CN111956731A - Traditional Chinese medicine composition with anti-allergic effect and preparation method thereof - Google Patents
Traditional Chinese medicine composition with anti-allergic effect and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a traditional Chinese medicine composition with an antiallergic effect and a preparation method thereof, wherein the traditional Chinese medicine composition comprises a first extracting solution, a second extracting solution, a third extracting solution, a fourth extracting solution, a surfactant and an auxiliary agent, wherein the first extracting solution is prepared from cortex dictamni, anhydrous pyridine, lecithin and other components, the cortex dictamni is dry root bark of dictamnus dasycarpus of Rutaceae and contains rich components such as polysaccharide, alkaloid, flavone and the like, and the traditional Chinese medicine composition has the effects of clearing heat, drying dampness, dispelling wind, detoxifying and removing damp-heat sore toxin, can be used for skin diseases such as skin pruritus, urticaria and eczema, and has strong antiallergic and antipruritic effects. The invention discloses a traditional Chinese medicine composition with an anti-allergic effect and a preparation method thereof, the process design is reasonable, the formula components are adaptive, the prepared traditional Chinese medicine composition has excellent antibacterial and anti-inflammatory effects, can treat allergic symptoms such as eczema and atopic dermatitis on the surface of skin, has long-term stability, and reduces the medicine loss.
Description
Technical Field
The invention relates to the technical field of traditional Chinese medicines, in particular to a traditional Chinese medicine composition with an anti-allergic effect and a preparation method thereof.
Background
Eczema is a skin inflammatory reaction with severe pruritus caused by various internal and external factors and is one of the most common skin allergy symptoms, and can be divided into an acute stage, a subacute stage and a chronic stage, wherein the acute stage has exudation tendency, and the chronic stage is infiltration and hypertrophy. Some patients directly show chronic eczema, and the eczema has the characteristics of polymorphism, symmetry, pruritus, easy repeated attack and the like.
Nowadays, with the progress and development of science and technology, skin eczema becomes a problem which is gradually paid attention to by people, but the formula of the medicine which can relieve symptoms such as eczema, atopic dermatitis, and the like is complex, the preparation process is complicated, the medicine contains natural plant extract, the component has poor stability and low solubility, and the treatment effect cannot meet the requirements of people.
Aiming at the problem, a traditional Chinese medicine composition with an anti-allergic effect and a preparation method thereof are designed, which are one of the technical problems to be solved urgently.
Disclosure of Invention
The invention aims to provide a traditional Chinese medicine composition with an anti-allergic effect and a preparation method thereof, and aims to solve the problems in the prior art.
In order to achieve the purpose, the invention provides the following technical scheme:
a traditional Chinese medicine composition with an anti-allergic effect comprises the following raw materials: 5-15 parts of first extracting solution, 8-16 parts of second extracting solution, 8-14 parts of third extracting solution, 10-12 parts of fourth extracting solution, 15-25 parts of surfactant and 6-10 parts of auxiliary agent.
According to an optimized scheme, the raw materials of each component of the first extracting solution comprise: by weight, 10-15 parts of cortex dictamni, 4-8 parts of anhydrous pyridine, 2-3 parts of chlorosulfonic acid, 4-6 parts of lecithin, 4-6 parts of cholesterol, 6-8 parts of N, N-dimethylformamide, 10-12 parts of 1, 2-propylene glycol and 5-9 parts of phosphate buffer solution.
According to an optimized scheme, the second extracting solution is prepared from cortex moutan, sulfur trioxide and distilled water.
According to an optimized scheme, the third extracting solution is prepared from onion, 1-butyl-3-methyl-imidazole hexafluorophosphate and alliinase solution.
According to an optimized scheme, the fourth extracting solution comprises the following raw materials: by weight, 15-25 parts of fructus aurantii, 10-20 parts of radix puerariae and 10-20 parts of artemisia capillaris.
According to an optimized scheme, the surfactant is a mixed solution of tween 40, tween 60 and tween 80, and the mass ratio of tween 40 to tween 60 to tween 80 is 1: 1: 1.
in an optimized scheme, the auxiliary agent is one or a mixture of 1, 2-propylene glycol, glycerol and polyethylene glycol.
According to a more optimized scheme, the preparation method of the traditional Chinese medicine composition with the anti-allergic effect comprises the following steps:
1) preparing materials;
2) preparing a first extracting solution: preparing a first extracting solution from cortex dictamni, anhydrous pyridine, chlorosulfonic acid, lecithin, cholesterol, N-dimethylformamide, 1, 2-propylene glycol and a phosphate buffer solution;
3) preparing a second extracting solution: extracting cortex moutan to obtain a second extractive solution;
4) preparing a third extracting solution: taking onion, 1-butyl-3-methyl-imidazole hexafluorophosphate and alliinase solution to prepare a third extracting solution;
5) preparing a fourth extracting solution: preparing a fourth extracting solution from fructus aurantii, radix puerariae and artemisia capillaries;
6) and (3) taking a surfactant, an auxiliary agent, a first extracting solution, a second extracting solution, a third extracting solution and a fourth extracting solution to prepare the traditional Chinese medicine composition.
The optimized scheme comprises the following steps:
1) preparing materials;
2) preparing a first extracting solution:
a) adding chlorosulfonic acid into anhydrous pyridine in an ice-water bath to obtain a material A; mixing lecithin and cholesterol, stirring, and adding absolute ethyl alcohol to dissolve to obtain a material B;
b) pulverizing cortex Dictamni Radicis, extracting with 90% ethanol under reflux, filtering, drying in the shade, extracting with water under reflux for 2-3 times, filtering, mixing filtrates, adding N, N-dimethylformamide, stirring, adding material A, stirring at 60-65 deg.C for reaction, cooling to room temperature, adjusting pH, precipitating with ethanol, centrifuging, filtering, and dialyzing to obtain a mixed solution;
c) mixing the mixed solution and 1, 2-propylene glycol, stirring, dissolving phosphate buffer solution, adding material B, performing ultrasonic treatment, placing in water bath at 40-45 deg.C, performing rotary evaporation under reduced pressure to form a membrane layer, adding phosphate buffer solution, performing ultrasonic treatment in ice water bath, and filtering with 0.22um microporous membrane to obtain first extractive solution;
3) preparing a second extracting solution: taking cortex moutan, placing the cortex moutan in an incubator at 72-75 ℃, transversely shearing the cortex moutan into small sections of 1-2cm, longitudinally splitting the cortex moutan to obtain crushed materials, placing the crushed materials in a reaction tank, treating the crushed materials for 1-1.2 hours in a sulfur trioxide gas environment at the temperature of 60-62 ℃, crushing and sieving the crushed materials after treatment, soaking the crushed materials in distilled water, distilling the materials by steam at the temperature of 100 ℃ and 105 ℃, extracting, standing overnight, and passing through a 0.45um microporous membrane to obtain a second extracting solution;
4) preparing a third extracting solution: mixing herba Alii Fistulosi and 1-butyl-3-methyl-imidazole hexafluorophosphate, stirring, performing ultrasonic treatment for 8-10min, placing in 40-45 deg.C water bath, adding alliinase solution, standing, slowly heating to 50-52 deg.C, and distilling under reduced pressure to obtain a third extractive solution;
5) preparing a fourth extracting solution:
a) cleaning fructus Aurantii, drying, pulverizing, sieving, soaking in distilled water for 30-60min, reflux extracting, and filtering to obtain filtrate C;
b) mixing herba Artemisiae Scopariae and radix Puerariae under stirring, soaking in 70% ethanol solution for 24-28 hr, and extracting with ethanol for 2-4 hr to obtain extractive solution D;
c) mixing and stirring the filtrate C and the extracting solution D to obtain a fourth extracting solution;
6) mixing and stirring a surfactant and an auxiliary agent, adding the third extracting solution and the fourth extracting solution, uniformly mixing in a water bath at 40-45 ℃, adding the first extracting solution and the second extracting solution, continuously stirring, slowly dropwise adding deionized water, stirring and dispersing to obtain the traditional Chinese medicine composition.
The optimized scheme comprises the following steps:
1) preparing materials;
2) preparing a first extracting solution:
a) adding chlorosulfonic acid into anhydrous pyridine in an ice-water bath to obtain a material A; mixing lecithin and cholesterol, stirring for 5-8min, and dissolving in anhydrous ethanol to obtain material B;
b) taking cortex dictamni, crushing, performing reflux extraction with 90% ethanol, filtering, drying in the shade, performing reflux extraction with water for 2-3 times, filtering, combining filtrates, adding N, N-dimethylformamide, stirring for 10-15min, adding material A, stirring and reacting at 60-65 ℃ for 3-3.5h, cooling to room temperature, adjusting pH to 7, precipitating with ethanol for 24-28h, performing centrifugal filtration, and dialyzing for 72h to obtain a mixed solution;
c) mixing the mixed solution and 1, 2-propylene glycol, stirring, dissolving phosphate buffer solution, adding material B, performing ultrasonic treatment for 30-50s, placing in water bath at 40-45 deg.C, performing rotary evaporation under reduced pressure to form a film layer, adding phosphate buffer solution, performing ultrasonic treatment for 30-40s in ice water bath, and filtering with 0.22um microporous membrane to obtain first extractive solution;
3) preparing a second extracting solution: taking cortex moutan, placing the cortex moutan in an incubator at 72-75 ℃ for standing for 12-18h, transversely shearing into small segments of 1-2cm, longitudinally splitting to obtain crushed materials, placing the crushed materials in a reaction tank, treating for 1-1.2h at the temperature of 60-62 ℃ in the environment of sulfur trioxide gas, crushing and sieving after treatment, placing in distilled water for soaking for 3-4h, distilling with steam at the temperature of 100 ℃ and 105 ℃, extracting for 1-1.5h, standing overnight, and passing through a 0.45um microporous membrane to obtain a second extracting solution;
4) preparing a third extracting solution: mixing and stirring onion and 1-butyl-3-methyl-imidazole hexafluorophosphate for 10-12min, then carrying out ultrasonic treatment for 8-10min under the ultrasonic power of 100-110w, then carrying out ultrasonic treatment, then placing in a water bath at the temperature of 40-45 ℃, adding alliinase solution, placing for 1-1.2h, then slowly heating to the temperature of 50-52 ℃, and carrying out reduced pressure distillation for 1.5-2h to obtain a third extracting solution;
5) preparing a fourth extracting solution:
a) cleaning fructus Aurantii, drying, pulverizing, sieving with 20 mesh sieve, soaking in distilled water for 30-60min, reflux extracting for 2-3 times, each for 4-5 hr, and filtering to obtain filtrate C;
b) mixing herba Artemisiae Scopariae and radix Puerariae under stirring for 10-20min, soaking in 70% ethanol solution for 24-28 hr, and extracting with ethanol at 50-70 deg.C for 2-4 hr to obtain extractive solution D;
c) mixing and stirring the filtrate C and the extracting solution D to obtain a fourth extracting solution;
6) mixing and stirring a surfactant and an auxiliary agent for 12-15min, adding a third extracting solution and a fourth extracting solution, uniformly mixing under the water bath condition of 40-45 ℃, adding a first extracting solution and a second extracting solution, continuously stirring for 20-30min, slowly dropwise adding deionized water, and dispersing at the rotating speed of 10000-11000r/min for 10-15min to obtain the traditional Chinese medicine composition.
Compared with the prior art, the invention has the beneficial effects that:
the invention discloses a traditional Chinese medicine composition with an antiallergic effect and a preparation method thereof, wherein the traditional Chinese medicine composition comprises a first extracting solution, a second extracting solution, a third extracting solution, a surfactant and an auxiliary agent, wherein the first extracting solution is prepared from cortex dictamni, anhydrous pyridine, lecithin and other components, the cortex dictamni is dry root bark of cortex dictamni of Rutaceae plants, contains rich components such as polysaccharide, alkaloid, flavone and steroid compounds, has the effects of clearing heat and drying dampness, dispelling wind and removing toxicity and treating damp-heat sore toxicity, can be used for skin diseases such as skin pruritus, urticaria and eczema, and has strong antiallergic and itching relieving effects.
When the preparation method is used, the dittany bark is firstly extracted by ethanol to obtain an extracting solution, and the extracting solution contains dictamnine, dittany polysaccharide and other components. Because the solubility of the dictamnus polysaccharide is poor and the bioactivity is low, the dictamnus polysaccharide is subjected to sulfation structural modification by adopting the components such as N, N-dimethylformamide, anhydrous pyridine and the like, so that the bioactivity of the dictamnus polysaccharide in the extracting solution is improved, and after the dictamnus polysaccharide is subjected to sulfation, the connection mode of sugar chains is optimized, so that the water solubility and bioactivity of the dictamnus polysaccharide can be improved, and the use effect of the dictamnus polysaccharide is improved; meanwhile, the extract is embedded by cholesterol and lecithin, so that the stability of the dictamnine component is improved, the long-acting slow-release effect of the medicament can be realized, and the using effect is more excellent.
The second extracting solution is prepared from cortex moutan, sulfur trioxide and distilled water, the cortex moutan is cortex moutan, the main effective component of the cortex moutan is paeonol, and the paeonol has excellent anti-inflammatory, antipyretic, antioxidant and antibacterial effects and can effectively inhibit the growth of fungi so as to treat diseases such as skin pruritus, eczema and the like; when the second extracting solution is prepared, the normal-pressure sulfur trioxide micro-thermal explosion technology is adopted for pretreatment, so that the yield and the purity of paeonol extracted by steam distillation are greatly improved, and the extracting solution is extracted by combining the steam distillation extracting technology to obtain the second extracting solution with excellent antibacterial property.
The third extract component of the invention comprises onion, 1-butyl-3-methyl-imidazole hexafluorophosphate and alliinase solution, the main bioactive component of the onion is a sulfur-containing compound, and thiosulfinate is used as the main component, and the invention has the pharmacological actions of antibiosis, antiphlogosis and antioxidation.
The fourth extracting solution of the invention comprises bitter orange, kudzu root and artemisia capillaris thumb, wherein the bitter orange is bitter, pungent and sour in taste and warm in nature; it has effects in invigorating spleen and stomach channels, and contains flavonoids, volatile oils, alkaloids, and saccharides; herba Artemisiae Scopariae, have effects of mainly rheumatism, chills and fever, pathogenic qi hot junction, yellow gallbladder, etc., herba Artemisiae Scopariae contains a large amount of coumarin, chromone, flavone, etc. ingredient, have pharmacological effects such as relieving fever, relieving pain, diminishing inflammation, etc.; the kudzu root mainly contains isoflavone compounds, such as alkaloid, coumarin and the like, and has pharmacological effects of resisting inflammation, resisting oxidation and the like; the fourth extracting solution is prepared by compatibility of the components such as the bitter orange, the artemisia capillaries, the kudzuvine root and the like, and has excellent pharmacological action on skin allergy symptoms such as skin eczema, atopic dermatitis and the like.
When the preparation method is used, the first extracting solution, the second extracting solution, the third extracting solution and the fourth extracting solution are embedded by using the surfactant and the auxiliary agent, so that the stability of each component can be effectively improved, the water solubility of each component is improved, and the absorption utilization rate of each component is further improved.
The invention discloses a traditional Chinese medicine composition with an anti-allergic effect and a preparation method thereof, the process design is reasonable, the formula components are adaptive, the prepared traditional Chinese medicine composition has excellent antibacterial and anti-inflammatory effects, can treat skin allergy symptoms such as eczema and atopic dermatitis on the surface of skin, has long-term stability, reduces medicine loss, improves the medicine absorption utilization rate, and has excellent practical effect.
Detailed Description
The technical solutions in the examples of the present invention will be described clearly and completely below, and it is obvious that the described examples are only a part of examples of the present invention, but not all examples. All other examples, which can be obtained by a person skilled in the art without making any creative effort based on the examples in the present invention, belong to the protection scope of the present invention.
Example 1:
s1: preparing materials;
s2: preparing a first extracting solution:
adding chlorosulfonic acid into anhydrous pyridine in an ice-water bath to obtain a material A; mixing lecithin and cholesterol, stirring for 5min, and dissolving with anhydrous ethanol to obtain material B;
crushing cortex dictamni, performing reflux extraction by 90% ethanol, filtering, performing reflux extraction by water for 2 times after drying in the shade, filtering, combining filtrates, adding N, N-dimethylformamide, stirring for 10min, adding the material A, stirring and reacting for 3h at 60 ℃, cooling to room temperature, adjusting the pH to 7, performing ethanol precipitation for 24h, performing centrifugal filtration, and dialyzing for 72h to obtain a mixed solution;
mixing the mixed solution and 1, 2-propylene glycol, stirring, dissolving phosphate buffer solution, adding material B, performing ultrasonic treatment for 30s, placing in water bath at 40 ℃, performing rotary evaporation under reduced pressure to form a film layer, adding phosphate buffer solution, performing ultrasonic treatment for 30s in ice water bath, and filtering with 0.22um microporous filter membrane to obtain a first extract;
s3: preparing a second extracting solution: taking cortex moutan, placing the cortex moutan in an incubator at 72 ℃ for standing for 12h, transversely shearing the cortex moutan into small segments of 1cm, longitudinally splitting the cortex moutan to obtain crushed materials, placing the crushed materials in a reaction tank, treating the crushed materials for 1h in a sulfur trioxide gas environment at the temperature of 60 ℃, crushing and sieving the crushed materials after treatment, placing the crushed materials in distilled water for soaking for 3h, carrying out steam distillation at the temperature of 100 ℃, extracting for 1h, standing overnight, and passing through a 0.45um microporous membrane to obtain a second extracting solution;
s4: preparing a third extracting solution: mixing and stirring onion and 1-butyl-3-methyl-imidazole hexafluorophosphate for 10min, performing ultrasonic treatment for 8min under 100w of ultrasonic power, performing ultrasonic treatment, adding alliinase solution in water bath at 40 ℃, standing for 1h, slowly heating to 50 ℃, and performing reduced pressure distillation for 1.5h to obtain a third extracting solution;
s5: preparing a fourth extracting solution:
cleaning fructus Aurantii, drying, pulverizing, sieving with 20 mesh sieve, soaking in distilled water for 30min, reflux extracting for 2 times, each for 4 hr, and filtering to obtain filtrate C;
mixing herba Artemisiae Scopariae and radix Puerariae under stirring for 10min, soaking in 70% ethanol solution for 24 hr, and extracting with ethanol at 50 deg.C for 2 hr to obtain extractive solution D;
mixing and stirring the filtrate C and the extracting solution D to obtain a fourth extracting solution;
s6: mixing and stirring surfactant and auxiliary agent for 12min, adding the third extract and the fourth extract, uniformly mixing in a water bath at 40 ℃, adding the first extract and the second extract, continuously stirring for 20min, slowly dropwise adding deionized water, and dispersing at the rotating speed of 10000r/min for 10min to obtain the traditional Chinese medicine composition.
In this example, the raw materials of each component of the traditional Chinese medicine composition include: the detergent comprises, by weight, 5 parts of a first extracting solution, 8 parts of a second extracting solution, 8 parts of a third extracting solution, 10 parts of a fourth extracting solution, 15 parts of a surfactant and 6 parts of an auxiliary agent.
Wherein the first extracting solution comprises the following raw materials: according to weight, 10 parts of cortex dictamni, 4 parts of anhydrous pyridine, 2 parts of chlorosulfonic acid, 4 parts of lecithin, 4 parts of cholesterol, 6 parts of N, N-dimethylformamide, 10 parts of 1, 2-propylene glycol and 5 parts of phosphate buffer solution.
The fourth extracting solution comprises the following raw materials: by weight, 15 parts of fructus aurantii, 10 parts of radix puerariae and 10 parts of artemisia capillaris.
The surfactant is a mixed solution of tween 40, tween 60 and tween 80, and the mass ratio of tween 40 to tween 60 to tween 80 is 1: 1: 1. the auxiliary agent is 1, 2-propylene glycol.
Example 2:
s1: preparing materials;
s2: preparing a first extracting solution:
adding chlorosulfonic acid into anhydrous pyridine in an ice-water bath to obtain a material A; mixing lecithin and cholesterol, stirring for 7min, and dissolving in anhydrous ethanol to obtain material B;
crushing cortex dictamni, performing reflux extraction by 90% ethanol, filtering, performing reflux extraction by water for 3 times after drying in the shade, filtering, combining filtrate, adding N, N-dimethylformamide, stirring for 12min, adding the material A, stirring and reacting for 3.2h at 63 ℃, cooling to room temperature, adjusting the pH to 7, performing ethanol precipitation for 26h, performing centrifugal filtration, and dialyzing for 72h to obtain a mixed solution;
mixing the mixed solution and 1, 2-propylene glycol, stirring, dissolving phosphate buffer solution, adding material B, performing ultrasonic treatment for 40s, placing in water bath at 43 ℃, performing rotary evaporation under reduced pressure to form a film layer, adding phosphate buffer solution, performing ultrasonic treatment for 35s in ice water bath, and filtering with 0.22um microporous filter membrane to obtain a first extract;
s3: preparing a second extracting solution: taking cortex moutan, placing in an incubator at 74 ℃ for standing for 15h, transversely shearing into small segments of 2cm, longitudinally splitting to obtain crushed materials, placing the crushed materials in a reaction tank, treating for 1.1h in a sulfur trioxide gas environment at 61 ℃, crushing and sieving after treatment, placing in distilled water for soaking for 3.5h, carrying out steam distillation at 103 ℃ for extracting for 1.3h, standing overnight, and passing through a 0.45-micrometer microporous membrane to obtain a second extracting solution;
s4: preparing a third extracting solution: mixing and stirring onion and 1-butyl-3-methyl-imidazole hexafluorophosphate for 11min, performing ultrasound treatment at 105w ultrasound power for 9min, performing ultrasound treatment, adding alliinase solution in water bath at 43 ℃, standing for 1.1h, slowly heating to 51 ℃, and performing reduced pressure distillation for 1.8h to obtain a third extract;
s5: preparing a fourth extracting solution:
cleaning fructus Aurantii, drying, pulverizing, sieving with 20 mesh sieve, soaking in distilled water for 45min, reflux extracting for 2 times, each for 4.5 hr, and filtering to obtain filtrate C;
mixing herba Artemisiae Scopariae and radix Puerariae under stirring for 15min, soaking in 70% ethanol solution for 26 hr, and extracting with ethanol for 3 hr at 60 deg.C to obtain extractive solution D;
mixing and stirring the filtrate C and the extracting solution D to obtain a fourth extracting solution;
s6: mixing and stirring surfactant and auxiliary agent for 14min, adding the third extract and the fourth extract, uniformly mixing in a water bath at 42 ℃, adding the first extract and the second extract, continuously stirring for 25min, slowly dropwise adding deionized water, and dispersing at the rotating speed of 10500r/min for 13min to obtain the traditional Chinese medicine composition.
In this example, the raw materials of each component of the traditional Chinese medicine composition include: the detergent comprises, by weight, 10 parts of a first extracting solution, 12 parts of a second extracting solution, 12 parts of a third extracting solution, 11 parts of a fourth extracting solution, 20 parts of a surfactant and 8 parts of an auxiliary agent.
Wherein the first extracting solution comprises the following raw materials: by weight, 13 parts of cortex dictamni, 6 parts of anhydrous pyridine, 2.5 parts of chlorosulfonic acid, 5 parts of lecithin, 5 parts of cholesterol, 7 parts of N, N-dimethylformamide, 11 parts of 1, 2-propylene glycol and 8 parts of phosphate buffer solution.
The fourth extracting solution comprises the following raw materials: by weight, 20 parts of fructus aurantii, 15 parts of radix puerariae and 15 parts of artemisia capillaris.
The surfactant is a mixed solution of tween 40, tween 60 and tween 80, and the mass ratio of tween 40 to tween 60 to tween 80 is 1: 1: 1. the auxiliary agent is glycerol.
Example 3:
s1: preparing materials;
s2: preparing a first extracting solution:
adding chlorosulfonic acid into anhydrous pyridine in an ice-water bath to obtain a material A; mixing lecithin and cholesterol, stirring for 8min, and dissolving with anhydrous ethanol to obtain material B;
crushing cortex dictamni, performing reflux extraction by 90% ethanol, filtering, performing reflux extraction by water for 3 times after drying in the shade, filtering, combining filtrate, adding N, N-dimethylformamide, stirring for 15min, adding the material A, stirring and reacting for 3.5h at 65 ℃, cooling to room temperature, adjusting the pH to 7, performing ethanol precipitation for 28h, performing centrifugal filtration, and dialyzing for 72h to obtain a mixed solution;
mixing the mixed solution and 1, 2-propylene glycol, stirring, dissolving phosphate buffer solution, adding material B, performing ultrasonic treatment for 50s, placing in water bath at 45 ℃, performing rotary evaporation under reduced pressure to form a film layer, adding phosphate buffer solution, performing ultrasonic treatment for 40s in ice water bath, and filtering with 0.22um microporous filter membrane to obtain a first extract;
s3: preparing a second extracting solution: taking cortex moutan, placing in an incubator at 75 ℃ for standing for 18h, transversely shearing into small segments of 2cm, longitudinally splitting to obtain crushed materials, placing the crushed materials in a reaction tank, treating for 1.2h in a sulfur trioxide gas environment at the temperature of 62 ℃, crushing and sieving after treatment, placing in distilled water for soaking for 4h, carrying out steam distillation at 105 ℃ to extract for 1.5h, standing overnight, and passing through a 0.45-micrometer microporous membrane to obtain a second extracting solution;
s4: preparing a third extracting solution: mixing and stirring onion and 1-butyl-3-methyl-imidazole hexafluorophosphate for 12min, performing ultrasound treatment for 10min under 110w of ultrasound power, placing in a water bath at 45 ℃ after the ultrasound treatment, adding alliinase solution, placing for 1.2h, slowly heating to 52 ℃, and performing reduced pressure distillation for 2h to obtain a third extracting solution;
s5: preparing a fourth extracting solution:
cleaning fructus Aurantii, drying, pulverizing, sieving with 20 mesh sieve, soaking in distilled water for 60min, reflux extracting for 3 times, each for 5 hr, and filtering to obtain filtrate C;
mixing herba Artemisiae Scopariae and radix Puerariae under stirring for 20min, soaking in 70% ethanol solution for 28 hr, and extracting with ethanol for 4 hr at 70 deg.C to obtain extractive solution D;
mixing and stirring the filtrate C and the extracting solution D to obtain a fourth extracting solution;
s6: mixing and stirring a surfactant and an auxiliary agent for 15min, adding a third extracting solution and a fourth extracting solution, uniformly mixing in a water bath at 45 ℃, adding a first extracting solution and a second extracting solution, continuously stirring for 30min, slowly dropwise adding deionized water, and dispersing at the rotating speed of 11000r/min for 15min to obtain the traditional Chinese medicine composition.
In this example, the raw materials of each component of the traditional Chinese medicine composition include: the detergent comprises, by weight, 15 parts of a first extracting solution, 16 parts of a second extracting solution, 14 parts of a third extracting solution, 12 parts of a fourth extracting solution, 25 parts of a surfactant and 10 parts of an auxiliary agent.
Wherein the first extracting solution comprises the following raw materials: by weight, 15 parts of cortex dictamni, 8 parts of anhydrous pyridine, 3 parts of chlorosulfonic acid, 6 parts of lecithin, 4-6 parts of cholesterol, 8 parts of N, N-dimethylformamide, 12 parts of 1, 2-propylene glycol and 9 parts of phosphate buffer solution.
The fourth extracting solution comprises the following raw materials: by weight, 25 parts of fructus aurantii, 20 parts of radix puerariae and 20 parts of artemisia capillaris.
The surfactant is a mixed solution of tween 40, tween 60 and tween 80, and the mass ratio of tween 40 to tween 60 to tween 80 is 1: 1: 1. the auxiliary agent is polyethylene glycol.
Comparative example 1:
s1: preparing materials;
s2: preparing a first extracting solution:
adding chlorosulfonic acid into anhydrous pyridine in an ice-water bath to obtain a material A; mixing lecithin and cholesterol, stirring for 8min, and dissolving with anhydrous ethanol to obtain material B;
crushing cortex dictamni, performing reflux extraction by 90% ethanol, filtering, performing reflux extraction by water for 3 times after drying in the shade, filtering, combining filtrate, adding N, N-dimethylformamide, stirring for 15min, adding the material A, stirring and reacting for 3.5h at 65 ℃, cooling to room temperature, adjusting the pH to 7, performing ethanol precipitation for 28h, performing centrifugal filtration, and dialyzing for 72h to obtain a mixed solution;
mixing the mixed solution and 1, 2-propylene glycol, stirring, dissolving phosphate buffer solution, adding material B, performing ultrasonic treatment for 50s, placing in water bath at 45 ℃, performing rotary evaporation under reduced pressure to form a film layer, adding phosphate buffer solution, performing ultrasonic treatment for 40s in ice water bath, and filtering with 0.22um microporous filter membrane to obtain a first extract;
s3: mixing and stirring surfactant and auxiliary agent for 15min, adding the first extract, continuously stirring for 30min under the condition of water bath at 45 ℃, slowly dropwise adding deionized water, and dispersing for 15min at the rotating speed of 11000r/min to obtain the traditional Chinese medicine composition.
In this example, the raw materials of each component of the traditional Chinese medicine composition include: 15 parts of first extracting solution, 25 parts of surfactant and 10 parts of auxiliary agent.
The surfactant is a mixed solution of Tween 40, Tween 60 and Tween 80, wherein the mass ratio of the Tween 40 to the Tween 60 to the Tween 80 is 1: 1: 1. the auxiliary agent is polyethylene glycol.
Comparative example 2:
s1: preparing materials;
s2: preparing a first extracting solution:
adding chlorosulfonic acid into anhydrous pyridine in an ice-water bath to obtain a material A; mixing lecithin and cholesterol, stirring for 8min, and dissolving with anhydrous ethanol to obtain material B;
crushing cortex dictamni, performing reflux extraction by 90% ethanol, filtering, performing reflux extraction by water for 3 times after drying in the shade, filtering, combining filtrate, adding N, N-dimethylformamide, stirring for 15min, adding the material A, stirring and reacting for 3.5h at 65 ℃, cooling to room temperature, adjusting the pH to 7, performing ethanol precipitation for 28h, performing centrifugal filtration, and dialyzing for 72h to obtain a mixed solution;
mixing the mixed solution and 1, 2-propylene glycol, stirring, dissolving phosphate buffer solution, adding material B, performing ultrasonic treatment for 50s, placing in water bath at 45 ℃, performing rotary evaporation under reduced pressure to form a film layer, adding phosphate buffer solution, performing ultrasonic treatment for 40s in ice water bath, and filtering with 0.22um microporous filter membrane to obtain a first extract;
s3: preparing a second extracting solution: taking cortex moutan, placing in an incubator at 75 ℃ for standing for 18h, transversely shearing into small segments of 2cm, longitudinally splitting to obtain crushed materials, placing the crushed materials in a reaction tank, treating for 1.2h in a sulfur trioxide gas environment at the temperature of 62 ℃, crushing and sieving after treatment, placing in distilled water for soaking for 4h, carrying out steam distillation at 105 ℃ to extract for 1.5h, standing overnight, and passing through a 0.45-micrometer microporous membrane to obtain a second extracting solution;
s4: mixing and stirring surfactant and adjuvant for 15min, adding the first extractive solution and the second extractive solution, stirring in 45 deg.C water bath for 30min, slowly adding deionized water dropwise, and dispersing at 11000r/min for 15min to obtain the Chinese medicinal composition.
In this example, the raw materials of each component of the traditional Chinese medicine composition include: 15 parts of first extracting solution, 16 parts of second extracting solution, 25 parts of surfactant and 10 parts of auxiliary agent.
Wherein the first extracting solution comprises the following raw materials: by weight, 15 parts of cortex dictamni, 8 parts of anhydrous pyridine, 3 parts of chlorosulfonic acid, 6 parts of lecithin, 4-6 parts of cholesterol, 8 parts of N, N-dimethylformamide, 12 parts of 1, 2-propylene glycol and 9 parts of phosphate buffer solution.
The surfactant is a mixed solution of tween 40, tween 60 and tween 80, and the mass ratio of tween 40 to tween 60 to tween 80 is 1: 1: 1. the auxiliary agent is polyethylene glycol.
Comparative example 3:
s1: preparing materials;
s2: preparing a first extracting solution:
adding chlorosulfonic acid into anhydrous pyridine in an ice-water bath to obtain a material A; mixing lecithin and cholesterol, stirring for 8min, and dissolving with anhydrous ethanol to obtain material B;
crushing cortex dictamni, performing reflux extraction by 90% ethanol, filtering, performing reflux extraction by water for 3 times after drying in the shade, filtering, combining filtrate, adding N, N-dimethylformamide, stirring for 15min, adding the material A, stirring and reacting for 3.5h at 65 ℃, cooling to room temperature, adjusting the pH to 7, performing ethanol precipitation for 28h, performing centrifugal filtration, and dialyzing for 72h to obtain a mixed solution;
mixing the mixed solution and 1, 2-propylene glycol, stirring, dissolving phosphate buffer solution, adding material B, performing ultrasonic treatment for 50s, placing in water bath at 45 ℃, performing rotary evaporation under reduced pressure to form a film layer, adding phosphate buffer solution, performing ultrasonic treatment for 40s in ice water bath, and filtering with 0.22um microporous filter membrane to obtain a first extract;
s3: preparing a second extracting solution: taking cortex moutan, placing in an incubator at 75 ℃ for standing for 18h, transversely shearing into small segments of 2cm, longitudinally splitting to obtain crushed materials, placing the crushed materials in a reaction tank, treating for 1.2h in a sulfur trioxide gas environment at the temperature of 62 ℃, crushing and sieving after treatment, placing in distilled water for soaking for 4h, carrying out steam distillation at 105 ℃ to extract for 1.5h, standing overnight, and passing through a 0.45-micrometer microporous membrane to obtain a second extracting solution;
s4: preparing a third extracting solution: mixing and stirring onion and 1-butyl-3-methyl-imidazole hexafluorophosphate for 12min, performing ultrasound treatment for 10min under 110w of ultrasound power, placing in a water bath at 45 ℃ after the ultrasound treatment, adding alliinase solution, placing for 1.2h, slowly heating to 52 ℃, and performing reduced pressure distillation for 2h to obtain a third extracting solution;
s5: mixing and stirring surfactant and auxiliary agent for 15min, adding the third extract, uniformly mixing in a water bath at 45 ℃, adding the first extract and the second extract, continuously stirring for 30min, slowly dropwise adding deionized water, and dispersing at the rotating speed of 11000r/min for 15min to obtain the traditional Chinese medicine composition.
In this example, the raw materials of each component of the traditional Chinese medicine composition include: 15 parts of first extract, 16 parts of second extract, 14 parts of third extract, 25 parts of surfactant and 10 parts of auxiliary agent.
Wherein the first extracting solution comprises the following raw materials: by weight, 15 parts of cortex dictamni, 8 parts of anhydrous pyridine, 3 parts of chlorosulfonic acid, 6 parts of lecithin, 4-6 parts of cholesterol, 8 parts of N, N-dimethylformamide, 12 parts of 1, 2-propylene glycol and 9 parts of phosphate buffer solution.
The surfactant is a mixed solution of tween 40, tween 60 and tween 80, and the mass ratio of tween 40 to tween 60 to tween 80 is 1: 1: 1. the auxiliary agent is polyethylene glycol.
Experiment:
in the above scheme, examples 1-3 are the preparation of the Chinese medicinal composition according to the scheme disclosed in the invention, and examples 1-3 are different only in processing parameters.
Comparative examples 1-3 form control experiments with example 3; comparative example 1 contained only the first extract, and the other influencing parameters were the same as in example 3; comparative example 2 contained only the first extract and the second extract, and the other influencing parameters were the same as in example 3; comparative example 3 contained only the first extract, the second extract and the third extract, and the other parameters were the same as in example 3.
1. And (3) testing the bacteriostatic activity:
taking an autoclaved common agar culture medium, cooling to about 50 ℃, uniformly mixing, spreading a plate while the plate is hot, pouring the plate into a culture dish with the diameter of 9cm, sucking 0.5mL of bacterial suspension (escherichia coli and staphylococcus aureus) after the culture medium in the plate is solidified, putting the bacterial suspension into the culture medium, and uniformly coating the bacterial suspension by using a coating rod.
The Chinese medicinal composition (100. mu.l) prepared in examples 1-3 and comparative examples 1-3 was put into a culture medium, and then placed in a constant temperature incubator at 38 ℃ for 36 hours, and the diameter (mm) of the zone of inhibition was observed and measured, respectively, and the average measurement value was taken.
| Item | Example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| Escherichia coli (mm) | 20 | 21 | 20 | 10 | 13 | 17 |
| Staphylococcus aureus (mm) | 23 | 22 | 21 | 12 | 14 | 19 |
2: mouse experiments:
dividing 60 mice into 6 groups of 10 mice, and performing eczema infection in advance; wherein 6 groups are the traditional Chinese medicine compositions prepared in examples 1-3 and comparative examples 1-3 respectively, 0.05ml/20g of the corresponding medicine is coated on the focus of each group of mice from the day of the test, the medicine is continuously applied for 5 days twice a day, and the recovery degree of the focus is observed.
After observation, 3 groups of mice in examples 1-3 all dry on the eczema focus, no exudation phenomenon occurs, and the eczema treatment effect is obvious.
The mice in comparative example 1 all had exudation, and eczema slightly improved; in comparative example 2, 4 mice all dry at the focus and have no exudation phenomenon, and 6 mice still have exudation phenomenon, but the treatment effect of eczema in comparative example 2 is better than that of comparative example 1. In the comparative example 3, 8 mice are dried at the focus without exudation, and the treatment effect of eczema in the comparative example 3 is better than that of the comparative examples 1 and 2 according to the exudation phenomenon of 2 old mice.
Experiment 3: typical cases are:
wangzhi, women, age 23, arm with large erythema and acute pruritus, was administered (the Chinese medicinal composition prepared in example 3 of the present invention was applied to the skin surface 3 times a day), and after 4 days, the erythema was totally resolved and no recurrence occurred.
Liu Yi, male and female, age 36, large reddish patch appeared on the back, and had pimple and herpes dunculatus, which were diagnosed with mild exudation and severe pruritus, and were administered (the Chinese medicinal composition prepared in example 2 of the present invention was applied 3 times a day on the skin surface), and after 5 days, the diagnosis was repeated, and the rash was completely resolved, and no recurrence occurred thereafter.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative examples and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present examples are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Claims (10)
1. A traditional Chinese medicine composition with an anti-allergic effect is characterized in that: the traditional Chinese medicine composition comprises the following raw materials: 5-15 parts of first extracting solution, 8-16 parts of second extracting solution, 8-14 parts of third extracting solution, 10-12 parts of fourth extracting solution, 15-25 parts of surfactant and 6-10 parts of auxiliary agent.
2. The traditional Chinese medicine composition with antiallergic effect according to claim 1, which is characterized in that: the first extracting solution comprises the following raw materials: by weight, 10-15 parts of cortex dictamni, 4-8 parts of anhydrous pyridine, 2-3 parts of chlorosulfonic acid, 4-6 parts of lecithin, 4-6 parts of cholesterol, 6-8 parts of N, N-dimethylformamide, 10-12 parts of 1, 2-propylene glycol and 5-9 parts of phosphate buffer solution.
3. The traditional Chinese medicine composition with antiallergic effect according to claim 1, which is characterized in that: the second extracting solution is prepared from cortex moutan, sulfur trioxide and distilled water.
4. The traditional Chinese medicine composition with antiallergic effect according to claim 1, which is characterized in that: the third extracting solution is prepared from onion, 1-butyl-3-methyl-imidazole hexafluorophosphate and alliinase solution.
5. The traditional Chinese medicine composition with antiallergic effect according to claim 1, which is characterized in that: the fourth extracting solution comprises the following raw materials: by weight, 15-25 parts of fructus aurantii, 10-20 parts of radix puerariae and 10-20 parts of artemisia capillaris.
6. The traditional Chinese medicine composition with antiallergic effect according to claim 1, which is characterized in that: the surfactant is a mixed solution of Tween 40, Tween 60 and Tween 80, and the mass ratio of the Tween 40 to the Tween 60 to the Tween 80 is 1: 1: 1.
7. the traditional Chinese medicine composition with antiallergic effect according to claim 1, which is characterized in that: the auxiliary agent is one or a mixture of 1, 2-propylene glycol, glycerol and polyethylene glycol.
8. A preparation method of a traditional Chinese medicine composition with an anti-allergic effect is characterized by comprising the following steps: the method comprises the following steps:
1) preparing materials;
2) preparing a first extracting solution: preparing a first extracting solution from cortex dictamni, anhydrous pyridine, chlorosulfonic acid, lecithin, cholesterol, N-dimethylformamide, 1, 2-propylene glycol and a phosphate buffer solution;
3) preparing a second extracting solution: extracting cortex moutan to obtain a second extractive solution;
4) preparing a third extracting solution: taking onion, 1-butyl-3-methyl-imidazole hexafluorophosphate and alliinase solution to prepare a third extracting solution;
5) preparing a fourth extracting solution: preparing a fourth extracting solution from fructus aurantii, radix puerariae and artemisia capillaries;
6) and (3) taking a surfactant, an auxiliary agent, a first extracting solution, a second extracting solution, a third extracting solution and a fourth extracting solution to prepare the traditional Chinese medicine composition.
9. The method for preparing a Chinese medicinal composition with antiallergic effect according to claim 8, wherein the method comprises the following steps: the method comprises the following steps:
1) preparing materials;
2) preparing a first extracting solution:
a) adding chlorosulfonic acid into anhydrous pyridine in an ice-water bath to obtain a material A; mixing lecithin and cholesterol, stirring, and adding absolute ethyl alcohol to dissolve to obtain a material B;
b) pulverizing cortex Dictamni Radicis, extracting with 90% ethanol under reflux, filtering, drying in the shade, extracting with water under reflux for 2-3 times, filtering, mixing filtrates, adding N, N-dimethylformamide, stirring, adding material A, stirring at 60-65 deg.C for reaction, cooling to room temperature, adjusting pH, precipitating with ethanol, centrifuging, filtering, and dialyzing to obtain a mixed solution;
c) mixing the mixed solution and 1, 2-propylene glycol, stirring, dissolving phosphate buffer solution, adding material B, performing ultrasonic treatment, placing in water bath at 40-45 deg.C, performing rotary evaporation under reduced pressure to form a membrane layer, adding phosphate buffer solution, performing ultrasonic treatment in ice water bath, and filtering with 0.22um microporous membrane to obtain first extractive solution;
3) preparing a second extracting solution: taking cortex moutan, placing the cortex moutan in an incubator at 72-75 ℃, transversely shearing the cortex moutan into small sections of 1-2cm, longitudinally splitting the cortex moutan to obtain crushed materials, placing the crushed materials in a reaction tank, treating the crushed materials for 1-1.2 hours in a sulfur trioxide gas environment at the temperature of 60-62 ℃, crushing and sieving the crushed materials after treatment, soaking the crushed materials in distilled water, distilling the materials by steam at the temperature of 100 ℃ and 105 ℃, extracting, standing overnight, and passing through a 0.45um microporous membrane to obtain a second extracting solution;
4) preparing a third extracting solution: mixing herba Alii Fistulosi and 1-butyl-3-methyl-imidazole hexafluorophosphate, stirring, performing ultrasonic treatment for 8-10min, placing in 40-45 deg.C water bath, adding alliinase solution, standing, slowly heating to 50-52 deg.C, and distilling under reduced pressure to obtain a third extractive solution;
5) preparing a fourth extracting solution:
a) cleaning fructus Aurantii, drying, pulverizing, sieving, soaking in distilled water for 30-60min, reflux extracting, and filtering to obtain filtrate C;
b) mixing herba Artemisiae Scopariae and radix Puerariae under stirring, soaking in 70% ethanol solution for 24-28 hr, and extracting with ethanol for 2-4 hr to obtain extractive solution D;
c) mixing and stirring the filtrate C and the extracting solution D to obtain a fourth extracting solution;
6) mixing and stirring a surfactant and an auxiliary agent, adding the third extracting solution and the fourth extracting solution, uniformly mixing in a water bath at 40-45 ℃, adding the first extracting solution and the second extracting solution, continuously stirring, slowly dropwise adding deionized water, stirring and dispersing to obtain the traditional Chinese medicine composition.
10. The method for preparing a Chinese medicinal composition with antiallergic effect according to claim 9, wherein the method comprises the following steps: the method comprises the following steps:
1) preparing materials;
2) preparing a first extracting solution:
a) adding chlorosulfonic acid into anhydrous pyridine in an ice-water bath to obtain a material A; mixing lecithin and cholesterol, stirring for 5-8min, and dissolving in anhydrous ethanol to obtain material B;
b) taking cortex dictamni, crushing, performing reflux extraction with 90% ethanol, filtering, drying in the shade, performing reflux extraction with water for 2-3 times, filtering, combining filtrates, adding N, N-dimethylformamide, stirring for 10-15min, adding material A, stirring and reacting at 60-65 ℃ for 3-3.5h, cooling to room temperature, adjusting pH to 7, precipitating with ethanol for 24-28h, performing centrifugal filtration, and dialyzing for 72h to obtain a mixed solution;
c) mixing the mixed solution and 1, 2-propylene glycol, stirring, dissolving phosphate buffer solution, adding material B, performing ultrasonic treatment for 30-50s, placing in water bath at 40-45 deg.C, performing rotary evaporation under reduced pressure to form a film layer, adding phosphate buffer solution, performing ultrasonic treatment for 30-40s in ice water bath, and filtering with 0.22um microporous membrane to obtain first extractive solution;
3) preparing a second extracting solution: taking cortex moutan, placing the cortex moutan in an incubator at 72-75 ℃ for standing for 12-18h, transversely shearing into small segments of 1-2cm, longitudinally splitting to obtain crushed materials, placing the crushed materials in a reaction tank, treating for 1-1.2h at the temperature of 60-62 ℃ in the environment of sulfur trioxide gas, crushing and sieving after treatment, placing in distilled water for soaking for 3-4h, distilling with steam at the temperature of 100 ℃ and 105 ℃, extracting for 1-1.5h, standing overnight, and passing through a 0.45um microporous membrane to obtain a second extracting solution;
4) preparing a third extracting solution: mixing and stirring onion and 1-butyl-3-methyl-imidazole hexafluorophosphate for 10-12min, then carrying out ultrasonic treatment for 8-10min under the ultrasonic power of 100-110w, then carrying out ultrasonic treatment, then placing in a water bath at the temperature of 40-45 ℃, adding alliinase solution, placing for 1-1.2h, then slowly heating to the temperature of 50-52 ℃, and carrying out reduced pressure distillation for 1.5-2h to obtain a third extracting solution;
5) preparing a fourth extracting solution:
a) cleaning fructus Aurantii, drying, pulverizing, sieving with 20 mesh sieve, soaking in distilled water for 30-60min, reflux extracting for 2-3 times, each for 4-5 hr, and filtering to obtain filtrate C;
b) mixing herba Artemisiae Scopariae and radix Puerariae under stirring for 10-20min, soaking in 70% ethanol solution for 24-28 hr, and extracting with ethanol at 50-70 deg.C for 2-4 hr to obtain extractive solution D;
c) mixing and stirring the filtrate C and the extracting solution D to obtain a fourth extracting solution;
6) mixing and stirring a surfactant and an auxiliary agent for 12-15min, adding a third extracting solution and a fourth extracting solution, uniformly mixing under the water bath condition of 40-45 ℃, adding a first extracting solution and a second extracting solution, continuously stirring for 20-30min, slowly dropwise adding deionized water, and dispersing at the rotating speed of 10000-11000r/min for 10-15min to obtain the traditional Chinese medicine composition.
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