CN115957262B

CN115957262B - Composition for treating acne and application thereof

Info

Publication number: CN115957262B
Application number: CN202310191805.8A
Authority: CN
Inventors: 宋志军; 闫炳雄; 姚彩云; 阮丽君; 吴云秋
Original assignee: Guangxi Botanical Garden of Medicinal Plants
Current assignee: Guangxi Botanical Garden of Medicinal Plants
Priority date: 2023-03-02
Filing date: 2023-03-02
Publication date: 2024-01-26
Anticipated expiration: 2043-03-02
Also published as: CN115957262A

Abstract

The invention discloses a composition for treating acne, which mainly comprises the following raw material components in parts by weight: 10-15 parts of cortex dictamni extract, 5-20 parts of cortex dictamni polysaccharide, 10-20 parts of fresh luffa juice, 1-2 parts of propylene glycol, 1-2 parts of laurocapram, 1-2 parts of glycerol, 1-3 parts of tween-80, 10-20 parts of hydroxypropyl-beta-cyclodextrin, 5-9 parts of sodium chloride, 7-12 parts of essence, 0.5-1 part of sodium benzoate and 900-1000 parts of water. The invention also provides a method for preparing the acne treatment spray from the composition for treating acne and application of the composition for treating acne in medicines for treating acne. The invention has safe effect and good permeability, can effectively remove acne, whelk and facial acne marks, and has the whitening effect.

Description

Composition for treating acne and application thereof

Technical Field

The invention belongs to the field of traditional Chinese medicine preparation. More particularly, the present invention relates to a composition for treating acne and its use.

Background

Acne is good for face, neck, chest and back etc. of young and young men, and has great influence on mental, social and life quality of teenagers. The main inducement is that puberty is mature, the level of male hormone in the body is increased, and epithelial cells which stimulate sebum and hair follicle to fall are gathered into yellow and white substances to plug in pores, so that acne is formed, the sebum is difficult to discharge, grey and white pimples are formed, the acne exposed outside hair follicle mouths is polluted by air dust and becomes black blackhead acne, a large amount of propionibacteria acnes exist in the hair follicle lumen, the sebum is decomposed into unsaturated fatty acids, different degrees of inflammation occur on the hair follicle and the periphery of the hair follicle, suppuration, nodules, cysts or atheroma occur, and the like, and the chronic and repeated inflammation can leave scars which are difficult to heal on the face, so that the skin is uneven and rough and unsightly. At present, the products for treating and relieving acne are mainly treated by adding chemical medicines and hormones, the disease is repeated, and the symptoms of pigmentation and scar are usually present after healing, so that the pure natural traditional Chinese medicines or the traditional Chinese medicine extraction medicines are less. Therefore, the development of the medicine taking the natural medicine extract and the effective active ingredients as the main raw materials has a great market prospect.

Disclosure of Invention

It is an object of the present invention to solve at least the above problems and to provide at least the advantages to be described later.

The invention aims to provide a composition for treating acne, which is safe in action, good in permeability, capable of effectively removing acne, whelk and facial acne marks, and has a whitening effect.

To achieve these objects and other advantages and in accordance with the purpose of the invention, there is provided a composition for treating acne, which comprises the following raw material components in parts by weight: 10-15 parts of cortex dictamni extract, 5-20 parts of cortex dictamni polysaccharide, 10-20 parts of fresh luffa juice, 1-2 parts of propylene glycol, 1-2 parts of laurocapram, 1-2 parts of glycerol, 1-3 parts of tween-80, 10-20 parts of hydroxypropyl-beta-cyclodextrin, 5-9 parts of sodium chloride, 7-12 parts of essence, 0.5-1 part of sodium benzoate and 900-1000 parts of water.

Preferably, the fresh fructus Luffae juice is prepared by cleaning fresh fructus Luffae, squeezing to obtain juice, filtering to remove residue, removing color, and purifying by MCI column chromatography.

Preferably, cortex Dictamni Radicis for extracting cortex Dictamni Radicis polysaccharide is processed by one of parching, salt parching, vinegar parching or wine parching.

Preferably, the salt stir-frying method of the dittany bark comprises the following steps: stirring the cortex dictamni with saline water uniformly, and moistening the cortex dictamni, wherein the mass ratio of the cortex dictamni, the salt and the water is 100-150:1-5:10-20, and stirring the mixture in the middle until the saline water is absorbed completely to obtain the moistening cortex dictamni; heating the stir-frying container, adding the steamed cortex Dictamni Radicis, stir-frying, taking out, oven drying at 60-95deg.C after a large amount of white frost is adhered to the surface of the medicinal materials, and parching with salt to obtain the processed cortex Dictamni Radicis.

Preferably, the extraction of the cortex dictamni extract and the cortex dictamni polysaccharide comprises the following steps:

1) Adding petroleum ether into the salt-fried cortex Dictamni Radicis, reflux extracting, filtering, and drying the residue to obtain dried residue;

2) Adding ethanol solution into the dried filter residue, reflux-extracting, filtering, concentrating the filtrate to obtain extract A, and oven drying the filter residue to obtain the residue;

3) Decocting the residue with water, extracting in a micro-pressure reaction kettle, filtering to obtain filtrate A and residue A, concentrating the filtrate A, adding Sevage reagent into the concentrated solution, mixing, oscillating, centrifuging, discarding the precipitate, adding ethanol into the supernatant for alcohol precipitation, standing, filtering to obtain filtrate B and residue B, washing the residue B with ethanol solution, and air drying to obtain cortex Dictamni Radicis polysaccharide; concentrating the filtrate B into extract to obtain extract B; adding ethanol solution into the filter residue A for reflux extraction, filtering, and concentrating the filtrate into extract to obtain extract C;

4) Mixing the extract A, the extract B and the extract C to obtain the cortex Dictamni Radicis extract.

Preferably, in the step 1), the feed liquid ratio of the salt stir-fried dittany bark to the petroleum ether is 1-5:10-20.

Preferably, in the step 2), the ratio of the dry filter residue to the ethanol solution is 1-5:10-20, the volume concentration of the ethanol solution is 80% -90%, and the reflux extraction is carried out for 2-3 times, each time for 50-100min.

Preferably, in the step 3), the feed liquid ratio of the medicine residue A to the water is 1-5:10-20, the extraction pressure in the micro-pressure reaction kettle is 0.05-0.1MPa, the temperature is 90-100 ℃, and the decoction time is 50-100min.

A method for preparing a spray for treating acne from a composition for treating acne comprising the steps of:

step one, uniformly mixing a dittany bark extract and fresh luffa juice to obtain a solution A;

dissolving sodium chloride in water and filtering to obtain solution B;

step three, adding hydroxypropyl-beta-cyclodextrin into water for dissolution to obtain a solution C;

step four, adding the solution A into the solution C, stirring and dissolving, adding tween-80 and glycerol, and stirring uniformly to obtain solution D;

step five, adding propylene glycol and laurocapram while stirring the solution D, and uniformly stirring and mixing to obtain the solution E;

and step six, adding the solution B, sodium benzoate and essence while stirring the solution E, and adding water and uniformly mixing to obtain the product.

Use of a composition for treating acne in a medicament for treating acne.

The invention at least comprises the following beneficial effects:

first, the invention can improve the extraction rate of the crude polysaccharide of the cortex dictamni by stir-frying, such as stir-frying, salt stir-frying, wine stir-frying or vinegar stir-frying.

Secondly, the invention uses petroleum ether to remove substances with small molecular polarity such as fat, tannin and the like in the cortex dictamni, so that the extracted components are fully contacted with the extraction solvent in the subsequent extraction process, the extraction rate of the effective components is increased, and the curative effect of the composition is improved.

Thirdly, the composition provided by the invention has the whitening effect on effectively removing acne, whelk and facial acne marks.

Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention.

Drawings

FIG. 1 is a wavelength scan of a glucose control;

FIG. 2 is a glucose standard graph;

FIG. 3 is a thin layer chromatogram;

FIG. 4 is a liquid chromatogram, wherein H is a control of phellodendron ketone; n is limonin reference substance; t is the test sample.

Detailed Description

The present invention is described in further detail below with reference to the drawings to enable those skilled in the art to practice the invention by referring to the description.

It will be understood that terms, such as "having," "including," and "comprising," as used herein, do not preclude the presence or addition of one or more other elements or groups thereof.

The experimental methods described in the following embodiments are conventional methods unless otherwise indicated, and the reagents and materials are commercially available.

The composition for treating acne mainly comprises the following raw material components in parts by weight: 10-15 parts of cortex dictamni extract, 5-20 parts of cortex dictamni polysaccharide, 10-20 parts of fresh luffa juice, 1-2 parts of propylene glycol, 1-2 parts of laurocapram, 1-2 parts of glycerol, 1-3 parts of tween-80, 10-20 parts of hydroxypropyl-beta-cyclodextrin, 5-9 parts of sodium chloride, 7-12 parts of essence, 0.5-1 part of sodium benzoate and 900-1000 parts of water.

In another technical scheme, the fresh luffa juice is prepared by taking fresh luffa, cleaning, squeezing to obtain luffa juice with a juicer, filtering to remove residues, removing color, and further separating and purifying with MCI column chromatography.

In another technical scheme, the essence is plant essence or hydrolat.

In another technical scheme, cortex dictamni used for extracting cortex dictamni polysaccharide is processed by one of a processing method of stir-frying, salt stir-frying, vinegar stir-frying or wine stir-frying.

In another technical scheme, the salt stir-frying method of the cortex dictamni comprises the following steps: stirring the cortex dictamni with saline water uniformly, and moistening the cortex dictamni, wherein the mass ratio of the cortex dictamni, the salt and the water is 100-150:1-5:10-20, and stirring the mixture in the middle until the saline water is absorbed completely to obtain the moistening cortex dictamni; heating the stir-frying container, adding the steamed cortex Dictamni Radicis, stir-frying, taking out, oven drying at 60-95deg.C after a large amount of white frost is adhered to the surface of the medicinal materials, and parching with salt to obtain the processed cortex Dictamni Radicis.

In another technical scheme, the extraction of the cortex dictamni extract and the cortex dictamni polysaccharide comprises the following steps:

3) Decocting the residue with water, extracting in a micro-pressure reaction kettle, filtering to obtain filtrate A and residue A, concentrating filtrate A by membrane separation system with reverse osmosis membrane to 0.5-0.7 times of original liquid medicine volume, adding Sevage reagent into the concentrated solution, mixing, oscillating, centrifuging, discarding precipitate, adding ethanol into supernatant for alcohol precipitation, standing, filtering to obtain filtrate B and residue B, washing residue B with ethanol solution, and air drying to obtain cortex Dictamni Radicis polysaccharide; concentrating the filtrate B into extract to obtain extract B; adding ethanol solution into the filter residue A for reflux extraction, filtering, and concentrating the filtrate into extract to obtain extract C;

In another technical scheme, in the step 1), the feed liquid ratio of the salt stir-fried dittany bark to the petroleum ether is 1-5:10-20.

In another technical scheme, in the step 2), the ratio of the dry filter residue to the ethanol solution is 1-5:10-20, the volume concentration of the ethanol solution is 80% -90%, and the reflux extraction is carried out for 2-3 times, 50-100min each time.

In another technical scheme, in the step 3), the feed liquid ratio of the medicine residue A to water is 1-5:10-20, the extraction pressure in the micro-pressure reaction kettle is 0.05-0.1MPa, the temperature is 90-100 ℃, and the decoction time is 50-100min.

dissolving sodium chloride in water and filtering to obtain solution B;

Use of a composition for treating acne in a medicament for treating acne. The composition and medically acceptable auxiliary materials are used for preparing medicaments in different dosage forms such as ointment, spray and the like, and the medicaments are all within the protection scope of the invention.

Example 1 ]

The composition for treating acne mainly comprises the following raw material components in parts by weight: 10g of cortex dictamni extract, 5g of cortex dictamni polysaccharide, 10g of fresh towel gourd juice, 1g of propylene glycol, 1g of laurocapram, 1g of glycerin, 1g of tween-80, 10g of hydroxypropyl-beta-cyclodextrin, 5g of sodium chloride, 7g of plant essence, 0.5g of sodium benzoate and 900mL of water;

the fresh fructus Luffae juice is prepared by cleaning fresh fructus Luffae, squeezing to obtain juice, filtering to remove residue, removing color, and purifying by MCI column chromatography;

the method for stir-frying the cortex dictamni for extracting the cortex dictamni polysaccharide comprises the following steps of: stirring the cortex dictamni with saline water uniformly, and moistening the cortex dictamni, wherein the mass ratio of the cortex dictamni, the salt and the water is 100:1:10, and turning the cortex dictamni in the middle, and obtaining the moistening cortex dictamni after the saline water is absorbed completely; heating the stir-frying container, adding the steamed cortex Dictamni Radicis, stir-frying, taking out and drying after a large amount of white frost is attached to the surface of the medicinal materials, and obtaining the salt stir-fried cortex Dictamni Radicis at 90 ℃;

the extraction of the cortex dictamni extract and the cortex dictamni polysaccharide comprises the following steps:

1) Adding petroleum ether into the salt-fried cortex Dictamni Radicis, reflux-extracting the salt-fried cortex Dictamni Radicis and petroleum ether at a feed liquid ratio of 1:10, filtering, and drying the residue to obtain dried residue;

2) Adding 90% ethanol solution into the dried residue, reflux-extracting for 2 times to extract monosaccharide and oligosaccharide, each time for 60min, vacuum-filtering, concentrating the filtrate under reduced pressure to obtain extract A (specific weight 1.25-1.30) at 80deg.C, and oven drying the residue to obtain residue;

3) Decocting the residue with water at a ratio of 1:10, extracting macromolecular polysaccharide component in a micro-pressure reaction kettle under 0.08MPa at 100deg.C for 60min, filtering to obtain filtrate A and residue A, concentrating filtrate A by membrane separation system with reverse osmosis membrane to 0.5 times of the original liquid, and adding Sevage reagent (chloroform: n-butanol=4: 1) Mixing the concentrated solution and Sevage reagent at a volume ratio of 5:1, oscillating, centrifuging, discarding the precipitate, adding 95% ethanol into the supernatant to make the ethanol concentration in the liquid medicine 80%, precipitating with ethanol, standing at 4deg.C for 24 hr, filtering to obtain filtrate B and residue B, washing the residue B with 95% ethanol solution for 2 times, and air drying to obtain cortex Dictamni Radicis polysaccharide; concentrating the filtrate B under reduced pressure to recover ethanol, concentrating under reduced pressure at 80deg.C, and concentrating to obtain extract B (specific weight 1.25-1.30); adding 50% ethanol solution into the filter residue A, reflux-extracting for 2 times to extract active substances such as flavone, mixing, filtering, concentrating under reduced pressure to recover ethanol, and concentrating the filtrate into extract C (specific gravity 1.25-1.30);

Example 2 ]

The composition for treating acne mainly comprises the following raw material components in parts by weight: 15g of cortex dictamni extract, 20g of cortex dictamni polysaccharide, 20g of fresh towel gourd juice, 2g of propylene glycol, 2g of laurocapram, 2g of glycerin, 3g of tween-80, 20g of hydroxypropyl-beta-cyclodextrin, 9g of sodium chloride, 12g of essence, 1g of sodium benzoate and 1000mL of water;

the method for stir-frying the cortex dictamni for extracting the cortex dictamni polysaccharide comprises the following steps of: stirring the cortex dictamni with saline water uniformly, and moistening the cortex dictamni, wherein the mass ratio of the cortex dictamni, the salt and the water is 150:5:20, and turning the cortex dictamni in the middle, and obtaining the moistening cortex dictamni after the saline water is absorbed completely; heating the stir-frying container, adding the steamed cortex Dictamni Radicis, stir-frying, taking out and drying after a large amount of white frost is attached to the surface of the medicinal materials, and obtaining the salt stir-fried cortex Dictamni Radicis at 90 ℃;

2) Adding 90% ethanol solution into the dried residue, reflux-extracting for 2 times at a ratio of 1:10 to ethanol solution of the dried residue for 60min each time, vacuum-concentrating the filtrate to obtain extract A (specific gravity of 1.25-1.30) at 80deg.C, and oven drying the residue to obtain residue A;

3) Decocting the residue A with water at a feed liquid ratio of 1:10, extracting in a micro-pressure reaction kettle under 0.08MPa at 100deg.C for 60min, filtering to obtain filtrate A and residue A, concentrating the filtrate A by membrane separation system with reverse osmosis membrane to 0.5 times of the original liquid volume, and adding Sevage reagent (chloroform: n-butanol=4: 1) Mixing the concentrated solution and Sevage reagent at a volume ratio of 5:1, oscillating, centrifuging, discarding the precipitate, adding 95% ethanol into the supernatant to make the ethanol concentration in the liquid medicine 70%, precipitating with ethanol, standing at 4deg.C for 24 hr, filtering to obtain filtrate B and residue B, washing the residue B with 95% ethanol solution for 2 times, and air drying to obtain cortex Dictamni Radicis polysaccharide; concentrating the filtrate B under reduced pressure to recover ethanol, concentrating under reduced pressure at 80deg.C, and concentrating to obtain extract B (specific weight 1.25-1.30); adding 50% ethanol solution into the filter residue A, reflux-extracting the filter residue A and the ethanol solution for 2 times at a ratio of 10 times, combining and filtering, concentrating under reduced pressure to recover ethanol, and concentrating the filtrate into extract C (specific gravity 1.25-1.30);

Example 3 ]

A method of preparing a spray for treating acne comprising the steps of:

step one, uniformly mixing 10g of dittany bark extract and 10g of fresh towel gourd juice to obtain solution A;

step two, adding 100mL of water into 9g of sodium chloride for dissolution and filtering to obtain solution B;

step three, adding 20g of hydroxypropyl-beta-cyclodextrin into 500mL of water for dissolution to obtain a solution C;

step four, adding the solution A into the solution C, stirring and dissolving, adding 1g of tween-80 and 1g of glycerol, and stirring uniformly to obtain solution D;

step five, adding 1g of propylene glycol and 1g of laurocapram while stirring the solution D, and uniformly stirring and mixing to obtain the solution E;

step six, adding the solution B, 1g of sodium benzoate and 10g of essence while stirring the solution E, adding 950mL of water, and sub-packaging and spraying the mixture into a bottle;

the method for stir-frying the cortex dictamni for extracting the cortex dictamni polysaccharide comprises the following steps of: stirring the cortex dictamni with saline water uniformly, and moistening the cortex dictamni, wherein the mass ratio of the cortex dictamni, the salt and the water is 100:2:10, and turning the cortex dictamni in the middle, and obtaining the moistening cortex dictamni after the saline water is absorbed completely; heating the stir-frying container, adding the steamed cortex Dictamni Radicis, stir-frying, taking out and drying after a large amount of white frost is attached to the surface of the medicinal materials, and obtaining the salt stir-fried cortex Dictamni Radicis at 90 ℃;

2) Adding 90% ethanol solution into the dried residue, reflux-extracting for 2 times at a ratio of 1:10 to ethanol solution of the dried residue for 60min each time, vacuum-concentrating the filtrate to obtain extract A (specific gravity of 1.25-1.30) at 80deg.C, and oven drying the residue to obtain residue;

3) Decocting the residue with water, extracting the residue A with water at a feed liquid ratio of 1:10 in a micro-pressure reaction kettle under the condition of 0.08MPa and 100 ℃ for 60min, filtering to obtain filtrate A and residue A, concentrating the filtrate A by membrane separation system with reverse osmosis membrane to 0.5 times of the volume of the original liquid medicine, and adding Sevage reagent (chloroform: n-butanol=4: 1) Mixing the concentrated solution and Sevage reagent at a volume ratio of 5:1, oscillating, centrifuging, discarding the precipitate, adding 95% ethanol into the supernatant to make the ethanol concentration in the liquid medicine 70%, precipitating with ethanol, standing at 4deg.C for 24 hr, filtering to obtain filtrate B and residue B, washing the residue B with 95% ethanol solution for 2 times, and air drying to obtain cortex Dictamni Radicis polysaccharide; concentrating the filtrate B under reduced pressure to recover ethanol, concentrating under reduced pressure at 80deg.C, and concentrating to obtain extract B (specific weight 1.25-1.30); adding 50% ethanol solution into the filter residue A, reflux-extracting the filter residue A and the ethanol solution for 2 times at a ratio of 10 times, combining and filtering, concentrating under reduced pressure to recover ethanol, and concentrating the filtrate into extract C (specific gravity 1.25-1.30);

Test one, comparing total polysaccharide content and extraction ratio of cortex Dictamni Radicis before and after processing by different processing methods

1.1 preparation of control solution and detection wavelength selection

Taking 2.5mg of anhydrous glucose reference substance, precisely weighing, placing into a 25mL measuring flask, adding a proper amount of water for dissolution, diluting to a scale, and shaking uniformly to obtain reference substance solution.

Precisely measuring 0.3mL of control solution in a test tube with a plug, adding water to supplement 1.0mL, adding 1mL of 80% phenol, shaking uniformly, rapidly adding 2.5mL of concentrated sulfuric acid, shaking uniformly, preserving heat in a water bath at 37 ℃ for 30min, taking out, cooling to room temperature, taking corresponding water as a blank, scanning the wavelength at 350-600nm by using an ultraviolet-visible spectrophotometer, measuring the maximum absorption wavelength, and displaying the maximum absorption wavelength as 491.12nm by the scanning result, wherein the result is shown in figure 1.

1.2 linear relationship investigation

Drawing standard curves, namely, drawing 0.10, 0.15, 0.20, 0.25, 0.30, 0.35 and 0.4mL of standard sample test solution in 7 dry test tubes, adding distilled water to make up to 1mL, and adding 1mL of distilled water as blank. 1mL of 80% phenol was added to each of the above 8 test tubes, and the mixture was shaken well and then 2.5mL of concentrated sulfuric acid was added rapidly, and after shaking well, the mixture was incubated in a water bath at 37℃for 30 minutes, the absorbance at 491nm was measured, and a glucose standard curve was drawn with the sugar mass mg as the abscissa and the absorbance at 491nm as the ordinate, as shown in Table 1, FIG. 2.

TABLE 1 Linear relationship test results

1.3 extraction of Dictamnus cortex Dictamni Total polysaccharide

The same batch of cortex Dictamni Radicis is divided into five parts, and is subjected to parching, salt parching, wine parching, and vinegar parching respectively, and is not processed as reference.

Parching: heating the stir-frying container, adding cortex Dictamni Radicis, stir-frying, taking out and oven-drying when the surface color of the medicinal materials is deepened, and oven-drying at 90deg.C to obtain the parched cortex Dictamni Radicis.

Parching with salt: stirring the cortex dictamni with saline water uniformly, and moistening the cortex dictamni, wherein the mass ratio of the cortex dictamni, the salt and the water is 100:1:10, and turning the cortex dictamni in the middle, and obtaining the moistening cortex dictamni after the saline water is absorbed completely; heating the stir-frying container, adding the steamed dittany bark, stir-frying, taking out and drying after the medicinal materials are nearly dry and the surface color is deepened and a large amount of white frost is attached on the surfaces of the medicinal materials, wherein the drying temperature is 90 ℃, and obtaining the salt stir-fried dittany bark.

Parching with wine: stirring the cortex dictamni with 95% alcohol solution uniformly, and stirring midway until the alcohol solution is absorbed completely to obtain the steamed cortex dictamni; heating the stir-frying container, adding the steamed cortex Dictamni Radicis, stir-frying, taking out and drying until the medicinal materials are nearly dry and the surface color is deepened, and obtaining the wine-fried cortex Dictamni Radicis at 90 ℃.

Parching with vinegar: stirring the raw cortex dictamni with an acetic acid solution uniformly, and stirring the raw cortex dictamni, acetic acid and water in a mass ratio of 100:1:10, and obtaining the steamed cortex dictamni after the acetic acid solution is absorbed completely; heating the stir-frying container, adding the steamed cortex Dictamni Radicis, stir-frying, taking out and drying until the medicinal materials are nearly dry and the surface color is deepened, and obtaining the vinegar-fried cortex Dictamni Radicis at 90 ℃.

Respectively weighing reference cortex Dictamni Radicis and processed cortex Dictamni Radicis, pulverizing into coarse powder (sieving with 10 mesh sieve), respectively weighing 500g according to the feed-liquid ratio of 1:10 Adding petroleum ether into (g/mL), reflux-extracting, filtering, and drying filter residue; decocting the dried residue with water for 2 times, adding 10 times of water (the water content is equivalent to the multiple of the weight of the medicinal materials), decocting for 1 hr each time, filtering with 200 mesh filter cloth, mixing filtrates, and adding Sevage reagent (chloroform: n-butanol=4:1) to the filtrate for 5:1 mixing, oscillating, centrifuging, discarding precipitate, adding 95% ethanol into supernatant to make ethanol concentration 80%, precipitating with ethanol, standing at 4deg.C for 24 hr, filtering, washing precipitate with 95% ethanol for 2 times, taking out, and air drying to obtain cortex Dictamni Radicis crude polysaccharide.

Crude polysaccharide extraction rate (%) =crude polysaccharide mass of cortex dictamni/mass of extracted medicinal material.

1.4 determination of Total polysaccharide content

Taking 10mg of each of the extracted crude polysaccharide of the dittany bark, precisely weighing, adding water for dissolution, transferring to a 50mL measuring flask, adding water for dilution to scale, shaking uniformly, precisely weighing 0.3mL, placing in a test tube with a plug, adding water to 1.0mL, adding 1mL of 80% phenol into the 8 test tubes respectively, shaking uniformly, rapidly adding 2.5mL of concentrated sulfuric acid, shaking uniformly, placing in a 37 ℃ water bath for heat preservation for 30min, measuring absorbance at 490nm, taking sugar mass mg as an abscissa, reading absorbance at 491nm, and reading the weight (mg) of glucose in a test solution from a standard curve according to the following formula:

total polysaccharide content (%) =total polysaccharide mass/cortex dictamni crude polysaccharide mass x 100%.

The calculation results are shown in table 2 below:

table 2 comparison of Dictamnus dasycarpus polysaccharide extraction rates before and after processing

From the results in Table 2, it is understood that the parching of the present invention is useful for improving the extraction rate of crude polysaccharide from cortex Dictamni Radicis and increasing the content of crude polysaccharide.

Test three, spray quality inspection

1. Thin layer chromatography inspection

The quality detection index components of limonin and phellodendron ketone are used as the quality detection index components of the spray, and the quality evaluation is carried out by using the two indexes, and the method comprises the following steps:

10mL of the product prepared in example 3 was extracted with ethyl acetate at a ratio of 1:1, concentrated to dryness under reduced pressure, and the residue was dissolved in 1mL of ethanol to prepare a sample solution. And respectively adding ethanol into limonin reference substance and phellodendron ketone reference substance to obtain solutions containing 1mg per 1mL, and taking the solutions as reference substance solutions. According to the test of thin layer chromatography (general rule 0502) of Chinese pharmacopoeia, 5-6 μl of each of the three solutions is sucked and respectively spotted on the same silica gel G thin layer plate, and the three solutions are unfolded, taken out and dried by taking n-hexane-ethyl acetate-methanol (1:1:1) as developing agents. Spraying 10% sulfuric acid ethanol vanillin test solution, and inspecting in sunlight. The spots of the same color appear on the sample chromatogram at the positions corresponding to the control chromatogram, and the results are shown in FIG. 3. In fig. 3, Z1, Z2, Z3, Z4, Z5, Z6 are different batches of products prepared by the method of example 3, B2 is a phellodendron ketone reference, and B3 is a limonin reference.

2. Liquid chromatography inspection

Taking 10mL of the product prepared in the example 3, adding the product into a pre-packed 200-300 mesh silica gel column, and using petroleum ether-acetone 2:1 eluting, discarding the eluent, eluting with petroleum ether-acetone 2:5, collecting the eluent, concentrating, drying, dissolving with methanol, and filtering with 0.45 μm microporous membrane to obtain sample solution.

Respectively, accurately weighing limonin reference substance and phellodendron ketone reference substance, adding methanol, and respectively preparing into 1mL standard reference substance solution containing 0.5 mg.

Chromatographic conditions: octadecyl bonded silica gel is used as a filler; acetonitrile is taken as a mobile phase A, a 0.1% phosphoric acid solution is taken as a mobile phase B, elution is carried out according to the gradient of the table, the detection wavelength is 210nm, the chromatographic column temperature is 30 ℃, and the theoretical plate number is calculated according to limonin peaks. The liquid chromatogram is shown in FIG. 4.

TABLE 3 mobile phase gradient setup

Time (minutes)	Mobile phase a (%)	Mobile phase B (%)
			0	8	92
27	100	0

Test III, effect test of products prepared by different methods

Comparative example 1: the process for preparing the product is the same as in example 3, except that no fresh luffa juice solution is present.

Comparative example 2: the process for preparing the product was the same as in example 3, except that the extract of dittany bark was not contained.

Comparative example 3: the process for the preparation of the product is the same as in example 3, except that the polysaccharide from dittany bark is absent.

Comparative example 4: the preparation method of the product is the same as in example 3, except that the salt stir-fried dittany bark is subjected to reflux extraction treatment by untreated petroleum ether.

1. Clinical data

Patients with grade 2 (moderate) acne were 45 persons aged 13-18 years, randomized equally divided into five groups, group a, group B, group C, group D and group E, respectively.

Wherein, group A uses the product prepared by comparative example 1, group B uses the product prepared by comparative example 2, group C uses the product prepared by comparative example 3, group D uses the product of comparative example 4, group E uses the product prepared by example 3, take 1 month as a course of treatment, take a follow-up diagnosis every two weeks each time in the morning and evening, add and subtract the dosage, take two courses of treatment, and the treatment effect evaluation is carried out after stopping the medication for 20 days.

All patients were volunteer subjects who had not taken antibiotics or other systemic treatment for acne for 4 weeks prior to treatment.

Notice that: all patients are washed by clear water before using the medicines each time, grease on the skin surface is removed, the medicines are sprayed on hands, then the medicines are coated on the application parts, and in the treatment course, the patients are fasted by high sugar, high fat, wine, spicy and other pungent foods, and eat more long fiber foods such as green vegetables and fruits.

2. Judgment standard:

the treatment course was determined by the skin lesion improvement degree = (number of skin lesions before treatment-number of skin lesions after treatment)/number of skin lesions before treatment 100%, and divided into the following four grades:

and (3) curing: the total skin loss after healing is reduced by more than or equal to 90 percent;

the effect is shown: the total skin loss is reduced by 60-89% after treatment;

the method is effective: the total skin loss is reduced by 20-59% after treatment;

invalidation: the total skin loss is reduced by less than 20% after treatment, or the reverse is increased.

3. Efficacy evaluation is shown in table 4.

Table 4 efficacy assessment

As can be seen from Table 5, the fresh luffa juice, the extract of dittany bark and the polysaccharide of dittany bark of the present invention act together. The effect of the group D is inferior to that of the group E, and the possible reason is that petroleum ether is utilized to remove substances with small molecular polarity such as fat, tannin and the like in the cortex dictamni, so that the extracted components are fully contacted with the extraction solvent in the subsequent extraction process, the extraction rate of the effective components is increased, and the effect of enhancing the curative effect is achieved.

Test four, different crowd effect test

1. Clinical data

Grade 2 (moderate) acne patients 18 persons, aged 13-18 years, were randomized equally divided into two groups, trial 1-1, and trial 1-2, respectively.

Patients with grade 3 (moderate) acne 28, aged 15-20 years, were randomized equally divided into two groups, trial 2-1, and trial 2-2, respectively.

Grade 4 (severe) acne patients 42 persons, aged 15-25 years, were randomized equally divided into two groups, trial 3-1, and trial 3-2, respectively.

Wherein, experiments 1-1, experiments 2-1 and experiments 3-1 take 1 month as a treatment course, the product prepared in example 3 is used for three times a day in the morning, in the evening, and is subjected to repeated diagnosis every two weeks, the dosage is increased and decreased along with symptoms, and after one treatment course is finished, the treatment effect evaluation is carried out after stopping the medicine for 20 days.

The experiment 1-2, experiment 2-2 and experiment 3-2 take 1 month as a treatment course, the product is prepared in example 2 every morning and evening, the treatment dosage is increased and decreased according to symptoms once every two weeks, the treatment course is two treatment courses, and the treatment effect evaluation is carried out after stopping the medicine for 20 days.

2. Judgment standard: the treatment course was determined by the skin lesion improvement degree = (number of skin lesions before treatment-number of skin lesions after treatment)/number of skin lesions before treatment 100%, and divided into the following four grades:

the effect is shown: the total skin loss is reduced by 60-89% after treatment;

3. Efficacy evaluation is shown in table 5.

Table 5 efficacy assessment

As can be seen from table 1, the treatment for patients with moderate acne all reached a significant outcome, and the treatment for patients with severe acne reached a significant outcome, and 1 case of failure occurred, mainly because the patients failed to fit well with the experimental plan during the treatment period, interrupting the treatment.

4. Typical cases

Huang Mou, male, 23 years old, the face of the patient begins to develop acne 4 years ago, once in need of treatment with a plurality of hospitals, although the disease conditions can be controlled after the medicine is taken, the acne recurs immediately after the medicine is stopped, and the symptoms tend to be more serious: the treatment method is used for treating the patients with 4-level (severe) acne by diagnosing a large number of papules, pustules and nodules on cheeks, forehead, nose bridges and chin, taking 2 months as a treatment course, carrying out repeated diagnosis once every two weeks in the morning, in the evening, adding and subtracting the dosage along with symptoms, wherein no acne is newly added in the first repeated diagnosis, the original acne nodules become soft, the color is diluted, no acne is newly added in the second repeated diagnosis, the characteristics of the acne nodules are further lightened, the protruding nodules and pimples are basically disappeared after one treatment course is ended, the repeated diagnosis is carried out once every two weeks, the dosage along with symptoms is added and subtracted once again after the treatment course is ended, the healing effect is achieved, and the acne marks and the scars on the face are little and are basically not seen.

Song Mou the female, 24 years old, the patient had a red pimple and a pimple on the face 1 year ago, the symptoms were not heavy, the patient had been squeezed by his own hands, the symptoms were aggravated, and the symptoms: the medicine is used for diagnosing 3-grade (moderate) acne patients with acnes and a large number of inflammatory papules and pustules at the cheek and forehead, is re-diagnosed every two weeks in the morning and evening, and is added or subtracted with the dosage, and the medicine is required to be applied to patients after one treatment course is ended, and is required to be re-diagnosed every two weeks only once a day, and is added or subtracted with the dosage, so that the healing effect is achieved after the other treatment course is ended.

Although embodiments of the present invention have been disclosed above, it is not limited to the details and embodiments shown and described, it is well suited to various fields of use for which the invention would be readily apparent to those skilled in the art, and accordingly, the invention is not limited to the specific details and illustrations shown and described herein, without departing from the general concepts defined in the claims and their equivalents.

Claims

1. The composition for treating acne is characterized by being prepared from the following raw material components in parts by weight: 10-15 parts of cortex dictamni extract, 5-20 parts of cortex dictamni polysaccharide, 10-20 parts of fresh luffa juice, 1-2 parts of propylene glycol, 1-2 parts of laurocapram, 1-2 parts of glycerol, 1-3 parts of tween-80, 10-20 parts of hydroxypropyl-beta-cyclodextrin, 5-9 parts of sodium chloride, 7-12 parts of essence, 0.5-1 part of sodium benzoate and 900-1000 parts of water;

the cortex Dictamni Radicis used for extracting cortex Dictamni Radicis polysaccharide is processed by one of parching, salt parching, vinegar parching or wine parching;

3) Decocting the residue with water, extracting in a micro-pressure reaction kettle, and filtering to obtain filtrate A and residue A; concentrating filtrate A, adding Sevage reagent into the concentrated solution, mixing, oscillating, centrifuging, discarding precipitate, adding ethanol into supernatant for ethanol precipitation, standing, filtering to obtain filtrate B and residue B, washing residue B with ethanol solution, and air drying to obtain cortex Dictamni Radicis polysaccharide; concentrating the filtrate B into extract to obtain extract B; adding ethanol solution into the filter residue A for reflux extraction, filtering, and concentrating the filtrate into extract to obtain extract C;

2. The composition for treating acne according to claim 1, wherein the fresh luffa juice is prepared by collecting fresh luffa, washing, squeezing with a juicer to obtain luffa juice, filtering to remove residue, removing color, and purifying by MCI column chromatography.

3. The composition for treating acne according to claim 1, wherein the salt-stir-frying method of the dittany bark comprises the following steps:

stirring the cortex dictamni with saline water uniformly, and moistening the cortex dictamni, wherein the mass ratio of the cortex dictamni, the salt and the water is 100-150:1-5:10-20, and stirring the mixture in the middle until the saline water is absorbed completely to obtain the moistening cortex dictamni;

heating the stir-frying container, adding the steamed cortex Dictamni Radicis, stir-frying, taking out, oven drying at 60-95deg.C after a large amount of white frost is adhered to the surface of the medicinal materials, and parching with salt to obtain the processed cortex Dictamni Radicis.

4. The composition for treating acne according to claim 1, wherein in step 1), the ratio of the salt-fried dittany bark to petroleum ether is 1-5:10-20.

5. The composition for treating acne according to claim 1, wherein in step 2), the ratio of the dry filter residue to the ethanol solution is 1-5:10-20, the volume concentration of the ethanol solution is 80% -90%, and the reflux extraction is performed for 2-3 times, each time for 50-100min.

6. The composition for treating acne according to claim 1, wherein in step 3), the ratio of the liquid to the residue a to water is 1-5:10-20, the extraction pressure in the micro-pressure reaction kettle is 0.05-0.1MPa, the temperature is 90-100 ℃, and the decoction time is 50-100min.

7. Use of a composition for treating acne according to any one of claims 1-6 in the manufacture of a medicament for treating acne.