Vitamin C compound as well as preparation method and application thereof

Abstract

The invention relates to a vitamin C compound as well as a preparation method and application thereof. The vitamin C compound comprises a component 1: vitamin C; a component 2: polydimethylsiloxane; the weight ratio of the component 1 to the component 2 is (6-12): (5-18). According to the vitamin C compound disclosed by the invention, the problem that vitamin C is difficult to apply is solved by selecting a proper dispersing agent, meanwhile, the compound is matched with a proper particle size, so that the obtained compound is good in stability and can be applied to a pure oil anhydrous system to prepare whitening cream with high vitamin C content, and the prepared whitening cream is high in vitamin C content, stable in performance and free of toxic and side effects. The whitening effect is excellent.

Description

Technical Field

[0001] The present invention relates to the field of cosmetics, and in particular to a vitamin C compound and a preparation method and application thereof. Background Art

[0002] Ascorbic acid (vitamin C) is a strong antioxidant that has anti-aging, acne-improving, and whitening and brightening effects. However, it is difficult to stabilize in an aqueous environment and is easily oxidized and inactivated. High-content ascorbic acid (vitamin C) products on the market are usually made by adding vitamin C derivatives or making them into two-dose dosage forms.

[0003] Some products are made into two-dose dosage forms, but after the products are mixed, they can only be used up within a short time. The packaging materials can only be small-capacity packaging, the packaging materials are relatively expensive, and they are not environmentally friendly.

[0004] For the derivative solution, on the one hand, the derivative solution has certain difficulties and limitations in the application of formulas. For example, the Chinese patent text CN115177548A discloses a vitamin C composition and a dispersion system including tetrahexyldecyl ascorbate and anhydrous silicone oil; wherein tetrahexyldecyl ascorbate is a derivative of vitamin C. However, the derivative solution has certain difficulties and limitations in the application of formulas. As in the solution in the above text, the introduction of the derivative hexyldecyl ascorbate solves the stability problem, but the texture of tetrahexyldecyl ascorbate itself is sticky, and it is mainly dissolved in various oils, so the skin feel problem of skin care products must be solved when it is applied. On the other hand, most of the derivatives used in the market are ascorbic acid (vitamin C) derivatives, such as tetrahexyldecyl ascorbate, sodium ascorbyl phosphate, magnesium ascorbyl phosphate, ascorbyl glucoside, 3-o-ethyl ascorbic acid, ascorbyl tetraisopalmitate, etc., which ultimately need to be hydrolyzed into ascorbic acid (vitamin C) to achieve better effects, and the efficiency of hydrolysis affects the use effect. Summary of the invention

[0005] Based on this, in order to solve at least one technical problem existing in the prior art, the present invention provides a vitamin C compound and a preparation method and application thereof, which can achieve the addition of high-content vitamin C.

[0006] The first aspect of the present invention provides a vitamin C compound, comprising component 1: vitamin C; component 2: polydimethylsiloxane, in a weight ratio of component 1: component 2 = 6-12: 5-18, preferably, component 1: component 2 = 6-8: 5-12.

[0007] Preferably, the particle size of the vitamin C compound is 1-100 μm, and the proportion of particles > 30 μm is ≤ 1wt%, so as to achieve better stability and use effect.

[0008] The second aspect of the present invention provides a method for preparing the above-mentioned vitamin C compound, comprising the steps of: Mix and disperse the components 1 and 2 in the formula until there is no obvious agglomeration, and then grind them.

[0009] Preferably, a three-roller mill is used for grinding, and during grinding, the gap between each roller is controlled at 0.04-0.06 mm, the rotation speed is controlled at 20-50 rpm / min, and grinding is performed twice. In this way, the material is evenly dispersed, the particle size is appropriate, and the product stability is better.

[0010] The third aspect of the present invention provides a skin care product comprising the above-mentioned vitamin C compound, wherein the skin care product is a pure oil-free water-free system.

[0011] The fourth aspect of the present invention provides a whitening cream with a high vitamin C content, comprising the vitamin C compound and acceptable excipients; the acceptable excipients may include one or more of emollients, emulsifying dispersants, and thickening suspending agents.

[0012] Furthermore, the whitening cream is composed of the following components in percentage by weight: 11-30% of the above-mentioned vitamin C compound, 0.5-1.5% of an emulsifying dispersant, 12%-20% of a thickening suspending agent, and 100% of an emollient.

[0013] Furthermore, the emollient is one or more of polydimethylsiloxane, cyclopentasiloxane, phenyl trimethicone, and hydrogenated polyisobutylene. In a preferred embodiment of the present invention, the emollient is polydimethylsiloxane.

[0014] Further, the emulsifying dispersant is one or more of PEG-10 polydimethylsiloxane, lauryl PEG-9 polydimethylsiloxyethyl polydimethylsiloxane, PEG / PPG-18 / 18 polydimethylsiloxane, and cetyl PEG / PPG-10 / 1 polydimethylsiloxane. In a preferred embodiment of the present invention, the emulsifying dispersant is PEG-10 polydimethylsiloxane.

[0015] Further, the thickening suspending agent is one or more of vinyl dimethicone / dimethicone silsesquioxane crosspolymer, disteardimonium hectorite, dimethicone / dimethicone vinyl crosspolymer. In a preferred embodiment of the present invention, the emulsifying dispersant is dimethicone / dimethicone vinyl crosspolymer.

[0016] In a preferred embodiment of the present invention, the whitening cream is composed of the following components in weight percentage: 11-30% vitamin C compound, 0.5-1.5% PEG-10 dimethicone, 12%-20% dimethicone / vinyl dimethicone cross-polymer, and dimethicone is supplemented to 100%. Further preferably, the vitamin C content in the whitening cream is between 7.5% and 15%, more preferably, between 7.5% and 13%, and most preferably, the vitamin C content is 13%.

[0017] Compared with the prior art, the present invention has the following beneficial effects: The vitamin C compound of the present invention solves the problem that vitamin C is difficult to apply by selecting a suitable dispersant, and at the same time, by combining a suitable particle size, the obtained compound has good stability and can be applied to a pure oil anhydrous system to prepare a whitening cream with a high vitamin C content. The prepared whitening cream has a high vitamin C content, stable performance and excellent whitening effect. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] Figure 1 The particle size change comparison of Example 1; Figure 2 The particle size change comparison of Example 2; Figure 3 The particle size change comparison of Example 3; Figure 4 The particle size change comparison of Example 4; Figure 5 The particle size change comparison of Example 5; Figure 6 The particle size change comparison of Example 6; Figure 7 The particle size change comparison of Example 7; Figure 8 The particle size change comparison of Example 8; Fig. 9 The particle size change comparison of Example 9; Fig.10 The particle size change comparison of Example 10; Fig.11 The particle size change comparison of Example 11; Fig.12 The particle size change comparison of Example 12; Fig.13 The particle size change comparison of Example 13; Fig.14 The particle size change comparison of Comparative Example 1; Fig.15 This is a comparison of the particle size changes in Comparative Example 2. DETAILED DESCRIPTION

[0019] In order to facilitate the understanding of the present invention, the present invention will be described more fully below with reference to relevant embodiments. Preferred embodiments of the present invention are given in the embodiments. However, the present invention can be implemented in many different forms and is not limited to the embodiments described herein. On the contrary, the purpose of providing these embodiments is to make the understanding of the disclosure of the present invention more thorough and comprehensive.

[0020] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as those commonly understood by those skilled in the art to which the present invention belongs. The terms used herein in the specification of the present invention are only for the purpose of describing specific embodiments and are not intended to limit the present invention. The term "and / or" used herein includes any and all combinations of one or more of the related listed items.

[0021] Unless otherwise specified, the sources of reagents used in the following examples and comparative examples are all commercially available; the methods used in the following examples and comparative examples, unless otherwise specified, are all achievable by conventional methods.

[0022] Example 1-5 Vitamin C compound The formula components of the vitamin C compound of each embodiment are shown in Table 1. The preparation method of the vitamin C compound is as follows, comprising the steps of: 1) Accurately weigh the ingredients of each formula; 2) Add component 1 and component 2 into the preparation container and stir until there is no obvious agglomeration.

[0023] 4) Transfer the dispersed material in step 2) to a three-roll mill for grinding. The gap between each roller of the three-roll mill is controlled at 0.05 mm, the speed is controlled at 40 rpm / min, and the grinding is performed twice.

[0024] 5) Take samples for testing, and discharge the materials after they are qualified.

[0025] Table 1 Formula components of Examples 1-5

[0026] The vitamin C compound samples of Examples 1-5 were placed in an environment of -10°C, 25°C, and 45°C for 30 days to observe whether the products showed unstable phenomena such as stratification, discoloration, and oiliness, and to investigate their stability. The particle size change data at 45°C for one month was investigated. The results are as follows: Figure 1-5 And as shown in Table 2. Among them, the test result in Example 4 is the best.

[0027] Table 2 Stability data of samples of Examples 1-5

[0028] Note: "ok" in the table means that there was no delamination, discoloration, oiling or other unstable phenomena during the test.

[0029] Example 6-14 Experiment on Optimization of Process Parameters for Preparation of Vitamin C Compound Examples 6-14 all use the ratio of the vitamin C compound of Example 4 to conduct comparative tests on the parameters of the preparation process, mainly selecting two parameters: roller gap and grinding speed. The experimental design is shown in Table 3, where the vertical column is the grinding speed in rpm / min and the horizontal column is the roller gap in mm.

[0030] Table 3 Schematic diagram of experimental design for process optimization of preparation method

[0031] The obtained samples were placed in -10℃, 25℃, and 45℃ environments for 30 days to observe whether the products showed unstable phenomena such as stratification, discoloration, and oil secretion, and to examine the stability. The particle size change data at 45℃ for one month was recorded. The results are as follows Figure 6-15 As shown in Table 4.

[0032] Table 4 Stability data of samples of Examples 6-14

[0033] Note: "ok" in the table means that there was no delamination, discoloration, oiling or other unstable phenomena during the test.

[0034] It can be seen from the above table that after the stability test, the particle size of the sample in Example 4 changed little and the grinding efficiency was relatively high, which is the preferred option.

[0035] Application and efficacy test of compound containing vitamin C 1. Preparation of whitening cream containing vitamin C compound Application Example 1 A whitening cream is composed of the following raw materials in percentage by weight: Vitamin C compound of Example 4: 26%, PEG-10 dimethicone: 1%, dimethicone / vinyl dimethicone crosspolymer: 17%, and dimethicone: to 100%.

[0036] The preparation method of the whitening cream comprises the following steps: 1) Stir and disperse dimethicone, PEG-10 dimethicone, and dimethicone / vinyl dimethicone crosspolymer until there are no particles, and then further homogenize and disperse them evenly.

[0037] 2) Adding the vitamin C compound, stirring and homogenizing to obtain the whitening cream.

[0038] Application Example 2 The same as Application Example 1, except that the ratio of the vitamin C compound in Example 4 is 15%, and the reduced amount is supplemented to 100% with polydimethylsiloxane.

[0039] Application Example 3 Same as Application Example 1, except that the ratio of the vitamin C compound in Example 4 is 30%, and the reduced amount is supplemented to 100% with polydimethylsiloxane. Comparative Example 3 Same as Application Example 1, except that, except for the polydimethylsiloxane in the vitamin C compound of Example 4, the remaining polydimethylsiloxane is replaced with isododecane, and the rest remains unchanged.

[0040] Comparative Example 4 Same as Application Example 1, except that the PEG-10 dimethicone in Application Example 1 is replaced with laureth-3, and the rest remains unchanged.

[0041] 2. Application examples and comparative examples of whitening cream performance tests: 1. Stability test: Each whitening cream was placed in an environment of -10°C, 25°C, and 45°C for 30 days to observe whether the product showed unstable phenomena such as stratification, discoloration, and oil secretion. A stability test was performed and the particle size change data for one month at 45°C was recorded. The results are shown in Table 5. It can be seen that the vitamin C compound of the embodiment of the present invention has good stability after being applied to the whitening cream.

[0042] Table 5 Stability of skin care products containing vitamin C compounds

[0043] Note: "ok" in the table means that there was no delamination, discoloration, oiling or other unstable phenomena during the test.

[0044] 2. Skin feel test: Ten subjects were selected to try each of the above whitening creams, and the skin feel of each sample was evaluated from three aspects: spreadability, absorbency, and stickiness. The test results are shown in Table 6.

[0045] Table 6 Skin feel test results of skin care products containing vitamin C compound

[0046] Evaluation indicators description: Spreadability refers to how easily a sample can be spread on the skin, with scores ranging from 1 to 9, with the spreadability ranging from difficult to easy; the higher the score, the easier it is to spread.

[0047] Absorbability refers to the speed at which the skin absorbs the sample during use; the score ranges from 1 to 9, and the absorption speed ranges from slow to fast, that is, from not easily absorbed to easily absorbed; the higher the score, the easier it is to absorb.

[0048] Stickiness refers to the residual sample on the skin surface after use, as well as the stickiness of the skin. The score ranges from 1 to 9, with the skin surface ranging from dry to sticky. The lower the score, the drier it is.

[0049] Conclusion: Judging from the average scores in the skin feel comparison test, the skin feel indicators in Application Examples 1 to 3 are relatively excellent and provide a good skin feel experience.

[0050] 3. Safety test of high-content vitamin C compound: According to Chapter 7 of the "Technical Specifications for Safety of Cosmetics" (2015 Edition) - Human Skin Patch Test, the skin occlusion patch test method was adopted to conduct human skin patch tests on the whitening cream products of the application example and the comparative example. The results are shown in Table 7.

[0051] Table 7 Human skin patch test results of skin care products containing vitamin C compounds (unit: person)

[0052] As can be seen from the table, the vitamin C compounds obtained in application examples 1 to 3 showed no suspicious or positive reactions in the skin occlusive patch test, showing excellent safety; while comparative examples 3 and 4 showed suspicious reactions. It can be seen that it is the selection of specific raw material types in the present invention that gives excellent safety.

[0053] 4. Tyrosinase activity inhibition experiment According to the Shanghai Daily Chemical Industry Association group standard "T / SHRH 015-2018 Cosmetics-Tyrosinase Activity Inhibition Test Method", kojic acid of different concentrations was used as the positive control, and the test product was a vitamin C aqueous solution of the same concentration as in the five application examples. Raw materials with tyrosinase activity inhibition can reduce the conversion of dopa into dopaquinone, thereby reducing the absorbance value. Based on the change in absorbance value, the inhibitory effect of the raw material on tyrosinase activity was evaluated. The experimental results are shown in Table 8-9: Table 8 Inhibition rate of kojic acid tyrosinase activity of positive control

[0054] Table 9 Tyrosinase activity inhibition rate of skin care products containing vitamin C compound

[0055] As can be seen from the above table, the inhibition rate of tyrosinase activity when the vitamin C concentration is 13% (Application Example 1) reaches 92.23%, while the inhibition rate of tyrosinase activity when the vitamin C concentration is 15% (Application Example 3) is not much different from that when the vitamin C concentration is 13%. Based on cost considerations, the vitamin C concentration of 13% (Application Example 1) is the preferred option.

[0056] 5. Whitening efficacy test The inspection shall be carried out in accordance with the specific requirements of the first method of testing the freckle removal and whitening efficacy of cosmetics - ultraviolet-induced human skin darkening model - and the second method of testing the freckle removal and whitening efficacy of cosmetics - Technical Specifications for Safety of Cosmetics (2015 edition).

[0057] 30 volunteers were selected to conduct a trial according to Example 1, once in the morning and once in the evening, and the MI and ITA° values ​​of the subjects' faces were tested using a skin color difference test probe before use and in the first, second, and fourth weeks. The negative control was a blank control.

[0058] The test results showed that the difference in ITAº before and after application of the test product was significantly higher than that of the negative control (P < 0.01), indicating that the test product has a whitening effect.

[0059] The technical features of the above-described embodiments may be arbitrarily combined. To make the description concise, not all possible combinations of the technical features in the above-described embodiments are described. However, as long as there is no contradiction in the combination of these technical features, they should be considered to be within the scope of this specification.

[0060] The above-mentioned embodiments only express several implementation methods of the present invention, and the descriptions thereof are relatively specific and detailed, but they cannot be understood as limiting the scope of the invention patent. It should be pointed out that, for ordinary technicians in this field, several variations and improvements can be made without departing from the concept of the present invention, and these all belong to the protection scope of the present invention. Therefore, the protection scope of the patent of the present invention shall be subject to the attached claims.

Claims

1. A vitamin C compound, characterized in that: include: Component 1: Vitamin C; Component 2: polydimethylsiloxane; According to weight ratio, component 1: component 2 = 6~12: 5~18.

2. The vitamin C compound according to claim 1, characterized in that The component 1:component 2 = 6~8:5~12.

3. The vitamin C compound according to claim 1 or 2, characterized in that: The particle size of the compound is 1-100 μm, and the proportion of particles larger than 30 μm is ≤1 wt %.

4. The method for preparing the vitamin C compound according to any one of claims 1 to 3, characterized in that: The method comprises the following steps: mixing and dispersing the components 1 and 2 in the formula until there is no obvious agglomeration, and then grinding the components by using a three-roller grinder. During grinding, the gap between each roller is controlled at 0.04-0.06 mm, the rotation speed is controlled at 20-50 rpm / min, and the grinding is performed twice.

5. A skin care product, comprising the vitamin C compound according to any one of claims 1 to 3, wherein the skin care product is a pure oil-free water-free system skin care product.

6. A whitening cream with high vitamin C content, characterized in that: The invention comprises the vitamin C compound according to any one of claims 1 to 3 and acceptable auxiliary materials.

7. The high vitamin C content whitening cream according to claim 6, characterized in that: The whitening cream is composed of the following components in percentage by weight: 11-30% of the vitamin C compound according to any one of claims 1 to 3, 0.5-1.5% of an emulsifying dispersant, 12-20% of a thickening suspending agent, and 100% of an emollient.

8. The high vitamin C content whitening cream according to claim 7, characterized in that: The emollient is one or more of polydimethylsiloxane, cyclopentasiloxane, phenyl trimethicone and hydrogenated polyisobutylene.

9. The high-vitamin C content whitening cream according to claim 7, characterized in that: The emulsifying dispersant is one or more of PEG-10 polydimethylsiloxane, PEG / PPG-18 / 18 polydimethylsiloxane, and cetyl PEG / PPG-10 / 1 polydimethylsiloxane.

10. The high vitamin C content whitening cream according to claim 7, characterized in that: The thickening suspending agent is one or more of vinyl polydimethylsiloxane / polymethylsiloxane silsesquioxane cross-linked polymer, disteardimethylammonium hectorite, and polydimethylsiloxane / vinyl polydimethylsiloxane cross-linked polymer.

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