CN111973529A

CN111973529A - Moisturizing whitening cream and preparation method thereof

Info

Publication number: CN111973529A
Application number: CN202010918558.3A
Authority: CN
Inventors: 周鸿立; 朱孟楠; 单佳乐; 曹冬雪; 翟婉辰; 张红菊; 申家萌
Original assignee: Jilin Institute of Chemical Technology
Current assignee: Jilin Institute of Chemical Technology
Priority date: 2020-09-04
Filing date: 2020-09-04
Publication date: 2020-11-24

Abstract

The invention provides a preparation method of moisturizing whitening cream, which comprises the following raw materials, by weight, 80-100 parts of wula sedge essence, 10-20 parts of glycerol, 2-4 parts of butanediol, 6-12 parts of propylene glycol, 0.1-0.4 part of sodium hyaluronate, 0.2-0.5 part of sodium carboxymethylcellulose, 2-5 parts of carbomer, 3-6 parts of triethanolamine, 0.5-2 parts of vitamin C, 0.5-2 parts of salicylic acid, 0.1-1 part of EDTA-2Na0.1 part of water-soluble azone, 0.1-0.5 part of cason, 0.1-0.3 part of ethylparaben and 0.1-0.3 part of essence. The moisturizing whitening cream disclosed by the invention is fresh in smell, contains various moisturizing agents and whitening agents, has dual effects of moisturizing and whitening, is added with natural plant essence, is non-toxic, can improve the skin state, meets the requirements of contemporary people on skin care products, and has a better development market.

Description

Moisturizing whitening cream and preparation method thereof

Technical Field

The invention relates to the technical field of daily cosmetics, in particular to a moisturizing and whitening cream containing Wula grass essence.

Background

Wula grass, a plant of the genus carex of the family Cyperaceae, is mainly distributed in the northeast three provinces of China, is one of the traditional three treasures of the northeast, and has a long civilian history. The leaf of the carex meyeriana is slender and soft, the fiber is tough, the carex meyeriana has very strong antifungal effect, mycorrhiza is not formed with fungi, and the natural plant type carex meyeriana is an attribute which is not possessed by common natural plants. The Wula sedge essence is used as a solvent of cosmetics, the pH values of the skin of most human beings and most essences are weak acid, and the plant essence can realize the effects of mildly nursing the skin, adjusting the pH value of the skin and promoting the absorption of nutrient substances. At present, researches on plant essence skin care products are few, skin care products prepared from the Wula grass essence are not developed, and if the plant essence can be widely applied to skin care products, the plant essence is convenient to use and has better treatment and maintenance effects on skin. Proves that the Wula grass essence also has wide application prospect in the field of cosmetics.

The degree of skin tenderness is mainly determined by the water content of the horny layer of the epidermis, and the reduction of the skin moisturizing function can cause various skin problems, when the skin lacks water, cell metabolism and information transmission are affected, the physiological structure of the skin is changed, such as dry skin, roughness, wrinkle increase, pigment increase and the like, and skin diseases, such as dermatitis, eczema, acne and the like, can be induced more seriously. Because the skin is exposed to the external environment for a long time and is easy to be damaged, the epidermal cells are damaged, and the components such as polysaccharide, protein, amino acid and the like extracted from plants contain a large amount of hydroxyl in the structure, can be combined with water in a hydrogen bond form, form a water locking film on the surface of the skin to prevent the water loss of the skin and achieve the effect of lasting moisture preservation.

The content and distribution of melanin affect the color of human skin, the structural function and quantity of melanocytes directly affect the content of melanin in skin and are also key factors for generating melanin, whitening products in the market at present mainly comprise physical whitening and biochemical whitening, the physical whitening is usually achieved by covering powder such as titanium dioxide, zinc oxide and the like, and the biochemical whitening is achieved by inhibiting the generation of melanin, blocking the transportation of melanin, accelerating the metabolism speed of epidermal cells, blocking a signal path in the melanin generation process and the like. The selection of the whitening raw materials must meet the requirements of national cosmetic hygiene standards and follow the safe and effective principle.

Disclosure of Invention

In the present invention, a moisturizing whitening cream was prepared using plant essences and evaluated.

The specific scheme is as follows:

2 parts of carbomer, 90 parts of Meyer sedge essence, 0.25 part of ethylparaben, 20 parts of glycerol, 12 parts of 1, 2-propylene glycol, 4 parts of butanediol, 0.2 part of EDTA-2Na0.2 part of triethanolamine, 0.1 part of sodium hyaluronate, 0.2 part of sodium carboxymethylcellulose, 0.4 part of vitamin C, 0.25 part of salicylic acid, 0.2 part of water-soluble azone, 0.2 part of cason and 0.2 part of essence.

A preparation method of moisturizing whitening cream comprises the following steps:

step 1, soaking 500 g of dried Meyer sedge and 8500 g of purified water for 2 h, extracting at 100 ℃ for 2 h to obtain Meyer sedge extracting solution, and distilling and collecting the Meyer sedge extracting solution to obtain Meyer sedge essence;

step 2, swelling carbomer in advance, adding glycerol, 1, 2-propylene glycol and butanediol after swelling, and stirring for dissolving for later use; dissolving ethylparaben and salicylic acid in anhydrous ethanol (85%), adding into the beaker solution, and stirring;

step 3, accurately weighing the components according to the weight;

step 4, dissolving vitamin C and EDTA-2Na by using the Wula sedge essence for later use, and dissolving hyaluronic acid and hydroxymethyl cellulose in the essence; finally, uniformly mixing the two solutions for later use;

step 5, mixing the solutions obtained in the step 2 and the step 3; adjusting the dosage of triethanolamine to make the pH value of the product neutral;

slowly adding water-soluble azone, kasong and essence, and fully mixing to obtain the carex wula moisturizing whitening cream;

step 7, packaging 3 batches of samples to be tested, performing stability experiment, and respectively detecting the color, aroma, state, pH value and whether layering phenomenon exists in the samples;

step 8, measuring the moisturizing activity of the carex meyeriana moisturizing and whitening cream by a weighing method through two aspects of moisture absorption rate and moisture retention rate;

step 9, taking a small part of the Carex meyeriana moisturizing and whitening cream to perform a tyrosinase activity test, calculating the inhibition rate of the Carex meyeriana moisturizing and whitening cream on tyrosinase, and judging the whitening effect of the essence;

step 10, selecting 10 subjects of 20-30 years old and different ages, carrying out magic mirror instrument detection, detecting components such as color spots, pigments, water and the like on the faces of the subjects 7 days after the subjects use the product, and recording. The two sets of data were analyzed in comparison.

Drawings

FIG. 1 is a graph of carbomer dosage versus viscosity;

FIG. 2 is a relationship between the pH value and the viscosity of the dosage of triethanolamine;

FIG. 3 is a graph of time versus moisture retention;

figure 4 is a comparison of the skin of a subject.

Detailed Description

The invention is described in detail below with reference to the figures and the detailed description of the embodiments.

The embodiment relates to a screening method of a Meyer sedge moisturizing whitening cream formula

1. Screening of the amount of carbomer and triethanolamine

The amounts of carbomer and triethanolamine were screened and the method examined the effect of different amounts of carbomer and triethanolamine on pH and viscosity, as shown in table 1.

TABLE 1 carbomer dosage vs whitening cream statusInfluence of viscosity and pH

Numbering	Carbomer/g	Triethanolamine/g	Viscosity (mpa.s)	pH	Status of state
						1	0.2	0.2	1000	4.6	Fluid state
2	0.4	0.4	11500	4.8	Fluid state
						3	0.6	0.6	63400	5.1	Fluid state
4	0.8	0.8	94000	6.4	Gel form
						5	1.0	1.0	206070	6.7	Gel form
6	1.2	1.2	294834	7.0	Gel form
						7	1.5	1.5	352741	7.2	Gel form

According to appendix VIH of Chinese pharmacopoeia, the pH value measuring method uses an acidimeter to measure the pH value of the moisturizing cream, and an NDJ-5S viscometer is used to test the viscosity of the product, so that the dosage of carbomer and triethanolamine is judged.

The relationship between carbomer amount and viscosity is shown in figure 1. It can be seen that the viscosity gradually increases with the increase of the amount of carbomer, the property of the product changes from a flowing state to a gel state, wherein the viscosity of the product is 200-400 Pa.s when the content of carbomer is 1.0-1.2 g, and the spreadability is good. The dosage of triethanolamine is selected according to the determined dosage of carbomer, and the relationship curve of the dosage of triethanolamine, the pH value of the moisturizing whitening cream and the viscosity of the moisturizing whitening cream is obtained. As can be seen from the relationship between the dosage of triethanolamine, the pH value and the viscosity in FIG. 2, the pH value of the product is in direct proportion to the dosage of triethanolamine, and the viscosity of the moisturizing whitening cream increases with the increase of the content of triethanolamine. When the content of triethanolamine is 1-1.5 g, the viscosity of the moisturizing whitening cream is 200-400 Pa.s, and the dispersibility is good. When the triethanolamine content is 1.0-1.5 g, the moisturizing whitening cream is in a gel shape, the transparency is best, the viscosity is moderate, the pH value is close to neutral, and the optimal triethanolamine amount is used.

2. Screening of dosage of compound humectant

The compound humectant comprises glycerol, propylene glycol, butanediol, sodium hyaluronate and sodium carboxymethylcellulose. The moisturizers of the 6 samples in Table 1 were applied to the skin of the test subjects at a temperature of 25 ℃ and a relative humidity of about 40%, respectively, to obtain a test area of about 5 cm by 5 cm. Testing the moisture content of the skin by using a digital skin moisture tester at 10 min, 30 min, 60 min, 90 min, 120 min, 150 min and 180 min respectively. Table 2 shows the amount ratio of the compound humectant in different samples.

The relationship between the compound humectant time and the moisturizing rate is shown in fig. 3. The results show that the 6# sample has higher moisture retention performance at a temperature of 25 ℃ and a relative humidity of 40% for each period of time than the other samples. In summary, 10 g of glycerin, 2 g of butylene glycol, 6 g of propylene glycol, 0.05 g of sodium hyaluronate and 0.1 g of sodium carboxymethylcellulose are the best in moisturizing performance.

TABLE 2 compounding humectant dosage ratio

Sample (I)	Glycerol/g	Propylene glycol/g	Butanediol/g	Hyaluronic acid sodium salt/g	Sodium carboxymethylcellulose/g
						1	4	3	2	0.05	0.05
2	6	4	2	0.05	0.05
						3	8	4	3	0.05	0.05
4	8	4	2	0.05	0.1
						5	10	4	3	0.05	0.1
6	10	6	2	0.05	0.1

3. Determination of dosage of whitening agent vitamin C and salicylic acid

Two whitening agents, namely vitamin C and salicylic acid, are mainly selected for screening. The vitamin C belongs to vitamin series, which has no harm to human skin but is unstable to light, so that the use time of the prepared moisturizing whitening cream is limited. Salicylic acid (Salicylic acid), B-kojic acid, has excellent exfoliating ability and high safety, and is commonly used for treating various chronic skin diseases such as acne, psoriasis and the like in dermatology; the salicylic acid can remove cutin, sterilize and diminish inflammation, and is suitable for treating pore blockage. In common acne-removing products, the content of salicylic acid is within the range of 0.5-2%, and excessive use of salicylic acid can cause acid-base imbalance of skin.

(1) Single factor experiment

Taking 30 g of a prepared sample, averagely dividing into 3 parts, placing the sample in a condition of 40 ℃ for 24 hours, then placing the sample in a condition of-15 ℃ for 24 hours, and finally placing the sample in a room temperature under the irradiation of sunlight for 24 hours, wherein the phenomenon of layering and deterioration of the sample is observed.

1) Effect of vitamin C content on moisturizing and whitening cream

Preparing 5 groups of moisturizing whitening creams, and adding 0.2 g, 0.4g, 0.6 g, 0.8 g and 1.0 g of vitamin C respectively, wherein the content of salicylic acid is 0.1 g, and the content of triethanolamine is 1.5 g. 5 parts of samples are respectively taken, and after 24 hours of high temperature and 24 hours of low temperature, the color, the fragrance and the fineness of the moisturizing and whitening cream are not changed, no layering occurs, and the pH value is not changed. The physicochemical properties of the moisturizing and whitening creams containing different amounts of vitamin C when left at room temperature for 7 days are shown in table 3. The absorbance of each set of tubes was measured at 475 nm using a uv-vis spectrophotometer, and the inhibition of tyrosinase by vitamin C was calculated from the data for each set to be 46.68%. The absorbance values of the vitamin C sample solutions measured for each group are shown in Table 4.

TABLE 3 physicochemical Properties of moisturizing whitening cream with different vitamin C contents

Vitamin C/g	Color and luster	Fragrance	Status of state	pH	Whether or not to stratify
						0.2	Colorless and transparent	Meyer sedge scent	Gel form	5.4	Whether or not
0.4	Colorless and transparent	Meyer sedge scent	Gel form	5.1	Whether or not
						0.6	Light yellow	Meyer sedge scent	Gel form	4.8	Whether or not
0.8	Light yellow	Meyer sedge scent	Fluid state	4.6	Whether or not
						1.0	Light yellow	Meyer sedge scent	Fluid state	4.4	Whether or not

TABLE 4 Absorbance of vitamin C sample solution

Absorbance of the solution	1	2	3	Mean value of
					A_C1	0.662	0.588	0.668	0.639
A_C2	0.028	0.029	0.027	0.028
					A_T1	0.349	0.368	0.351	0.356
A_T2	0.030	0.028	0.028	0.029

As can be seen from Table 3, the samples containing 0.6 g, 0.8 g and 1.0 g of vitamin C showed significant discoloration, while the samples containing 0.2 g and 0.4g of vitamin C showed no change and showed good stability. The larger the content of vitamin C, the smaller the pH value, the poorer the physicochemical properties of the moisturizing and whitening cream, and the content of vitamin C can be determined to be 0.2 g-0.4g along with the prolonging of time and the increase of vitamin C.

2) Effect of salicylic acid on whitening cream

Preparing 5 groups of moisturizing whitening creams, and respectively adding 0.1 g, 0.15 g, 0.2 g, 0.25 g and 0.3 g of salicylic acid, wherein the content of vitamin C is 0.2 g, and the content of triethanolamine is 1.5 g. 5 parts of samples are respectively taken, and after 24 hours of high temperature and 24 hours of low temperature, the color, the fragrance and the fineness of the moisturizing and whitening cream are not changed, and no layering and no pH value change occur. The physicochemical properties of the moisturizing whitening creams with different salicylic acid contents when left at room temperature for 7 days are shown in table 5. And measuring the absorbance of each group of test tubes by using an ultraviolet-visible spectrophotometer, and calculating the inhibition rate of the salicylic acid on the tyrosinase to be 11.33% according to the data of each group. The measured absorbance of each group of salicylic acid sample solutions is shown in table 6.

TABLE 5 physicochemical properties of moisturizing whitening cream with different salicylic acid contents

Salicylic acid/g	Color and luster	Fragrance	Status of state	pH	Whether or not to stratify
						0.1	Colorless and transparent	Meyer sedge scent	Gel form	5.1	Whether or not
0.15	Colorless and transparent	Meyer sedge scent	Gel form	4.8	Whether or not
						0.2	Colorless and transparent	Meyer sedge scent	Gel form	4.6	Whether or not
0.25	Colorless and transparent	Meyer sedge scent	Fluid state	4.4	Whether or not
						0.3	Light yellow	Meyer sedge scent	Fluid state	4.2	Whether or not

TABLE 6 absorbance of salicylic acid sample solutions

Absorbance of the solution	1	2	3	Mean value of
					A_C1	0.774	0.710	0.726	0.737
A_C2	0.030	0.032	0.030	0.031
					A_T1	0.674	0.650	0.648	0.657
A_T2	0.031	0.031	0.031	0.031

According to the table 5, the color of the moisturizing whitening cream added with 0.3 g of salicylic acid is obviously changed, other samples are not deteriorated, the larger the amount of the salicylic acid is, the smaller the pH value is, the poorer the physical and chemical properties are along with the increase of the salicylic acid, and the dosage of the salicylic acid can be 0.1-0.2 g along with the extension of time and the increase of the salicylic acid.

And (3) placing the sample in a drying constant temperature cabinet at 40 ℃ for 12 h, then placing the sample in a refrigerator at-15 ℃ for 12 h, and circulating for 7 days to finish the cold-hot circulation test. And finally, continuously placing the sample for 24 hours under the condition of natural illumination, and observing that the sample does not have color change, odor change or other abnormal phenomena. The results of the experiment are shown in Table 7. The preparation of 9 kinds of moisturizing whitening creams with different dosages of vitamin C, salicylic acid and triethanolamine, through a heat-resistant and cold-resistant alternation experiment for 7 days, and by combining the data of color, state, pH value and the like in a table, the conclusion is drawn that the data of the color, state and pH value of the sample 5 are better than other data, so that the addition of 0.2 g of vitamin C, 0.15 g of salicylic acid and 1.5 g of triethanolamine is determined.

TABLE 7 results of orthogonal experiments

Serial number	Vitamin C	Salicylic acid	Triethanolamine	Color and luster	Fragrance	Status of state	pH	Whether or not to stratify
									1	0.1	0.10	0.5	Colorless and transparent	Meyer sedge scent	Fluid state	4.0	Whether or not
2	0.1	0.15	1.0	Light yellow	Meyer sedge scent	Gel form	5.1	Whether or not
									3	0.1	0.20	1.5	Light yellow	Meyer sedge scent	Gel form	4.6	Whether or not
4	0.2	0.10	1.0	Light yellow	Meyer sedge scent	Gel form	4.8	Whether or not
									5	0.2	0.15	1.5	Colorless and transparent	Meyer sedge scent	Gel form	6.1	Whether or not
6	0.2	0.20	0.5	Colorless and transparent	Meyer sedge scent	Fluid state	4.1	Whether or not
									7	0.3	0.10	1.5	Light yellow	Meyer sedge scent	Gel form	5.8	Whether or not
8	0.3	0.15	0.5	Colorless and transparent	Meyer sedge scent	Fluid state	4.4	Whether or not
									9	0.3	0.20	1.0	Light yellow	Meyer sedge scent	Gel form	4.6	Whether or not

Formula of moisturizing and whitening cream

TABLE 8 formula of moisturizing whitening cream

Raw material numbering	Chemical name	Dosage per gram	Function of
				1	Carbomer	1.00	Gel agent
2	Pure dew	Proper amount of	Solvent(s)
				3	Nipagin ethyl ester	0.15	Preservative
4	Glycerol	10.00	Moisture-retaining agent
				5	1, 2-propanediol	6.00	Moisture-retaining agent
6	Butanediol	2.00	Moisture-retaining agent
				7	EDTA-2Na	0.10	Bacteriostatic agent
8	Triethanolamine	1.50	Wetting agent
				9	Hyaluronic acid sodium salt	0.05	Moisture-retaining agent
10	Sodium carboxymethylcellulose	0.10	Moisture-retaining agent
				11	Vitamin C	0.20	Whitening agent
12	Salicylic acid	0.15	Whitening agent
				13	Water-soluble azones	0.10	Penetrant
14	Kathon	0.10	Preservative
				15	Essence	Proper amount of	Flavoring agent

(1) Placing carbomer in a beaker 1 for pre-swelling, adding glycerol and propylene glycol after swelling, and placing in a 90 ℃ water bath kettle for stirring and dissolving for later use; adding ethylparaben and EDTA-2Na into beaker 2 with essence, dissolving in 90 deg.C water bath, adding into beaker 1, stirring for 10 min under heat preservation;

(2) dissolving vitamin C and salicylic acid essence in a beaker 3 for later use, adding hyaluronic acid and hydroxymethyl cellulose in a beaker 4 for dissolving, and finally uniformly mixing the beaker 3 and the beaker 4 for later use;

(3) uniformly mixing the solutions (1) and (2);

(4) cooling to 60 ℃, and adding triethanolamine until the pH value of the gel is neutral;

(5) cooling to 45 ℃, respectively adding water-soluble azone, kasong and essence into the system, and fully mixing to obtain the Meyer sedge moisturizing whitening cream.

Quality evaluation of three-moisturizing whitening cream in embodiment

1. Stability test

Packaging 3 (1 and 2) batches of samples to be tested, and standing one batch of samples for 7 days at 54 ℃ and 75% of relative humidity in a dark condition; the other part is placed at about-5 ℃ for 7 days in the dark, and high and low temperature comparison is carried out, so that the color, the fragrance, the state and the pH value of the sample are all changed, and the layering phenomenon does not occur. The results are shown in tables 9 and 10:

table 9 heat and light resistance test results.

TABLE 10 Cold and light resistance test results

Implementation example functional evaluation of five-moisturizing whitening cream

After the product is tested and compared by a magic mirror instrument for 7 days, 23 test subjects are selected, 20-30-year-old women are all non-systemic diseases, have no allergic history to skin care cosmetics, and record data of skin stains, pigments, moisture and the like before and after use, and the comparison result of the skin data of the test subjects is shown in figure 4. The comparison result shows that the pigment and the color spots on the face of the subject are obviously reduced, and further shows that the moisturizing whitening cream has good effect.

Claims

1. A preparation method of a carex moisture-retaining whitening cream is characterized by comprising the following raw materials, by weight, 80-100 parts of carex extract, 10-20 parts of glycerol, 2-4 parts of butanediol, 6-12 parts of 1, 2-propylene glycol, 0.1-0.4 part of sodium hyaluronate, 0.2-0.5 part of sodium carboxymethylcellulose, 2-5 parts of carbomer, 3-6 parts of triethanolamine, 0.5-2 parts of vitamin C, 0.5-2 parts of salicylic acid, 0.1-1 part of EDTA-2Na0.1, 0.1-0.5 part of water-soluble azone, 0.1-0.3 part of cason, 0.1-0.3 part of ethylparaben and 0.1-0.3 part of essence.

2. The method for preparing a moisturizing whitening cream according to claim 1, wherein the pH value of the sample is 6.57 +/-0.06, and the spreadability is good.

3. The method for preparing a moisturizing whitening cream according to claim 1, characterized in that the sample moisturizing rate is 82%.

4. The method for preparing the moisturizing whitening cream according to claim 1, wherein the tyrosinase inhibition rate of the sample is 88.26%.

5. The method for preparing the moisturizing and whitening cream as claimed in claim 1, wherein the pigment and the color spots on the face of the subject are obviously reduced after the sample is tested by a magic mirror instrument and compared with the product used for 7 days.