CN111888276A - Lip care compositions containing novel phytosterol additives and methods of making same - Google Patents
Lip care compositions containing novel phytosterol additives and methods of making same Download PDFInfo
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- CN111888276A CN111888276A CN201910372219.7A CN201910372219A CN111888276A CN 111888276 A CN111888276 A CN 111888276A CN 201910372219 A CN201910372219 A CN 201910372219A CN 111888276 A CN111888276 A CN 111888276A
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- 238000000034 method Methods 0.000 title claims description 16
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- NOPFSRXAKWQILS-UHFFFAOYSA-N docosan-1-ol Chemical compound CCCCCCCCCCCCCCCCCCCCCCO NOPFSRXAKWQILS-UHFFFAOYSA-N 0.000 claims abstract description 52
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- WNIFXKPDILJURQ-JKPOUOEOSA-N octadecyl (2s,4as,6ar,6as,6br,8ar,10s,12as,14br)-10-hydroxy-2,4a,6a,6b,9,9,12a-heptamethyl-13-oxo-3,4,5,6,6a,7,8,8a,10,11,12,14b-dodecahydro-1h-picene-2-carboxylate Chemical compound C1C[C@H](O)C(C)(C)[C@@H]2CC[C@@]3(C)[C@]4(C)CC[C@@]5(C)CC[C@@](C(=O)OCCCCCCCCCCCCCCCCCC)(C)C[C@H]5C4=CC(=O)[C@@H]3[C@]21C WNIFXKPDILJURQ-JKPOUOEOSA-N 0.000 description 1
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- VLPFTAMPNXLGLX-UHFFFAOYSA-N trioctanoin Chemical compound CCCCCCCC(=O)OCC(OC(=O)CCCCCCC)COC(=O)CCCCCCC VLPFTAMPNXLGLX-UHFFFAOYSA-N 0.000 description 1
- 235000019165 vitamin E Nutrition 0.000 description 1
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- GVJHHUAWPYXKBD-IEOSBIPESA-N α-tocopherol Chemical compound OC1=C(C)C(C)=C2O[C@@](CCC[C@H](C)CCC[C@H](C)CCCC(C)C)(C)CCC2=C1C GVJHHUAWPYXKBD-IEOSBIPESA-N 0.000 description 1
Images
Classifications
-
- 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
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/63—Steroids; Derivatives thereof
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
- A61Q19/001—Preparations for care of the lips
-
- 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
- A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
- A61K2800/59—Mixtures
- A61K2800/592—Mixtures of compounds complementing their respective functions
- A61K2800/5922—At least two compounds being classified in the same subclass of A61K8/18
Landscapes
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Dermatology (AREA)
- Birds (AREA)
- Epidemiology (AREA)
- Cosmetics (AREA)
Abstract
The invention discloses a lip care composition containing a novel phytosterol additive, which is prepared by taking phytosterol and phytosterol ester as active ingredients, selecting cetyl alcohol and behenyl alcohol to improve the solubility and the melting point of a system, and mixing the components in a better weight part ratio. The components of the lip care composition take effect synergistically, can effectively exert the characteristics of the phytosterol additive, and effectively improve the skin-friendly property of the product. The prepared lipstick has the effects of long-acting moisture retention, moistening and lip gloss improvement.
Description
Technical Field
The invention relates to a lip care composition, in particular to a lip care composition added with a novel phytosterol additive and a preparation method thereof.
Background
The lip skin has only 3-5 layers of corneocytes, and the thickness is 1/6 of the stratum corneum of the facial skin. The lips can not secrete grease by themselves because of no sebaceous glands, and the lips are not protected by a sebaceous layer, so that the water evaporation speed can reach six times of that of the facial skin. Therefore, the skin of the lips is easily affected by the external environment and physical conditions, resulting in dry, flaky, dull, and lusterless conditions.
Lip balm application is a common method for improving the dryness and the peeling of the lips and improving the glossiness of the lips. However, the lip balm sold on the market at present generally improves the lip problems in a short time by utilizing the sealing property of solid grease, and the lip balm cannot have the effect of long-term repair after the lip balm is stopped being used and the symptoms are repeated.
The phytosterol is used in lip care products, and has the effects of keeping the moisture on the skin surface of lips, improving the dryness and the peeling of the lips and improving the glossiness of the lips. However, the phytosterol is difficult to be added into lip care products, because free phytosterol is extremely difficult to dissolve in water and has low oil solubility, the solubility in ethanol is only 1.17g/100mL (23 ℃), the phytosterol is difficult to be applied to a lip care formula, and the low solubility also directly influences the efficacy of the phytosterol in the lip care products. The melting point of the phytosterol is higher and is 130-180 ℃, the highest preparation temperature in lipstick production is generally not more than 100 ℃, and the preparation temperature is lower for cosmetics containing plant extracts, so that the operability of adding the phytosterol in the cosmetics is greatly limited by the preparation method of the cosmetics.
In order to improve the solubility and melting point, those skilled in the art generally modify the phytosterol molecules by physical and chemical methods, wherein the physical modification is mainly to improve the dispersibility, and the chemical modification is to graft lipophilic/hydrophilic groups on the phytosterol molecules to improve the solubility. The conventional modification method is to disperse the phytosterol in an aqueous-oil system (such as liposome) by using an emulsifier, but the emulsifying system is not favorable for the release of the phytosterol on the skin surface, and the utilization efficiency of the phytosterol is influenced. The phytosterol is catalyzed to form phytosterol ester, the solubility and the melting point of the phytosterol ester can also be improved, and the phytosterol ester is increasingly widely applied to cosmetics, however, the phytosterol ester needs pancreatic cholesterol esterase to be hydrolyzed into free sterol in a human body to be absorbed, so that the phytosterol ester is used in the cosmetics to influence the skin effect of the phytosterol ester. In addition, the phytosterol ester is grafted with long-chain fatty acid, so that the proportion of active groups is reduced, and the efficacy is reduced compared with that of free phytosterol.
The inventors of the present invention found that: cholesterol is an important skin structure lipid and is essential for maintaining skin structure and function. Cholesterol and cholesterol ester exist in the skin at the same time, and the cholesterol ester is converted into cholesterol under the action of enzyme, so that structural lipid is continuously provided for the skin. Phytosterols have a similar structure to cholesterol and can exert cholesterol-like effects on the skin. If the phytosterol and the phytosterol ester are simultaneously applied to cosmetics, the skin structure lipid can be simulated, and the ratio of sterol active groups in the formula can be increased. However, the simultaneous use of phytosterol and phytosterol ester has a great technical problem that phytosterol and phytosterol ester are not mutually soluble, the simultaneous addition has poor solubility and poor efficacy, and the problem causes the limitation of the combined application of phytosterol and phytosterol ester.
How to solve the above technical problems is still the focus of research by those skilled in the art.
Disclosure of Invention
The invention aims to provide a novel phytosterol additive which can improve the intersolubility of phytosterol and phytosterol ester, enables the phytosterol and the phytosterol ester to be simultaneously added into cosmetics and has good solubility and low melting point, and the obtained cosmetics have strong formula operability and improved skin-friendly property.
A second object of the present invention is to propose a lip care composition containing the above additive.
The third purpose of the invention is to provide a preparation method of the lip care composition.
The fourth purpose of the invention is to provide the lipstick which is prepared by the method and has the effects of long-acting moisture retention, moistening and lip gloss improvement.
In order to achieve the purpose, the invention adopts the following technical scheme:
a lip care composition containing a novel phytosterol additive, wherein the composition consists of a phase A, a phase B and a phase C, and the phase A, the phase B and the phase C consist of the following raw materials:
0.08-8.00 wt% of A-phase phytosterol additive
B phase petrolatum balance
5.00-15.00 wt% of beeswax
2.00-8.00 wt% of glyceryl behenate/eicosanoate
3.00-15.00 wt% of C-phase octyl polymethylsiloxane
0 to 10.00 wt% of hydrogenated polyisobutene
1-10.00 wt% of shea butter
0.10-2.00 wt% of tocopherol acetate
Butylated hydroxytoluene 0.03-0.20 wt%
0.10-0.14 wt% of propyl hydroxybenzoate;
the A-phase phytosterol additive is prepared from behenyl alcohol, cetyl alcohol, phytosterol and phytosterol ester, and the weight parts of the raw materials are as follows:
1 to 5 portions of behenyl alcohol, 1 to 5 portions of cetyl alcohol, 1 to 5 portions of phytosterol and 0.1 to 10 portions of phytosterol ester.
Preferably, the weight ratio of the phytosterol to the phytosterol ester in the phytosterol additive is 1: 0.1 to 2.
Preferably, the preparation method of the phytosterol additive comprises the following steps:
(1) preparing the raw materials according to the weight part ratio;
(2) mixing the behenyl alcohol, the cetyl alcohol and the phytosterol, heating to 70-100 ℃, stirring at a rotating speed of 100-400 rpm, and reacting for 5-60 minutes to obtain a first solution;
(3) and cooling the solution I to 60-90 ℃, adding the phytosterol ester into the solution I, stirring at the rotating speed of 100-400 r/min, continuously reacting for 1-30 min, and cooling to room temperature to obtain the phytosterol ester.
A method for preparing the lip care composition, wherein the method comprises the following steps:
(1) mixing and heating the raw materials of the phase B until the material body becomes transparent for later use;
(2) mixing the raw materials of the phase C with the phase A, and heating and stirring until the raw materials are completely dissolved;
(3) adding the mixture of the phase C and the phase A prepared in the step (2) into the phase B prepared in the step (1), and uniformly stirring;
(4) cooling to 60-65 ℃, filling and demolding to obtain the product.
Preferably, the heating temperature in the step (1) is 40-70 ℃.
Preferably, the heating temperature in the step (2) is 40-70 ℃, and the stirring speed is 100-300 r/min.
A lipstick containing a novel phytosterol additive is prepared by the method.
The preparation method of the composition is a better preparation method recommended by the inventor, has strong operability, and has the main invention point that the preparation method can select other preparation methods known by the technicians in the field on the selection and the compounding of raw materials, and the product effect is not influenced.
The preparation method of the lip care composition can be selected from the lip care product preparation methods known by persons skilled in the art, and the method is a preferred preparation method recommended by the inventor and is not limited by the invention.
The invention has the beneficial effects that:
the invention takes the phytosterol and the phytosterol ester as active ingredients, selects the cetyl alcohol and the behenyl alcohol to improve the solubility and the melting point of a system, and obtains the phytosterol composition through a better weight part ratio, thereby solving the problem of poor intersolubility of the phytosterol and the phytosterol ester which are simultaneously added in the prior art, simultaneously obtaining the composition with good oil solubility and low melting point, having strong operability in the formula of the lip care composition, and being beneficial to the industrial application of the phytosterol to cosmetics. The components of the lip care composition take effect synergistically, can effectively exert the characteristics of the phytosterol additive, and effectively improve the skin-friendly property of the product. The prepared lipstick has the effects of long-acting moisture retention, moistening and lip gloss improvement.
Drawings
FIG. 1 is a DSC plot of five samples;
FIG. 2 is a microscope photograph of the experiment of dissolving caprylic/capric triglyceride;
fig. 3 is a comparison of the essential oil deposition phenomenon prepared in example 1 and comparative example 6(3 wt%).
Detailed Description
All of the starting materials used in this example were commercially available. The raw material sources used in the examples of the present invention are shown in Table 1, and the names and manufacturers of the instruments used in the present invention are shown in Table 2.
TABLE 1
TABLE 2
| Name of instrument | Model number | Manufacturer of the product |
| Electronic balance | TB-2002 | Beijing Sadolis Instrument systems, Inc |
| Intelligent temperature-control heating stirrer | SZCL | Instrument Limited of consolidated City |
| Electric heating constant temperature water bath | HH·S1-M | Beijing Changan scientific instrument factory |
EXAMPLE 1 preparation of the phytosterol additive of the present invention
(1) Preparing the raw materials according to the following weight part ratio;
50g of behenyl alcohol, 150g of cetyl alcohol, 150g of phytosterol and 150g of phytosterol ester;
(2) mixing behenyl alcohol, cetyl alcohol and phytosterol, heating to 80 ℃, stirring at the rotating speed of 100 revolutions per minute, and reacting for 40 minutes to obtain a solution I;
(3) and cooling the solution I to 60 ℃, adding the phytosterol ester into the solution I, stirring at the rotating speed of 100 revolutions per minute, continuing to react for 20 minutes, and cooling to room temperature to obtain the phytosterol ester.
EXAMPLE 2 preparation of the phytosterol additive of the present invention
(1) Preparing the raw materials according to the following weight part ratio;
20g of behenyl alcohol, 100g of cetyl alcohol, 100g of phytosterol and 200g of phytosterol ester;
(2) mixing behenyl alcohol, cetyl alcohol and phytosterol, heating to 70 ℃, stirring at the rotating speed of 200 revolutions per minute, and reacting for 60 minutes to obtain a solution I;
(3) and cooling the solution I to 60 ℃, adding the phytosterol ester into the solution I, stirring at the rotating speed of 200 revolutions per minute, continuously reacting for 10 minutes, and cooling to room temperature to obtain the phytosterol ester.
EXAMPLE 3 preparation of the phytosterol additive of the present invention
(1) Preparing the raw materials according to the following weight part ratio;
100g of behenyl alcohol, 100g of cetyl alcohol, 100g of phytosterol and 100g of phytosterol ester;
(2) mixing behenyl alcohol, cetyl alcohol and phytosterol, heating to 100 ℃, stirring at the rotating speed of 400 r/min, and reacting for 5 minutes to obtain a solution I;
(3) and cooling the solution I to 90 ℃, adding the phytosterol ester into the solution I, stirring at the rotating speed of 300 revolutions per minute, continuing to react for 20 minutes, and cooling to room temperature to obtain the phytosterol ester.
EXAMPLE 4 preparation of the phytosterol additive of the present invention
(1) Preparing the raw materials according to the following weight part ratio;
20g of behenyl alcohol, 50g of cetyl alcohol, 100g of phytosterol and 50g of phytosterol ester;
(2) mixing behenyl alcohol, cetyl alcohol and phytosterol, heating to 90 ℃, stirring at the rotating speed of 200 revolutions per minute, and reacting for 30 minutes to obtain a solution I;
(3) and cooling the solution I to 70 ℃, adding the phytosterol ester into the solution I, stirring at the rotating speed of 400 r/min, continuously reacting for 30 min, and cooling to room temperature to obtain the phytosterol ester.
EXAMPLE 5 preparation of the phytosterol additive of the present invention
(1) Preparing the raw materials according to the following weight part ratio;
50g of behenyl alcohol, 100g of cetyl alcohol, 150g of phytosterol and 15g of phytosterol ester;
(2) mixing behenyl alcohol, cetyl alcohol and phytosterol, heating to 100 ℃, stirring at the rotating speed of 300 r/min, and reacting for 20 minutes to obtain a solution I;
(3) and cooling the solution I to 60 ℃, adding the phytosterol ester into the solution I, stirring at the rotating speed of 200 revolutions per minute, continuously reacting for 1 minute, and cooling to room temperature to obtain the phytosterol ester.
EXAMPLE 6 preparation of the phytosterol additive of the present invention
(1) Preparing the raw materials according to the following weight part ratio;
50g of behenyl alcohol, 100g of cetyl alcohol, 50g of phytosterol and 5g of phytosterol ester;
(2) mixing behenyl alcohol, cetyl alcohol and phytosterol, heating to 80 ℃, stirring at the rotating speed of 200 revolutions per minute, and reacting for 15 minutes to obtain a solution I;
(3) and cooling the solution I to 60 ℃, adding the phytosterol ester into the solution I, stirring at the rotating speed of 200 revolutions per minute, continuing to react for 15 minutes, and cooling to room temperature to obtain the phytosterol ester.
EXAMPLE 7 preparation of a lipstick according to the invention
Raw materials and dosage are shown in table 3:
TABLE 3
The preparation method comprises the following steps:
(1) mixing and heating the raw materials of the phase B until the material body becomes transparent for later use;
(2) mixing the raw materials of the phase C with the phase A, and heating and stirring until the raw materials are completely dissolved;
(3) adding the mixture of the phase C and the phase A prepared in the step (2) into the phase B prepared in the step (1), and uniformly stirring;
(4) cooling to 60 deg.C, bottling, and demolding.
EXAMPLE 8 preparation of a lipstick according to the invention
Raw materials and dosage are shown in table 4:
TABLE 4
The preparation method comprises the following steps:
(1) mixing and heating the raw materials of the phase B until the material body becomes transparent for later use;
(2) mixing the raw materials of the phase C with the phase A, and heating and stirring until the raw materials are completely dissolved;
(3) adding the mixture of the phase C and the phase A prepared in the step (2) into the phase B prepared in the step (1), and uniformly stirring;
(4) cooling to 60 deg.C, bottling, and demolding.
Example 9 preparation of a lipstick according to the invention
Raw materials and dosage are shown in table 5:
TABLE 5
The preparation method comprises the following steps:
(1) mixing and heating the raw materials of the phase B until the material body becomes transparent for later use;
(2) mixing the raw materials of the phase C with the phase A, and heating and stirring until the raw materials are completely dissolved;
(3) adding the mixture of the phase C and the phase A prepared in the step (2) into the phase B prepared in the step (1), and uniformly stirring;
(4) cooling to 60 deg.C, bottling, and demolding.
EXAMPLE 10 preparation of a lipstick according to the invention
Raw materials and amounts are shown in table 6:
TABLE 6
The preparation method comprises the following steps:
(1) mixing and heating the raw materials of the phase B until the material body becomes transparent for later use;
(2) mixing the raw materials of the phase C with the phase A, and heating and stirring until the raw materials are completely dissolved;
(3) adding the mixture of the phase C and the phase A prepared in the step (2) into the phase B prepared in the step (1), and uniformly stirring;
(4) cooling to 60 deg.C, bottling, and demolding.
EXAMPLE 11 preparation of a lipstick according to the invention
Raw materials and amounts, see table 7:
TABLE 7
The preparation method comprises the following steps:
(1) mixing and heating the raw materials of the phase B until the material body becomes transparent for later use;
(2) mixing the raw materials of the phase C with the phase A, and heating and stirring until the raw materials are completely dissolved;
(3) adding the mixture of the phase C and the phase A prepared in the step (2) into the phase B prepared in the step (1), and uniformly stirring;
(4) cooling to 60 deg.C, bottling, and demolding.
EXAMPLE 12 preparation of a lipstick according to the invention
Raw materials and dosage are shown in table 8:
TABLE 8
The preparation method comprises the following steps:
(1) mixing and heating the raw materials of the phase B until the material body becomes transparent for later use;
(2) mixing the raw materials of the phase C with the phase A, and heating and stirring until the raw materials are completely dissolved;
(3) adding the mixture of the phase C and the phase A prepared in the step (2) into the phase B prepared in the step (1), and uniformly stirring;
(4) cooling to 60 deg.C, bottling, and demolding.
Efficacy test of the present invention
Selection of compounding agent
The inventors have defined the final product as a solid state that facilitates storage, transport and cosmetic addition. The selection of the compounding agent of a solid product has great limitation, the selection of a proper compounding agent is favorable for improving the overall performance and effect of the product, and the selectable compounding agents are as follows: stearic acid, palmitic acid, coconut oil, cocoa butter and cetyl alcohol.
(1) The test method comprises the following steps: heating stearic acid, palmitic acid, coconut oil, cocoa butter and cetyl alcohol to dissolve the phytosterol, wherein the ratio of the solvent to the phytosterol is 2:1, the dissolving temperature is not more than 80 ℃, and observing the dissolving phenomenon.
(2) The results are shown in Table 9.
TABLE 9
| Compounding of raw materials | Solubility in water |
| Stearic acid + phytosterols | Not dissolving |
| Palmitic acid + phytosterols | Not dissolving |
| Coconut oil + phytosterols | Partially dissolved |
| Cocoa butter + phytosterols | Not dissolving |
| Cetyl alcohol + phytosterols | Soluble and uniformly stable |
(3) And (4) experimental conclusion:
finally, cetyl alcohol with good solubility is selected, in addition, a compound agent with a structure similar to that of the cetyl alcohol is selected, and finally, the compound effect of the behenyl alcohol is selected to be optimal.
Second, differential scanning calorimetry measures the endothermic peak of the sample
Differential Scanning Calorimetry (DSC) is a thermal analysis method. The DSC is used for analyzing the product and the four raw materials, so that the phase transition temperature can be determined, and the operability in the cosmetic preparation process can be compared.
(1) The test method comprises the following steps: five samples were tested experimentally, operating according to the operating protocol of differential scanning calorimetry, N2The atmosphere is measured in the range of 0-200 ℃, and the heating rate is 10 ℃/min.
(2) Test samples:
sample 1: inventive example 1 a phytosterol additive was prepared.
Sample 2: phytosterol ester samples.
Sample 3: a phytosterol sample.
Sample 4: behenyl alcohol samples.
Sample 5: a sample of cetyl alcohol.
(3) The experimental results are as follows: referring to fig. 1 and table 10, in fig. 1 (a) is sample 1; (b) sample 2; (c) sample 3; (d) sample 4; (e) sample 5 was obtained.
TABLE 10 endothermic peaks for samples
(4) And (4) experimental conclusion:
two endothermic peaks at 44.77 ℃ and 25.20 ℃ can be seen in the DSC curve of the sample phytosterol ester starting material (sample 2). In general, the appearance of two peaks in the DSC curve of an organic can be attributed to two cases: (1) the two peaks correspond to the transformation of the crystalline phase and the solid-liquid phase transformation respectively; (2) the organic matter is a mixture, and the compatibility of the components in the mixture is poor. The phytosterol ester raw material (sample 2) is milky opaque viscous liquid at room temperature (about 28 ℃), and changes into light yellow transparent oily liquid when heated to 50 ℃, which indicates that the peak at 25.20 ℃ in the DSC curve is not the transformation of crystalline phase, i.e. the sample is a mixture, and the compatibility of the components is poor.
Behenyl alcohol (sample 4) and cetyl alcohol (sample 5) both have long-chain hydrocarbon groups and hydroxyl groups, and have certain surface activity, so that on one hand, the inclusion effect on phytosterol (sample 3) is realized, and the solubility of phytosterol can be enhanced; on the other hand, the phytosterol ester can form an emulsifying solvent type mixed solvent with the phytosterol ester, so that the solubility of the phytosterol is further improved. At the same time, the presence of two alcohols also helps to enhance the phase solubility of the components in the phytosterol ester. Thus, the phytosterol composition of example 1 was obtained with only one melting endotherm at 45.42 ℃.
From a formulation point of view, it is desirable to obtain a uniform, stable product with a low melting temperature. Only one melting endothermic peak at 45.42 ℃ can be observed in the DSC curve of the sample 1, which shows that the product has good intersolubility of all components and is not easy to phase separate and uneven due to temperature rise and temperature drop in the using process of the product. Meanwhile, the proper melting point also ensures the operability of the product and avoids the problem of overhigh melting temperature of the phytosterol. The melting point of the product is close to the skin temperature, and the product has better skin-friendly property. The inventor repeats the above experiment with the product prepared by other embodiments of the invention, and the experimental conclusion is consistent.
Dissolution test of Tricaprylic/capric triglyceride
Caprylic/capric triglyceride is common oil for cosmetics, is prepared by esterifying caprylic acid, capric acid and glycerol, and can be used as base material of moisturizing factor, stabilizer, antifreeze and homogenizing agent for cosmetics. The dispersion of the sample in the oil base matrix was confirmed by dissolving the phytosterol composition and phytosterol of example 1 in caprylic/capric triglyceride as a solvent and observing the resulting solution with an optical microscope.
(1) The test method comprises the following steps: the phytosterol composition (sample 1) and the phytosterol (sample 2) in example 1 were dissolved in caprylic/capric triglyceride as a solvent at 70 ℃ under stirring at 100 rpm for 30 minutes. The dissolution was observed under an optical microscope.
(2) The experimental results are as follows: as shown in FIG. 2, the phytosterol composition (a) of example 1 has no visible insoluble matter and is well dissolved; the phytosterol (b) picture shows that the solid is insoluble and the dissolution is poor.
(3) And (4) experimental conclusion: the phytosterol additive prepared by the invention improves the solubility of the phytosterol in an oil-soluble system, can efficiently exert the activity of the phytosterol and improves the utilization rate of active ingredients. The inventor repeats the above experiment with the product prepared by other embodiments of the invention, and the experimental conclusion is consistent.
Fourth, solubility and melting point test
(1) The experimental method comprises the following steps: 7 groups of experiments are totally carried out, and the influence of different combinations of the phytosterol, the phytosterol ester, the behenyl alcohol and the cetyl alcohol and the experiment steps on the solubility and the melting point of the product is researched. The melting point was determined by the capillary method.
(2) Sample preparation:
comparative example 1: weighing 100g of phytosterol and 100g of phytosterol ester, heating to 80 ℃, and reacting for 60min at a stirring speed of 100 rad/min; cooling to room temperature.
Comparative example 2: weighing 100g of cetyl alcohol and 100g of phytosterol, heating to 80 ℃, and reacting for 60min at a stirring speed of 100 rad/min; cooling to room temperature.
Comparative example 3: weighing 100g of cetyl alcohol, 100g of phytosterol and 100g of phytosterol ester, heating to 80 ℃, and reacting for 60min at a stirring speed of 100 rad/min; cooling to room temperature.
Comparative example 4: weighing 100g of cetyl alcohol and 100g of phytosterol, heating to 80 ℃, and reacting for 40min at the stirring speed of 100 rad/min; adding 100g of phytosterol ester, and continuing to react for 20min at the stirring speed of 100 rad/min; cooling to room temperature.
Comparative example 5: weighing 100g of cetyl alcohol and 100g of phytosterol ester, heating to 80 ℃, and reacting for 40min at the stirring speed of 100 rad/min; adding 100g of phytosterol, continuing to react for 20min, and stirring at the rotating speed of 100 rad/min; cooling to room temperature.
Comparative example 6: weighing 50g of cetyl alcohol, 150g of behenyl alcohol and 50g of phytosterol, heating to 80 ℃, and reacting for 40min at the stirring speed of 100 rad/min; adding 50g of phytosterol ester, and continuing to react for 20min at the stirring speed of 100 rad/min; cooling to room temperature.
Comparative example 7: weighing 100g of cetyl alcohol, 10g of behenyl alcohol and 100g of phytosterol, heating to 80 ℃, and reacting for 40min at a stirring speed of 100 rad/min; adding 100g of phytosterol ester, and continuing to react for 20min at the stirring speed of 100 rad/min; cooling to room temperature.
(3) The experimental results are as follows:
TABLE 11 solubility and melting points for comparative examples 1-7
(4) And (4) experimental conclusion:
from the above table, it can be seen that the phytosterol and the phytosterol ester are not mutually soluble (comparative example 1), whereas example 1 is a uniform transparent liquid at 80 ℃ and a white solid at room temperature, which shows that the invention effectively solves the problem that the phytosterol and the phytosterol ester cannot be simultaneously applied, and the two are uniformly dispersed in the system and have good compatibility.
Comparative examples 3 and 5 are solid-liquid mixtures at 80 c, indicating that the two products are poorly soluble. The embodiment 1 of the invention is a uniform transparent liquid, and solves the problems of poor solubility of the phytosterol and immiscible phytosterol and phytosterol ester.
Compared with comparative examples 2 and 4, the melting point of example 1 is obviously reduced, which shows that the invention solves the problems of high melting point and poor use of phytosterol by optimizing the formula.
The compositions of comparative example 1, comparative example 3, comparative example 5 and comparative example 7 did not form a uniform system, i.e., the phytosterols were not uniformly dispersed in the system, and the phytosterols and phytosterol esters were not well compatible, and thus could not be added to the formulation for relevant tests. Comparative example 6 is a uniform transparent liquid (80 ℃), but precipitates as shown in the right diagram of fig. 3 when added to the essential oil (fig. 3 provides a color diagram for more clearly seeing the precipitation), which indicates that comparative example 6 fails to uniformly disperse the phytosterol in the system, or the phytosterol and the phytosterol ester are not well compatible, so that the relevant test is not performed. The left figure of fig. 3 is a diagram of the essential oil added in example 1, and the fact that the essential oil in example 1 has good solubility, is clear and transparent and has stable properties can be seen.
Comparative example 7 failed to form a uniform dispersion system, demonstrating that the present invention solves the problem of poor application of phytosterols in cosmetics by optimizing the formulation.
In conclusion, the invention effectively solves the problems of high melting point and poor solubility of the phytosterol and incompatibility of the phytosterol and the phytosterol ester by optimizing the formula proportion and the preparation method, so that the phytosterol is better applied to cosmetics. The inventor repeats the above experiment with the product prepared by other embodiments of the invention, and the experimental conclusion is consistent.
Fifthly, the performances of the lipstick, the comparative example and the commercial product are compared
The phytosterol additive composition simulates skin structure lipid, can level the stratum corneum, prevent water loss, and improve the symptoms of lip peeling, darkness and lackluster.
1. The experimental sample:
comparative example 1: lipstick containing only phytosterol
TABLE 12
(1) Mixing and heating the phase A until the material body becomes transparent for later use;
(2) phase B is heated and stirred until the phase B is completely dissolved;
(3) adding the phase B into the dissolved phase A, and uniformly stirring;
(4) cooling to 60 deg.C, filling and demoulding.
Comparative example 2: lipstick containing phytosterol ester only
Watch 13
(1) Mixing and heating the phase A until the material body becomes transparent for later use;
(2) phase B is heated and stirred until the phase B is completely dissolved;
(3) adding the phase B into the dissolved phase A, and uniformly stirring;
(4) cooling to 60-65 deg.C, bottling, and demolding.
Comparative example 3: lipstick containing phytosterol and phytosterol ester
TABLE 14
(1) Mixing and heating the phase A until the material body becomes transparent for later use;
(2) phase B is heated and stirred until the phase B is completely dissolved;
(3) adding the phase B into the dissolved phase A, and uniformly stirring;
(4) cooling to 60 deg.C, filling and demoulding.
Comparative example 4: adding phytosterol, phytosterol ester, and cetyl alcohol
Watch 15
(1) Weighing 150g of cetyl alcohol and 150g of phytosterol in the phase A, heating to 80 ℃, and reacting for 40min at the stirring speed of 100 rad/min; adding 150g of phytosterol ester, and continuing to react for 20min at the stirring speed of 100 rad/min; cooling to room temperature for later use.
(2) Mixing and heating the phase B until the material body becomes transparent for later use;
(3) mixing the phase C with the phase A, heating and stirring until the phase C is completely dissolved;
(3) adding the phase A and the phase C into the dissolved phase B, and uniformly stirring;
(4) cooling to 60-65 deg.C, bottling, and demolding.
Comparative example 5: lipstick blank base
TABLE 16
(1) Mixing and heating the phase A until the material body becomes transparent for later use;
(2) phase B is heated and stirred until the phase B is completely dissolved;
(3) adding the phase B into the dissolved phase A, and uniformly stirring;
(4) cooling to 60 deg.C, filling and demoulding.
Comparative example 6: commercially available lip balm, ingredients: lanolin oil, caprylic/capric triglyceride, candelilla (Euphorbiaceae) wax, lanolin, beeswax, stearic acid, squalane, paraffin, olive (Olea EUROPAEA) fruit oil, 1, 2-pentanediol, tocopherol (vitamin E), phenoxyethanol, stearyl glycyrrhetinate, Ginseng radix (Panax GINSENG) root extract, and Aloe BARBADENSIS (Aloe BARBADENSIS) leaf extract.
2. The experimental method comprises the following steps: the method comprises the steps of selecting 60 volunteers with age of 18-40 years and dry lip symptoms, wherein the lip is the test area. The volunteers were divided into 6 groups of 10 persons each, and the samples were applied to the lips 5 times a day, and were discontinued after 10 days of application. Before use, after 5 days use, after 10 days use, after 5 days rest, after 10 days rest, the following tests were carried out in order: skin moisture content, skin moisture loss, ITA degree parameter analysis, and questionnaire survey.
3. The experimental results are as follows:
(1) moisture content of skin
The moisturizing properties of the samples can be evaluated by skin moisture content testing. The results of the skin moisture content test before use (initial value), after 5 days of use, after 10 days of use, after 5 days of rest, and after 10 days of rest are shown in Table 18. The greater the skin moisture content value, the higher the skin moisture content.
TABLE 17 skin moisture content test
The lip moisture content increased after use for each sample compared to the initial value; after the use was stopped, the lipstick prepared in example 7 of the present invention maintained its moisturizing effect better than the other samples, indicating that the phytosterol additive of the present invention has superior efficacy to the comparative example. The inventors repeated the above experiments with the phytosterol additives prepared in other examples, and the conclusions were the same and are not repeated here.
(2) Rate of skin moisture loss
The skin moisture loss test also allows the samples to be evaluated for their moisturizing properties. The results of the skin moisture loss rate before (initial) use, after 5 days of use, after 10 days of use, after 5 days of rest, and after 10 days of rest are shown in the following table. The smaller the skin moisture loss rate is, the better the moisturizing effect is.
TABLE 18 skin moisture loss test
Compared with the initial value, the skin moisture loss rate of each sample is reduced after the sample is used; example 7 maintained its moisturizing effect better than the other samples after discontinuation of use, demonstrating the superior efficacy of the phytosterol additive described herein over the comparative example. The inventors repeated the above experiments with the phytosterol additives prepared in other examples, and the conclusions were the same and are not repeated here.
(3) ITA ° parameter analysis
The ITA ° parametric analysis allows the evaluation of the effect of the sample on skin gloss. The skin ITA ° parameters before (initial) use, after 5 days use, after 10 days use, after 5 days rest, and after 10 days rest for the samples are shown in the table below. The larger the skin color parameter ITA DEG value, the brighter the skin color.
TABLE 19 skin color ITA ° parameter
The sample of example 7 of the present invention had a significant effect on lip color enhancement, and the lips remained glossy after the use was stopped. The effect of the phytosterol additive is better than that of the comparative example. The inventors repeated the above experiments with the phytosterol additives prepared in other examples, and the conclusions were the same and are not repeated here.
(4) Questionnaire survey
And investigating the long-acting moisture retention, long-acting moisturizing and lip gloss improvement of the sample.
Grading standard: 0-1.9-low strength; 2-3.9-lower strength; 4-5.9-moderate; 6-7.9-higher strength; 8-10-high strength.
The experimental results are as follows: see the following Table
TABLE 20 evaluation of population suitability
| Index name | Example 7 | Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 | Comparative example 5 | Comparative example 6 |
| Long-acting moisture retention | 7.2 | 3.8 | 4.9 | 5.6 | 6.2 | 3.2 | 6.5 |
| Long-acting moistening | 7.6 | 5.1 | 5.9 | 6.1 | 6.5 | 3.9 | 5.4 |
| Improving luster | 6.3 | 4.1 | 5.2 | 5.5 | 5.9 | 3.5 | 5.8 |
According to questionnaire survey, the example 7 can achieve good effects of long-acting moisture retention, long-acting moisturizing and lip gloss improvement by optimizing the formula composition and the process. In the formula of comparative example 1, phytosterol is directly added, and the phytosterol has good antioxidant effect, but is difficult to dissolve and melt, and the formula has poor applicability, so that the phytosterol has no good effect. In comparative example 2, phytosterol ester was added directly, which had better solubility than phytosterol, so comparative example 2 had enhanced efficacy over comparative example 1. The formula of the comparative example 3 is simultaneously added with the phytosterol and the phytosterol ester, the two active raw materials have synergistic effect, the effect is slightly better than that of the comparative examples 1 and 2, but the phytosterol and the phytosterol ester are not mutually soluble, so the effect of the invention is not good. In comparative example 4, cetyl alcohol was added to improve the effect of phytosterol, but the solubility of the formulation was not completely improved, and the functional ingredients were not fully exerted, so the technical effect was not as good as that of the present invention. Comparative example 5 is a sample of lipstick base, which was not ideal in each efficacy. The inventors repeated the above experiments with the phytosterol additives prepared in other examples, and the conclusions were the same and are not repeated here.
(5) And (4) experimental conclusion: the lip balm prepared by the invention has better long-acting moisturizing, moistening and lip gloss improving effects, and the novel phytosterol additive provided by the invention has the advantages of good solubility in a formula system, synergistic effect of functional components, full play of the effect of functional groups and good application prospect.
Claims (8)
1. A lip care composition containing a novel phytosterol additive is characterized by consisting of a phase A, a phase B and a phase C, wherein the phase A, the phase B and the phase C consist of the following raw materials:
0.08-8.00 wt% of A-phase phytosterol additive
B phase petrolatum balance
5.00-15.00 wt% of beeswax
2.00-8.00 wt% of glyceryl behenate/eicosanoate
3.00-15.00 wt% of C-phase octyl polymethylsiloxane
0 to 10.00 wt% of hydrogenated polyisobutene
1-10.00 wt% of shea butter
0.10-2.00 wt% of tocopherol acetate
Butylated hydroxytoluene 0.03-0.20 wt%
0.10-0.14 wt% of propyl hydroxybenzoate;
the A-phase phytosterol additive is prepared from behenyl alcohol, cetyl alcohol, phytosterol and phytosterol ester, and the weight parts of the raw materials are as follows:
1 to 5 portions of behenyl alcohol, 1 to 5 portions of cetyl alcohol, 1 to 5 portions of phytosterol and 0.1 to 10 portions of phytosterol ester.
2. A lip care composition according to claim 1 wherein: the weight ratio of the phytosterol to the phytosterol ester in the phytosterol additive is 1: 0.1 to 2.
3. A lip care composition according to claim 1 or 2, wherein: the preparation method of the phytosterol additive comprises the following steps:
(1) preparing the raw materials according to the weight part ratio;
(2) mixing the behenyl alcohol, the cetyl alcohol and the phytosterol, heating to 70-100 ℃, stirring at a rotating speed of 100-400 rpm, and reacting for 5-60 minutes to obtain a first solution;
(3) and cooling the solution I to 60-90 ℃, adding the phytosterol ester into the solution I, stirring at the rotating speed of 100-400 r/min, continuously reacting for 1-30 min, and cooling to room temperature to obtain the phytosterol ester.
4. A process for preparing a lip care composition according to claim 1 or 2, characterized in that said process comprises the steps of:
(1) mixing and heating the raw materials of the phase B until the material body becomes transparent for later use;
(2) mixing the raw materials of the phase C with the phase A, and heating and stirring until the raw materials are completely dissolved;
(3) adding the mixture of the phase C and the phase A prepared in the step (2) into the phase B prepared in the step (1), and uniformly stirring;
(4) cooling to 60-65 ℃, filling and demolding to obtain the product.
5. A method of making a lip care composition according to claim 3, characterized in that said method comprises the steps of:
(1) mixing and heating the raw materials of the phase B until the material body becomes transparent for later use;
(2) mixing the raw materials of the phase C with the phase A, and heating and stirring until the raw materials are completely dissolved;
(3) adding the mixture of the phase C and the phase A prepared in the step (2) into the phase B prepared in the step (1), and uniformly stirring;
(4) cooling to 60-65 ℃, filling and demolding to obtain the product.
6. A method of making a lip care composition according to claim 5, wherein: the heating temperature in the step (1) is 40-70 ℃.
7. A method of making a lip care composition according to claim 5, wherein: in the step (2), the heating temperature is 40-70 ℃, and the stirring speed is 100-300 r/min.
8. A lipstick containing a novel phytosterol additive is characterized in that: the lipstick prepared by the method of any one of claims 5 to 7.
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Cited By (4)
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| CN113925793A (en) * | 2021-09-03 | 2022-01-14 | 太和康美(北京)中医研究院有限公司 | Skin care essence oil containing phytosterol and phytosterol ester and preparation method thereof |
| CN113925788A (en) * | 2021-09-03 | 2022-01-14 | 太和康美(北京)中医研究院有限公司 | Sleep mask containing phytosterol and phytosterol ester and preparation method thereof |
| CN113940900A (en) * | 2021-09-24 | 2022-01-18 | 广州那比昂生物科技有限公司 | Lip protecting ointment for softening lip cutin and improving lip state and preparation method thereof |
| CN113952242A (en) * | 2021-09-03 | 2022-01-21 | 太和康美(北京)中医研究院有限公司 | Emulsion containing phytosterol and phytosterol ester and preparation method thereof |
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| CN113925793A (en) * | 2021-09-03 | 2022-01-14 | 太和康美(北京)中医研究院有限公司 | Skin care essence oil containing phytosterol and phytosterol ester and preparation method thereof |
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