CN113693974A - Persimmon leaf clear paste and preparation method thereof, freckle removing composition and application thereof, freckle removing preparation and preparation method of freckle removing paste - Google Patents
Persimmon leaf clear paste and preparation method thereof, freckle removing composition and application thereof, freckle removing preparation and preparation method of freckle removing paste Download PDFInfo
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- CN113693974A CN113693974A CN202011028212.2A CN202011028212A CN113693974A CN 113693974 A CN113693974 A CN 113693974A CN 202011028212 A CN202011028212 A CN 202011028212A CN 113693974 A CN113693974 A CN 113693974A
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
- A61K8/9783—Angiosperms [Magnoliophyta]
- A61K8/9789—Magnoliopsida [dicotyledons]
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/98—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution of animal origin
- A61K8/987—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution of animal origin of species other than mammals or birds
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P17/00—Drugs for dermatological disorders
- A61P17/04—Antipruritics
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
- A61Q19/005—Preparations for sensitive skin
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
- A61Q19/02—Preparations for care of the skin for chemically bleaching or whitening the skin
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/80—Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
- A61K2800/805—Corresponding aspects not provided for by any of codes A61K2800/81 - A61K2800/95
Abstract
The application relates to the technical field of cosmetics, and particularly discloses a persimmon leaf clear paste and a preparation method thereof, a freckle removing composition and application thereof, a freckle removing preparation and a preparation method of a freckle removing paste, wherein the preparation method of the persimmon leaf clear paste comprises the following steps: adding purified water into folium kaki, decocting for 25-33min at 95-102 deg.C twice, filtering the decoction with filter screen, and mixing to obtain extractive solution; and concentrating the extracting solution under reduced pressure at the concentration temperature of 60-80 ℃ to obtain the persimmon leaf clear paste, wherein the relative density of the persimmon leaf clear paste is 1.10-1.15. Also provides the persimmon leaf clear paste prepared by the preparation method, a freckle removing composition containing the persimmon leaf clear paste, application of the freckle removing composition, a freckle removing preparation prepared by the freckle removing composition, and a preparation method of the freckle removing paste. The method can effectively improve the extraction efficiency of the persimmon leaf extract.
Description
Technical Field
The application relates to the technical field of cosmetics, in particular to persimmon leaf clear paste and a preparation method thereof, a freckle removing composition and application thereof, a freckle removing preparation and a preparation method of freckle removing cream.
Background
The persimmon leaves are bitter in taste, cold in nature and nontoxic, are specially used in lung channels, and have the effects of astringing to arrest diarrhea, moistening skin and relieving itching. The main effective component of persimmon leaf is flavone, and in addition, the persimmon leaf also contains phenols, organic acid, chlorophyll, carotene, a large amount of vitamin C, amino acids and various trace elements, etc., and has extensive pharmacological actions, such as antioxidation, epidermal cell activity enhancement, antianaphylaxis, bacteriostasis, anti-inflammation, immunity enhancement, etc. Research proves that the persimmon leaves can obviously inhibit the tyrosinase activity of melanocytes and the generation of melanin, and compared with the local chemical medicament hydroquinone which is commonly used for treating chloasma clinically, the substances such as flavonoids in the persimmon leaves have stable chemical properties, small cytotoxicity and safe use.
At present, when persimmon leaves are used as raw materials to prepare a freckle removing product, the mode of adding the persimmon leaves into the freckle removing product generally has two forms, one is to directly add the whole persimmon leaves into the freckle removing product, and the other is to obtain a persimmon leaf extract from the persimmon leaves.
In view of the above-mentioned related art, the inventors have considered that it is necessary to provide a method for extracting a persimmon leaf extract from persimmon leaves to improve the extraction efficiency of the persimmon leaf extract from persimmon leaves.
Disclosure of Invention
In order to improve the extraction efficiency of the persimmon leaf extract obtained from persimmon leaves, the application provides a persimmon leaf fluid extract and a preparation method thereof, a freckle removing composition and application thereof, a freckle removing preparation and a preparation method of a freckle removing paste.
In a first aspect, the application provides a preparation method of persimmon leaf fluid extract, which adopts the following technical scheme:
a preparation method of persimmon leaf clear paste is characterized by comprising the following steps: the method specifically comprises the following steps:
a-1, extracting: according to the persimmon leaf: purified water is 1: (8-10) adding purified water into the persimmon leaves, decocting for 25-33min at 95-102 ℃ twice, filtering and combining the obtained cooking liquor with a 100-mesh 120-mesh filter screen to obtain an extracting solution;
a-2, concentrating an extracting solution: and D, concentrating the extracting solution obtained in the step A-1 under reduced pressure, wherein the concentration temperature is 60-80 ℃, and thus obtaining the persimmon leaf clear paste, and the relative density of the persimmon leaf clear paste is 1.10-1.15.
By adopting the technical scheme, the persimmon leaves are used as raw materials, various components in the persimmon leaves are extracted, the extracting solution is concentrated, and finally various components extracted from the persimmon leaves are presented in the form of persimmon leaf clear paste. Through experimental analysis, the preparation method can effectively extract various components in the persimmon leaves and improve the content of persimmon leaf clear paste extracted from the persimmon leaves.
The persimmon leaf is steamed at high temperature, and flavonoids, phenols, organic acids, chlorophyll and the like in the persimmon leaf can be transferred from the persimmon leaf to the persimmon leaf clear paste, so that the persimmon leaf clear paste has wide pharmacological effects, such as oxidation resistance, epidermal cell activity enhancement, allergy resistance, bacteriostasis, inflammation resistance, immunity enhancement and the like, and the persimmon leaf clear paste also has the effect of removing freckles.
In the process of extracting folium kaki fluid extract from folium kaki, decocting with water at 95-102 deg.C for 25-33min, filtering the decoction to obtain first decoction and residue; adding water into the filter residue for cooking continuously, wherein the cooking condition is the same as the first cooking condition, and obtaining a second cooking liquid; filtering the first and second cooking liquids, respectively, and mixing to obtain extractive solutions. In the high-temperature cooking process, the cooking temperature is not too high or too low, the activity of partial effective freckle-removing ingredients in the persimmon leaves is reduced or lost due to too high temperature, and the extraction efficiency is lower due to too low temperature; the cooking time is not suitable to be too long or too short, and the activity of the cooked effective components is reduced because the cooked effective components are in a high-temperature condition for a long time, or the cooked components are cooked, so that the components of the persimmon leaves can not be cooked from the persimmon leaves even if the cooking is carried out for a long time, and the waste of time is caused; if the cooking time is too short, the ingredients that can be cooked are not all cooked, resulting in a reduction in the final cooking efficiency. Therefore, the selection of the proper cooking time and cooking temperature is very important for the final cooking efficiency. The flavonoids in folium kaki are physiologically active substances, and are extracted from plants by heating to about 60 deg.C under normal pressure, and if heating is continued, reducing pressure is required. Experiments prove that in the extraction process of the persimmon leaf clear paste, the stewing temperature of the persimmon leaves is controlled within the range of 95-102 ℃ under normal pressure, the stewing time is controlled within the range of 25-33-7min, and the final stewing efficiency is optimal.
In addition, it has been found through experiments that a large amount of flavonoids are still contained in persimmon leaves and are not cooked out by only one cooking, and therefore, a second cooking of persimmon leaves is required. Since the cooked components are not suitable for a long time at a high temperature, and the components in the cooking liquor are saturated to prevent the components in the persimmon leaves from being transferred from the persimmon leaves to the cooking liquor, the persimmon leaves cannot be cooked by the operation of reducing the number of times of cooking and increasing the cooking time. In order to remove impurities in the first cooking liquor and the second cooking liquor, the first cooking liquor and the second cooking liquor are respectively filtered by using 100-120-mesh filter screens.
Concentrating the combined extract at 60-80 deg.C under-0.04 Mpa to-0.08 Mpa, stopping concentrating when the relative density of the concentrated solution is 1.10-1.15 at 60 deg.C, and obtaining folium kaki fluid extract. Various components in persimmon leaves are extracted through twice cooking operations, persimmon leaf clear paste is obtained through concentration, and finally the persimmon leaf clear paste with the concentration of 1.10-1.15 is added into a freckle removing product, so that the freckle removing effect of the freckle removing product can be effectively improved.
In a second aspect, the present application provides a persimmon leaf fluid extract prepared by the above preparation method.
In a third aspect, the application provides a spot-removing composition, which adopts the following technical scheme:
the freckle removing composition prepared from the persimmon leaf clear paste comprises the following raw material components in parts by weight: 0.5-1.1 parts of pearl; 46-94 parts of persimmon leaf clear paste; 56-64 parts of glycerol; 1.2-1.8 parts of sodium hydroxide; 1.6-2.2 parts of potassium hydroxide; 56-64 parts of octadecanol; 46-54 parts of liquid paraffin; 56-64 parts of stearic acid; 14.2-15.8 parts of glyceryl mono-distearate; 9.2-10.8 parts of lanolin; 4.7-5.3 parts of a preservative; 0.5-1.0 part of lily essence.
By adopting the technical scheme, the persimmon leaf clear paste is taken as clear paste extracted from persimmon leaves, has wide pharmacological effects of the persimmon leaves, such as oxidation resistance, epidermal cell activity enhancement, allergy resistance, bacteriostasis, inflammation resistance, immunity enhancement and the like, can obviously inhibit the tyrosinase activity of melanocytes and the generation of melanin, is stable in chemical property with a local chemical medicament hydroquinone which is clinically used for treating chloasma, and is low in cytotoxicity and safe to use.
The pearl powder contains five major components for changing skin types, namely collagen fiber consisting of glycine, methionine, taurine, photic phosphoamino acid and alkaline phosphate, wherein the collagen fiber can keep moisture from inside to outside for a long time, the methionine can increase the luster and the elasticity of the skin, the taurine can improve the skin environment, the photic phosphoamino acid can improve the skin environment, and the alkaline phosphate can enhance the activity of human epidermis and delay senility. The pearl is added into the freckle removing composition, so that the skin environment can be effectively improved, and the freckle removing effect is promoted.
The persimmon leaf clear paste and pearl powder are matched with other components to prepare the freckle removing composition, so that freckles can be effectively removed. Through experimental analysis, when the components of the raw materials are in the range, the prepared freckle removing composition has a good freckle removing effect.
In order to improve the stability of the freckle removing composition, the pH value of the whole freckle removing composition is adjusted by utilizing the functions of sodium hydroxide and potassium hydroxide, and the pH value of the whole freckle removing composition is stabilized within the range of 7-9.
Preferably, the freckle removing composition comprises the following raw material components in parts by weight: 0.7-0.9 part of pearl; 48-92 parts of persimmon leaf clear paste; 58-62 parts of glycerol; 1.4-1.6 parts of sodium hydroxide; 1.8-2.0 parts of potassium hydroxide; 58-62 parts of octadecanol; 48-52 parts of liquid paraffin; 58-62 parts of stearic acid; 14.5-15.5 parts of glyceryl mono-distearate; 9.5-10.5 parts of lanolin; 4.5-5.5 parts of a preservative; 0.7-0.9 part of lily essence.
By adopting the technical scheme, through experimental analysis, when the raw material components are in the range, the freckle removing effect of the freckle removing composition prepared by the preparation method is better.
Preferably, the pearl is added into the freckle removing composition in the form of pearl powder, and the particle size of the pearl powder is less than or equal to 150 mu m.
By adopting the technical scheme, in order to promote the absorption of the skin to the freckle-removing composition and improve the freckle-removing effect of the freckle-removing composition, the particle size of pearl powder prepared from pearls in the freckle-removing composition is controlled to be below 150 microns.
In a fourth aspect, the present application provides the use of a spot-removing composition for the manufacture of a medicament for the treatment of chloasma, freckles and allergic itching.
In a fifth aspect, the application provides a spot-removing preparation, which adopts the following technical scheme:
the freckle removing preparation comprises the freckle removing composition, and is lotion, liniment, paste or patch.
By adopting the technical scheme, the freckle removing preparation prepared by the freckle removing composition can be in various forms, and can be lotion, liniment, paste or patch.
In a sixth aspect, the application provides a preparation method of a spot-removing cream, which adopts the following technical scheme:
the preparation method of the freckle removing paste specifically comprises the following steps:
b-1, preparation of an aqueous phase: dissolving the folium kaki fluid extract, glycerol, sodium hydroxide and potassium hydroxide in purified water to obtain solution A; preparation of oil phase: dissolving liquid paraffin, stearic acid, glyceryl monostearate and lanolin in octadecanol to obtain solution B; preparation of pearl powder: pulverizing Margarita into fine powder, and sieving with 200-400 mesh sieve;
b-2, emulsification and homogenization: filtering the solution A and the solution B by using a filter screen of 80-100 meshes, mixing and homogenizing in a homogenizer at the rotating speed of 30-55rpm/min, 1200-2400rpm/min and 3-7min to obtain a homogeneous solution C;
b-3, adding materials and homogenizing: adding the pearl powder, the preservative and the lily essence into the homogeneous liquid C and homogenizing, wherein the rotating speed of a stirring system is 20-30rpm/min, and the rotating speed of a homogenizer is 1200-2400rpm/min to obtain a homogeneous liquid D;
b-4, standing: standing the homogenized solution D for more than 12h to obtain the freckle removing paste;
wherein the raw materials comprise the following components in parts by weight: 0.5-1.1 parts of pearl; 46-94 parts of persimmon leaf clear paste; 56-64 parts of glycerol; 1.2-1.8 parts of sodium hydroxide; 1.6-2.2 parts of potassium hydroxide; 56-64 parts of octadecanol; 46-54 parts of liquid paraffin; 56-64 parts of stearic acid; 14.2-15.8 parts of glyceryl mono-distearate; 9.2-10.8 parts of lanolin; 4.7-5.3 parts of a preservative; 0.5-1.0 part of lily essence.
By adopting the technical scheme, the preparation method of the freckle-removing paste comprises a preliminary preparation stage, an emulsification and homogenization stage, a feeding and homogenization stage and a standing stage, wherein the preparation of a water phase, the preparation of an oil phase and the crushing of pearls are completed in the preliminary preparation stage to respectively obtain a solution A, a solution B and pearl powder, the solution A and the solution B are emulsified and homogenized in the homogenization stage, lanolin as a lipophilic emulsifier is dissolved in the oil phase, glycerin as a hydrophilic emulsifier is dissolved in the water phase, the solution A and the solution B are mixed and homogenized and emulsified by the method; and (3) when the temperature is reduced to 35-40 ℃, adding the pearl powder, the preservative and the lily essence into the homogenized liquid C. The homogeneous liquid obtained after the homogeneous emulsification has better surface tension, and the stability of each component in the homogeneous liquid is improved. And finally, standing to obtain the freckle removing cream.
Through experimental analysis, parameter control of each stage in the preparation method of the freckle removing cream has a great influence on the freckle removing effect of the finally prepared freckle removing cream, and verification proves that the freckle removing effect of the simultaneously existing pearl powder and persimmon leaf clear paste in the freckle removing cream is far greater than the sum of the freckle removing effect of the independently existing pearl powder in the freckle removing cream and the freckle removing effect of the independently existing persimmon leaf clear paste in the freckle removing cream.
Preferably, the raw materials comprise the following components in parts by weight: 0.7-0.9 part of pearl; 48-92 parts of persimmon leaf clear paste; 58-62 parts of glycerol; 1.4-1.6 parts of sodium hydroxide; 1.8-2.0 parts of potassium hydroxide; 58-62 parts of octadecanol; 48-52 parts of liquid paraffin; 58-62 parts of stearic acid; 14.5-15.5 parts of glyceryl mono-distearate; 9.5-10.5 parts of lanolin; 4.5-5.5 parts of a preservative; 0.7-0.9 part of lily essence.
By adopting the technical scheme, through experimental analysis, when the raw material components are in the range, the freckle removing cream prepared by the preparation method has a better freckle removing effect.
Preferably, the particle size of the pearl powder is less than or equal to 150 mu m.
By adopting the technical scheme, in order to exert the function of the pearl powder in the freckle removing cream to the maximum and facilitate the absorption of the pearl powder by skin, the particle size of the finally prepared pearl powder is controlled below 150 mu m.
In summary, the present application has the following beneficial effects:
1. the application discloses a preparation method of persimmon leaf clear paste and the persimmon leaf clear paste prepared by the preparation method, and the preparation method can effectively extract various components in persimmon leaves; compared with the related technology, the extraction efficiency of the persimmon leaf clear paste in the application can reach more than 9.1 percent.
2. The application also discloses a freckle removing composition prepared from the persimmon leaf clear paste, a freckle removing preparation prepared from the freckle removing composition and application of the freckle removing preparation, and a preparation method of the freckle removing cream in the freckle removing preparation.
3. In order to better promote the freckle-removing cream to act on the skin and promote the absorption of the skin on the freckle-removing cream, the pearl powder in the freckle-removing composition and the freckle-removing cream is controlled to have the grain diameter less than or equal to 150 mu m, so that the freckle-removing composition or the freckle-removing cream is promoted to act on the skin, and the freckle-removing effect of the freckle-removing cream is improved.
Drawings
Fig. 1 is a flow chart of a preparation method of persimmon leaf fluid extract provided by the application.
Fig. 2 is a flowchart of a method for preparing a spot removing cream provided by the present application.
Detailed Description
The application provides a preparation method of persimmon leaf extract, which specifically comprises the following steps:
(1) according to the persimmon leaf: purified water 1: (8-10) adding purified water into the persimmon leaves to cook at the temperature of 95-102 ℃ for 27-33min according to the mass ratio, and filtering by using a filter screen with the specification of 100 and 120 meshes to obtain a first cooking liquid and filter residue A;
(2) according to the persimmon leaf: purified water 1: (8-10) adding purified water into the filter residue A for cooking at the temperature of 95-102 ℃ for 27-33min, filtering by using a filter screen with the specification of 100 and 120 meshes to obtain a second cooking liquid and a filter residue B, and discarding the filter residue B;
(3) mixing the first cooking liquor and the second cooking liquor to obtain an extracting solution;
(4) and (4) concentrating the extracting solution obtained in the step (3) under reduced pressure, wherein the concentration temperature is 60-80 ℃, and the vacuum degree is-0.04 Mpa to-0.08 Mpa, so that the persimmon leaf clear paste is obtained, and the relative density of the persimmon leaf clear paste is 1.10-1.15.
The application also discloses the persimmon leaf clear paste prepared by the preparation method. The application also discloses a freckle removing composition prepared from the persimmon leaf clear paste, and the freckle removing composition comprises the following raw material components in parts by weight: 0.5-1.1 parts of pearl; 46-94 parts of persimmon leaf clear paste; 56-64 parts of glycerol; 1.2-1.8 parts of sodium hydroxide; 1.6-2.2 parts of potassium hydroxide; 56-64 parts of octadecanol; 46-54 parts of liquid paraffin; 56-64 parts of stearic acid; 14.2-15.8 parts of glyceryl mono-distearate; 9.2-10.8 parts of lanolin; 4.7-5.3 parts of a preservative; 0.5-1.0 part of lily essence.
Further, the freckle removing composition comprises the following raw material components in parts by weight: 0.7-0.9 part of pearl; 48-92 parts of persimmon leaf clear paste; 58-62 parts of glycerol; 1.4-1.6 parts of sodium hydroxide; 1.8-2.0 parts of potassium hydroxide; 58-62 parts of octadecanol; 48-52 parts of liquid paraffin; 58-62 parts of stearic acid; 14.5-15.5 parts of glyceryl mono-distearate; 9.5-10.5 parts of lanolin; 4.5-5.5 parts of a preservative; 0.7-0.9 part of lily essence. The composition can be used for treating chloasma, freckle and allergic pruritus.
In addition to the above, the application also discloses a freckle removing preparation containing the freckle removing composition, and the freckle removing preparation is a lotion, a liniment, an ointment or a patch. Meanwhile, the application also specifically discloses a preparation method of the spot removing paste in the spot removing preparation, namely the preparation method of the spot removing paste, wherein the spot removing paste comprises the following raw material components in parts by weight: 0.5-1.1 parts of pearl; 46-94 parts of persimmon leaf clear paste; 56-64 parts of glycerol; 1.2-1.8 parts of sodium hydroxide; 1.6-2.2 parts of potassium hydroxide; 56-64 parts of octadecanol; 46-54 parts of liquid paraffin; 56-64 parts of stearic acid; 14.2-15.8 parts of glyceryl mono-distearate; 9.2-10.8 parts of lanolin; 4.7-5.3 parts of a preservative; 0.5-1.0 part of lily essence.
The preparation method of the freckle removing paste comprises the following steps:
(1) preparation of the aqueous phase: adding the persimmon leaf clear paste, glycerol, sodium hydroxide and potassium hydroxide into purified water according to the requirements of raw material components, mixing and stirring at the stirring speed of 500-600rpm/min and the water phase temperature of 95-100 ℃, and keeping the temperature for 27-33min to obtain a solution A.
(2) Preparation of oil phase: adding liquid paraffin, stearic acid, glyceryl monostearate and lanolin into octadecanol according to the requirements of raw material components, mixing and stirring at the stirring speed of 500-600rpm/min, the oil phase temperature of 75-85 ℃, and the heat preservation time of 27-33min to obtain solution B.
(3) Preparation of pearl powder: firstly, crushing pearls into primary powder to obtain pearl coarse powder; putting the pearl coarse powder into a ball mill, grinding the pearl coarse powder into fine powder, wherein the grinding speed is 180-250rpm/min, the grinding mode is that the pearl coarse powder and the pearl coarse powder are alternately operated in a turning mode, the pearl coarse powder and the pearl coarse powder are operated for 5min at an interval of 5min, and the accumulated grinding operation time is 10-60 min; finally sieving the pearl powder by using a 200-plus 400-mesh sieve to obtain the pearl powder; the pearl powder has a particle size of less than or equal to 150 μm.
(4) Emulsification and homogenization: filtering the solution A and the solution B by using a filter screen of 80-100 meshes respectively, mixing and stirring the solution A and the solution B in a homogenizer at the rotating speed of 30-55rpm/min, the rotating speed of the homogenizer of 1200-2400rpm/min, the homogenizing time of 3-7min and the vacuum degree of-0.06-0.1 MPa to obtain a homogeneous liquid C, and cooling;
(5) and (3) low-temperature homogenization: when the homogeneous liquid C is cooled to 35-40 ℃, adding the pearl powder, the preservative and the lily essence into the homogeneous liquid C and stirring, wherein the rotating speed of a stirring system is 20-30rpm/min, the rotating speed of a homogenizer is 1200-2400rpm/min, the homogenizing time is 7-13min, and the vacuum degree is-0.06 MPa-0.1 MPa, so as to obtain a homogeneous liquid D;
(6) cooling and discharging: and (4) cooling the homogenized liquid D to 30-35 ℃, standing for more than 12h, and discharging to obtain the freckle removing cream.
The speckle removing paste prepared by the preparation method is light brown ointment with fragrant smell and particle size less than or equal to 180 μm.
Further, the freckle removing cream comprises the following raw material components in parts by weight: 0.7-0.9 part of pearl; 48-92 parts of persimmon leaf clear paste; 58-62 parts of glycerol; 1.4-1.6 parts of sodium hydroxide; 1.8-2.0 parts of potassium hydroxide; 58-62 parts of octadecanol; 48-52 parts of liquid paraffin; 58-62 parts of stearic acid; 14.5-15.5 parts of glyceryl mono-distearate; 9.5-10.5 parts of lanolin; 4.5-5.5 parts of a preservative; 0.7-0.9 part of lily essence.
The application discloses a preparation method of persimmon leaf clear paste and the persimmon leaf clear paste prepared by the preparation method, and the preparation method can effectively extract various components in persimmon leaves; compared with the prior art, the persimmon leaf clear paste extracted is added into the freckle removing product, so that the freckle removing effect of the freckle removing product can be effectively improved.
The application also discloses a freckle removing composition prepared from the persimmon leaf clear paste, a freckle removing preparation prepared from the freckle removing composition and application of the freckle removing preparation, and a preparation method of the freckle removing cream in the freckle removing preparation.
The present application will be described in further detail below with reference to FIGS. 1 to 2, examples 1 to 11, and comparative examples 1 to 10.
Examples
Example 1
The embodiment provides a preparation method of persimmon leaf clear paste, which specifically comprises the following steps:
(1) according to the persimmon leaf: purified water 1: 10, adding 240kg of purified water into 24kg of persimmon leaves, cooking at 95 ℃ for 33min, and filtering with a filter screen with the specification of 100 meshes to obtain a first cooking liquid and filter residue A;
(2) according to the persimmon leaf: purified water 1: 8, adding 192kg of purified water into the filter residue A, cooking at 95 ℃ for 33min, filtering by using a filter screen with the specification of 100 meshes to obtain a second cooking liquid and a filter residue B, and discarding the filter residue B;
(3) mixing the first cooking liquor and the second cooking liquor to obtain an extracting solution;
(4) and (4) concentrating the extracting solution obtained in the step (3) under reduced pressure, wherein the concentration temperature is 80 ℃, and the vacuum degree is-0.04 Mpa to-0.08 Mpa, so that the persimmon leaf clear paste is obtained, and the relative density of the persimmon leaf clear paste is 1.10.
Example 2
The embodiment provides a preparation method of persimmon leaf clear paste, which specifically comprises the following steps:
(1) according to the persimmon leaf: purified water 1: 8, adding 192kg of purified water into 24kg of persimmon leaves, cooking at 102 ℃ for 27min, and filtering by using a filter screen with the specification of 120 meshes to obtain a first cooking liquid and filter residue A;
(2) according to the persimmon leaf: purified water 1: 10, adding 240kg of purified water into the filter residue A, cooking at 102 ℃ for 27min, filtering by using a filter screen with the specification of 120 meshes to obtain a second cooking liquid and a filter residue B, and discarding the filter residue B;
(3) mixing the first cooking liquor and the second cooking liquor to obtain an extracting solution;
(4) and (4) concentrating the extracting solution obtained in the step (3) under reduced pressure, wherein the concentration temperature is 60 ℃, and the vacuum degree is-0.04 Mpa to-0.08 Mpa, so that the persimmon leaf clear paste is obtained, and the relative density of the persimmon leaf clear paste is 1.15.
Example 3
The embodiment provides a preparation method of a freckle removing cream, which specifically comprises the following steps:
(1) preparation of the aqueous phase: adding 6.72kg of glycerol, 0.144kg of sodium hydroxide, 0.192kg of potassium hydroxide and 78.6kg of purified water into 5.52kg of the persimmon leaf clear paste, mixing and stirring at the stirring speed of 500rpm/min and the water phase temperature of 95 ℃ for 33min to obtain a solution A.
(2) Preparation of oil phase: mixing and stirring 6.72kg of octadecanol, 5.52kg of liquid paraffin, 6.72kg of stearic acid, 1.704kg of glyceryl monostearate and 1.104kg of lanolin at the stirring speed of 500rpm/min, the oil phase temperature of 75 ℃ and the heat preservation time of 33min to obtain a solution B.
(3) Grinding pearls: firstly, 0.06kg of pearl is crushed into primary powder to obtain pearl coarse powder; putting the pearl coarse powder into a ball mill, grinding the pearl coarse powder into fine powder, wherein the grinding speed is 180rpm/min, the grinding mode is that the pearl coarse powder is alternately operated in a turning mode, the pearl coarse powder is operated for 5min, the interval is 5min, and the grinding accumulated operation time is 60 min; finally sieving with 200 mesh sieve to obtain Margarita powder; the pearl powder has a particle size of less than or equal to 150 μm.
(4) Emulsification and homogenization: filtering the solution A and the solution B by using a filter screen of 80 meshes respectively, mixing and stirring the solution A and the solution B in a homogenizer at the rotating speed of 30rpm/min, 1200rpm/min, 7min for homogenization and-0.06-0.1 MPa for vacuum degree to obtain a homogenized solution C, and cooling;
(5) and (3) low-temperature homogenization: when the homogenized liquid C is cooled to 40 ℃, adding 0.564kg of pearl powder, 0.564kg of preservative and 0.06kg of lily essence into the homogenized liquid C and stirring, wherein the rotating speed of a stirring system is 30rpm/min, the rotating speed of a homogenizer is 2400rpm/min, the homogenizing time is 7min, and the vacuum degree is-0.06 MPa to-0.1 MPa, so as to obtain homogenized liquid D;
(6) cooling and discharging: and (5) cooling the homogenized liquid D to 35 ℃, standing for 12 hours, and discharging to obtain the freckle removing cream.
The speckle removing paste prepared by the preparation method is light brown ointment with fragrant smell and particle size less than or equal to 180 μm.
Examples 4 to 9
Examples 4 to 9 are different from example 3 in the content of each raw material component for preparing the spot removing cream, and the content of each component for preparing the spot removing cream in examples 3 to 9 is shown in table 1.
Table 1 summary of the components of the raw materials in examples 3-9
Example 10
The difference between this embodiment and embodiment 3 lies in the different parameters in the preparation method of the spot-removing cream, which specifically include:
(1) in the preparation of the water phase, the stirring speed is 550rpm/min, the temperature of the water phase is 100 ℃, and the heat preservation time is 30min, so as to obtain a solution A.
(2) In the preparation of the oil phase: stirring speed is 550rpm/min, oil phase temperature is 80 ℃, and heat preservation time is 30min to obtain solution B.
(3) In the grinding of pearls: grinding at 200rpm/min, and sieving with 400 mesh sieve to obtain Margarita powder.
(4) In emulsification and homogenization: filtering the solution A and the solution B by using a filter screen of 80 meshes respectively, mixing and stirring the solution A and the solution B in a homogenizer at the rotating speed of 55rpm/min, 1200rpm/min, 5min for homogenization and-0.06-0.1 MPa for vacuum degree to obtain a homogenized solution C, and cooling;
(5) low-temperature homogenization: and when the homogenized liquid C is cooled to 35 ℃, adding the pearl powder, the preservative and the lily essence into the homogenized liquid C and stirring, wherein the rotating speed of a stirring system is 30rpm/min, the rotating speed of a homogenizer is 2400rpm/min, the homogenizing time is 10min, and the vacuum degree is-0.06 MPa-0.1 MPa, so as to obtain homogenized liquid D.
The remaining preparation steps and parameters were the same as in example 3.
Example 11
The difference between this embodiment and embodiment 3 lies in the different parameters in the preparation method of the spot-removing cream, which specifically include:
(1) in the preparation of the water phase, the stirring speed is 600rpm/min, the temperature of the water phase is 102 ℃, and the heat preservation time is 27min, so as to obtain a solution A.
(2) In the preparation of the oil phase: stirring speed is 600rpm/min, oil phase temperature is 85 ℃, and heat preservation time is 27min, thus obtaining solution B.
(3) In the grinding of pearls: grinding at 250rpm/min, and sieving with 400 mesh sieve to obtain Margarita powder.
(4) In emulsification and homogenization: filtering the solution A and the solution B by using a 100-mesh filter screen respectively, mixing and stirring the solution A and the solution B in a homogenizer at the rotating speed of 55rpm/min, 2400rpm/min, the homogenizing time of 3min and the vacuum degree of-0.06 MPa to-0.1 MPa to obtain a homogeneous liquid C, and cooling;
(5) low-temperature homogenization: and when the homogenized liquid C is cooled to 35 ℃, adding the pearl powder, the preservative and the lily essence into the homogenized liquid C and stirring, wherein the rotating speed of a stirring system is 20rpm/min, the rotating speed of a homogenizer is 1200rpm/min, the homogenizing time is 13min, and the vacuum degree is-0.06 MPa-0.1 MPa, so as to obtain homogenized liquid D.
The remaining preparation steps and parameters were the same as in example 3.
Comparative example
Comparative example 1
The comparative example provides a preparation method of persimmon leaf clear paste, and the difference between the comparative example and the example 1 is that the persimmon leaves are steamed only once to obtain a steaming liquid, the steaming liquid is directly concentrated to obtain the final persimmon leaf clear paste, and the rest operation steps and parameters are the same as those of the example 1.
Comparative example 2
The comparative example provides a preparation method of persimmon leaf clear paste, and is different from the comparative example 1 in that the temperature of twice-cooked persimmon leaves is 60 ℃, and the rest operation steps and parameters are the same as those of the example 1.
Comparative example 3
The comparative example is different from the example 1 in that the time for steaming the persimmon leaves twice is 20min, and the rest operation steps and parameters are the same as those of the example 1.
Comparative example 4
The comparative example is different from the example 1 in that the time for steaming the persimmon leaves twice is 40min, and the rest operation steps and parameters are the same as those of the example 1.
Comparative example 5
The present comparative example provides a method for extracting a persimmon leaf extract selected from the group consisting of inhibition of tyrosinase by a persimmon leaf extract, published in agricultural science of Anhui, Journal of Anhui Agri.Sci.2015,43(26) 8-10, 26. The preparation method of the persimmon leaf extract comprises the following steps:
(1) pulverizing folium kaki, and sieving with 50 mesh sieve;
(2) taking 200g of powder, wherein the material-liquid ratio is 1: 10, adding the powder into absolute methanol containing 1.2 percent of hydrochloric acid, performing ultrasonic extraction at the temperature of 55 ℃ for 60min, filtering, and performing reduced pressure concentration to obtain the persimmon leaf extracting solution.
Comparative example 6
The comparative example discloses a preparation method of a freckle removing paste, and is different from the embodiment 3 in that pearl coarse powder is put into a ball mill during grinding of pearls, the grinding speed is 150rpm/min, and the accumulated grinding running time is 20 min; finally sieving with 150 mesh sieve to obtain Margarita powder; the particle size of the pearl powder is less than or equal to 200 mu m, and the rest operation steps and parameters are the same as those of the embodiment 3.
Comparative example 7
The comparative example discloses a preparation method of the freckle removing cream, and the difference between the comparative example and the example 3 is as follows: in the emulsification and homogenization in the step (4), the rotating speed of a homogenizer is 1000rpm/min, the homogenization time is 2min, and a homogenized liquid C is obtained and cooled; step (5), low-temperature homogenization: when the homogenized liquid C is cooled to 40 ℃, adding the pearl powder, the preservative and the lily essence into the homogenized liquid C and stirring, wherein the rotating speed of a homogenizer is 1000rpm/min, the homogenizing time is 5min, and the vacuum degree is-0.06 MPa to-0.1 MPa, so as to obtain homogenized liquid D; and (6) cooling and discharging: and (5) cooling the homogenized liquid D to 35 ℃, standing for 12 hours, and discharging to obtain the freckle removing cream. The freckle-removing paste prepared by the preparation method is light brown ointment with fragrance and particle size less than or equal to 250 microns, and the rest operation steps and parameters are the same as those of the embodiment 3.
Comparative example 8
The comparative example discloses a preparation method of the freckle removing cream, and is different from the example 3 in that a pearl powder component is not added in the preparation process, and the rest operation steps and parameters are the same as those of the example 3.
Comparative example 9
The comparative example discloses a preparation method of the freckle removing paste, and is different from the example 3 in that the persimmon leaf clear paste is not added in the preparation process, and the rest operation steps and parameters are the same as those of the example 3.
Comparative example 10
The comparative example is different from example 3 in that the persimmon leaf clean cream in the spot-removing cream was replaced with the persimmon leaf extract obtained by the preparation method provided in comparative example 5, and the remaining operation steps and parameters were the same as those of example 3.
Performance test
Test No.)
The persimmon leaf fluid extracts prepared in the examples 1-2 and the comparative examples 1-5 are compared in properties, 200g of the persimmon leaf fluid extract prepared in the examples 1-2 and the comparative examples 1-4 and the persimmon leaf extract prepared in the comparative example 5 are respectively taken, the persimmon leaf fluid extracts are placed in a constant-temperature drying oven at 80 ℃ for drying for 48h, and the mass of the finally obtained dried sample is recorded and counted as the dry weight. The comparison results and the detection results are shown in table 2. The calculation formula of the relative density is shown as a formula (1), the calculation formula of the preparation efficiency is shown as a formula (2), and the formula (1) and the formula (2) are respectively shown as follows:
TABLE 2 Property ratios of persimmon leaf fluid extracts prepared in examples 1 to 2 and comparative examples 1 to 5
As shown in Table 2, as can be seen from the comparison of examples 1-2 with comparative examples 1-5, the persimmon leaf components prepared from the persimmon leaf fluid extracts prepared by the preparation methods of examples 1-2 were more abundant, and the cooking degree of the persimmon leaves of examples 1-2 was more sufficient, as can be seen from the state of the final residue, from the relative density, viscosity, color, dry weight and preparation efficiency of the persimmon leaf fluid extracts prepared by the preparation methods of examples 1-2. Therefore, the preparation method provided by the application can be used for effectively improving the preparation efficiency of the persimmon leaf clear paste.
Test No. two
The spot-removing cream prepared by the preparation method of examples 3 to 11 was subjected to corresponding detection in accordance with WS3-B-3897-98, which is a standard of Chinese medicinal component preparations of drug standards of the ministry of health, and the detection results are shown in Table 3.
TABLE 3 test results of examples 3 to 11
As shown in table 3, it can be seen that the spot-removing cream prepared by the preparation method of the present application all meets the corresponding detection standards.
Experiment three
The freckle-removing paste prepared by the preparation method provided by the application can be applied to preparation of medicines for treating chloasma, freckles and allergic itching. The spot removing cream prepared by the present application is used for treating chloasma as an example, and the spot removing cream prepared by the examples 3 to 11 and the comparative examples 6 to 10 are used in the following detection tests, respectively.
Firstly, an effect detection test grouping: according to the preparation rule (draft) of chloasma animal model (Chinese medicine new drug and clinical pharmacology 2017, 9.7.28, 5 th), a mouse chloasma model is prepared by using progesterone general attack, a female mouse with the age of 6-8 weeks is selected, the weight of the female mouse is 18-22g, and progesterone injection (20m g kg) is injected into hind limb muscle-1) 1 time daily, 35 days of continuous injection, two hind limbs alternatedAnd (5) injecting progesterone to prepare a mouse chloasma model. Randomly dividing the prepared chloasma model mice into two groups, namely a test group and a control group; meanwhile, selecting a spot-free mouse to be smeared with the spot-removing cream as a control; selecting 2X 2cm of the back of each mouse2The mouse hair was removed and used as the test point.
The test mode is as follows: test groups: respectively smearing 0.2g of freckle-removing cream on the test point of a mouse 2 times a day, wherein the interval between every two times is 12h, and the smearing period is 30 days; control group: mice were each dosed with 0.2g of purified water 2 times a day, 12h apart, for a 30 day dosing period. After 30 days, the mice were sacrificed after administration, and the chloasma area at the test site on the back of each mouse was observed and was measured by an image analyzer. Skin tissues (1X 1 cm) of the test site were taken2) 10% formalin, sections embedded in normal paraffin, deparaffinized to water, antigen retrieval, and immunohistochemical visualization of melanin granules in the epidermis using HMB45 (melanoma) as the primary antibody to visualize the distribution of melanocytes in the epidermis. The results are shown in Table 4.
TABLE 4 test results for removing chloasma and freckles in examples 3 to 11 and comparative examples 6 to 10
As shown in table 4, it can be seen from the detection results of examples 3 to 11 that the freckle removing cream prepared by the preparation method of the freckle removing cream provided by the present application has a good effect of removing chloasma. As can be seen from the comparison between example 3 and comparative examples 6 to 7, the particle size of the pearl powder in the spot-removing cream and the particle size of the spot-removing cream have a great influence on the final spot-removing effect of the spot-removing cream. As can be seen from the comparison between example 3 and comparative examples 8-9, the spot-removing effect of the spot-removing cream with the pearl powder and the persimmon leaf fluid extract is much greater than the sum of the spot-removing effect of the pearl powder alone and the spot-removing effect of the persimmon leaf fluid extract alone.
In addition, as can be seen from comparison between example 3 and comparative example 10, the application of the persimmon leaf fluid extract prepared by the preparation method of the present application to the freckle removing effect is superior to the application of the persimmon leaf extract prepared by the preparation method of the related art to the freckle removing effect of the freckle removing cream, and thus, the application of the persimmon leaf fluid extract prepared by the preparation method of the present application to the freckle removing cream can effectively improve the freckle removing effect of the freckle removing cream.
II, grouping toxicity test tests: selecting model mice established by the method, and selecting 2X 2cm back of each mouse2Removing mouse hair to serve as a test point; the freckle-removing paste prepared in the examples 3-11 is respectively smeared on the test points of mice according to the mass ratio of 0.05g, 0.1g, 0.2g, 0.5g and 1g, 2 times a day with 12h intervals, and the smearing period is 30 days. After 30 days, the test site on the back of each mouse was observed for the presence of abnormality, and the results are shown in Table 5.
TABLE 5 toxicity test results
As shown in table 5, it is understood from the test results of examples 3 to 11 that when the spot removing cream prepared by the preparation method provided by the present application is used for the toxicity test of mice, no toxicity reaction is observed in the spot removing cream prepared by the preparation method provided by the present application in the test range, and the skin at the test point tends to be better in the test range.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.
Claims (10)
1. A preparation method of persimmon leaf clear paste is characterized by comprising the following steps: the method specifically comprises the following steps:
a-1, extracting: according to the persimmon leaf: purified water is 1: (8-10) adding purified water into the persimmon leaves, decocting for 25-33min at 95-102 ℃ twice, filtering and combining the obtained cooking liquor with a 100-mesh 120-mesh filter screen to obtain an extracting solution;
a-2, concentrating an extracting solution: and D, concentrating the extracting solution obtained in the step A-1 under reduced pressure, wherein the concentration temperature is 60-80 ℃, and thus obtaining the persimmon leaf clear paste, and the relative density of the persimmon leaf clear paste is 1.10-1.15.
2. A persimmon leaf fluid extract prepared by the preparation method of claim 1.
3. A freckle removing composition prepared from the persimmon leaf clear paste of claim 2 is characterized by comprising the following raw material components in parts by weight: 0.5-1.1 parts of pearl; 46-94 parts of persimmon leaf clear paste; 56-64 parts of glycerol; 1.2-1.8 parts of sodium hydroxide; 1.6-2.2 parts of potassium hydroxide; 56-64 parts of octadecanol; 46-54 parts of liquid paraffin; 56-64 parts of stearic acid; 14.2-15.8 parts of glyceryl mono-distearate; 9.2-10.8 parts of lanolin; 4.7-5.3 parts of a preservative; 0.5-1.0 part of lily essence.
4. The freckle removing composition according to claim 3, wherein the freckle removing composition comprises the following raw material components in parts by weight: 0.7-0.9 part of pearl; 48-92 parts of persimmon leaf clear paste; 58-62 parts of glycerol; 1.4-1.6 parts of sodium hydroxide; 1.8-2.0 parts of potassium hydroxide; 58-62 parts of octadecanol; 48-52 parts of liquid paraffin; 58-62 parts of stearic acid; 14.5-15.5 parts of glyceryl mono-distearate; 9.5-10.5 parts of lanolin; 4.5-5.5 parts of a preservative; 0.7-0.9 part of lily essence.
5. A spot-removing composition according to claim 3 or 4, wherein: the pearl is added into the freckle removing composition in the form of pearl powder, and the particle size of the pearl powder is less than or equal to 150 mu m.
6. Use of a spot-removing composition according to any of claims 3 to 5, wherein: the freckle removing composition is applied to the preparation of medicines for treating chloasma, freckles and allergic itching.
7. A spot-removing preparation is characterized in that: the freckle removing preparation comprises the freckle removing composition according to any one of claims 3 to 5, and the freckle removing preparation is lotion, liniment, paste or patch.
8. The preparation method of the freckle removing paste is characterized by comprising the following steps:
b-1, preparation of an aqueous phase: dissolving the folium kaki fluid extract, glycerol, sodium hydroxide and potassium hydroxide in purified water to obtain solution A;
preparation of oil phase: dissolving liquid paraffin, stearic acid, glyceryl monostearate and lanolin in octadecanol to obtain solution B;
preparation of pearl powder: pulverizing Margarita into fine powder, and sieving with 200-400 mesh sieve;
b-2, emulsification and homogenization: filtering the solution A and the solution B by using a filter screen of 80-100 meshes, mixing and homogenizing in a homogenizer at the rotating speed of 30-55rpm/min, 1200-2400rpm/min and 3-7min to obtain a homogeneous solution C;
b-3, adding materials and homogenizing: adding the pearl powder, the preservative and the lily essence into the homogeneous liquid C and homogenizing, wherein the rotating speed of a stirring system is 20-30rpm/min, and the rotating speed of a homogenizer is 1200-2400rpm/min to obtain a homogeneous liquid D;
b-4, standing: standing the homogenized solution D for more than 12h to obtain the freckle removing paste;
wherein the raw materials comprise the following components in parts by weight: 0.5-1.1 parts of pearl; 46-94 parts of persimmon leaf clear paste; 56-64 parts of glycerol; 1.2-1.8 parts of sodium hydroxide; 1.6-2.2 parts of potassium hydroxide; 56-64 parts of octadecanol; 46-54 parts of liquid paraffin; 56-64 parts of stearic acid; 14.2-15.8 parts of glyceryl mono-distearate; 9.2-10.8 parts of lanolin; 4.7-5.3 parts of a preservative; 0.5-1.0 part of lily essence.
9. The preparation method of the spot-removing cream according to claim 8, wherein the raw materials comprise, by weight: 0.7-0.9 part of pearl; 48-92 parts of persimmon leaf clear paste; 58-62 parts of glycerol; 1.4-1.6 parts of sodium hydroxide; 1.8-2.0 parts of potassium hydroxide; 58-62 parts of octadecanol; 48-52 parts of liquid paraffin; 58-62 parts of stearic acid; 14.5-15.5 parts of glyceryl mono-distearate; 9.5-10.5 parts of lanolin; 4.5-5.5 parts of a preservative; 0.7-0.9 part of lily essence.
10. The method for preparing a freckle-removing cream according to claim 8, wherein the pearl powder has a particle size of less than or equal to 150 μm.
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