CN109692142B

CN109692142B - Poria cocos facial cleanser and preparation method thereof

Info

Publication number: CN109692142B
Application number: CN201910170239.6A
Authority: CN
Inventors: 戴鑫汶; 戴甲木; 孙梦锦; 刘刚; 龙孝金; 王帆; 邹奇
Original assignee: Hunan Busky Pharmaceutical Co ltd
Current assignee: Hunan Busky Pharmaceutical Co ltd
Priority date: 2019-03-07
Filing date: 2019-03-07
Publication date: 2022-01-04
Anticipated expiration: 2039-03-07
Also published as: CN109692142A

Abstract

The invention provides a poria cocos facial cleanser which is prepared from a component A, a component B, a component C, a component D and a component E, wherein the component A comprises water, glycerol, allantoin and methyl hydroxybenzoate, and the component B comprises 16-18 alcohol, dimethicone, isooctyl palmitate, sodium lauryl sulfate and betaine; the component C is 50% of triethanolamine, the component D comprises DMDM hydantoin, carboxymethyl pachyman, shea butter, a sophora flower bud extract and a fenugreek extract, and the component E comprises plant essential oil and essence. The poria cocos facial cleanser disclosed by the invention has the effects of resisting inflammation, resisting cell division, relieving itching and keeping skin elasticity, can be used for healthy skin, preventing and treating skin diseases, relieving the damage of radiation to the skin, delaying aging, cleaning and tendering the skin, and has a good application prospect.

Description

Poria cocos facial cleanser and preparation method thereof

Technical Field

The invention relates to the technical field of cosmetics, and particularly relates to poria cocos facial cleanser.

Background

The facial cleanser is a skin care product for cleaning dirt on the face and protecting the skin, and is one of indispensable daily necessities in our daily life. It is a milky product formed from oil phase material, water phase material, surfactant and nutrient. Mainly plays a role in cleaning residual substances of skin grease, dirt, aged cuticle, skin care cosmetics and the like.

Poria, also known as Yuling, Fu Ling, Wanling Gui and Fu Tu, is one of the traditional Chinese medicines, namely four monarch eight delicacies, is the dried sclerotium of the Poria cocos, which is a fungus of the family Hymenomycetes, is usually parasitic on the root of pine, is in the shape of a sweet potato, a sphere, light brown or dark brown in outer skin and pink or white in inner part, and has the effects of promoting diuresis, excreting dampness, strengthening spleen and calming heart. Medical research further proves that the tuckahoe has various effects of resisting tumor, inducing diuresis to alleviate edema, enhancing immunity, calming nerves, inhibiting bacteria and the like. Poria contains multiple chemical components, the most important of which is pachyman, and its content can be up to 84% of dry weight of Poria. Pachyman is easily dissolved in medium and strong alkaline solution, and hardly dissolved in water, and has a main structure of beta- (1 → 3) -bonded glucose linear structure and a structure of beta- (1 → 6) -bonded glucose branched chain. Scientific research shows that chemical modification is carried out on pachyman by a carboxymethylation semisynthesis derivatization method to increase the solubility and improve the bioactivity, the higher the substitution degree is, the higher the solubility in water is, the higher the bioavailability is and the stronger the bioactivity is.

The carboxymethyl pachyman is a polysaccharide with carboxymethyl on pachyman, has high water solubility, has obvious physiological activities of resisting tumor, improving immunity, protecting liver, reducing transaminase, resisting viruses, relieving radiation side reaction, reducing blood sugar, improving leukocyte function, invigorating stomach, soothing nerves, resisting aging and the like, is developed into a medicament or health-care food for resisting tumor and enhancing immunity, has obvious effect and has excellent market prospect.

The Chinese patent with application number of CN200610163425.X discloses a carboxymethyl pachyman with high degree of substitution, its preparation method and application, wherein water or water-alcohol solution is used as medium, pachyman, chloroacetic acid and proper excess sodium hydroxide are subjected to substitution reaction to prepare carboxymethyl pachyman (CMP) with high degree of substitution, and the degree of substitution is more than 1. The method comprises the steps of extracting pachymaran from poria cocos, replacing with chloroacetic acid, keeping a higher reaction temperature, obtaining carboxymethyl pachymaran, decoloring and purifying, wherein the liquid phase is a liquid-phase non-oscillation process, alkali liquor and chloroacetic acid solution need to be prepared in advance in the reaction, and the total production time is long. In the active carboxymethyl pachyman disclosed in the Chinese patent with the application number of CN101724091B and the production process and application thereof, firstly, tuckahoe powder is degreased by ethanol, and in an ethanol phase system, 15-20% of chloroacetic acid is added by a secondary alkalization method (the addition of alkali is 2-10% of the amount of tuckahoe), so as to obtain the carboxymethyl pachyman with medium substitution degree. The invention with application number of CN104387482B adopts an ethanol phase system, a secondary alkalization process and utilizes a catalyst to promote the substitution reaction process. The two processes both need a secondary alkalization and ethanol reaction system, so the operation steps are more and a large amount of ethanol is consumed.

In order to provide more choices of products in rich markets and meet the requirements of people on high-quality cosmetics, the traditional Chinese medicine facial cleanser which has the effects of moisturizing, resisting aging and preventing radiation, can effectively clean skin, is mild and has no stimulation is needed to be developed.

Disclosure of Invention

In order to solve the technical problems, the invention provides the poria cocos facial cleanser and the preparation method thereof, and aims to provide the poria cocos facial cleanser which has good water solubility due to the addition of carboxymethyl pachymaran, and the prepared moisturizing emulsion has good oxidation resistance, radiation side reaction reduction, anti-aging, bacteriostasis and moisturizing effects.

The invention provides poria cocos facial cleanser which is prepared from a component A, a component B, a component C, a component D and a component E, wherein the component A comprises the following raw materials in parts by weight: the composition comprises water, glycerol, allantoin and methyl hydroxybenzoate, wherein the component B comprises the following raw materials in parts by weight: 16-18 alcohol, simethicone, isooctyl palmitate, sodium lauryl sulfate and betaine; the component C is 50% triethanolamine, and the component D is prepared from the following raw materials in parts by weight: the composition comprises DMDM hydantoin, carboxymethyl pachyman, shea butter, a sophora flower bud extract and a fenugreek extract, wherein the component E comprises the following raw materials in parts by weight: plant essential oils and essences.

As a further improvement of the invention, the component A consists of the following raw materials: 75-80 parts of water, 4-8 parts of glycerol, 0.05-0.15 part of allantoin and 0.1-0.2 part of methylparaben; the component B consists of the following raw materials: 0.5-1 part of 16-18 alcohol, 1-1.5 parts of dimethyl silicone oil, 4-8 parts of isooctyl palmitate, 0.5-1 part of sodium lauryl sulfate and 0.3-0.7 part of betaine; the component C is 0.1 to 0.5 portion of 50 percent triethanolamine; the component D consists of the following raw materials: 0.1-0.5 part of DMDM hydantoin, 0.01-0.05 part of carboxymethyl pachyman, 0.1-0.5 part of shea butter, 0.01-0.03 part of sophora flower bud extract and 0.01-0.03 part of fenugreek extract; the component E consists of the following raw materials: 0.1-0.3 part of plant essential oil and 0.005-0.015 part of essence.

As a further improvement of the invention, the component A consists of the following raw materials: 76-78 parts of water, 2-4 parts of glycerol, 0.07-0.12 part of allantoin and 0.12-0.18 part of methylparaben; the component B consists of the following raw materials: 0.6-0.8 part of 16-18 alcohol, 1.2-1.4 parts of simethicone, 2-4 parts of isooctyl palmitate, 0.6-0.8 part of sodium lauryl sulfate and 0.4-0.6 part of betaine; the component C is 0.2 to 0.4 portion of 50 percent triethanolamine; the component D consists of the following raw materials: 0.2-0.4 part of DMDM hydantoin, 0.02-0.04 part of carboxymethyl pachyman, 0.2-0.4 part of shea butter, 0.015-0.025 part of sophora flower bud extract and 0.015-0.025 part of fenugreek extract; the component E consists of the following raw materials: 0.15 to 0.25 portion of vegetable essential oil and 0.007 to 0.012 portion of essence.

As a further improvement of the invention, the component A consists of the following raw materials: 77 parts of water, 3 parts of glycerol, 0.1 part of allantoin and 0.15 part of methylparaben; the component B consists of the following raw materials: 0.7 part of 16-18 alcohol, 1.3 parts of simethicone, 3 parts of isooctyl palmitate, 0.7 part of sodium lauryl sulfate and 0.5 part of betaine; the component C is 0.3 part of 50 percent triethanolamine; the component D consists of the following raw materials: 0.3 part of DMDM hydantoin, 0.03 part of carboxymethyl pachyman, 0.3 part of shea butter, 0.02 part of sophora flower bud extract and 0.02 part of fenugreek extract; the component E consists of the following raw materials: 0.2 part of plant essential oil and 0.01 part of essence.

As a further improvement of the invention, the carboxymethyl pachyman is prepared by the following method:

s1, culturing poria cocos: inoculating Poria mycelium in malt wort liquid culture medium under sterile condition, and culturing at 28 deg.C for 4-5 days;

s2, preparation of pachyman: fermenting cultured Poria culture medium at 35 deg.C for 2 days, heating to slightly boil, extracting for 1-2 hr, filtering, adding mixed solvent of chloroform and n-butanol, oscillating, centrifuging, adding 3 times of 95% ethanol, standing overnight, filtering to obtain precipitate, and washing with diethyl ether for 2-3 times to obtain pachyman;

s3, preparing pachyman: adding pachymaran into sodium periodate solution for selective oxidation, adjusting pH to 3-4 with trifluoroacetic acid, performing acidolysis, filtering, and washing solid with water to obtain pachymaran;

s4, preparing carboxymethyl pachyman: dissolving pachymaran in an alkali solution, slowly adding 35% hydrogen peroxide under stirring for decolorization until the solution turns white, adding a mixed solution of isopropyl alcohol and tert-butyl alcohol of chloroacetic acid, controlling the concentration of the mixed solvent of isopropyl alcohol and tert-butyl alcohol in a reaction system to be 65% -70%, carrying out etherification reaction at 60-80 ℃ for 2-3h to obtain a reaction system in a pasty state, pouring out an upper layer of liquid, adding a dilute hydrochloric acid solution into a lower layer of the reaction system to adjust the pH to 6.0, violently stirring, adding 95% ethanol, filtering, dissolving the solid in water, precipitating with ethanol, filtering, and drying to obtain a white powdery solid, namely carboxymethyl pachymaran.

As a further improvement of the invention, the acidolysis time is 30min-1h, the mixing volume ratio of isopropanol and tert-butanol is 3:1, the mixing volume ratio of chloroform and n-butanol is (4-6):1, the alkali solution is a KOH solution, and the mass concentration of the sodium periodate solution is 0.5mol/L-1.5 mol/L.

As a further improvement of the present invention, the plant essential oil is selected from one of tea tree essential oil, lavender essential oil, rosemary essential oil, bergamot essential oil, lemon essential oil, rose essential oil, clove essential oil, mint essential oil, cinnamon essential oil and thyme essential oil.

The invention further provides a preparation method of the poria cocos facial cleanser, which comprises the following steps:

s1, weighing the raw materials of the component A in proportion, adding the raw materials into a container A, heating, stirring until the raw materials are completely dissolved, and controlling the temperature to 80 ℃;

s2, weighing the raw materials of the component B according to a proportion, adding the raw materials into a container B, heating, stirring until the raw materials are completely dissolved, and controlling the temperature to 80 ℃;

s3, adding the solution obtained in the step S1 into the solution obtained in the step S2 while the solution is hot, quickly homogenizing and stirring for 2-3 min to form an emulsion;

s4, heating the emulsion in the step S3 to 70 ℃, adding the component C, homogenizing for 2min-3min, stirring, cooling to 45 ℃, adding the components D and E, stirring uniformly, naturally cooling to room temperature, and tubing to obtain the emulsion.

As a further improvement of the invention, the stirring speed in steps S1 and S2 is 300r/min-500 r/min.

As a further improvement of the invention, the homogenizing rotating speed in the steps S3 and S4 is 4000r/min-6000 r/min.

The invention has the following beneficial effects:

1. in the preparation of the carboxymethyl pachymaran, the traditional isopropanol or ethanol is replaced by the mixed solution of isopropanol and tertiary butanol, the isopropanol is secondary alcohol, the tertiary butanol is tertiary alcohol, the steric hindrance of the isopropanol and the tertiary butanol is large, the SN2 substitution reaction is favorable for reducing the side reaction, the dosage of chloroacetic acid is reduced, the production cost is reduced, the reaction is mild, the substitution degree of the prepared carboxymethyl pachymaran is higher, the distribution of substituents is uniform, and the defect that the carboxymethyl pachymaran prepared by using the isopropanol or ethanol as a medium is easy to agglomerate is overcome; the substitution degree of the carboxymethyl pachymaran can be improved by controlling the concentration of the isopropanol and the tertiary butanol; the trifluoroacetic acid adopted by the invention has the advantages of weak acidity and oxidability, good hydrolysis effect and small influence on pachyman structure, and is used as an acid for acidolysis to break the glucosidic bond of pachyman; according to the invention, the substitution degree is further improved by controlling the appropriate etherification reaction temperature, and researches show that the temperature is too low and the substitution degree is too low; the etherification temperature is too high, the substitution degree is reduced, and experiments show that the substitution degree is the highest when the temperature is 60-80 ℃;

2. the carboxymethyl pachyman prepared by the method has good water solubility, the solubility at 20 ℃ is 0.105-0.109mg/mL, the substitution degree is 1.55-1.59, and the carboxymethyl pachyman has good effects of resisting oxidation, relieving radiation side reaction, resisting aging, inhibiting bacteria and preserving moisture; the sophora flower bud extract and the fenugreek extract have good antioxidant, whitening and moisturizing effects; the plant essential oil has antibacterial, fragrance enhancing, skin caring, wound healing, tranquilizing, and refreshing effects; the shea butter is pure natural green plant source solid oil, can promote the regeneration of epidermal cells, endows the skin with the function of nutrition, is easy to be absorbed by the human body, can prevent drying and cracking, further recovers and maintains the natural elasticity of the skin, and simultaneously can play a role in diminishing inflammation;

3. the poria cocos facial cleanser disclosed by the invention has the effects of resisting inflammation, resisting cell division, relieving itching and keeping skin elasticity, can be used for healthy skin, preventing and treating skin diseases, relieving the damage of radiation to the skin, delaying aging, cleaning and tendering the skin, and has a good application prospect.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is obvious that the embodiments described are only some representative embodiments of the present invention, rather than all embodiments, and all other embodiments obtained by a person skilled in the art without creative efforts belong to the protection scope of the present invention.

Example 1

The carboxymethyl pachyman is prepared by the following method:

s1, culturing poria cocos: inoculating Poria mycelium in malt wort liquid culture medium under sterile condition, and culturing at 28 deg.C for 4 days;

s2, preparation of pachyman: fermenting cultured Poria culture medium at 35 deg.C for 2 days, heating to slightly boil, extracting for 1h, filtering, adding 3 times of mixed solvent of chloroform and n-butanol at a volume ratio of 4:1, oscillating, centrifuging, adding 3 times of 95% ethanol, standing overnight, filtering to obtain precipitate, and washing with diethyl ether for 2 times to obtain pachyman;

s3, preparing pachyman: adding 10g pachymaran into 100mL0.5mol/L sodium periodate solution for selective oxidation, adjusting pH to 3 with trifluoroacetic acid, carrying out moderate acidolysis for 30min, filtering, and washing the solid with water to obtain pachymaran;

s4, preparing carboxymethyl pachyman: dissolving 1g of pachymaran in 20mL of 0.1mol/L KOH solution, slowly adding 35% of hydrogen peroxide for decolorization under stirring until the solution becomes white, adding 50mL of a mixed solution of isopropyl alcohol and tert-butyl alcohol of chloroacetic acid with the volume ratio of 3:1, controlling the concentration of the mixed solvent of isopropyl alcohol and tert-butyl alcohol in a reaction system to be 65%, carrying out etherification reaction at 60 ℃ for 2 hours to obtain a pasty reaction system, pouring out an upper layer of liquid, adding a dilute hydrochloric acid solution into a lower layer to adjust the pH to be 6.0, violently stirring, adding 95% of ethanol, filtering, dissolving the solid in water, precipitating with ethanol, filtering, and drying to obtain a white powdery solid, namely the carboxymethyl pachymaran.

The carboxymethyl pachyman has a degree of substitution of 1.55, and a solubility of 0.105mg/mL at 20 deg.C.

Example 2

The carboxymethyl pachyman is prepared by the following method:

s1, culturing poria cocos: inoculating Poria mycelium in malt wort liquid culture medium under sterile condition, and culturing at 28 deg.C for 5 days;

s2, preparation of pachyman: fermenting cultured Poria culture medium at 35 deg.C for 2 days, heating to slightly boil, extracting for 2 hr, filtering, adding 5 times volume of mixed solvent of chloroform and n-butanol at a volume ratio of 6:1, oscillating, centrifuging, adding 3 times volume of 95% ethanol, standing overnight, filtering to obtain precipitate, and washing with diethyl ether for 3 times to obtain pachyman;

s3, preparing pachyman: adding 10g of pachymaran into 30mL of 1.5mol/L sodium periodate solution for selective oxidation, adjusting the pH value to 4 with trifluoroacetic acid, carrying out moderate acidolysis for 1h, filtering, and washing the solid with water to obtain pachymaran;

s4, preparing carboxymethyl pachyman: dissolving 1g of pachymaran in 20mL of 0.1mol/L KOH solution, slowly adding 35% hydrogen peroxide for decolorization under stirring until the solution becomes white, adding 50mL of a mixed solution of isopropanol and tert-butyl alcohol of 2mol/L chloroacetic acid, wherein the volume ratio is 3:1, controlling the concentration of the mixed solvent of the isopropanol and the tert-butyl alcohol in a reaction system to be 70%, etherifying at 80 ℃ for 3 hours, pouring out the upper layer of liquid, adding a dilute hydrochloric acid solution into the lower layer to adjust the pH to be 6.0, violently stirring, adding 95% ethanol, filtering, dissolving the solid in water, precipitating with ethanol, filtering, and drying to obtain a white powdery solid, namely the carboxymethyl pachymaran.

The carboxymethyl pachyman has a degree of substitution of 1.57 and a solubility of 0.106mg/mL at 20 deg.C.

Example 3

The carboxymethyl pachyman is prepared by the following method:

s2, preparation of pachyman: fermenting cultured Poria culture medium at 35 deg.C for 2 days, heating to slightly boil, extracting for 2 hr, filtering, adding mixed solvent of chloroform and n-butanol at a volume ratio of 5:1, oscillating, centrifuging, adding 3 times of 95% ethanol, standing overnight, filtering to obtain precipitate, and washing with diethyl ether for 3 times to obtain pachyman;

s3, preparing pachyman: adding 10g pachymaran into 50mL of 1.0mol/L sodium periodate solution for selective oxidation, adjusting pH to 3.6 with trifluoroacetic acid, carrying out moderate acidolysis for 45min, filtering, and washing the solid with water to obtain pachymaran;

s4, preparing carboxymethyl pachyman: dissolving 1g of pachymaran in 20mL of 0.1mol/LKOH solution, slowly adding 35% hydrogen peroxide while stirring for decolorization until the solution turns white, adding 50mL of a mixed solution of isopropanol and tert-butanol of 2mol/L chloroacetic acid with the volume ratio of 3:1, controlling the concentration of the mixed solvent of the isopropanol and the tert-butanol in a reaction system to be 68%, carrying out etherification reaction at 70 ℃ for 2.5 hours to obtain a pasty reaction system, pouring out an upper layer of liquid, adding a dilute hydrochloric acid solution into a lower layer to adjust the pH to be 6.0, carrying out vigorous stirring, adding 95% ethanol, filtering, dissolving the solid in water, precipitating with ethanol, filtering, and drying to obtain a white powdery solid, namely the carboxymethyl pachymaran.

The carboxymethyl pachyman has a degree of substitution of 1.59 and a solubility of 0.109mg/mL at 20 deg.C.

Comparative example 1

The carboxymethyl pachyman is prepared according to the method of Chinese invention patent CN 104188900B.

The test shows that the degree of substitution of the carboxymethyl pachyman is 1.02, and the solubility at 20 ℃ is 0.085 mg/mL.

Test example 1 oxidation resistance test

Tris-HCl buffer solution with pH of 8.2 was put into a colorimetric tube, each of the carboxymethyl pachyman sample solutions prepared in examples 1 to 3 and comparative example 1 was added to the colorimetric tube, and then, a water bath was carried out at 37 ℃ followed by addition of a preheated pyrogallol solution, and after mixing, quenching reaction was carried out with hydrochloric acid after treatment for 5min, and the absorbance at 320nm was measured. The control group was vitamin C, and carboxymethyl pachyman prepared in comparative example 1, respectively. The test results are expressed as the clearance E (%). The results are shown in Table 1.

TABLE 1

Sample \ concentration mg/mL

0.1

0.5

1.0

2.0

5.0

10.0

Example 1

14.1±1.6

17.4±1.1

28.3±2.2

38.4±1.6

48.3±3.7

60.3±1.5

Example 2

14.5±1.3

16.7±1.7

27.3±0.8

36.9±1.8

47.7±2.4

59.1±1.2

Example 3

15.6±0.7

18.1±1.4

29.3±1.2

39.6±1.6

51.1±0.9

63.6±1.8

Vitamin C

42.3±0.8

91.7±1.3

92.1±1.5

91.8±1.7

91.8±1.3

92.1±1.6

Comparative example 1

9.3±1.3

12.4±0.8

16.6±1.1

25.4±1.8

33.6±3.7

38.3±2.5

As can be seen from the above table, the carboxymethyl pachyman prepared in examples 1-3 of the present invention has good antioxidant activity, and the activity is significantly better than that of comparative example 1.

Test example 2 degree of substitution (D. S) of carboxymethyl pachyman

The carboxymethyl pachyman prepared in examples 1-3 and comparative example 1 was subjected to the degree of substitution test by the following method:

accurately weighing 0.4g (accurate to 4 decimal places) of carboxymethyl pachyman sample, placing in a 150ml beaker, heating in 80 ℃ water bath, stirring for dissolving, cooling, adjusting pH to 4.0 with 2mol L hydrochloric acid solution, adding 100ml of absolute ethanol, stirring uniformly, standing overnight, centrifugally separating alcohol precipitate, repeatedly washing the alcohol precipitate with 95% ethanol until the washing solution does not contain chloride ions. Washing alcohol precipitate, dissolving with 40.00ml of 0.1000mol/L NaOH standard solution, back titrating with 0.1000mol/L standard hydrochloric acid solution immediately after the solution is transparent until the red color of phenolphthalein indicator is just faded, and recording the volume of 0.1000mol/L hydrochloric acid standard solution consumed by back titration as V_HCl。

The degree of substitution (D.S) of carboxymethyl pachyman was calculated according to the following formula:

in the formula:

a is the m mol number of NaOH consumed to neutralize 1g of acid form carboxymethyl pachyman sample;

C_NaOHthe concentration of the NaOH standard solution (0.1000 mol/L);

V_NaOHis the volume number of the added 0.1000mol/L NaOH standard solution (40.00 ml);

C_HClthe concentration of a hydrochloric acid standard solution for back titration (0.1000 mol/L);

V_HClthe volume of 0.1000mol/L hydrochloric acid standard solution consumed for the back titration.

The results are shown in Table 2.

TABLE 2

Group of	Degree of substitution
		Example 1	1.55
Example 2	1.57
		Example 3	1.59
Comparative example 1	1.02

From the results, it can be seen that the carboxymethyl pachyman prepared in examples 1-3 of the present invention has a higher degree of substitution (1.55-1.59), which is significantly better than that of comparative example 1.

Example 4

The raw materials comprise the following components in parts by weight:

the component A consists of the following raw materials: 75 parts of water, 1 part of glycerol, 0.05 part of allantoin and 0.1 part of methylparaben;

the component B consists of the following raw materials: 0.5 part of cetostearyl alcohol, 1 part of dimethyl silicone oil, 1 part of isooctyl palmitate, 0.5 part of sodium lauryl sulfate and 0.3 part of betaine;

the component C is 0.1 part of 50 percent triethanolamine;

the component D consists of the following raw materials: 0.1 part of DMDM hydantoin, 0.01 part of carboxymethyl pachyman, 0.1 part of shea butter, 0.01 part of sophora flower bud extract and 0.01 part of fenugreek extract;

the component E consists of the following raw materials: 0.1 part of rose essential oil and 0.005 part of essence.

A preparation method of poria cocos facial cleanser comprises the following steps:

s1, weighing the raw materials of the component A according to a proportion, adding the raw materials into a container A, heating, stirring until the raw materials are completely dissolved, controlling the rotating speed to be 300r/min, and controlling the temperature to be 80 ℃;

s2, weighing the raw materials of the component B according to a proportion, adding the raw materials into the container B, heating, stirring until the raw materials are completely dissolved, controlling the rotating speed to be 300r/min, and controlling the temperature to be 80 ℃;

s3, adding the solution obtained in the step S1 into the solution obtained in the step S2 while the solution is hot, and quickly homogenizing and stirring the mixture for 2min to form an emulsion;

s4, heating the emulsion in the step S3 to 70 ℃, adding the component C, homogenizing for 2min at the rotation speed of 4000r/min, cooling to 45 ℃, adding the components D and E, stirring uniformly at the rotation speed of 300r/min, naturally cooling to room temperature, and tubing to obtain the emulsion.

Example 5

The raw materials comprise the following components in parts by weight:

the component A consists of the following raw materials: 80 parts of water, 5 parts of glycerol, 0.15 part of allantoin and 0.2 part of methylparaben;

the component B consists of the following raw materials: 1 part of cetearyl alcohol, 1.5 parts of simethicone, 5 parts of isooctyl palmitate, 1 part of sodium lauryl sulfate and 0.7 part of betaine;

the component C is 0.5 part of 50 percent triethanolamine;

the component D consists of the following raw materials: 0.5 part of DMDM hydantoin, 0.05 part of carboxymethyl pachyman, 0.5 part of shea butter, 0.03 part of sophora flower bud extract and 0.03 part of fenugreek extract;

the component E consists of the following raw materials: 0.3 part of lavender essential oil and 0.015 part of essence.

s1, weighing the raw materials of the component A according to a proportion, adding the raw materials into a container A, heating, stirring until the raw materials are completely dissolved, wherein the rotating speed is 500r/min, and controlling the temperature to 80 ℃;

s2, weighing the raw materials of the component B according to a proportion, adding the raw materials into the container B, heating, stirring until the raw materials are completely dissolved, controlling the rotating speed to be 500r/min, and controlling the temperature to be 80 ℃;

s3, adding the solution obtained in the step S1 into the solution obtained in the step S2 while the solution is hot, quickly homogenizing and stirring for 3min to form an emulsion;

s4, heating the emulsion in the step S3 to 70 ℃, adding the component C, homogenizing for 3min at the rotating speed of 6000r/min, cooling to 45 ℃, adding the components D and E, stirring uniformly at the rotating speed of 500r/min, naturally cooling to room temperature, and tubing to obtain the emulsion.

Example 6

The raw materials comprise the following components in parts by weight:

the component A consists of the following raw materials: 76 parts of water, 2 parts of glycerol, 0.07 part of allantoin and 0.12 part of methylparaben;

the component B consists of the following raw materials: 0.6 part of cetostearyl alcohol, 1.2 parts of dimethyl silicone oil, 2 parts of isooctyl palmitate, 0.6 part of sodium lauryl sulfate and 0.4 part of betaine;

the component C is 0.2 part of 50 percent triethanolamine;

the component D consists of the following raw materials: 0.2 part of DMDM hydantoin, 0.02 part of carboxymethyl pachyman, 0.2 part of shea butter, 0.015 part of sophora flower bud extract and 0.015 part of fenugreek extract;

the component E consists of the following raw materials: 0.15 part of tea tree essential oil and 0.007 part of essence.

s1, weighing the raw materials of the component A according to a proportion, adding the raw materials into a container A, heating, stirring until the raw materials are completely dissolved, controlling the rotating speed to be 350r/min, and controlling the temperature to be 80 ℃;

s2, weighing the raw materials of the component B according to a proportion, adding the raw materials into the container B, heating, stirring until the raw materials are completely dissolved, controlling the rotating speed to be 350r/min, and controlling the temperature to be 80 ℃;

s4, heating the emulsion in the step S3 to 70 ℃, adding the component C, homogenizing for 2min at the rotating speed of 4500r/min, cooling to 45 ℃, adding the components D and E, stirring uniformly at the rotating speed of 350r/min, naturally cooling to room temperature, and tubing to obtain the emulsion.

Example 7

The raw materials comprise the following components in parts by weight:

the component A consists of the following raw materials: 78 parts of water, 4 parts of glycerol, 0.12 part of allantoin and 0.18 part of methylparaben;

the component B consists of the following raw materials: 0.8 part of cetostearyl alcohol, 1.4 parts of dimethyl silicone oil, 4 parts of isooctyl palmitate, 0.8 part of sodium lauryl sulfate and 0.6 part of betaine;

the component C is 0.4 part of 50 percent triethanolamine;

the component D consists of the following raw materials: 0.4 part of DMDM hydantoin, 0.04 part of carboxymethyl pachyman, 0.4 part of shea butter, 0.025 part of sophora flower bud extract and 0.025 part of fenugreek extract;

the component E consists of the following raw materials: 0.25 part of bergamot essential oil and 0.012 part of essence.

s1, weighing the raw materials of the component A in proportion, adding the raw materials into a container A, heating, stirring until the raw materials are completely dissolved, wherein the rotating speed is 450r/min, and controlling the temperature to 80 ℃;

s2, weighing the raw materials of the component B according to a proportion, adding the raw materials into the container B, heating, stirring until the raw materials are completely dissolved, controlling the rotating speed to be 450r/min, and controlling the temperature to be 80 ℃;

s4, heating the emulsion in the step S3 to 70 ℃, adding the component C, homogenizing for 3min at the rotation speed of 5500r/min, cooling to 45 ℃, adding the components D and E, stirring uniformly at the rotation speed of 450r/min, naturally cooling to room temperature, and tubing to obtain the product.

Example 8

The raw materials comprise the following components in parts by weight:

the component A consists of the following raw materials: 77 parts of water, 3 parts of glycerol, 0.1 part of allantoin and 0.15 part of methylparaben;

the component B consists of the following raw materials: 0.7 part of cetostearyl alcohol, 1.3 parts of dimethyl silicone oil, 3 parts of isooctyl palmitate, 0.7 part of sodium lauryl sulfate and 0.5 part of betaine;

the component C is 0.3 part of 50 percent triethanolamine;

the component D consists of the following raw materials: 0.3 part of DMDM hydantoin, 0.03 part of carboxymethyl pachyman, 0.3 part of shea butter, 0.02 part of sophora flower bud extract and 0.02 part of fenugreek extract;

the component E consists of the following raw materials: rosemary essential oil 0.2 parts and essence 0.01 parts.

s1, weighing the raw materials of the component A according to a proportion, adding the raw materials into a container A, heating, stirring until the raw materials are completely dissolved, wherein the rotating speed is 400r/min, and controlling the temperature to 80 ℃;

s2, weighing the raw materials of the component B according to a proportion, adding the raw materials into the container B, heating, stirring until the raw materials are completely dissolved, controlling the rotating speed to be 400r/min, and controlling the temperature to be 80 ℃;

s3, adding the solution obtained in the step S1 into the solution obtained in the step S2 while the solution is hot, quickly homogenizing and stirring for 2.5min to form an emulsion;

s4, heating the emulsion in the step S3 to 70 ℃, adding the component C, homogenizing for 2.5min at the rotation speed of 5000r/min, cooling to 45 ℃, adding the components D and E, stirring uniformly at the rotation speed of 400r/min, naturally cooling to room temperature, and tubing to obtain the emulsion.

Comparative example 1

The preparation method is the same as that of example 8, and the carboxymethyl pachyman is replaced by the carboxymethyl pachyman prepared in comparative example 1 compared with the formula of example 8.

Comparative example 2

The preparation method is the same as that of the example 8, and compared with the formula of the example 8, the formula does not contain shea butter.

Comparative example 3

The preparation method is the same as that of example 8, and the formula does not contain the sophora flower bud extract and the fenugreek extract compared with example 8.

Test example 1 patch test for human skin

1. The test substance: poria cocos cleanser prepared in example 8

2. Negative control: deionized water

3. Subject: the total number of 30 people, male 0 person and female 30 people, the age is 21-48 years, and the volunteer enrollment criteria of the subject are met.

4. The spot pasting method comprises the following steps: a qualified spot tester is selected, a closed spot test method is adopted, a tested substance and a negative control about 0.020-0.025 mL (semifluid) are dripped into the spot tester, an external special adhesive tape is pasted on the back of the tested substance, the tested substance is removed after 24 hours, skin reactions are observed after 0.5, 24 and 48 hours after the tested substance is removed respectively, and the results are recorded according to the skin reaction grading standard in the cosmetic hygiene Specification (2007 edition). The test results are shown in table 3:

TABLE 3 test results of human skin patches

The result of the human body skin patch test shows that: adverse skin reactions occurred in 0 of 30 people; the poria cocos facial cleanser is safe to use.

The skin patch test of the human body was performed using the poria cocos cleansers obtained in examples 4 to 7 in the above-described manner, and test results consistent with the above-described test results were obtained.

Test example 2 Effect test

A first part: the poria cocos facial cleanser disclosed by the invention has a moisturizing effect.

Firstly, testing a test article: the poria cocos cleansers prepared in examples 4 to 8, the cleanser prepared in comparative examples 1 to 3, and a commercial cleanser.

II, the tested people group:

sex number: woman, 200 persons.

Age: between 22 and 45 years old.

Health condition: the skin of the subject is healthy, has no allergic history of the skin disease, and meets the voluntary selection standard of the subject.

Grouping: divided into 10 groups of 20 people each.

Thirdly, a testing method: after a subject washes the face with clear water, the moisture content of the skin of the forehead, the left face, the right face and the chin is respectively tested by using a Fischerer SK-I skin moisture detector, the arithmetic mean value is taken, the subject wets the face with warm water, then the face is cleaned by using the poria cocos facial cleanser, the face is washed with clear water, the skin moisture content of the forehead, the left face, the right face and the chin at the same positions is tested by using a skin moisture tester, and the arithmetic mean value is taken. The results were arithmetically averaged for each group of 20 subjects. The results are shown in Table 4.

Table 4 table of skin moisture content measurement results

As can be seen from table 1, compared with the commercially available facial cleanser, the poria facial cleanser of examples 4-8 of the present invention can maintain the moisture of the skin without losing and damaging the natural sebum membrane of the facial skin, and can moisturize the skin in time, wherein the moisturizing effect of the poria facial cleanser of example 8 is the best. The carboxymethyl pachyman prepared by other methods in the prior art (comparative example 1) has a water supplementing effect which is not as good as that of the carboxymethyl pachyman prepared by the method of the present invention used in examples 4-8, and comparative examples 2-3 lack certain components compared with example 8, and have no water supplementing effect as good as those of examples 4-8, which shows that the additive components of the present invention have synergistic effect.

A second part: the poria cocos facial cleanser has the using effect

Firstly, testing a test article: poria cocos facial cleansers prepared in examples 4-8 and comparative examples 1-3 and a commercial facial cleanser.

II, the tested people group:

sex number: woman, 200 persons.

Age: between 22 and 50 years old.

Grouping: divided into 10 groups of 20 people each.

Thirdly, a testing method: the facial cleansing and the feeling of use were observed and felt using the poria cocos facial cleansers prepared in examples 4 to 8 and comparative examples 1 to 3, respectively, and the commercial facial cleansers. The using method comprises the following steps: the subject directly uses the tested product once a day in the morning and evening, the face is wetted with warm water before use, a proper amount of face cleaning cream is squeezed out of the palm, a small amount of clear water is added to rub rich foam, and the face is washed clean with clear water after being massaged for a moment. The patient keeps on using the traditional Chinese medicine for one month, and is checked at least once a week to know whether systemic and local adverse reactions exist or not, and the result is recorded in detail. The test evaluation results are shown in Table 5.

TABLE 5 summary of the probation (one month) feedback of tuckahoe facial cleanser

As can be seen from the above table, compared with commercially available facial cleansers, the poria facial cleanser prepared in the embodiments 4 to 8 of the present invention has fine foam, good cleansing effect, certain anti-inflammatory and wound healing effects, elegant and natural fragrance, and can tighten skin and maintain skin elasticity and moisture; the carboxymethyl pachyman (comparative example 1) prepared by other methods of the prior art has rough use feeling and poor anti-inflammatory and wound healing effects; in the comparative example 2, ceramide and squalene are not added, so that the moisture retention and the compactness are greatly reduced; comparative example 3, in which shea butter was not added, the degree of skin lubrication was general in use; the pagodatree flower bud extract and fenugreek seed extract are not added in the comparative example 4, so that the anti-aging, skin-tightening and moisturizing effects of the facial cleanser are reduced.

Compared with the prior art, the preparation of the carboxymethyl pachyman uses the mixed solution of isopropanol and tertiary butanol to replace the traditional isopropanol or ethanol, the isopropanol is secondary alcohol, the tertiary butanol is tertiary alcohol, the steric hindrance of the isopropanol and the tertiary butanol is large, the SN2 substitution reaction is favorable for reducing side reaction, the dosage of chloroacetic acid is reduced, the production cost is reduced, the reaction is mild, the substitution degree of the prepared carboxymethyl pachyman is higher, the distribution of substituent groups is uniform, and the defect that the carboxymethyl pachyman prepared by using the isopropanol or ethanol as a medium is easy to agglomerate is overcome; the substitution degree of the carboxymethyl pachymaran can be improved by controlling the concentration of the isopropanol and the tertiary butanol; the trifluoroacetic acid adopted by the invention has the advantages of weak acidity and oxidability, good hydrolysis effect and small influence on pachyman structure, and is used as an acid for acidolysis to break the glucosidic bond of pachyman; according to the invention, the substitution degree is further improved by controlling the appropriate etherification reaction temperature, and researches show that the temperature is too low and the substitution degree is too low; the etherification temperature is too high, the substitution degree is reduced, and experiments show that the substitution degree is the highest when the temperature is 60-80 ℃;

the carboxymethyl pachyman prepared by the method has good water solubility, the solubility at 20 ℃ is 0.105-0.109mg/mL, the substitution degree is 1.55-1.59, and the carboxymethyl pachyman has good effects of resisting oxidation, relieving radiation side reaction, resisting aging, inhibiting bacteria and preserving moisture; the sophora flower bud extract and the fenugreek extract have good antioxidant, whitening and moisturizing effects; the plant essential oil has antibacterial, fragrance enhancing, skin caring, wound healing, tranquilizing, and refreshing effects; the shea butter is pure natural green plant source solid oil, can promote the regeneration of epidermal cells, endows the skin with the function of nutrition, is easy to be absorbed by the human body, can prevent drying and cracking, further recovers and maintains the natural elasticity of the skin, and simultaneously can play a role in diminishing inflammation;

the poria cocos facial cleanser disclosed by the invention has the effects of resisting inflammation, resisting cell division, relieving itching and keeping skin elasticity, can be used for healthy skin, preventing and treating skin diseases, relieving the damage of radiation to the skin, delaying aging, cleaning and tendering the skin, and has a good application prospect.

Various modifications may be made to the above without departing from the spirit and scope of the invention as defined by the appended claims. The scope of the invention is therefore intended to be limited not by the above description, but rather by the scope of the appended claims.

Claims

1. The poria cocos facial cleanser is characterized by being prepared from a component A, a component B, a component C, a component D and a component E, wherein the component A is prepared from the following raw materials: 75-80 parts of water, 4-8 parts of glycerol, 0.05-0.15 part of allantoin and 0.1-0.2 part of methylparaben; the component B consists of the following raw materials: 0.5-1 part of 16-18 alcohol, 1-1.5 parts of dimethyl silicone oil, 4-8 parts of isooctyl palmitate, 0.5-1 part of sodium lauryl sulfate and 0.3-0.7 part of betaine; the component C is 0.1 to 0.5 portion of 50 percent triethanolamine; the component D consists of the following raw materials: 0.1-0.5 part of DMDM hydantoin, 0.01-0.05 part of carboxymethyl pachyman, 0.1-0.5 part of shea butter, 0.01-0.03 part of sophora flower bud extract and 0.01-0.03 part of fenugreek extract; the component E consists of the following raw materials: 0.1-0.3 part of plant essential oil and 0.005-0.015 part of essence;

the carboxymethyl pachyman is prepared by the following method:

s4, preparing carboxymethyl pachyman: dissolving pachymaran in an alkali solution, slowly adding 35% hydrogen peroxide under stirring for decolorization until the solution becomes white, adding a mixed solution of isopropyl alcohol and tert-butyl alcohol of chloroacetic acid, controlling the concentration of the mixed solvent of isopropyl alcohol and tert-butyl alcohol in a reaction system to be 65% -70%, performing etherification reaction at 60-80 ℃ for 2-3h to obtain a reaction system in a pasty state, pouring out an upper layer of liquid, adding a dilute hydrochloric acid solution into a lower layer to adjust the pH to be 6.0, violently stirring, adding 95% ethanol, filtering, dissolving solids in water, precipitating with ethanol, filtering, and drying to obtain a white powdery solid, namely carboxymethyl pachymaran;

the acidolysis time is 30min-1h, the mixing volume ratio of isopropanol to tert-butanol is 3:1, the mixing volume ratio of chloroform to n-butanol is (4-6):1, the alkali solution is a KOH solution, and the mass concentration of the sodium periodate solution is 0.5mol/L-1.5 mol/L.

2. The poria cocos facial cleanser according to claim 1, wherein the component A is prepared from the following raw materials: 76-78 parts of water, 2-4 parts of glycerol, 0.07-0.12 part of allantoin and 0.12-0.18 part of methylparaben; the component B consists of the following raw materials: 0.6-0.8 part of 16-18 alcohol, 1.2-1.4 parts of simethicone, 2-4 parts of isooctyl palmitate, 0.6-0.8 part of sodium lauryl sulfate and 0.4-0.6 part of betaine; the component C is 0.2 to 0.4 portion of 50 percent triethanolamine; the component D consists of the following raw materials: 0.2-0.4 part of DMDM hydantoin, 0.02-0.04 part of carboxymethyl pachyman, 0.2-0.4 part of shea butter, 0.015-0.025 part of sophora flower bud extract and 0.015-0.025 part of fenugreek extract; the component E consists of the following raw materials: 0.15 to 0.25 portion of vegetable essential oil and 0.007 to 0.012 portion of essence.

3. The poria cocos facial cleanser according to claim 2, wherein the component A is prepared from the following raw materials: 77 parts of water, 3 parts of glycerol, 0.1 part of allantoin and 0.15 part of methylparaben; the component B consists of the following raw materials: 0.7 part of 16-18 alcohol, 1.3 parts of simethicone, 3 parts of isooctyl palmitate, 0.7 part of sodium lauryl sulfate and 0.5 part of betaine; the component C is 0.3 part of 50 percent triethanolamine; the component D consists of the following raw materials: 0.3 part of DMDM hydantoin, 0.03 part of carboxymethyl pachyman, 0.3 part of shea butter, 0.02 part of sophora flower bud extract and 0.02 part of fenugreek extract; the component E consists of the following raw materials: 0.2 part of plant essential oil and 0.01 part of essence.

4. The poria cocos cleanser according to claim 1, wherein the plant essential oil is one selected from tea tree essential oil, lavender essential oil, rosemary essential oil, bergamot essential oil, lemon essential oil, rose essential oil, clove essential oil, mint essential oil, cinnamon essential oil and thyme essential oil.

5. The preparation method of the poria cocos facial cleanser according to any one of claims 1 to 4, wherein the poria cocos facial cleanser is prepared according to the following method:

s3, adding the solution obtained in the step S1 into the solution obtained in the step S2 while the solution is hot, homogenizing and stirring for 2-3 min to form an emulsion;

s4, heating the emulsion in the step S3 to 70 ℃, adding the component C, homogenizing and stirring for 2-3 min, cooling to 45 ℃, adding the components D and E, stirring uniformly, naturally cooling to room temperature, and tubing to obtain the emulsion.

6. The method for preparing the poria cocos facial cleanser according to claim 5, wherein the stirring rotation speed in steps S1 and S2 is 300-500 r/min.

7. The method for preparing the poria cocos facial cleanser according to claim 5, wherein the homogenizing rotating speed in steps S3 and S4 is 4000r/min-6000 r/min.