CN114129467A - Anti-aging composition for stabilizing high-concentration retinol stock solution and preparation method thereof - Google Patents
Anti-aging composition for stabilizing high-concentration retinol stock solution 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
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/67—Vitamins
- A61K8/671—Vitamin A; Derivatives thereof, e.g. ester of vitamin A acid, ester of retinol, retinol, retinal
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- A61K8/00—Cosmetics or similar toiletry preparations
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- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
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- A61K8/00—Cosmetics or similar toiletry preparations
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- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
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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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- 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
- A61Q19/08—Anti-ageing preparations
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Abstract
The invention discloses an anti-aging composition of stable high-concentration retinol stock solution and a preparation method thereof, and the composition comprises, by weight, 40-50 parts of retinol, 1-10 parts of antioxidant, 40-49 parts of grease, and 0.1-5 parts of oil-soluble anti-allergic active substance; the composition obtained by the invention is safe, mild and non-irritant; the anti-aging composition of the high-concentration retinol stock solution is applied to essential oil, essence, emulsion, cream and the like. The composition is simple in preparation method and easy to add in a formula, and effectively solves the problems of application stability of single retinol in cosmetics, irritation of commercially available high-concentration retinol stock solution, limitation of formula application and the like.
Description
Technical Field
The invention belongs to the technical field of cosmetics, and particularly relates to an anti-aging composition for stabilizing a high-concentration retinol stock solution and a preparation method thereof.
Background
Skin is an important organ for maintaining human life and health, however, it gradually begins to age with the aging and the influence of external factors. With the research and development of cosmetic science and the increasing demand of consumers for the efficacy of cosmetics, anti-aging skin care becomes one of the most important consumer demands. Retinol, also known as a alcohol, is a precursor of tretinoin, a very classic skin care ingredient with anti-aging effect. The medicine is firstly marketed in 70-80 years in the United states as a medicine for treating acne, has a good anti-aging effect, has a collagen synthesis promoting effect, has great advantages in the aspects of improving skin photoaging, fine lines, wrinkles and pigmentation, and is an important functional component in a plurality of fields such as cosmetics, medical cosmetology and the like. However, the high-purity (more than or equal to 99 percent) retinol monomer is unstable and very active, and if the high-purity retinol monomer is not protected, the high-purity retinol monomer changes in the process of detecting the content and the purity by adopting a high performance liquid chromatograph, so that the purity and the content are reduced, and the activity is also reduced. Therefore, the monomeric retinol cannot be directly used in cosmetics, and the content and activity thereof cannot be guaranteed by storage under ordinary conditions. In order to improve the practical application problem of retinol, the retinol with the highest concentration in the world is solubilized mainly by high-content tween-20 to obtain stock solution with the concentration of about 50 percent. Tween 20(Tween 20), also called polysorbate-20 (polysorbate 20), is a nonionic surfactant, has strong hydrophilicity and chemical undissociation, and has good solubilizing effect on liposoluble active ingredients. However, with the intensive pharmacological research in recent years, people recognize that the polysorbate surfactant has certain biological and pharmacological activities, can induce cells to generate a degranulation effect to cause the release of allergic active substances, and unsaturated fatty acid of the polysorbate surfactant is also very easy to be oxidized and degraded to generate a plurality of toxic components, and is related to adverse reactions such as dyspnea, nausea, vomiting, rash and the like in the clinical medicine. Therefore, there is a need to develop a relatively green, mild and stable high concentration (50%) retinol stock solution composition that can solve the conventional storage of monomeric retinol under conditions and solve the problem of its use in cosmetics.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides the anti-aging composition of the stable high-concentration retinol stock solution, the anti-aging composition can solve the application of a retinol monomer in cosmetics, and the relatively green, mild and stable high-concentration retinol stock solution is obtained, so that a foundation is laid for further realizing the application of the retinol stock solution in the formula by subsequent formulators.
The technical scheme adopted by the invention is as follows:
an anti-aging composition for stabilizing a high-concentration retinol stock solution, which is characterized by comprising the following raw material components:
40-50 parts of retinol;
1-10 parts of antioxidant;
40-49 parts of grease;
0.1-5.0 parts by weight of oil-soluble anti-allergy soothing active substance;
further preferably, the raw material components of the anti-aging composition for stabilizing the high-concentration retinol stock solution comprise:
45-50 parts of retinol;
3-6 parts of antioxidant;
42-46 parts of grease;
0.1-1.0 weight part of oil-soluble anti-allergy and relieving active substance;
in another aspect of the present invention, the antioxidant in the anti-aging composition for stabilizing a stock solution of retinol at a high concentration is a mixture of 1 or 2 or more of tocopherol, tocopheryl acetate, tocopheryl succinate, butylated hydroxytoluene, butylated hydroxyanisole, and diethylhexyl syringylidenemalonate.
In another aspect of the present invention, the anti-aging composition for stabilizing a high concentration retinol stock solution is a mixture of 1 or 2 or more of caprylic/capric triglyceride, tocopheryl acetate, tocopheryl succinate, tocopherol, diethoxyethyl succinate, glycerol tri (ethyl hexanoate), diisooctyl adipate, pentaerythritol tetraisostearate, isostearyl stearate, diisostearyl malate, isooctyl palmitate, isopropyl myristate, diisopropyl adipate, mineral oil (No. 15), diethoxy diglycol cyclohexane 1, 4-dicarboxylate, and babassu oil glyceryl polyether-8 ester.
In another aspect of the present invention, the anti-aging composition containing stable high concentration retinol stock solution comprises 1 or 2 or more of oat extract, bisabolol, and stearyl glycyrrhetinate.
On the other hand, the anti-aging composition of the stable high-concentration retinol stock solution can be applied to cosmetics with anti-aging efficacy, and the application mass percentage of the anti-aging composition is 0.1-1%.
The invention has the beneficial effects that: 1. the problem of conventional condition storage of the retinol is solved, the relatively green, mild and stable high-concentration retinol stock solution 2 is obtained, a foundation is laid for formulators to further develop the application of the retinol in cosmetics, and researchers can research and pack retinol dosage forms with more specifications and contents and more convenient application on the basis.
Drawings
FIG. 1 shows the stability of retinol stock solution compositions obtained in each example at 4 ℃.
FIG. 2 shows stability test of retinol stock solution compositions obtained in each example under room temperature condition.
FIG. 3 shows stability test of retinol stock solution compositions obtained in each example at 45 ℃.
Detailed Description
The invention is further described below with reference to specific examples, but the invention is not limited in any way.
In the following examples, 1 part by weight represents 1 g.
Example 1
The embodiment provides an anti-aging composition for stabilizing a high-concentration retinol stock solution, which comprises the following raw material components in parts by weight:
50 parts by weight of retinol;
butylated hydroxytoluene, 2.0 parts by weight;
3.0 parts by weight of tocopherol acetate;
butylated hydroxyanisole, 1.0 part by weight;
caprylic/capric triglyceride, 43.7 parts by weight;
0.3 part by weight of bisabolol;
the preparation method of the anti-aging composition for stabilizing the high-concentration retinol stock solution comprises the following steps:
(1) mixing butylated hydroxytoluene, tocopherol acetate, butylated hydroxyanisole, caprylic/capric triglyceride and bisabolol, heating to 60 ℃ at a stirring speed of 500r/min to dissolve the raw materials into a uniform and transparent state, and then keeping the temperature for later use to obtain a component A;
(2) adding retinol powder into the component A under the condition of nitrogen introduction and stirring, and stirring at the stirring speed of 200r/min until the retinol crystal powder is dissolved into a uniform and transparent state, thus obtaining the anti-aging composition of the stable high-concentration retinol stock solution.
Example 2
The embodiment provides an anti-aging composition for stabilizing a high-concentration retinol stock solution, which comprises the following raw material components in parts by weight:
50 parts by weight of retinol;
butylated hydroxytoluene, 3.0 parts by weight;
2.0 parts by weight of tocopherol acetate;
butylated hydroxyanisole, 1.0 part by weight;
diethoxyethyl succinate, 43.9 parts by weight;
0.1 part by weight of oat extract;
the preparation method of the anti-aging composition for stabilizing the high-concentration retinol stock solution comprises the following steps:
(1) mixing butylated hydroxytoluene, tocopherol acetate, butylated hydroxyanisole, diethoxyethyl succinate and oat extract, heating to 60 ℃ at a stirring speed of 500r/min, dissolving the raw materials into a uniform transparent state, and keeping the temperature for later use to obtain a component A;
(2) adding retinol powder into the component A under the condition of nitrogen introduction and stirring, and stirring at the stirring speed of 200r/min until the retinol crystal powder is dissolved into a uniform and transparent state, thus obtaining the anti-aging composition of the stable high-concentration retinol stock solution.
Example 3
The embodiment provides an anti-aging composition for stabilizing a high-concentration retinol stock solution, which comprises the following raw material components in parts by weight:
50 parts by weight of retinol;
1.5 parts by weight of butylated hydroxytoluene;
tocopheryl acetate, 47.3 parts by weight;
butylated hydroxyanisole, 1.0 part by weight;
0.2 part by weight of stearyl glycyrrhetinate;
the preparation method of the anti-aging composition for stabilizing the high-concentration retinol stock solution comprises the following steps:
(1) mixing butylated hydroxytoluene, tocopherol acetate, butylated hydroxyanisole and stearyl glycyrrhetinate, heating to 60 deg.C at a stirring speed of 500r/min, dissolving the above raw materials into uniform transparent state, and keeping the temperature for use to obtain component A;
(2) adding retinol powder into the component A under the condition of nitrogen introduction and stirring, and stirring at the stirring speed of 200r/min until the retinol crystal powder is dissolved into a uniform and transparent state, thus obtaining the anti-aging composition of the stable high-concentration retinol stock solution.
Example 4
This example provides a preparation method of VA anti-aging essential oil
The raw materials required by the VA anti-aging essential oil are weighed according to the following table 1.
The preparation method of the VA anti-aging essential oil comprises the following steps: weighing A phase raw materials respectively, heating to 80-85 ℃, dissolving and stirring uniformly, and cooling. ② the phase A raw material is cooled to 60 ℃, the phase B raw material is slowly added under the condition of stirring, stirred and dissolved evenly, and cooled. Cooling to below 30 ℃, adding the anti-aging composition of the stable high-concentration retinol stock solution prepared in the example 2 and the residual raw materials of the C phase, and uniformly stirring to obtain the VA anti-aging essential oil.
TABLE 1 VA formula table of anti-aging essential oil
The following test methods were used in the practice:
safety test of skin patch
The number of the test persons is 50 (the number of the blank group and the number of the test group are both 50, and the male and the female are half and half, and the age is between 30 and 60 years), and the test persons all meet the standard of the test subjects.
The VA anti-aging essence oil prepared in example 4 is put into a spot tester cell, and the dosage is about 0.2-0.25 mL. The control well was a blank control (without any substance), and the plaque test device with the test substance was applied to one of the curved sides of the forearm of the subject with a hypoallergenic tape (manufacturer: Shanghai medical instruments (group) Co., Ltd., hygienic materials works, plaque tape product No. 09000251116) and the other curved side of the forearm being a blank group, and the test device was applied to the skin uniformly by pressing the palm for 24 hours. The skin reactions were observed at 30min (after disappearance of the indentation), 24h and 48h after removal of the test article plaque test device, respectively, according to the following table standards and the observation results were recorded, see tables 2 and 3.
TABLE 2 skin closure Patch test skin response grading Standard
Table 3 test results of the patch for human skin of example 4 of the present invention
As can be seen from table 3, the VA anti-aging essential oil prepared by adding the anti-aging composition of stable high-concentration retinol stock solution in example 4 of the present invention is mild and has no irritation to skin.
Second, stability test
2.1 instruments and appliances
High performance liquid chromatograph (HPLC-DAD) electronic balance (precision 0.01mg), chromatographic column (Welch Ultimate series XB-C18 chromatographic column, 250mm 4.6mm, 5 μm), several volumetric flasks
2.2 reagents, solutions, controls
Reagent: acetonitrile (chromatographic grade), formic acid (chromatographic grade) and ultrapure water
Comparison products: retinol, purity over 99.5%, manufacturer: keqin laboratory self-made (-20 ℃, sealed in dark place, vacuum storage)
Blank solvent: acetonitrile-0.1% formic acid (95/5) solution
2.3 sample preparation
Control solution: precisely weighing about 10.0mg of a pure retinol crystal reference substance, placing the pure retinol crystal reference substance into a 20mL brown measuring flask, firstly adding a proper amount of antioxidant BHT (butylated hydroxytoluene) and BHA (butylated hydroxyanisole), then adding a proper amount of acetonitrile, carrying out dark ultrasound and diluting to a scale, shaking up, and preparing 2 parts in parallel.
Solution of test article a: precisely weighing about 0.1g of the anti-aging composition of the stable high-concentration retinol stock solution obtained in the above example 1, placing the anti-aging composition into a 100mL brown measuring flask, adding an appropriate amount of acetonitrile, carrying out dark ultrasound, diluting to a scale, shaking up, and preparing 2 parts in parallel.
Solution of test article B: precisely weighing about 0.1g of the anti-aging composition of the stable high-concentration retinol stock solution obtained in the above example 2, placing the anti-aging composition into a 100mL brown measuring flask, adding an appropriate amount of acetonitrile, carrying out dark ultrasound, diluting to a scale, shaking up, and preparing 2 parts in parallel.
Solution of test article C: precisely weighing about 0.1g of the anti-aging composition of the stable high-concentration retinol stock solution obtained in the above example 3, placing the anti-aging composition into a 100mL brown measuring flask, adding a proper amount of acetonitrile, performing ultrasonic treatment, diluting to a scale, shaking up, and preparing 2 parts in parallel.
Solution of test article D: precisely weighing about 0.1g of a commercial retinol stock solution sample, placing the sample in a 100mL brown measuring flask, adding a proper amount of acetonitrile, performing ultrasonic treatment, diluting to a scale, shaking up, and preparing 2 parts in parallel.
Negative control solution: precisely weighing about 10.0mg of a pure retinol crystal reference substance, placing the pure retinol crystal reference substance into a 20mL brown measuring flask, adding no antioxidant such as BHT (butylated hydroxytoluene), BHA (butylated hydroxyanisole), tocopherol acetate and the like, adding a proper amount of acetonitrile, carrying out ultrasonic treatment, diluting to a scale, shaking uniformly, and preparing 2 parts in parallel.
2.4 chromatographic conditions
Mobile phase: acetonitrile of phase A; b phase 0.1% formic acid-water
Column temperature: 25 deg.C
Flow rate: 1.0mL/min
Wavelength: 325nm
Sample introduction volume: 10 μ L
The isocratic elution procedure is shown in table 4 below:
TABLE 4 Retinol elution schedule
Retention time t of retinol is about 9.2min
2.5 testing
Operating according to the operating procedures of using and maintaining the high performance liquid chromatograph:
i) blank solvent, injecting 2 needles, and recording the chromatogram for 30 minutes;
II) continuously performing at least 3 times on the reference substance solution 1, and recording the chromatogram for 30 minutes;
III) a reference substance solution 2 is injected into a sample 2 needle, and the chromatogram is recorded for 30 minutes;
IV) 2 parts of sample solution, 2 needles for each sample introduction, and recording the chromatogram for 30 minutes;
and V) adjusting the chromatogram measuring range, integrating and printing.
2.6 System suitability test
RSD of 2 parts of main peak correction factors of the reference solution is not more than 3.0%;
in the chromatogram of the control solution, the theoretical plate number is not less than 3000 calculated according to retinol, and the tailing factor is not more than 2.0.
2.7 calculation of the content
In the formula: cr represents the concentration of the control solution (mg/mL);
mr represents the weight of the control (mg);
p represents reference substance content assignment; here, P ═ 99.50% provided by the ketjen laboratory;
vr represents the dilution factor of the control solution;
f represents a correction factor for retinol;
ar represents the main peak area of the reference solution;
as represents the main peak area of the test solution;
vs represents the dilution factor of the test solution;
ms represents the sample weight (mg) of the test sample;
ws represents the moisture content of the sample, and if there is no moisture, Ws is 0.00%
2.8 stability test results
As a result: the stability examination of FIG. 1, FIG. 2 and FIG. 3 shows that the retinol stock anti-aging compositions obtained in examples 1 to 3 have better stability at room temperature and 4 ℃ than the negative control. Especially, the content is still higher than 98 percent after being placed for one month at the temperature of 4 ℃, basically no degradation is caused, and the stability is very high.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention, and all the changes or substitutions should be covered within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.
Claims (6)
1. An anti-aging composition for stabilizing a high-concentration retinol stock solution, which is characterized by comprising the following raw material components: 40-50 parts of retinol;
1-10 parts of antioxidant;
40-49 parts of grease;
0.1-5 parts of oil-soluble anti-allergic active substance.
2. The anti-aging composition for stabilizing a high concentration retinol stock solution in accordance with claim 1, wherein the stock ingredients comprise:
45-50 parts of retinol;
3-6 parts of antioxidant;
42-46 parts of grease;
0.1-1 weight part of oil-soluble anti-allergic active matter.
3. The anti-aging composition according to claim 1, wherein the antioxidant is a mixture of 1 or 2 or more of tocopherol, tocopheryl acetate, tocopheryl succinate, butylated hydroxytoluene, butylated hydroxyanisole, diethylhexyl syringylidenemalonate.
4. The anti-aging composition for stabilizing a high concentration retinol stock solution according to claim 1, wherein said oil is 1 or 2 and more mixtures of caprylic/capric triglyceride, tocopheryl acetate, tocopheryl succinate, tocopherol, diethoxyethyl succinate, glycerol tri (ethylhexanoate), diisooctyl adipate, pentaerythritol tetraisostearate, isostearyl stearate, diisostearyl malate, isooctyl palmitate, isopropyl myristate, diisopropyl adipate, mineral oil (No. 15), bis-ethoxy diglycol cyclohexane 1, 4-dicarboxylate, babassu oil glyceryl polyether-8 ester.
5. The anti-aging composition according to claim 1, wherein the oil-soluble anti-allergic active is a mixture of 1 or 2 or more selected from the group consisting of oat extract, bisabolol, and stearyl glycyrrhetinate.
6. The anti-aging composition of claim 1, wherein the stable high concentration retinol stock solution can be used in cosmetics with anti-aging effect, and the application weight percentage is 0.1-1.0%.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114939079A (en) * | 2022-05-19 | 2022-08-26 | 上海奥利实业有限公司 | Preparation method and application of retinol and derivative inclusion thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20050028544A (en) * | 2003-09-18 | 2005-03-23 | 한국콜마 주식회사 | Anti-wrinkle cosmetic composition and its manufacturing method containing a pure retinol stabilized with a nano size of multiple liquid crystal membrane capsule |
| CN109700753A (en) * | 2019-02-14 | 2019-05-03 | 成都市葆姿健康管理有限公司 | A kind of skin care compositions and its application and preparation method with moisturizing anti-oxidation efficacy |
| CN112656695A (en) * | 2019-10-15 | 2021-04-16 | 嘉兴睿肤丽生物科技有限公司 | Preparation of retinol nano-emulsion with low irritation and high stability |
-
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- 2021-11-22 CN CN202111385146.9A patent/CN114129467A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20050028544A (en) * | 2003-09-18 | 2005-03-23 | 한국콜마 주식회사 | Anti-wrinkle cosmetic composition and its manufacturing method containing a pure retinol stabilized with a nano size of multiple liquid crystal membrane capsule |
| CN109700753A (en) * | 2019-02-14 | 2019-05-03 | 成都市葆姿健康管理有限公司 | A kind of skin care compositions and its application and preparation method with moisturizing anti-oxidation efficacy |
| CN112656695A (en) * | 2019-10-15 | 2021-04-16 | 嘉兴睿肤丽生物科技有限公司 | Preparation of retinol nano-emulsion with low irritation and high stability |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114939079A (en) * | 2022-05-19 | 2022-08-26 | 上海奥利实业有限公司 | Preparation method and application of retinol and derivative inclusion thereof |
| CN114939079B (en) * | 2022-05-19 | 2024-04-23 | 上海奥利实业有限公司 | Preparation method and application of retinol and its derivative inclusion |
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