A vitamin C complex, its preparation method and application

Abstract

The present invention relates to a vitamin C complex and its preparation method and application. The vitamin C complex includes component 1: vitamin C; component 2: polydimethylsiloxane; by weight ratio, component 1: component 2 = 6-12: 5-18. The vitamin C complex of the present invention solves the problem that vitamin C is difficult to apply by selecting a suitable dispersant. At the same time, with a suitable particle size, the obtained complex 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.

Description

Technical Field

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

[0002] Ascorbic acid (vitamin C) is a strong antioxidant, which has the functions of anti-aging, improving acne-prone skin, and whitening and brightening. However, it is very difficult to be stable in an aqueous environment and is easily oxidized and inactivated. Usually, high-content ascorbic acid (vitamin C) products on the market are usually prepared by adding vitamin C derivatives or making them into a two-component dosage form.

[0003] There are also some products made into a two-component dosage form, but they can only be used up within a short time after mixing, and the packaging materials can only be used in small-capacity packages, and the packaging material costs are relatively expensive and not environmentally friendly.

[0004] For the derivative solution, on the one hand, the derivative solution has certain difficulties and limitations in formula application. For example, Chinese patent text CN115177548A discloses a vitamin C composition including tetrahexyl decyl ascorbate and an anhydrous silicone oil dispersion system; tetrahexyl decyl ascorbate is a derivative of vitamin C. However, the derivative solution has certain difficulties and limitations in formula application. For the solution in the above text, introducing the derivative hexyl decyl ascorbate solves the stability problem, but tetrahexyl decyl ascorbate itself has a sticky texture and is mainly dissolved in various oils, so the skin feel problem of skin care products also needs to be solved during application. On the other hand, most of the derivatives of ascorbic acid (vitamin C) are currently used in the market, such as: tetrahexyl decyl ascorbate, sodium ascorbyl phosphate, magnesium ascorbyl phosphate, ascorbyl glucoside, 3-O-ethyl ascorbic acid, ascorbyl tetraisopalmitate, etc. Finally, it needs to be hydrolyzed into ascorbic acid (vitamin C) to achieve better effects, and the hydrolysis efficiency 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 complex, a preparation method thereof, and an application thereof, which can achieve the addition of a high content of vitamin C.

[0006] In the first aspect of the present invention, a vitamin C complex is provided, including component 1: vitamin C; component 2: polydimethylsiloxane. According to the weight ratio, 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 complex is 1-100 μm, and the proportion of >30 μm is ≤1 wt%, so as to achieve better stability and use effect.

[0008] In a second aspect of the present invention, there is provided a method for preparing the above vitamin C complex, comprising the steps of:

[0009] Mix and disperse the components 1 and 2 in the formula amount until there is no obvious agglomeration, and then perform grinding treatment.

[0010] Preferably, a three-roll mill is used for grinding. During grinding, the gap between each roller is controlled at 0.04 - 0.06 mm, and the rotation speed during grinding 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.

[0011] In a third aspect of the present invention, there is provided a skin care product containing the above vitamin C complex, and the skin care product is a pure oil anhydrous system.

[0012] In a fourth aspect of the present invention, there is provided a whitening cream with a high vitamin C content, comprising the above vitamin C complex and acceptable excipients; the acceptable excipients may include one or more of emollients, emulsifying and dispersing agents, thickening and suspending agents.

[0013] Further, the whitening cream is composed of the following components in weight percentages: 11 - 30% of the above vitamin C complex, 0.5 - 1.5% of the emulsifying and dispersing agent, 12% - 20% of the thickening and suspending agent, and the emollient is made up to 100%.

[0014] Further, the emollient is one or several of polydimethylsiloxane, cyclopentasiloxane, phenyltrimethicone, hydrogenated polyisobutene. In a preferred embodiment of the present invention, the emollient is polydimethylsiloxane.

[0015] Further, the emulsifying and dispersing agent is one or several of PEG-10 polydimethylsiloxane, lauryl PEG-9 polydimethylsiloxyethyl polydimethylsiloxane, PEG / PPG-18 / 18 polydimethylsiloxane, cetyl PEG / PPG-10 / 1 polydimethylsiloxane. In a preferred embodiment of the present invention, the emulsifying and dispersing agent is PEG-10 polydimethylsiloxane.

[0016] Further, the thickening and suspending agent is one or several of vinyl polydimethylsiloxane / polymethylsiloxane sesquisiloxane cross-linked polymer, dimethyldistearylammonium lithium montmorillonite, polydimethylsiloxane / vinyl polydimethylsiloxane cross-linked polymer. In a preferred embodiment of the present invention, the emulsifying and dispersing agent is polydimethylsiloxane / vinyl polydimethylsiloxane cross-linked polymer.

[0017] In a preferred embodiment of the present invention, the whitening cream is composed of the following components in weight percentages: 11 - 30% of vitamin C complex, 0.5 - 1.5% of PEG - 10 dimethicone, 12% - 20% of dimethicone / vinyl dimethicone cross - polymer, and the balance up to 100% of dimethicone. Further preferably, in the whitening cream, the vitamin C content is between 7.5 - 15%, more preferably between 7.5 - 13%, and most preferably, the vitamin C content is 13%.

[0018] Compared with the prior art, the present invention has the following beneficial effects:

[0019] The vitamin C complex of the present invention solves the problem of difficult application of vitamin C by selecting a suitable dispersant. At the same time, with a suitable particle size, the obtained complex has good stability and can be applied to a pure oil and 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

[0020] Figure 1 For the comparison of particle size changes in Example 1;

[0021] Figure 2 For the comparison of particle size changes in Example 2;

[0022] Figure 3 For the comparison of particle size changes in Example 3;

[0023] Figure 4 For the comparison of particle size changes in Example 4;

[0024] Figure 5 For the comparison of particle size changes in Example 5;

[0025] Figure 6 For the comparison of particle size changes in Example 6;

[0026] Figure 7 For the comparison of particle size changes in Example 7;

[0027] Figure 8 For the comparison of particle size changes in Example 8;

[0028] Figure 9 For the comparison of particle size changes in Example 9;

[0029] Figure 10 For the comparison of particle size changes in Example 10;

[0030] Figure 11 For the comparison of particle size changes in Example 11;

[0031] Figure 12Particle size change comparison for Example 12;

[0032] Figure 13 Particle size change comparison for Example 13;

[0033] Figure 14 Particle size change comparison for Comparative Example 1;

[0034] Figure 15 Particle size change comparison for Comparative Example 2. Detailed implementation mode

[0035] To facilitate the understanding of the present invention, the present invention will be described more comprehensively 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, these embodiments are provided to make the understanding of the disclosure of the present invention more thorough and comprehensive.

[0036] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by those skilled in the technical field to which the present invention belongs. The terms used in the description of the present invention herein 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.

[0037] Unless otherwise specified, the reagents used in the following examples and comparative examples are commercially available; unless otherwise specified, the methods used in the following examples and comparative examples can be realized by conventional methods.

[0038] Examples 1-5 Vitamin C complex

[0039] The formula components of the vitamin C complex in each example are shown in Table 1.

[0040] The preparation method of the vitamin C complex is as follows, including the steps:

[0041] 1), Accurately weigh the components of each formula amount;

[0042] 2), Add Component 1 and Component 2 to the preparation container and stir and disperse until there is no obvious agglomeration.

[0043] 4), Transfer the dispersed material in step 2) to a three-roll grinder for grinding, control the gap of each roller of the three-roll grinder at 0.05 mm, control the rotation speed at 40 rpm / min during grinding, and grind twice.

[0044] 5), Take samples for detection, and after passing, discharge the material.

[0045] Table 1 Formula components of Examples 1-5

[0046]

[0047] The vitamin C complex samples of Examples 1-5 were respectively placed in environments of -10°C, 25°C, and 45°C for 30 days, and whether unstable phenomena such as layering, discoloration, and oil separation occurred in the products was observed to investigate their stability, and the particle size change data at 45°C for one month was also investigated. The results are as Figures 1-5 and Table 2 show. Among them, the test result in Example 4 is the best.

[0048] Table 2 Stability data of samples of Examples 1-5

[0049]

[0050] Note: "ok" in the table indicates that no unstable phenomena such as layering, discoloration, and oil separation occurred during the test.

[0051] Examples 6-14 Experiment on optimization of process parameters for the preparation method of vitamin C complex

[0052] In Examples 6-14, the ratio of the vitamin C complex in Example 4 was used, and the parameters of the preparation process were compared and tested. The main selection was for two parameters, the roller gap and the grinding speed. The experimental design is shown in Table 3. The vertical column is the grinding speed, with the unit of rpm / min, and the horizontal row is the roller gap, with the unit of mm.

[0053] Table 3 Schematic diagram of experimental design for process optimization of the preparation method

[0054]

[0055] The obtained samples were respectively placed in environments of -10°C, 25°C, and 45°C for 30 days, and whether unstable phenomena such as layering, discoloration, and oil separation occurred in the products was observed to investigate the stability, and the particle size change data at 45°C for one month was recorded. The results are as Figures 6-15 and Table 4 show.

[0056] Table 4 Stability data of samples of Examples 6-14

[0057]

[0058] Note: "ok" in the table indicates that no unstable phenomena such as layering, discoloration, and oil separation occurred during the test.

[0059] As can be seen from the above table, after the stability test of the sample in Example 4, the particle size change was small and the grinding efficiency was relatively high, which was the preferred option.

[0060] Application and efficacy test of the vitamin C complex

[0061] I. Preparation of Whitening Cream Containing Vitamin C Complex

[0062] Application Example 1

[0063] A whitening cream, by weight percentage, consists of the following raw materials: Vitamin C complex in Example 4: 26%, PEG-10 dimethicone: 1%, dimethicone / vinyl dimethicone crosspolymer: 17%, dimethicone: up to 100%.

[0064] The preparation method of the whitening cream includes the following steps:

[0065] 1) Stir and disperse dimethicone, PEG-10 dimethicone, and dimethicone / vinyl dimethicone crosspolymer until there are no particles, and then further homogenize and disperse evenly.

[0066] 2) Add the Vitamin C complex, stir, homogenize, and disperse evenly to obtain the whitening cream.

[0067] Application Example 2

[0068] Same as Application Example 1, except that the proportion of the Vitamin C complex in Example 4 is 15%, and the reduced amount is supplemented with dimethicone to 100%.

[0069] Application Example 3

[0070] Same as Application Example 1, except that the proportion of the Vitamin C complex in Example 4 is 30%, and the reduced amount is supplemented with dimethicone to 100%

[0071] Comparative Example 3

[0072] Same as Application Example 1, except that except for the dimethicone in the Vitamin C complex in Example 4, the remaining dimethicone is replaced with isododecane, and the rest remains unchanged.

[0073] Comparative Example 4

[0074] 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.

[0075] II. Performance Tests of Whitening Creams in Application Examples and Comparative Examples:

[0076] 1. Stability Test:

[0077] Place each whitening cream in environments of -10°C, 25°C, and 45°C for 30 days, observe whether the product shows unstable phenomena such as layering, discoloration, and oiling, conduct stability tests, and record the particle size change data at 45°C for one month. The results are shown in Table 5. It can be seen that the vitamin C complex of the embodiment of the present invention has good stability after being applied to the whitening cream.

[0078] Table 5 Stability of Skin Care Products Containing Vitamin C Complex

[0079]

[0080] Note: "ok" in the table indicates that no unstable phenomena such as layering, discoloration, and oiling occurred during the test period.

[0081] 2. Skin Feel Test:

[0082] Select 10 subjects to try the above-mentioned whitening creams respectively, and evaluate the skin feel of each sample from three aspects: spreadability, absorbability, and stickiness. The test results are shown in Table 6.

[0083] Table 6 Skin Feel Test Results of Skin Care Products Containing Vitamin C Complex

[0084]

[0085] Description of Evaluation Indexes:

[0086] Spreadability refers to the ease of spreading the sample on the skin. The score ranges from 1 to 9, and the ease of spreading ranges from difficult to easy in turn; the higher the score, the easier it is to spread.

[0087] Absorbability refers to the absorption speed of the skin on the sample during the use of the sample; the score ranges from 1 to 9, and the absorption speed ranges from slow to fast in turn, that is, from difficult to absorb to easy to absorb; the higher the score, the easier it is to absorb.

[0088] Stickiness refers to the residue of the sample on the skin surface and the sticky feeling of the skin after using the sample. The score ranges from 1 to 9, and the skin surface ranges from dry to sticky in turn. The lower the score, the drier it is.

[0089] Conclusion: From the average scores in the skin feel comparison test, several skin feel indexes in Application Examples 1-3 are relatively excellent, and have a good skin feel experience.

[0090] 3. Safety Test of High-Content Vitamin C Complex:

[0091] According to Chapter 7 of the "Technical Specifications for Cosmetics Safety" (2015 Edition) - Test Methods for Human Safety - Human Skin Patch Test, adopt the method of skin closed patch test to conduct human skin patch tests on the whitening cream products of the application examples and the comparative examples. The results are shown in Table 7.

[0092] Table 7 Results of human skin patch test of skin care products containing vitamin C complex (unit: person)

[0093]

[0094] As can be seen from the table, no suspicious or positive reactions occurred in the skin occlusion patch test with the vitamin C complexes obtained from Application Examples 1 to 3, showing excellent safety; suspicious reactions occurred in Comparative Examples 3 and 4. It can be seen that it is the selection of specific raw material types in the present invention that endows excellent safety.

[0095] 4. Tyrosinase activity inhibition experiment

[0096] According to the group standard of Shanghai Daily Chemical Industry Association, "T / SHRH 015-2018 Cosmetics - Test Method for Tyrosinase Activity Inhibition", different concentrations of kojic acid were used as positive control products, and the test products were vitamin C aqueous solutions with the same concentrations as those in the 5 application examples. Raw materials with tyrosinase activity inhibition can reduce the conversion of dopa to dopaquinone, thereby reducing the absorbance value. According to the change of the absorbance value, the inhibitory effect of the raw material on tyrosinase activity was evaluated. The experimental results are shown in Tables 8-9:

[0097] Table 8 Inhibition rate of tyrosinase activity of positive control product kojic acid

[0098]

[0099] Table 9 Inhibition rate of tyrosinase activity of skin care products containing vitamin C complex

[0100]

[0101] As can be seen from the above table, when the vitamin C concentration was 13% (Application Example 1), the inhibition rate of tyrosinase activity reached 92.23%. The inhibition rate of tyrosinase activity when the vitamin C concentration was 15% (Application Example 3) was not much different from that when the vitamin C concentration was 13%. Considering the cost, a vitamin C concentration of 13% (Application Example 1) is the preferred option.

[0102] 5. Whitening efficacy test

[0103] The test was carried out in accordance with the specific requirements of the first method of the test method for the freckle and whitening efficacy of cosmetics in the "Technical Specifications for Cosmetics Safety" (2015 edition), the post-method of the test method for the freckle and whitening efficacy of the ultraviolet-induced human skin darkening model

[0104] Thirty volunteers were selected to try Application Example 1, once in the morning and once in the evening. The MI value and ITA° value of the subjects' faces were measured using a skin color difference test probe before use and at the first week, second week, and fourth week respectively. The negative control was a blank control.

[0105] The test results showed that the difference in ITAº before and after applying the test product was highly significant compared with the negative control (P < 0.01), indicating that the test product had whitening efficacy.

[0106] The technical features of the above-described embodiments can be combined arbitrarily. For the sake of brevity of description, 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, it should be considered as falling within the scope described in this specification.

[0107] The above-described embodiments merely represent several implementation manners of the present invention. The description is relatively specific and detailed, but it should not be construed as a limitation on the scope of the invention patent. It should be noted that for those of ordinary skill in the art, without departing from the concept of the present invention, several modifications and improvements can still be made, and these all belong to the protection scope of the present invention. Therefore, the protection scope of the present invention patent shall be subject to the appended claims.

Claims

1. A vitamin C compound, characterized in that: Composed of component 1: vitamin C; And component 2: polydimethylsiloxane; according to the weight ratio, component 1: component 2 = 6~8:5~12; The particle size of the vitamin C compound is 1-100 μm, and the proportion of particles larger than 30 μm is ≤1wt%; The vitamin C compound is prepared by the following steps: mixing and dispersing the components 1 and 2 in the formula amount until no obvious agglomeration occurs, and then grinding the components by a three-roller grinder, wherein 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.

2. A skin care product comprising the vitamin C compound according to claim 1, wherein the skin care product is a pure oil-free water-free system skin care product.

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

4. The high-vitamin C content whitening cream according to claim 3, 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 claim 1, 0.5-1.5% of an emulsifying dispersant, 12-20% of a thickening suspending agent, and 100% of an emollient.

5. The high vitamin C content whitening cream according to claim 4, characterized in that: The emollient is one or more of polydimethylsiloxane, cyclopentasiloxane, phenyl trimethicone and hydrogenated polyisobutylene.

6. The high-vitamin C content whitening cream according to claim 4, 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.

7. The high vitamin C content whitening cream according to claim 4, 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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