcohols and silicone oils as main ingredients. The semitransparent cream disclosed by the invention is moist in skin feel and easy to operate. However, since silicones are volatile, the persistence of moisture retention remains to be examined.
CN109330903A discloses a preparation method and application of a transparent water-in-oil formulation, and the invention aims to provide a product with transparent quality and better usability. However, the transparency is too high, which inevitably limits the addition of the effective components.
Therefore, the development of a cream with translucent appearance, moisturizing, stability and good use feeling is a strong demand for the consumers in the market.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide the water-in-oil frost, the preparation method and the application thereof, the water-in-oil frost has the advantages of elastic and light texture, refreshing but not greasy, and excellent moisture retention, is the frost with both moisture retention and fresh skin feel, and meets the market demands of vast consumers at present.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the invention provides a water-in-oil frost, which is characterized in that the water-in-oil frost comprises the following components in percentage by weight based on 100% of the total mass of the water-in-oil frost: 13-18% of oil phase raw material, 2-4% of emulsifier, 3-5% of suspending agent, 18-28% of humectant and the balance of water; the oil phase raw materials comprise a fat-liquoring emollient and silicone oil with the viscosity of less than 10 cst.
The invention combines the raw materials together according to a certain mass ratio for the first time to obtain the frost cream with good water replenishing, moisture preserving, stability and use feeling. The water-in-oil frost disclosed by the invention is a W/O type system, has closed water locking property, and can be used for efficiently and durably moisturizing. Wherein, the oil phase raw material selects silicone oil with the viscosity of less than 10cst, the volatility is strong, the skin feel is fresh and cool, the smearing is easy, and simultaneously the grease-added emollient is reasonably matched, so that the obtained water-in-oil frost has the texture of fresh skin feel and moisturizing.
The oil phase raw material may be 13 to 18%, for example, 13%, 13.5%, 14%, 14.5%, 15%, 15.5%, 16%, 16.5%, 17%, 17.5%, 18%, or the like.
The emulsifier is 2 to 4%, and may be, for example, 2%, 2.3%, 2.5%, 2.8%, 3%, 3.2%, 3.5%, 3.7%, 3.8%, 3.9%, or 4%.
The suspending agent is 3 to 5%, and may be, for example, 3%, 3.2%, 3.5%, 3.6%, 3.8%, 4%, 4.1%, 4.3%, 4.5%, 4.8%, or 5%.
The humectant may be 18 to 28%, for example, 18%, 19%, 20%, 21%, 22%, 23%, 24%, 25%, 26%, 27%, 28%, or the like.
Preferably, the mass ratio of the fat-added emollient to the silicone oil with the viscosity of less than 10cst is 1 (5-15), and can be 1:5, 1:6, 1:7, 1:8, 1:9, 1:10, 1:11, 1:12, 1:13, 1:14 or 1:15, for example.
The invention preferably controls the mass ratio of the fat-liquoring emollient to the silicone oil with the viscosity of less than 10cst in the above range, mainly because when the mass ratio of the fat-liquoring emollient to the silicone oil is lower than 1:15, namely the content of the fat-liquoring emollient is less, the moisture and residual feeling of the water-in-oil cream can be reduced, and the skin feeling experience and long-acting moisture retention can be obviously reduced; when the mass ratio of the two is higher than 1:5, namely the content of the silicone oil with the viscosity of less than 10cst is reduced, the water-in-oil frost is easily too sticky and has poor skin feel, and meanwhile, the stability of the formula is also influenced due to the excessive content and strong polarity of the fat-type emollient; .
Preferably, the silicone oil with the viscosity below 10cst is polydimethylsiloxane with the viscosity below 10 cst.
Preferably, the lipidated emollient is a polar ester and/or a triglyceride.
Preferably, the polar ester is selected from any one of or a combination of at least two of diisostearyl malate, di-C12-13 alcohol malate, or jojoba oil.
Preferably, the humectant comprises a polyhydric alcohol.
Preferably, the amount of the polyhydric alcohol added is 18 to 22%, for example, 18%, 19%, 20%, 21%, 22%, or the like, based on 100% by mass of the total water-in-oil cream.
The reason why the amount of the polyhydric alcohol added is preferably controlled within the above range in the present invention is that the water phase component in the water-in-oil frost can be made to have a refractive index similar to that of the oil phase component only by limiting the content of the polyhydric alcohol within a fixed range, so that the resulting water-in-oil frost has a translucent appearance, and in addition, the excessive content of the polyhydric alcohol in the system causes the frost to generate heat significantly during use.
Preferably, the polyol is selected from any one of glycerol, sorbitol, butylene glycol or propylene glycol or a combination of at least two thereof.
Preferably, the humectant further comprises an alkyl amide and/or a saccharide.
The humectant of the present invention preferably further comprises alkylamides and/or saccharides, since alkylamides and/or saccharides can have a moisturizing synergistic effect with the polyhydric alcohol.
Preferably, the alkylamide is DL-lactamide.
Preferably, the saccharide is selected from any one of or a combination of at least two of beta-glucan, oat polysaccharide or tremella polysaccharide.
Preferably, the water-in-oil frost further comprises a stabilizer.
Preferably, the stabilizer is added in an amount of 0.5-1.5% based on 100% by mass of the water-in-oil cream.
Preferably, the stabilizer is magnesium sulfate and/or sodium chloride.
Preferably, the emulsifier has an HLB value of 3 to 6, and may be, for example, 3, 3.5, 4, 4.5, 5, 5.5, or 6, etc.
Preferably, the emulsifier consists of lauryl PEG-9 dimethiconoethyl dimethicone and PEG-10 dimethicone.
Preferably, the mass ratio of the lauryl PEG-9 polydimethylsiloxane to the PEG-10 polydimethylsiloxane is 1 (1-4), and can be 1:1, 1:2, 1:3, 1:4 and the like.
According to the invention, the two specific emulsifiers are preferably selected and the mass ratio of the two specific emulsifiers is controlled, so that the HLB value of the compounded composite emulsifier meets the range, and the frost-forming agent has good stability.
Preferably, the suspending agent is dimethylalkylammonium hectorite and/or distearyldimethylammonium chloride treated magnesium aluminum silicate.
The organic modified clay is preferably used as a suspending agent in the invention, so that the stability of the formula can be ensured, and the fluffy, elastic and moist texture of the frost can be improved.
Preferably, the water-in-oil cream further comprises a preservative.
Preferably, the preservative is phenoxyethanol and/or benzyl alcohol.
Preferably, the preservative is added in an amount of 0.1 to 1%, for example, 0.1%, 0.2%, 0.3%, 0.4%, 0.5%, 0.6%, 0.7%, 0.8%, 0.9% or 1% based on 100% of the total mass of the water-in-oil cream.
Preferably, the water-in-oil cream further comprises a perfume.
Preferably, the amount of the essence added is 0.05-0.3%, for example, 0.05%, 0.1%, 0.15%, 0.2%, 0.25%, 0.3%, or the like, based on 100% by mass of the water-in-oil cream.
In a second aspect, the present invention also provides a method for preparing the water-in-oil frost according to the first aspect, which comprises the following steps:
1) mixing a humectant, optionally a stabilizer, and water to obtain a first mixture;
2) mixing silicone oil with the viscosity of less than 10cst, a fat-added emollient, an emulsifier and a suspending agent to obtain a second mixture;
3) mixing and homogenizing the first mixture obtained in the step 1) and the second mixture obtained in the step 2) to obtain a third mixture;
4) adding an optional preservative and an optional essence into the third mixture obtained in the step 3), and mixing to obtain the water-in-oil frost.
The preparation method of the water-in-oil frost disclosed by the invention has the advantages that the system does not need to be heated, the operation process is simple, and the time and energy cost can be effectively reduced.
Preferably, the mixing method in step 1) is stirring at 500-1000rpm for 10-30 min.
The 500-1000rpm may be, for example, 500rpm, 600rpm, 700rpm, 800rpm, 900rpm, 1000rpm, or the like.
The time is 10-30min, such as 10min, 15min, 20min, 25min or 30 min.
Preferably, the mixing method in step 2) is stirring at the rotation speed of 1000-1500rpm for 10-30 min.
The 1000-1500rpm may be, for example, 1000rpm, 1100rpm, 1200rpm, 1300rpm, 1400rpm, 1500rpm, or the like.
The time period of 10-30min may be, for example, 10min, 15min, 20min, 25min or 30 min.
Preferably, step 3) comprises: pumping the first mixture obtained in the step 1) into the second mixture obtained in the step 2) by utilizing negative pressure, stirring, homogenizing, and defoaming in vacuum.
Preferably, the first mixture is pumped in for 20-30min, such as 20min, 22min, 25min, 27min or 30 min.
Preferably, the stirring time is 20-30min, such as 20min, 22min, 25min, 27min or 30 min.
Preferably, the rotation speed of the stirring is 1000-.
Preferably, the homogenizing rotation speed is 1500-.
Preferably, the homogenization time is 10-20min, such as 10min, 11min, 12min, 13min, 14min, 15min, 16min, 17min, 18min, 19min or 20 min.
Preferably, the mixing method in step 4) is stirring at the rotation speed of 1000-1500rpm for 3-10 min.
The 1000-1500rpm may be, for example, 1000rpm, 1100rpm, 1200rpm, 1300rpm, 1400rpm, 1500rpm, or the like.
The above-mentioned 3-10min may be, for example, 3min, 4min, 5min, 6min, 7min, 8min, 9min or 10 min.
In a third aspect, the present invention also provides the use of a water-in-oil cream according to the first aspect as a foundation, sunscreen or moisturising cream.
Compared with the prior art, the invention has the following beneficial effects:
(1) the oil-in-water cream is a W/O system, has closed water locking property, is efficient and durable in moisture retention, can present a semitransparent appearance, is good in stability, unique in texture, and is capable of preserving moisture and not greasy.
(2) The preparation method of the water-in-oil frost disclosed by the invention has the advantages that the system does not need to be heated, the operation process is simple, and the time and energy cost can be effectively reduced.
Drawings
FIG. 1(a) is a schematic diagram of the water-in-oil frost obtained in example 9.
FIG. 1(b) is a diagram showing a water-in-oil frost obtained in comparative example 8.
Detailed Description
The present invention is described in further detail below. The following examples are merely illustrative of the present invention and do not represent or limit the scope of the claims, which are defined by the claims.
The manufacturers and designations of some of the raw materials used in the examples are as follows:
polydimethylsiloxane (viscosity 5CST available from Dow Corning under the PMX200/5CS designation);
diisostearyl malate (available from sasol corporation under the designation COSMOL 222);
di-C12-13 alcohol malate (available from Nisshin under the trademark COSMACOL EMI);
lauryl PEG-9 Dimethylsiloxyethyl polydimethylsiloxane (available from shin-Etsu Co., Ltd., trade name KF-6038);
PEG-10 polydimethylsiloxane (available from shin-Etsu corporation under the trademark KF-6017);
a mixture of disteardimonium hectorite, cyclopentadimethylsiloxane and propylene carbonate (available from ELEMENTIS under the brand name BENTONE GEL VS-5PCV, where cyclopentadimethylsiloxane and propylene carbonate are solvents only, aid only, and do not suspend).
Examples 1 to 2
The embodiment provides a water-in-oil frost and a preparation method thereof.
Wherein the specific formula is shown in table 1.
The preparation method of this example includes the following steps:
1) sequentially adding the phase A raw materials into a water phase pot, and stirring for 20min to obtain a first mixture, wherein the stirring speed is 1000 rpm/min;
2) sequentially adding the phase B raw materials into an emulsifying pot, and stirring for 20min to obtain a second mixture, wherein the stirring speed is 1500 rpm/min;
3) pumping the first mixture obtained in the step 1) into the second mixture obtained in the step 2) by utilizing negative pressure, controlling the pumping time to be 25min, pumping while stirring, wherein the stirring rotation speed is 1500rpm, homogenizing for 10min at the stirring rotation speed of 3000rpm/min after pumping, and keeping vacuum defoaming;
4) adding a C-phase raw material into the third mixture obtained in the step 3), and stirring for 5min to obtain the water-in-oil frost, wherein the stirring speed is 1500 rpm/min; the steps 1) to 4) are all carried out in the normal temperature environment.
TABLE 1
Figure BDA0002262377210000081
Examples 3 to 5
The embodiment provides a water-in-oil frost and a preparation method thereof.
The preparation method of this group of examples was the same as that in examples 1-2.
Wherein the specific formula is shown in table 2.
TABLE 2
Figure BDA0002262377210000092
Examples 6 to 8
The present group of embodiments provides a water-in-oil frost and a method for preparing the same.
Wherein the specific formula is shown in table 3.
The preparation method of this group of examples was the same as that in examples 1-2.
TABLE 3
Figure BDA0002262377210000101
Example 9
The embodiment provides a water-in-oil frost and a preparation method thereof.
Wherein, the specific formula is shown in table 4.
The preparation method of this example was the same as that in example 1-2.
TABLE 4
Examples 10 to 13 and comparative example 1
The pair proportion provides a water-in-oil frost and a preparation method thereof.
Wherein, the specific formula is shown in table 5.
The preparation method of this comparative example was the same as that of example 1-2.
TABLE 5
Figure BDA0002262377210000112
Comparative examples 2 to 4
The pair proportion provides a water-in-oil frost and a preparation method thereof.
Wherein, the specific formula is shown in table 6.
The preparation method of this comparative example was the same as that of example 1-2.
TABLE 6
Figure BDA0002262377210000121
Comparative examples 5 to 7
The pair proportion provides a water-in-oil frost and a preparation method thereof.
Wherein, the specific formula is shown in table 7.
The preparation method of this comparative example was the same as that of example 1-2.
TABLE 7
Figure BDA0002262377210000131
Comparative example 8
The present comparative example provides a common moisturizing cream with a formulation as shown in table 8.
TABLE 8
Performance testing
1. Evaluation of skin appearance: the creams obtained in examples and comparative examples were evaluated for transparency, freshness and moisture retention.
Selecting 100 persons, taking the same amount of cream, and evaluating the transparency, the freshness and the moisture retention degree by visual inspection and hands, wherein each test is the arithmetic average of all person evaluation values.
The evaluation criteria are as follows:
transparency: completely transparent A, semi-transparent B, slightly transparent C, milky D;
refreshing degree: very fresh A, fresh B, a little greasy C and a very greasy D;
moisture preservation: very good moisture retention A, general moisture retention B, no feel C, and dryness D.
The specific evaluation results are shown in table 9, and fig. 1(a) and 1(b) show physical diagrams of the frosts obtained in example 9 and comparative example 8, respectively.
Comparing fig. 1(a) and fig. 1(b), it can be seen visually that the cream of example 9 of the present invention has a translucent appearance, is easy to push and apply, has unique texture, and has long moisture retention; the paste of comparative example 8 was milky white in appearance and clearly distinguished.
2. And (3) stability testing: placing 30g of paste in a PET bottle, performing temperature cycle test at-15 deg.C and 48 deg.C, changing temperature every 12h, recovering to room temperature after 1 week, and observing state change of the paste.
The evaluation criteria are as follows:
stability: and (3) completely separating oil from water A, wherein the oil permeability (referred to the operation process and the calculation method in QB/T1857-2013) is about 5 percent B, and the oil-water separation is obvious C.
The specific test results are shown in table 9.
TABLE 9
Figure BDA0002262377210000151
From the results in table 9, it can be seen that all the creams prepared by the examples of the present invention have a translucent appearance, a fresh and non-greasy skin feel, good moisture retention and good stability.
The two emulsifiers, namely lauryl PEG-9 polydimethylsiloxyethyl polydimethylsiloxane and PEG-10 polydimethylsiloxane, are compounded in the cream prepared in the embodiments 1 and 2, so that the skin feeling quality and the stability of the cream are superior to those of the cream prepared by using a single emulsifier in the embodiments 10 to 11, and the skin feeling and the stability of the cream can be effectively improved by using the two emulsifiers; in addition, the skin feel quality and stability of the cream prepared in examples 1-2 are superior to those of examples 12-13, because the two emulsifiers of the invention can be matched with each other only by compounding within a certain mass range, so that the skin feel and stability can be effectively improved only by controlling the HLB value within a proper range. In addition, in comparative example 1, the emulsifier content was high, the skin feel was heavy and the spreadability was slightly poor as compared with examples 1 and 2, because in a water-in-oil emulsion system, the higher the emulsifier content, the more stable the emulsifier content was, and when the emulsifier content was higher than a certain range, the stability of the system was often reduced. That is, the amount of the emulsifier is controlled within the range of the present invention to ensure good stability of the system. Therefore, controlling the amount of the two emulsifiers and the mass ratio of the two emulsifiers is the key to excellent skin feel and stability.
The appropriate internal-external phase ratio will improve the stability of the system, while the consistency of the W/O system is mainly dependent on the emulsifier and internal-external phase ratio. In order to achieve fresh skin feel and good spreadability, polydimethylsiloxane with low viscosity and high volatility is specifically selected as a main oil phase raw material, and solid and semi-solid grease is abandoned and other high-viscosity grease-added emollients are compounded in consideration of the fact that the W/O system needs to meet the characteristic of easiness in spreading. Compared with the examples 3-5, the cream prepared in the comparative example 2 has high silicon oil content and high system transparency, but the moisture retention is obviously lower than that of the cream prepared in the examples 3-5 of the compound moisturizing grease; the stability, transparency and freshness of the frost obtained by the comparative examples 3-4 with too high fat content of the fatliquoring type are all as in the examples 3-5, which shows that the stability of the formula is influenced by high polarity of the fat, the use feeling is thick and sticky, and the transparency is reduced. Therefore, the skin feeling can be ensured to be fresh and cool by selecting the grease with proper proportion for compounding, and the moisture retention and the stability are good.
Polyols are classic cosmetic moisturizers, also concerning the low temperature stability of W/O systems. As can be seen from Table 9, the polyol content in comparative example 7 was too high, and the transparency was higher in appearance than those of examples 6 to 8, but the heat sensation during use was significant; comparative examples 5-6 the creams had lower polyol content and lower clarity than examples 6-8; thus, a moderate amount of polyol content contributes to the translucent appearance. The variety of the selected polyhydric alcohol comprehensively considers skin feel, raw material price and diversity, so that the skin feel is avoided from being sticky, a semitransparent appearance is formed, and the timely supply and reasonable cost of the raw materials are ensured.
3. Test for moisture Retention of human body
(1) An experimental instrument: skin moisture Corneometer test probe manufactured by CK, Germany.
(2) The experimental method comprises the following steps: selecting 20 females with the age of 25-45 years. Before the test, the subject is required to wash both arms, and after 2 hours of washing, the subject sits statically for 30min in a constant temperature and humidity room with the temperature of 22 +/-1 ℃ and the humidity of 50 +/-5%, and is kept in a relaxed state.
The creams obtained in the examples and comparative examples according to the invention were applied and tested on the subjects' double forearms according to the double-blind principle, respectively, at T0(initial state), T0.5h(after 30min of sample application), T4h(after 4h of application), T8hThe skin hydration measurements were performed (8 h after application).
The results of the specific tests are shown in Table 10.
Watch 10
Figure BDA0002262377210000181
As can be seen from the results in Table 10, the skin moisture content of the cream prepared in the example of the present invention after application was significantly higher than that of the O/W system of comparative example 8, and the skin moisture content decreased less than that of comparative example 8 with the increase of the application time. This shows that the cream obtained by the embodiment of the invention has good moisture retention and the moisture retention also has durability.
Compared with the examples, the water content of the skin of the cream prepared in the comparative example 2 is obviously lower after the cream is applied to the skin of a human body, and the reduction range of the water content of the skin is higher than the examples along with the increase of the application time, which shows that the higher the content of the selected low-viscosity polydimethylsiloxane is, the poorer the moisturizing effect and the moisturizing durability of the selected low-viscosity polydimethylsiloxane on the skin are, and the higher the content of the low-viscosity polydimethylsiloxane is, the moisturizing capability of the prepared water-in-oil cream on the skin is also reduced; the moisture content of the creams prepared in the comparative examples 3 and 4 is higher than that of the examples after the creams are applied to human skin, and the reduction range of the moisture content of the skin is lower than that of the examples along with the increase of the application time, because the higher the content of the fat-added type emollient is, the residual feeling is strong, the film strength is high, the moisturizing capability of the cream on the skin is obviously enhanced, but the stability, the transparency and the refreshing feeling of the cream are obviously reduced, so the skin feeling is fresh and cool, and the moisturizing property and the stability can be considered only by selecting two kinds of fats in a reasonable range for compounding.
In conclusion, the W/O frost cream prepared by the invention has more obvious water retention capacity on skin, can effectively increase the water content of the horny layer, reduce the water loss of the horny layer of the skin and improve the moistening degree and smoothness of the skin.
4. Human skin irritation test
The experimental method comprises the following steps: 60 women with healthy skin were selected, and the age ranged from 20 to 50 years. The skin on both sides of the arm is the tested part, 0.03g of the frost cream prepared in the embodiment and the comparative example is respectively coated on the tested part, and then the spot tester adhesive tape added with the spot test substance is firmly pasted; the patch test time is 48h, then the patch tester is removed, the test result is observed and recorded after 30min, and 6 patch tests are carried out totally. The identification criteria are shown in Table 11 and the results are shown in Table 12.
TABLE 11
TABLE 12
Figure BDA0002262377210000192
Figure BDA0002262377210000201
As can be seen from table 13, the cream prepared in the examples is not irritating to the skin, while the cream prepared in comparative example 7 has a remarkable heat-generating and irritating feeling due to the use of a large amount of polyol; the experiments prove that the water-in-oil frost cream prepared by the invention is safe, mild and non-irritant.
5. Human body trial evaluation experiment
The experimental method comprises the following steps: 60 volunteers aged 20-40 years are selected as test objects, the frost cream obtained in the example 9 and the comparative example 8 is subjected to human body trial evaluation, the period is one month, and the skin feeling preference, the humidity preservation degree, the glossiness and the irritation evaluation are performed on the sample in the using process, wherein the highest score is 5, and the lowest score is 0. Filling out a trial evaluation table according to the sensory evaluation, collecting the half-face experiment trial evaluation table, taking the arithmetic mean of the evaluation scores, and obtaining the statistical result shown in the table 13.
Watch 13
Evaluation results Example 9 Comparative example 8
Skin feel preference 5 points of 4.8 points
Moisture retention 5 points of 3 points of
Degree of gloss 4.5 points 3 points of
Irritation property 0 point (min) 0 point (min)
As can be seen from the results in Table 13, the results of human half-face test evaluation can be compared with those of example 9 and comparative example 8, and it can be seen that the skin feel and moisture retention of the cream prepared by the present invention are more satisfactory to consumers without irritation or side effects.
In conclusion, the water-in-oil cream disclosed by the invention is good in stability, good in appearance and skin feel, remarkable in moisture retention, mild and non-irritant, and can restore the dry skin to a moist, smooth, glossy and fine health state. With the expansion of market and consumer demands, the W/O translucent cream system is increasingly applied to various care products, such as foundation liquid, sunscreen cream, moisturizing cream and various curative products.
The applicant declares that the present invention illustrates the detailed structural features of the present invention through the above embodiments, but the present invention is not limited to the above detailed structural features, that is, it does not mean that the present invention must be implemented depending on the above detailed structural features. It should be understood by those skilled in the art that any modifications of the present invention, equivalent substitutions of selected components of the present invention, additions of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.

Claims (10)

1. The water-in-oil frost is characterized by comprising the following components in percentage by weight according to 100 percent of the total mass: 13-18% of oil phase raw material, 2-4% of emulsifier, 3-5% of suspending agent, 18-28% of humectant and the balance of water;
the oil phase raw materials comprise a fat-liquoring emollient and silicone oil with the viscosity of less than 10 cst.
2. The water-in-oil cream according to claim 1, characterized in that the mass ratio of the fat-added emollient to the silicone oil having a viscosity of 10cst or less is 1 (5-15);
preferably, the silicone oil with the viscosity of below 10cst is polydimethylsiloxane with the viscosity of below 10 cst;
preferably, the lipidated emollient is a polar ester and/or a triglyceride;
preferably, the polar ester is selected from any one of or a combination of at least two of diisostearyl malate, di-C12-13 alcohol malate, or jojoba oil.
3. Water-in-oil cream according to claim 1 or 2, characterized in that said humectant comprises a polyhydric alcohol;
preferably, the addition amount of the polyhydric alcohol is 18-22% based on the total mass of the water-in-oil frost cream as 100%;
preferably, the polyhydric alcohol is selected from any one or a combination of at least two of glycerol, sorbitol, butylene glycol or propylene glycol;
preferably, the humectant further comprises a surfactant selected from alkyl amides or saccharides;
preferably, the alkylamide is DL-lactamide;
preferably, the saccharide is selected from any one or a combination of at least two of beta-glucan, oat polysaccharide or tremella polysaccharide;
preferably, the water-in-oil frost further comprises a stabilizer;
preferably, the addition amount of the stabilizer is 0.5-1.5% based on the total mass of the water-in-oil frost;
preferably, the stabilizer is magnesium sulfate and/or sodium chloride.
4. The water-in-oil cream according to any one of claims 1 to 3, characterized in that the emulsifier has an HLB value of 3 to 6;
preferably, the emulsifier consists of lauryl PEG-9 polydimethylsiloxyethyl dimethicone and PEG-10 dimethicone;
preferably, the mass ratio of the lauryl PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane to the PEG-10 polydimethylsiloxane is 1 (1-4).
5. The water-in-oil cream according to any one of claims 1 to 4, characterized in that the suspending agent is dimethylalkylammonium hectorite and/or distearyldimethylammonium chloride treated magnesium aluminum silicate.
6. Water-in-oil cream according to any of claims 1 to 5, characterized in that it further comprises a preservative;
preferably, the preservative is phenoxyethanol and/or benzyl alcohol;
preferably, the addition amount of the preservative is 0.1-1% based on the total mass of the water-in-oil frost cream as 100%;
preferably, the water-in-oil cream further comprises a perfume;
preferably, the adding amount of the essence is 0.05-0.3% by taking the total mass of the water-in-oil frost as 100%.
7. A method of making a water-in-oil frost according to any of claims 1 to 6, comprising the steps of:
1) mixing a humectant, optionally a stabilizer, and water to obtain a first mixture;
2) mixing silicone oil with the viscosity of less than 10cst, a fat-added emollient, an emulsifier and a suspending agent to obtain a second mixture;
3) mixing and homogenizing the first mixture obtained in the step 1) and the second mixture obtained in the step 2) to obtain a third mixture;
4) adding an optional preservative and an optional essence into the third mixture obtained in the step 3), and mixing to obtain the water-in-oil frost.
8. The method as claimed in claim 7, wherein the mixing step 1) is performed by stirring at 500-1000rpm for 10-30 min;
preferably, the mixing method in step 2) is stirring at the rotation speed of 1000-1500rpm for 10-30 min.
9. The method of manufacturing according to claim 7 or 8, wherein step 3) includes: pumping the first mixture obtained in the step 1) into the second mixture obtained in the step 2) by utilizing negative pressure, stirring, homogenizing, and defoaming in vacuum;
preferably, the first mixture is pumped in for 20-30 min;
preferably, the stirring time is 20-30 min;
preferably, the rotation speed of the stirring is 1000-;
preferably, the rotation speed of the homogenizing device is 1500-;
preferably, the homogenization time is 10-20 min;
preferably, the mixing method in step 4) is stirring at the rotation speed of 1000-1500rpm for 3-10 min.
10. Use of the water-in-oil cream according to any one of claims 1 to 6 as a foundation, sunscreen or moisturizer.
CN201911075737.9A 2019-11-06 2019-11-06 Water-in-oil frost and preparation method and application thereof Active CN110721097B (en)

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CN115475107A (en) * 2022-09-09 2022-12-16 广州环亚化妆品科技股份有限公司 Water-in-oil type skin cream and preparation method thereof
CN115804733A (en) * 2022-12-29 2023-03-17 羽楠(广州)化妆品有限公司 Gel-in-oil moisturizing composition and preparation method and application thereof

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CN105832574A (en) * 2016-06-07 2016-08-10 广州立白企业集团有限公司 Sun-screening and skin-protecting day cream with water mist cream characteristic and preparation method thereof
CN106726713A (en) * 2016-12-14 2017-05-31 诺斯贝尔化妆品股份有限公司 A kind of translucent moisturizing cream
CN109330903A (en) * 2018-11-29 2019-02-15 四川省中医药科学院 A kind of clean oil packet water aqua type preparation method and applications

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CN105832574A (en) * 2016-06-07 2016-08-10 广州立白企业集团有限公司 Sun-screening and skin-protecting day cream with water mist cream characteristic and preparation method thereof
CN106726713A (en) * 2016-12-14 2017-05-31 诺斯贝尔化妆品股份有限公司 A kind of translucent moisturizing cream
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CN115475107A (en) * 2022-09-09 2022-12-16 广州环亚化妆品科技股份有限公司 Water-in-oil type skin cream and preparation method thereof
CN115804733A (en) * 2022-12-29 2023-03-17 羽楠(广州)化妆品有限公司 Gel-in-oil moisturizing composition and preparation method and application thereof

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