CN114617815A

CN114617815A - Preparation method and application of moisturizing and whitening gel containing three ingredients

Info

Publication number: CN114617815A
Application number: CN202210354607.4A
Authority: CN
Inventors: 王晓慧; 孙双姣; 李成舰; 曾立; 张运良; 黄春花; 杨铁桥
Original assignee: Shaoyang University
Current assignee: Shaoyang University
Priority date: 2022-04-06
Filing date: 2022-04-06
Publication date: 2022-06-14

Abstract

The invention discloses a preparation method and application of a moisturizing and whitening gel, which comprises the following steps: step one, preparing an angelica dahurica extraction stock solution, an atractylodes macrocephala extraction stock solution and a poria cocos extraction stock solution; step two, preparing 2% carbomer 940 gel matrix, then respectively mixing radix angelicae extraction stock solution, rhizoma atractylodis macrocephalae extraction stock solution, poria alba extraction stock solution, glycerol, 0.5% trehalose, 5% ethylparaben methanol solution and water, then adding PBS, then adding triethanolamine to adjust the pH value to 6.8, and continuing stirring until the gel is glittering and translucent, thus obtaining the gel. According to the invention, the radix angelicae, the bighead atractylodes rhizome and the white poria are subjected to stock solution extraction, and the most appropriate proportion is determined, so that the removal rate of DPPH free radicals of the three-white moisturizing and whitening gel is effectively improved, and the ultraviolet resistance and the moisturizing rate of the three-white moisturizing and whitening gel are also improved.

Description

Preparation method and application of moisturizing and whitening gel containing three ingredients

Technical Field

The invention relates to the technical field of skin care product processing, in particular to a preparation method and application of a three-white moisturizing and whitening gel.

Background

Radix Angelicae Dahuricae is dry root of radix Angelicae Dahuricae of Umbelliferae, Poria is dry sclerotium of Poria cocos (Schw.) wolf of Polyporaceae, and Atractylodis rhizoma is dry rhizome of Atractylodis rhizoma of Compositae. The angelica dahurica serving as one of ingredients of a palace secret recipe for whitening and moisturizing becomes the favor of researchers, the angelica dahurica and the bighead atractylodes rhizome serving as main ingredients of 'Qibaisan' are commonly used for treating dark spots of the skin and whitening the skin, and modern medical research proves that unsaturated alkene compounds in the angelica dahurica volatile oil have antioxidant activity and the effect of inhibiting tyrosinase activity ER; the Poria cocos anhydrous ethanol extract has an inhibition rate of 91.7% on tyrosinase, and has a good melanin deposition preventing effect^[3]. The volatile oil in Atractylodis rhizoma has melanin inhibiting effect, and can prevent pigment from depositing on skin surface, thereby achieving effects of resolving macula, whitening skin, and caring skin^[5]。

The gel is semisolid transdermal preparation prepared from the medicine and gel auxiliary materials. Compared with cream, the gel has the advantages of crystal appearance, easy coating, simple preparation method, easily available raw materials, and is favored by researchers and patients due to the slow release effect of the transdermal preparation. The application range of the gel is continuously widened, and the prospect is very wide.

Disclosure of Invention

In order to solve the problems, the invention discloses a preparation method and application of a three-white moisturizing and whitening gel.

In order to achieve the purpose, the technical scheme of the invention is as follows:

a preparation method of a three-white moisturizing and whitening gel comprises the following steps:

preparing an angelica dahurica extraction stock solution, a bighead atractylodes rhizome extraction stock solution and a white poria cocos extraction stock solution;

and step two, preparing 2% carbomer 940 gel matrix, mixing the radix angelicae extract stock solution, the rhizoma atractylodis macrocephalae extract stock solution, the poria cocos extract stock solution, glycerol, 0.5% trehalose, 5% ethylparaben methanol solution and water respectively, adding PBS, adding triethanolamine to adjust the pH value to 6.8, and continuing stirring until the gel is glittering and translucent to obtain the gel.

Further improvement, in the second step, 50g of 2% carbomer 940 gel matrix is prepared, then 2-7mL of radix angelicae extraction stock solution, 2-7mL of rhizoma atractylodis macrocephalae extraction stock solution, 2-7mL of poria alba extraction stock solution, 10mL of glycerol, 4mL of trehalose, 2.0mL of 0.5% trehalose and 5% ethylparaben methanol solution are respectively taken to be mixed with water until the total weight is 100g, then 4mL of PBS is added, triethanolamine is added to adjust the pH value to 6.8, and stirring is continued until the gel is glittering and translucent, so that the three-white gel is obtained.

In a further improvement, the addition amount of the radix angelicae extraction stock solution is 5.0mL, the addition amount of the rhizoma atractylodis macrocephalae extraction stock solution is 5.0mL, and the addition amount of the poria cocos extraction stock solution is 5.0 mL.

In a further improvement, the preparation method of the radix angelicae extraction stock solution comprises the following steps:

weighing radix angelicae dahuricae decoction pieces, cutting into pieces, adding water, distilling for 3 times until no oil is discharged, collecting effluent, dissolving the effluent with methanol, and diluting with water to obtain 0.01 mL/mL-1 radix angelicae dahuricae stock solution, wherein the volume-mass ratio of the water to the radix angelicae dahuricae decoction pieces is 15:1mL/g during distillation.

Further improvement, the preparation method of the rhizoma atractylodis macrocephalae extract stock solution comprises the following steps:

respectively weighing 50g of rhizoma atractylodis macrocephalae powder, adding 500mL of 75% ethanol, carrying out ultrasonic treatment for 20min, carrying out reflux extraction at 60-70 ℃ for 0.5h, continuously carrying out 2 times, carrying out hot reduced pressure filtration, combining filtrates, recovering a solvent until no alcohol smell exists, continuously concentrating to one tenth of the volume of 75% ethanol, namely a stock solution with the mass concentration of 1.0 g/mL < -1 > to obtain a rhizoma atractylodis macrocephalae extract stock solution, and storing at 4 ℃ for later use; the preparation mass ratio of the 75% ethanol to the white atractylodes rhizome powder is 10:1 ml/g.

The preparation method of the three-white moisturizing and whitening gel according to claim 1, wherein the preparation method of the white poria cocos extract stock solution comprises the following steps:

respectively weighing 50g of white poria cocos powder, adding 500mL of 75% ethanol, performing ultrasonic treatment for 20min, performing reflux extraction at 60-70 ℃ for 0.5h, continuously performing 2 times, filtering under reduced pressure while the white poria cocos powder is hot, combining filtrates, recovering a solvent until no alcohol smell exists, continuously concentrating the mixed filtrates to one tenth of the volume of 75% ethanol, namely a stock solution with the mass concentration of 1.0 g/mL < -1 > to obtain a stock solution of the white atractylodes rhizome extract, and storing the stock solution at 4 ℃ for later use; the preparation mass ratio of the 75% ethanol to the white atractylodes rhizome powder is 10:1 ml/g.

Use of a three-white moisturizing and whitening gel prepared by the preparation method of the three-white moisturizing and whitening gel according to any one of claims 1 to 6; the whitening and moisturizing gel is used as cosmetics or medicines for improving the DPPH free radical clearance rate and improving the ultraviolet resistance and the moisturizing rate.

The invention has the beneficial effects that:

the radix angelicae, the bighead atractylodes rhizome and the white poria are subjected to stock solution extraction, and the most appropriate proportion of the raw materials is determined, so that the removal rate of DPPH free radicals of the three-white moisturizing and whitening gel is effectively improved, and the ultraviolet resistance and the moisturizing rate of the three-white moisturizing and whitening gel are also improved.

Drawings

FIG. 1 is a graph showing the effect of the usage of radix Angelicae Dahuricae extractive solution, Atractylodis rhizoma extractive solution, and Poria extractive solution on the comprehensive index;

FIG. 2 is a graph showing the effect of the dosage of the Atractylodis rhizoma extract stock solution and the Poria cocos extract stock solution on the comprehensive index;

FIG. 3 is a graph showing the effect of the usage of Poria cocos Wolff extract stock solution on the comprehensive index.

Detailed Description

Specific embodiments of the present invention are described in further detail below.

(one) extraction of active substances

Preparation of angelica dahurica extract stock solution

Extracting by steam distillation. Weighing 50g of angelica dahurica decoction pieces, cutting the angelica dahurica decoction pieces into a round-bottom flask, adding 750mL of water, and distilling for 3 times until the angelica dahurica decoction pieces are discharged without oil each time. Taking 0.5mL of effluent, dissolving in methanol, adding 50mL of water, and diluting to 0.01 mL/mL^-1The radix angelicae dahuricae stock solution.

② preparation of white atractylodes rhizome, poria extract stock solution

Weighing 50g of rhizoma atractylodis macrocephalae and poria alba powder respectively, adding 500mL of 75% ethanol, performing ultrasonic reflux extraction for 20min at 60-70 ℃ for 0.5h, continuously performing reflux extraction for 2 times, filtering under reduced pressure while the solution is hot, combining the filtrates, recovering the solvent until no alcohol smell exists, and continuously concentrating to 50mL, namely obtaining the extract with the mass concentration of 1.0 g/mL^-1The stock solution is used as a test solution and stored at 4 ℃ for later use.

Preparation of (II) 'Sanbai' gel

Weighing carbomer 940 and water, naturally swelling for more than 8h, and uniformly stirring to obtain 50g of 2% carbomer 940 gel matrix. Taking proper amount of radix angelicae extract stock solution, proper amount of rhizoma atractylodis macrocephalae and white poria extract stock solution, 10mL of glycerol, 4mL of 0.5% trehalose, 2.0mL of 5% ethylparaben methanol solution and proper amount of water, uniformly stirring, mixing with 50g of 2% carbomer 940 matrix to obtain 100g of mixture, adding 4mL of PBS (pH6.8), dropwise adding triethanolamine to adjust pH6.8, continuously stirring until the mixture is glittering and translucent, obtaining 'three white' gel, and storing at normal temperature for later use.

(III) optimization of gel prescription

(ii) Single factor analysis

Six levels of A, B, C three influencing factors are preliminarily selected, and the response value of the factors is determined by single factor analysis by taking a comprehensive index value (50% of DPPH free radical removal rate + 50% of tyrosinase activity inhibition rate) as a research index. The factor-level is shown in table 1, and the influence result of each factor on the comprehensive evaluation value is shown in table 1.

TABLE 1 factor-horizon table (Single factor analysis)

Fig. 1-3 show that 5.0mL of the extract of radix angelicae, bighead atractylodes rhizome and poria alba achieves satisfactory comprehensive effect, and the increase of dosage does not increase the effect, which shows that the removal limit of the active ingredients of radix angelicae, bighead atractylodes rhizome and poria alba is reached, thus indicating that the antioxidant activity of the active ingredients of radix angelicae, bighead atractylodes rhizome and poria alba is saturated.

② orthogonal design experiment

TABLE 2 factor and horizon table (orthogonal design experiment)

TABLE 3 orthogonal design L₉(3⁴) Results of the experiment

TABLE 4 analysis of variance results of orthogonal experiments

Note: f_0.01(2，4)＝18.00，F_0.05(2，4)＝6.94。

The optimal prescription scheme is C2A3B2 through visual analysis, and the sequence of primary and secondary influence factors is C > A > B; the orthogonal design results are consistent with visual analysis, and the effect test difference between bodies is obvious (P < 0.05). When the volume of the radix angelicae extraction stock solution is 5.0mL, and the volume of the rhizoma atractylodis macrocephalae extraction stock solution is 5.0mL, the optimal preparation process parameters are obtained.

Third verification experiment

According to the scheme of C2A3B2, the radix Angelicae Dahuricae extract stock solution, Atractylodis rhizoma and Poria extract stock solution are respectively 5.0mL, and are prepared in parallel in 3 parts, and the comprehensive index results are shown in Table 5.

TABLE 5 results of confirmatory experiments (n ═ 3)

(V) "Sanbai" moisture-keeping and whitening gel functionality assay

Preparation of sample test solution

Weighing "three white" gel and commercially available gel 5g each, and centrifuging at high speed (10000 r.min)^-1) Then 5mL of supernatant was aspirated, and the volume was diluted with distilled water to 100 mL.

Firstly, the clearance rate of DPPH free radical is measured

2mL of sample test solution with a concentration of 20. mu.g/mL was precisely transferred^-12mL of diphenyl picrylphenylhydrazine (DPPH) solution is added into the same test tube with a plug in sequence, shaken up, kept stand for 30min in a dark room at room temperature, and then the absorbance A of the sample is measured at the wavelength of 517 nm. The DPPH radical clearance (K) of the sample was calculated according to the following formula (1)

K(％)＝[1-(A_i-A_j)/A_c]×100％。 (1)

Wherein A is_iIs the absorbance of the mixture of DPPH solution and sample test solution, Aj is the absorbance of the sample test solution, A_cAbsorbance of DPPH solution was taken and F was used. The results are shown in Table 1.

② determination of tyrosinase inhibitory Activity

PBS (pH6.8), sample test solution and tyrosine solution (1.0 mg/mL) were added in sequence according to the procedure^-1) After being bathed in water at 35 ℃ for 10min, 1.0mL of tyrosinase solution is added, shaken up, quickly transferred to a colorimetric tube, and the absorbance A is measured at 475 nm.

TABLE 6 determination of tyrosinase inhibitory activity

The inhibition ratio (I) of tyrosinase was calculated according to the following formula (2)

Wherein: A1-A4 are absorbance values of the test sample groups 1-4 at 475 nm. The results are shown in Table 7.

TABLE 7 "SAIBAI" gel and commercially available aloe gel for DPPH radical scavenging and tyrosinase activity inhibition.

③ measurement of anti-ultraviolet property

Evaluation method of sunscreen effect of UVB area of sunscreen according to QB/T2410-1998^[11]. Respectively weighing 'three white' moisturizing and whitening gel and commercially available aloe whitening and freckle removing moisturizing gel, uniformly coating 2g of each gel on a 3M medical breathable adhesive tape, pasting the gel on the inner wall of a cuvette, taking the medical breathable adhesive tape of a sample as a reference, measuring the wavelength within the wavelength range of 280-360 nm, scanning every 10nm to record absorbance A, and judging the sun protection effect of the sample in a UVB region (280-320 nm) according to the average value of the absorbance^[12]. The results are shown in Table 8.

TABLE 8 measurement results of ultraviolet ray resistance (. + -. s, n. 6)

Note:

table 3 shows that there is a significant difference in uv resistance between "three white" gels and commercially available gels. Can be used for protecting medium ultraviolet radiation.

Determination of moisture retention

At room temperature, 2.0g of gel was directly and uniformly applied to a medical breathable adhesive tape (simulating human skin), and the mass W was accurately recorded₀Then placing the sample in a humidity dryer with relative humidity of 45% and 80%, taking out the breathable adhesive tape after 4, 8, 12 and 24 hours respectively, immediately and accurately weighing each sample mass, and recording as W_iThe moisture retention rate was calculated according to the following formula (3)

The results are shown in Table 9.

TABLE 9 results of the gel in vitro moisturisation experiment (+/-s, n ═ 6)

Table 4 shows that the moisturizing rates of the 'three-white' gel and the commercial gel are not obviously different in 8-24 h under the environment with the humidity of 45% and 80%.

Performance characterization investigation

The product has white gel appearance, fine and uniform texture, glittering and translucent property, proper viscosity and good spreadability. The pH value is checked, and the test solution is taken, and the measured value of the pH value is 6.8.

The cold and hot experiment is carried out by packaging the product in a transparent cosmetic bottle, respectively placing the bottle at 4, 25 and 50 ℃, sampling and observing the bottle at 7, 30 and 180 days, and the gel has no phenomena of layering, caking, mildew and discoloration.

The product is packaged in centrifugal test tube for 2000 r.min^-1And the gel appearance is free from layering and caking phenomena after sampling observation at 5min, 10min and 15 min.

In the strong light irradiation experiment, the product is placed in a light cabinet with a fluorescent lamp with the illumination of 4500Lx for 15 days, and sampling detection is carried out on 7 th and 15 th days, so that the transparency, the pH value and the viscosity of the gel are unchanged.

And (4) placing the sample into a packaging box, covering and sealing the packaging box, placing the packaging box at room temperature for 1 month, and detecting according to a quality standard, wherein the result has no obvious change.

Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope defined by the claims.

Claims

1. A preparation method of a three-white moisturizing and whitening gel is characterized by comprising the following steps:

step one, preparing an angelica dahurica extraction stock solution, an atractylodes macrocephala extraction stock solution and a poria cocos extraction stock solution;

2. The method for preparing the tri-white moisturizing and whitening gel as claimed in claim 1, wherein in the second step, 50g of 2% carbomer 940 gel matrix is prepared, then 2-7mL of radix angelicae extract stock solution, 2-7mL of rhizoma atractylodis macrocephalae extract stock solution, 2-7mL of poria cocos extract stock solution, 10mL of glycerol, 4mL of trehalose, 2.0mL of 0.5% trehalose, and 5% ethylparaben methanol solution are respectively mixed with water to total weight of 100g, then 4mL of PBS is added, then triethanolamine is added to adjust the pH to 6.8, and the mixture is continuously stirred until the gel is glittering and translucent, thus obtaining the tri-white gel.

3. The preparation method of the Sanbai moisturizing and whitening gel as claimed in claim 2, wherein the addition amount of the radix angelicae extract stock solution is 5.0mL, the addition amount of the rhizoma atractylodis macrocephalae extract stock solution is 5.0mL, and the addition amount of the white poria extract stock solution is 5.0 mL.

4. The preparation method of the three-white moisturizing and whitening gel according to claim 1, wherein the preparation method of the radix angelicae extraction stock solution comprises the following steps:

5. The preparation method of the three-white moisturizing and whitening gel according to claim 1, wherein the preparation method of the white atractylodes rhizome extract stock solution comprises the following steps:

respectively weighing 50g of rhizoma atractylodis macrocephalae powder, adding 500mL of 75% ethanol, performing ultrasonic extraction for 20min, performing reflux extraction for 0.5h at 60-70 ℃, continuously performing 2 times, filtering under reduced pressure while the solution is hot, combining the filtrates, recovering the solvent until no alcohol smell exists, continuously concentrating to one tenth of the volume of 75% ethanol, namely a stock solution with the mass concentration of 1.0 g/mL < -1 > to obtain a rhizoma atractylodis macrocephalae extraction stock solution, and storing at 4 ℃ for later use; the preparation mass ratio of the 75% ethanol to the white atractylodes rhizome powder is 10:1 ml/g.

6. The preparation method of the three-white moisturizing and whitening gel according to claim 1, wherein the preparation method of the white poria cocos extract stock solution comprises the following steps:

7. Use of the three-white moisturizing and whitening gel, which is characterized in that the three-white moisturizing and whitening gel is prepared by the preparation method of the three-white moisturizing and whitening gel according to any one of claims 1 to 6; the Sanbai moisturizing and whitening gel is used as a cosmetic or a medicine for improving the removal rate of DPPH free radicals and improving the ultraviolet resistance and the moisturizing rate.