CN110664887B - Compound traditional Chinese medicine composition for treating cold and extraction method thereof - Google Patents

Compound traditional Chinese medicine composition for treating cold and extraction method thereof Download PDF

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CN110664887B
CN110664887B CN201910982566.1A CN201910982566A CN110664887B CN 110664887 B CN110664887 B CN 110664887B CN 201910982566 A CN201910982566 A CN 201910982566A CN 110664887 B CN110664887 B CN 110664887B
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梁烽焱
张�浩
李霞
谭余庆
刘丽
于海翠
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Yili Pharmaceutical Co ltd
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Abstract

The invention belongs to the technical field of traditional Chinese medicines, and particularly relates to a compound cold traditional Chinese medicine composition and an extraction method thereof. The compound cold traditional Chinese medicine composition comprises the following raw materials in parts by weight: 350-600 parts of scutellaria baicalensis, 400-600 parts of fructus forsythiae, 400-650 parts of elsholtzia, 400-600 parts of pogostemon cablin, 700-900 parts of honeysuckle stem, 400-650 parts of wild chrysanthemum flower, 300-600 parts of sweet wormwood and 400-600 parts of evodia lepta. The invention improves the extraction method of decocting the whole formula in water in the prior art, namely the invention extracts the volatile oil from the Chinese mosla herb and the cablin potchouli herb by steam distillation, then carries out inclusion by cyclodextrin or cyclodextrin derivatives, and extracts the other six Chinese medicines by decoction in water and concentration.

Description

Compound traditional Chinese medicine composition for treating cold and extraction method thereof
Technical Field
The invention belongs to the technical field of traditional Chinese medicines, and particularly relates to a compound cold traditional Chinese medicine composition and an extraction method thereof.
Background
Common cold is a common clinical disease, which occurs all the year round, especially in winter and spring, and especially in alternate seasons and sudden climate change, the incidence rate is higher. The patients with cold only show symptoms of nasal obstruction, watery nasal discharge, sneezing and the like in light patients, symptoms of high fever, headache, body pain and the like in heavy patients, and even more serious patients can cause deficiency of vital qi after cold, and diseases such as acute bronchitis, pneumonia, nasosinusitis, neuritis and the like are caused secondarily, so that the life is threatened, the work and life of the patients are seriously influenced, and the pain is brought to the patients.
At present, no specific treatment method for upper respiratory tract infection caused by virus is available in Western medicine, and symptomatic or supportive treatment is mainly adopted, and antiviral drugs such as ribavirin are commonly used in Western medicine for symptomatic treatment. The antiviral drug is easy to generate drug resistance after being taken for a long time, particularly for some people with special physique, such as children, pregnant women and old people, the antiviral drug for treating cold is easy to induce various adverse symptoms such as gastrointestinal discomfort, nausea, vomiting and the like, at the moment, the traditional Chinese medicine for treating cold is safer, and can treat both symptoms and root causes.
In the prior art, the extraction of the traditional Chinese medicine composition generally adopts water decoction of the whole formula, the water decoction of the whole formula has the advantage of simple operation process, but a large amount of precipitates can be generated in the water decoction process of the whole formula, and the effective components of the extract which can act on the upper respiratory tract infection are difficult to be ensured. Therefore, the method for effectively extracting the effective components in the traditional Chinese medicine composition has profound significance for promoting the inheritance and development of the traditional Chinese medicine.
Disclosure of Invention
In order to overcome the problems in the prior art, the invention provides a traditional Chinese medicine composition capable of effectively relieving upper respiratory tract infection symptoms such as cold and the like and an extraction method thereof, and the defects in the prior art are overcome by improving the extraction method and the extraction process.
In order to realize the purpose of the invention, the invention provides a compound cold traditional Chinese medicine composition which comprises the following raw materials in parts by weight: 350-600 parts of scutellaria baicalensis, 400-600 parts of fructus forsythiae, 400-650 parts of elsholtzia, 400-600 parts of pogostemon cablin, 700-900 parts of honeysuckle stem, 400-650 parts of wild chrysanthemum flower, 300-600 parts of sweet wormwood and 400-600 parts of evodia lepta.
Further, the compound cold traditional Chinese medicine composition comprises the following raw materials in parts by weight: 400-500 parts of scutellaria baicalensis, 450-550 parts of fructus forsythiae, 450-550 parts of elsholtzia, 450-550 parts of pogostemon cablin, 750-850 parts of honeysuckle stem, 500-550 parts of wild chrysanthemum flower, 450-520 parts of sweet wormwood herb and 450-550 parts of evodia lepta.
Preferably, the compound cold traditional Chinese medicine composition comprises the following raw materials in parts by weight: 500 parts of scutellaria baicalensis, 500 parts of fructus forsythiae, 500 parts of elsholtzia, 500 parts of pogostemon cablin, 833.3 parts of honeysuckle stem, 500 parts of wild chrysanthemum flower, 500 parts of sweet wormwood herb and 500 parts of thin evodia.
The invention also provides an extraction method of the compound cold traditional Chinese medicine composition, which comprises the following steps:
s1, adding water, and extracting herba Moslae and herba Agastaches by steam distillation to obtain volatile oil;
s2, clathrating the volatile oil obtained in the step S1 with cyclodextrin or cyclodextrin derivatives, drying, and pulverizing to obtain volatile oil clathrate;
s3, decocting fructus forsythiae, honeysuckle stem, wild chrysanthemum flower, sweet wormwood herb, thin evodia leaf and radix scutellariae with water to obtain decoction, filtering the decoction, and concentrating the decoction to obtain extract with the relative density of 1.10-1.14 at 50 ℃;
s4, adding ethanol into the extract obtained in the step S3, standing, filtering, concentrating to form thick paste with the relative density of 1.25-1.30 at 50 ℃, drying, and crushing to obtain concentrated powder;
s5, mixing the volatile oil inclusion compound in the step S2 and the concentrated powder in the step S4 to obtain the volatile oil inclusion compound.
Further, in step S1, the weight of the water is 5 to 8 times of the weight of the elsholtzia and the patchouli.
Preferably, in step S1, the weight of water is 6 times of the weight of the elsholtzia and pogostemon cablin.
Further, in step S1, the extraction time is 3-5 h.
Preferably, in step S1, the extraction time is 4 h.
Further, in step S2, the weight ratio of the volatile oil to the cyclodextrin or cyclodextrin derivative is 1: 10-20.
Preferably, in step S2, the weight ratio of the volatile oil and the cyclodextrin or cyclodextrin derivative is 1: 16.
Further, the cyclodextrin is one of alpha-cyclodextrin, beta-cyclodextrin and gamma-cyclodextrin.
Further, the cyclodextrin derivative can be one or more of carboxymethyl-beta-cyclodextrin, glucosyl-beta-cyclodextrin and hydroxyethyl-beta-cyclodextrin.
Further, the inclusion method in step S2 is one of a water-saturated solution method, a colloid mill method, and a grinding method.
The water saturated solution method comprises weighing 8 times of beta-cyclodextrin, adding 80 times of water, heating to dissolve until the beta-cyclodextrin is clear, adding 4.0g of volatile oil under stirring, magnetically stirring at 45-55 ℃ for 2h (rotation speed of 750 r.min < -1 >), cooling to room temperature, refrigerating overnight, filtering, taking precipitate, and drying in an oven at 45 ℃ for 4h to obtain the clathrate.
Colloid milling method: weighing 8 times of beta-cyclodextrin, adding 32 times of water, mixing, adding volatile oil, slowly adding into a colloid mill while stirring, refrigerating overnight, centrifuging, collecting clathrate, and oven drying at 45 deg.C for 4 hr.
The grinding method comprises weighing beta-cyclodextrin 6 times, adding volatile oil 4.0g, grinding, mixing, drying in the shade, grinding and pulverizing.
Further, in step S3, the number of times of water adding and decocting is 2, 6-10 times of water is added in the first time of decoction, the decoction is carried out for 1-3 hours, 5-8 times of water is added in the second time of decoction, the decoction is carried out for 1-3 hours, the decoction solutions are combined, the decoction solution is filtered and concentrated to an extract with the relative density of 1.10-1.14 at 50 ℃; in step S3, the charging sequence of the traditional Chinese medicines is as follows: decocting fructus forsythiae, honeysuckle stem, wild chrysanthemum flower, sweet wormwood herb and thin evodia leaf in water until the temperature of a water extracting solution reaches 85-95 ℃, and then adding scutellaria baicalensis.
Preferably, in step S3, the number of times of decocting with water is 2, 8 times of water is added for the first time of decoction, and 1.5 hours of decoction is performed, 6 times of water is added for the second time of decoction, and 1.5 hours of decoction is performed, the decoctions are combined, filtered, and concentrated to obtain an extract with a relative density of 1.10-1.14 at 50 ℃; in step S3, the charging sequence of the traditional Chinese medicines is as follows: decocting fructus forsythiae, caulis Lonicerae, flos Chrysanthemi Indici, herba Artemisiae Annuae, and thin Evodia in water, adding Scutellariae radix when the water extractive solution reaches 90 deg.C.
Further, in step S4, the volume ratio of the ethanol to the extract is 6-10: 3.
Preferably, in step S4, the volume ratio of the ethanol to the extract is 7: 3.
Preferably, in step S4, ethanol is added to the extract in step S3, the volume ratio of the ethanol to the extract is 7:3, the mixture is left standing for 2 hours, filtered and concentrated to a thick paste with the relative density of 1.25-1.30 at 50 ℃, and the thick paste is dried in vacuum at 75 ℃ and crushed to obtain concentrated powder.
Scutellaria baicalensis: the product is prepared from plants of Scutellaria of Labiatae; bitter and cold; it enters lung, gallbladder, spleen, stomach, large intestine and small intestine meridians; has effects in clearing away heat, eliminating dampness, purging pathogenic fire, removing toxic substances, stopping bleeding, and preventing miscarriage; it can be used for treating chest distress, emesis, dysentery, jaundice, cough due to lung heat, hyperpyrexia, polydipsia, hematemesis, carbuncle, swelling, sore, and threatened abortion.
Fructus forsythiae: the product is fruit of Forsythia suspensa (Thunb.) Vahl) belonging to the family Oleaceae; bitter and slightly cold; it enters lung, heart and gallbladder meridians; has the effects of clearing away heat and toxic materials, eliminating carbuncle and resolving hard mass, and can be used for treating affection of exogenous wind-heat, fever due to epidemic febrile disease, pyocutaneous disease, swelling and pain, and lymphoid tuberculosis.
Herba Moslae: the product is prepared from plants of Elsholtzia of Labiatae; pungent taste and slightly warm nature; entering lung and stomach meridians; has effects of inducing sweat, relieving exterior syndrome, eliminating dampness, regulating the middle warmer, inducing diuresis, and relieving edema, and can be used for treating summer-heat and dampness exterior syndrome, edema and dysuresia.
Patchouli: the product is Labiatae plant, perennial upright plant of herbaceous plant; pungent and mild-warm; spleen, stomach and lung meridians entered; has the effects of eliminating turbid pathogen with aromatics, regulating the middle warmer, relieving vomit, relieving exterior syndrome, and relieving summer-heat; it can be used for treating damp obstruction in middle warmer, abdominal distention, emesis, summer-heat dampness syndrome, early stage of damp-warm syndrome, fever, listlessness, chest distress, cold-dampness, summer-heat, abdominal pain, emesis, diarrhea, nasosinusitis, headache, etc.
Honeysuckle stem: the product is a plant belonging to Caprifoliaceae of Rubiales; sweet and cold; entering heart and lung meridians; has effects of clearing away heat and toxic materials, and dredging collaterals; it is mainly used for treating fever due to epidemic febrile disease, dysentery with bloody stool due to heat toxin, infectious hepatitis, carbuncle, swelling, sore, and arthralgia and myalgia.
Wild chrysanthemum flower: the product is perennial herb of Compositae; bitter, pungent and slightly cold; entering liver and heart meridians; has effects of clearing away heat and toxic materials, purging pathogenic fire, and calming liver; it can be used for treating furuncle, carbuncle, swelling, conjunctival congestion, swelling and pain, headache, and vertigo.
Sweet wormwood herb: the product is dried aerial part of Artemisia annua L of Compositae; bitter, pungent and cold; it enters liver and gallbladder meridians; has effects in clearing away summer-heat, removing steam, and preventing malaria; can be used for treating fever due to summer-heat, fever due to yin deficiency, night fever with early coolness, malaria with cold and heat, damp-heat jaundice, etc.
Bitter taste in trigeminal: the product is Rutaceae plant; bitter taste and cold nature; the Chinese medicinal composition has effects of clearing away heat and toxic materials, dispelling pathogenic wind, and removing dampness; can be used for treating swelling and pain of throat, rheumatalgia, malaria, jaundice, eczema, dermatitis, traumatic injury, insect bite, snake bite, etc.
The applicant discovers that main chemical components in the sweet wormwood comprise flavonoids, coumarins, terpenoids, phenylpropanoids, various volatile oils, coumarins scopoletin and the like through component analysis of eight traditional Chinese medicines, wherein most of the chemical components in the sweet wormwood extract are fat-soluble, and the applicant unexpectedly discovers that the effect of the water-soluble components in the sweet wormwood extract on the upper respiratory infection symptoms is more remarkable than that of the fat-soluble components in the test process. By classifying the eight traditional Chinese medicines, the volatile oil extracted from the elsholtzia and the patchouli is included by cyclodextrin or cyclodextrin derivatives, so that the effective components acting on the upper respiratory tract infection in the elsholtzia and the patchouli can be better reserved. In addition, the scutellaria baicalensis contains baicalase, which can carry out enzymolysis on the baicalin at a certain temperature and humidity to form unstable o-trihydroxyflavone which is easily oxidized to become a green quinone derivative to influence the extraction of the baicalin content, so that in the six-ingredient water-decocted traditional Chinese medicine, the scutellaria baicalensis is taken as a later ingredient, and the forsythia, the honeysuckle stem, the wild chrysanthemum, the sweet wormwood and the thin evodia are decocted by adding water until the water extract reaches 90 ℃, and then the baicalin can be better extracted.
Therefore, compared with the prior art, the extraction method has the following beneficial effects:
(1) the volatile oil extracted from the elsholtzia and the patchouli is included by the cyclodextrin or the cyclodextrin derivative, so that the method abandons the direct extraction by a steam extraction method in the traditional process, better preserves the active ingredients of the extracts of the elsholtzia and the patchouli acting on the upper respiratory tract infection, and is beneficial to enhancing the integral efficacy of the compound cold traditional Chinese medicine composition.
(2) The invention extracts the water-soluble components in the six medicines of forsythia, honeysuckle stem, wild chrysanthemum, sweet wormwood, thin evodia and scutellaria better by steam distillation. The water extracts of the five medicines are effective to the upper respiratory tract infection as can be obtained by mouse pneumonia model data caused by the infection of H1N1 influenza virus (FM1/PR8 strain). Aiming at the property difference of different traditional Chinese medicines, the invention obtains the compound cold traditional Chinese medicine composition capable of effectively relieving the upper respiratory tract infection by improving the extraction process of the traditional Chinese medicines.
Detailed Description
The present invention is further illustrated by the following description of specific embodiments, which are not intended to limit the invention, and various modifications and improvements can be made by those skilled in the art based on the basic idea of the invention, but within the scope of the invention, without departing from the basic idea of the invention.
Example 1
The compound cold traditional Chinese medicine composition of the embodiment 1 is prepared from the following raw materials in parts by weight: 350 parts of scutellaria baicalensis, 600 parts of fructus forsythiae, 400 parts of elsholtzia, 600 parts of pogostemon cablin, 700 parts of honeysuckle stem, 400 parts of wild chrysanthemum flower, 600 parts of sweet wormwood and 600 parts of thin evodia.
The extraction method of the compound cold traditional Chinese medicine composition of the embodiment 1 is as follows:
s1, adding water which is 5 times of the total weight of the Chinese mosla herb and the patchouli, and extracting the Chinese mosla herb and the patchouli by steam distillation for 3 hours to obtain volatile oil;
s2, clathrating the volatile oil obtained in the step S1 by an alpha-cyclodextrin colloid mill, drying and crushing to obtain a volatile oil clathrate compound, wherein the weight ratio of the volatile oil to the alpha-cyclodextrin is 1: 10;
s3, adding water 10 times of the total weight of fructus forsythiae, caulis Lonicerae, flos Chrysanthemi Indici, herba Artemisiae Annuae, thin Evodia and radix Scutellariae, decocting, adding fructus forsythiae, caulis Lonicerae, flos Chrysanthemi Indici, herba Artemisiae Annuae and thin Evodia, adding radix Scutellariae after the water extractive solution of fructus forsythiae, caulis Lonicerae, flos Chrysanthemi Indici, herba Artemisiae Annuae and thin Evodia reaches 85 deg.C, decocting for 3h, filtering, and pouring out the first decoction; adding 8 times of water into the residual dregs, continuously decocting for 3 hours to obtain a second decoction, mixing the decoctions, filtering the decoction, and concentrating to obtain an extract with the relative density of 1.10-1.14 at 50 ℃;
s4, adding ethanol into the extract obtained in the step S3, wherein the volume ratio of the ethanol to the extract is 6:3, standing for 2 hours, filtering, concentrating to obtain thick paste with the relative density of 1.25-1.30 at 50 ℃, drying at 75 ℃, and crushing to obtain concentrated powder;
s5, mixing the volatile oil inclusion compound in the step S2 and the concentrated powder in the step S4 to obtain the volatile oil inclusion compound.
Example 2
The compound cold traditional Chinese medicine composition of the embodiment 2 is prepared from the following raw materials in parts by weight: 600 parts of scutellaria baicalensis, 400 parts of fructus forsythiae, 650 parts of elsholtzia, 400 parts of pogostemon cablin, 900 parts of honeysuckle stem, 650 parts of wild chrysanthemum flower, 300 parts of sweet wormwood and 400 parts of thin evodia.
The extraction method of the compound cold traditional Chinese medicine composition of the embodiment 2 is as follows:
s1, adding water which is 8 times of the total weight of the Chinese mosla herb and the patchouli, and extracting the Chinese mosla herb and the patchouli by steam distillation for 5 hours to obtain volatile oil;
s2, clathrating the volatile oil obtained in the step S1 by a gamma-cyclodextrin colloid mill, drying and crushing to obtain a volatile oil clathrate compound, wherein the weight ratio of the volatile oil to the gamma-cyclodextrin is 1: 20;
s3, adding 6 times of water of fructus forsythiae, caulis Lonicerae, flos Chrysanthemi Indici, herba Artemisiae Annuae, thin Evodia and radix Scutellariae, decocting, adding fructus forsythiae, caulis Lonicerae, flos Chrysanthemi Indici, herba Artemisiae Annuae and thin Evodia, adding radix Scutellariae after the water extractive solution of fructus forsythiae, caulis Lonicerae, flos Chrysanthemi Indici, herba Artemisiae Annuae and thin Evodia reaches 95 deg.C, decocting for 1h, and pouring out the first decoction; adding 5 times of water into the residual dregs, decocting for 1 hour to obtain a second decoction, mixing the decoctions, filtering the decoction, and concentrating to obtain an extract with the relative density of 1.10-1.14 at 50 ℃;
s4, adding ethanol into the extract obtained in the step S3, wherein the volume ratio of the ethanol to the extract is 10:3, standing for 2 hours, filtering, concentrating to obtain thick paste with the relative density of 1.25-1.30 at 50 ℃, drying at 75 ℃, and crushing to obtain concentrated powder;
s5, mixing the volatile oil inclusion compound in the step S2 and the concentrated powder in the step S4 to obtain the volatile oil inclusion compound.
Example 3
The compound cold traditional Chinese medicine composition of embodiment 3 is prepared from the following raw materials in parts by weight: 500 parts of scutellaria baicalensis, 500 parts of fructus forsythiae, 500 parts of elsholtzia, 500 parts of pogostemon cablin, 833.3 parts of honeysuckle stem, 500 parts of wild chrysanthemum flower, 500 parts of sweet wormwood herb and 500 parts of thin evodia.
The extraction method of the compound cold traditional Chinese medicine composition of the embodiment 3 is as follows:
s1, adding water 6 times of the total weight of the herba Moslae and the herba Agastaches, and extracting the herba Moslae and the herba Agastaches by steam distillation for 4h to obtain volatile oil;
s2, clathrating the volatile oil obtained in the step S1 by a beta-cyclodextrin colloid mill method, drying and crushing to obtain a volatile oil clathrate compound, wherein the weight ratio of the volatile oil to the beta-cyclodextrin is 1: 16;
s3, adding 8 times of water of fructus forsythiae, caulis Lonicerae, flos Chrysanthemi Indici, herba Artemisiae Annuae, thin Evodia and radix Scutellariae, decocting, adding fructus forsythiae, caulis Lonicerae, flos Chrysanthemi Indici, herba Artemisiae Annuae and thin Evodia, adding radix Scutellariae after the water extractive solution of fructus forsythiae, caulis Lonicerae, flos Chrysanthemi Indici, herba Artemisiae Annuae and thin Evodia reaches 90 deg.C, decocting for 1.5h, and pouring out the first decoction; continuously adding 6 times of water into the residual dregs, decocting for 1.5h to obtain a second decoction, mixing the decoctions, filtering the decoction, and concentrating to obtain an extract with the relative density of 1.10-1.14 at 50 ℃;
s4, adding ethanol into the extract obtained in the step S3, wherein the volume ratio of the ethanol to the extract is 7:3, standing for 2 hours, filtering, concentrating to obtain thick paste with the relative density of 1.25-1.30 at 50 ℃, drying at 75 ℃, and crushing to obtain concentrated powder;
s5, mixing the volatile oil inclusion compound in the step S2 and the concentrated powder in the step S4 to obtain the volatile oil inclusion compound.
Example 4
The compound cold traditional Chinese medicine composition of embodiment 4 is prepared from the following raw materials in parts by weight: 500 parts of scutellaria baicalensis, 450 parts of fructus forsythiae, 550 parts of elsholtzia, 450 parts of pogostemon cablin, 800 parts of honeysuckle stem, 500 parts of wild chrysanthemum flower, 520 parts of sweet wormwood and 500 parts of evodia lepta.
The extraction method of the compound cold traditional Chinese medicine composition of the embodiment 4 is as follows:
s1, adding water 7 times of the total weight of the herba Moslae and the herba Agastaches, and extracting the herba Moslae and the herba Agastaches by steam distillation for 3.5h to obtain volatile oil;
s2, clathrating the volatile oil obtained in the step S1 by a hydroxyethyl-beta-cyclodextrin colloid mill, drying and crushing to obtain a volatile oil clathrate compound, wherein the weight ratio of the volatile oil to the hydroxyethyl-beta-cyclodextrin is 1: 14;
s3, adding water 7 times of the total weight of fructus forsythiae, caulis Lonicerae, flos Chrysanthemi Indici, herba Artemisiae Annuae, thin Evodia and radix Scutellariae, decocting, adding fructus forsythiae, caulis Lonicerae, flos Chrysanthemi Indici, herba Artemisiae Annuae and thin Evodia, adding radix Scutellariae after the extractive solution of fructus forsythiae, caulis Lonicerae, flos Chrysanthemi Indici, herba Artemisiae Annuae and thin Evodia reaches 90 deg.C, decocting for 2h, and pouring out the first decoction; continuously adding 6 times of water into the residual dregs, decocting for 1.5h to obtain a second decoction, mixing the decoctions, filtering the decoction, and concentrating to obtain an extract with the relative density of 1.10-1.14 at 50 ℃;
s4, adding ethanol into the extract obtained in the step S3, wherein the volume ratio of the ethanol to the extract is 8:3, standing for 2 hours, filtering, concentrating to obtain thick paste with the relative density of 1.25-1.30 at 50 ℃, drying at 75 ℃, and crushing to obtain concentrated powder;
s5, mixing the volatile oil inclusion compound in the step S2 and the concentrated powder in the step S4 to obtain the volatile oil inclusion compound.
Comparative example 1
The raw material composition and the parts by weight of the compound cold traditional Chinese medicine composition in the comparative example 1 are the same as those in the example 3;
the compound cold traditional Chinese medicine composition of the comparative example 1 is prepared by adopting an extraction process of decocting the whole formula with water, and the extraction process comprises the following steps:
s1, adding water 8 times of the total weight of radix Scutellariae, fructus forsythiae, herba Moslae, herba Agastaches, caulis Lonicerae, flos Chrysanthemi Indici, herba Artemisiae Annuae and thin Evodia, decocting for 1.5h, and pouring out the first decoction; adding 6 times of water into the dregs of a decoction, continuously decocting for 1.5 hours to obtain a second decoction, mixing the decoctions, filtering the decoction, and concentrating to obtain an extract with the relative density of 1.10-1.14 at 50 ℃;
s2, adding ethanol into the extract obtained in the step S3, wherein the volume ratio of the ethanol to the extract is 7:3, standing for 2 hours, filtering, concentrating to obtain thick paste with the relative density of 1.25-1.30 at 50 ℃, drying at 75 ℃, and crushing to obtain concentrated powder;
comparative example 2
The raw material composition and the parts by weight of the compound cold traditional Chinese medicine composition in the comparative example 2 are the same as those in the example 3;
the extraction process of the compound cold traditional Chinese medicine composition of the comparative example 2 comprises the following steps: extracting herba Artemisiae Annuae with 65% ethanol to obtain herba Artemisiae Annuae extract; decocting herba Moslae and herba Agastaches with water separately to extract volatile oil, clathrating with beta-cyclodextrin colloid mill, drying, and pulverizing; decocting the rest five medicinal materials such as Scutellariae radix with water, concentrating the extractive solution, precipitating with ethanol to remove impurities, mixing with the ethanol extract of herba Artemisiae Annuae, drying, and pulverizing. The specific extraction method comprises the following steps:
s1, adding water 6 times of the total weight of the herba Moslae and the herba Agastaches, and extracting the herba Moslae and the herba Agastaches by steam distillation for 4h to obtain volatile oil;
s2, clathrating the volatile oil obtained in the step S1 by a beta-cyclodextrin colloid mill method, drying and crushing to obtain a volatile oil clathrate compound, wherein the weight ratio of the volatile oil to the beta-cyclodextrin is 1: 16;
s2 extracting herba Artemisiae Annuae with 65% ethanol for 1.5 hr to obtain herba Artemisiae Annuae ethanol extract;
s3, adding 8 times of water of fructus forsythiae, caulis Lonicerae, flos Chrysanthemi Indici, thin Evodia and Scutellariae radix, decocting, adding Scutellariae radix after the extractive solution of fructus forsythiae, caulis Lonicerae, flos Chrysanthemi Indici and thin Evodia reaches 90 deg.C, decocting for 1.5h, and pouring out the first decoction; continuously adding 6 times of water into the residual dregs, decocting for 1.5h to obtain a second decoction, mixing the decoctions, filtering the decoction, and concentrating to obtain an extract with the relative density of 1.10-1.14 at 50 ℃;
s4, adding ethanol into the extract obtained in the step S3, wherein the volume ratio of the ethanol to the extract is 7:3, standing for 2 hours, filtering to obtain a filtrate, adding the arteannuol extract obtained in the step S2 into the filtrate, concentrating to form a thick paste with the relative density of 1.25-1.30 at 50 ℃, drying at 75 ℃, and crushing to obtain concentrated powder;
s5, mixing the volatile oil inclusion compound in the step S2 and the concentrated powder in the step S4 to obtain the volatile oil inclusion compound.
Comparative example 3
The raw material composition and the parts by weight of the compound cold traditional Chinese medicine composition in the comparative example 3 are the same as those in the example 3;
except for the different charging sequence of the scutellaria (namely, the scutellaria is not used as a later medicine), the other extraction methods are the same as the embodiment 3, namely, the scutellaria in the compound cold traditional Chinese medicine composition of the comparative example 3 is extracted together with the forsythia, the honeysuckle stem, the wild chrysanthemum, the sweet wormwood and the thin evodia at the beginning.
Comparative example 4
The raw material composition and the parts by weight of the compound cold traditional Chinese medicine composition in the comparative example 4 are the same as those in the example 3;
in the compound traditional Chinese medicine composition for treating cold of comparative example 4, the sweet wormwood is extracted by 65% ethanol to obtain sweet wormwood extract; decocting herba Moslae and herba Agastaches separately with water to extract volatile oil, filtering the medicinal liquid for use, decocting the rest five Chinese medicinal materials including Scutellariae radix with water, mixing with the medicinal liquid obtained by extracting volatile oil from herba Moslae and herba Agastaches, concentrating, precipitating with ethanol to remove impurities, mixing with herba Artemisiae Annuae ethanol extract, and its extraction method comprises:
s1, adding water 6 times of the total weight of the herba Moslae and the herba Agastaches, and extracting the herba Moslae and the herba Agastaches by steam distillation for 4h to obtain volatile oil;
s2 extracting herba Artemisiae Annuae with 65% ethanol for 1.5 hr to obtain herba Artemisiae Annuae ethanol extract;
s3, adding 8 times of water of fructus forsythiae, caulis Lonicerae, flos Chrysanthemi Indici, thin Evodia and Scutellariae radix, decocting, adding Scutellariae radix after the extractive solution of fructus forsythiae, caulis Lonicerae, flos Chrysanthemi Indici and thin Evodia reaches 90 deg.C, decocting for 1.5h, and pouring out the first decoction; continuously adding 6 times of water into the residual dregs, decocting for 1.5h to obtain a second decoction, mixing the decoctions, filtering the decoction, and concentrating to obtain an extract with the relative density of 1.10-1.14 at 50 ℃;
s4, adding ethanol into the extract obtained in the step S3, keeping the volume ratio of the ethanol to the extract at 7:3, standing for 2 hours, filtering to obtain a filtrate, adding the volatile oil obtained in the step S1 and the arteannuol extract obtained in the step S2 into the filtrate, concentrating to form a thick paste with the relative density of 1.25-1.30 at 50 ℃, drying at 75 ℃, and crushing to obtain concentrated powder.
Test example 1 Effect of different extraction methods on pulmonary index and pulmonary index inhibition ratio of FMI-infected mice
A mouse pneumonia model caused by H1N1 influenza virus (FM1/PR8 strain) infection is adopted, and the effectiveness evaluation is carried out on samples of examples 1-4 and comparative examples 1-4 by different extraction methods by taking a lung index and an inhibition rate thereof as indexes.
330 ICR mice (license number: SCXK (Jing) 2016-. Wherein, the positive medicament ribavirin granules: the clinical dosage of the human is 450mg/60kg/d, and the equivalent dosage converted into the mouse is 82.5 mg/kg; the amounts used in examples 1 to 4 and comparative examples 1 to 4 were 2.75g extract/kg body weight, corresponding to 14.3/g crude drug/kg body weight. Except for a normal control group, the mice were lightly anesthetized with ether, infected with 15 LD50 influenza virus liquid (FMI strain) by nasal drip, each 35 μ l, the administration was started on the day of infection, each time, the administration was started on the weight of 0.2ml/10g, the administration was performed 1 time per day for 4 consecutive days, the normal control group and the model control group were gavaged with distilled water under the same conditions, the mice were weighed on the 5 th day, dissected, the lungs were taken and weighed, and the lung index inhibition rate were calculated. In order to ensure the truth and the completeness of experimental data, the maximum value and the minimum value of each group of lung index are removed and then statistical calculation is carried out, and the results are statistically processed by using an inter-group comparison t test. The pulmonary index and pulmonary index inhibition rate are shown in formulas (I) and (II), respectively:
(I) lung index ═ lung wet weight (g) × 100/body weight (g)
Figure BDA0002234933220000121
TABLE 1 comparison of samples of different process routes for infant Elsholtzia ciliata granules for treating common cold
Figure BDA0002234933220000122
Note: # P <0.01 compared to normal control group; p <0.05, P <0.01, compared to model control group
Table 1 the results show that: after a normal mouse is infected by the influenza virus FMI, the lung index of the mouse is obviously increased, and the mouse has significant difference (P <0.01) compared with a normal control group, wherein except the elsholtzia granules No. 1 small dose group, the other groups have significant difference (P <0.01 and P <0.05) compared with a model control group. After 4 days of continuous administration of the elsholtzia granules, the lung indexes of mice infected by FMI strains are obviously reduced in examples 1-4, wherein the effect of example 3 is most obvious, and the inhibition rate of the lung indexes reaches 88.72%.
The preparation process route of the compound traditional Chinese medicine composition for treating cold in the comparative example 1 is to decoct the whole formula with water, and as the main drug effect parts of the elsholtzia and the patchouli are volatile oil components, the decoction can cause that the drug effect components of the elsholtzia and the patchouli in the compound traditional Chinese medicine composition for treating cold can not be exerted, so that the lung index is not obviously reduced, and the inhibition rate of the lung index is only 42.87%, which is far lower than that in the embodiment 3 of the invention.
The artemisia apiacea in the compound traditional Chinese medicine composition for treating the cold in the comparative example 2 is extracted by 65% ethanol, and the lung index inhibition rate of the artemisia apiacea is lower than that of the artemisia apiacea in the example 3, because the effective components of the artemisia apiacea for the upper respiratory tract infection are mainly water-soluble, the effect of extracting the artemisia apiacea by using water vapor is more advantageous than that of extracting the artemisia apiacea by 65% ethanol.
The scutellaria baicalensis in the compound cold traditional Chinese medicine composition in the comparative example 3 is not taken as a later medicine, namely, the scutellaria baicalensis is extracted together with forsythia, honeysuckle stem, wild chrysanthemum, sweet wormwood and thin evodia at the beginning, and the lung index inhibition rate is obviously lower than that in the example 3, probably because the baicalein is inactivated by high temperature after the scutellaria baicalensis is put, the baicalin cannot be enzymolyzed, and the baicalin content of an extracting solution is improved.
The compound traditional Chinese medicine composition for treating cold in the comparative example 4 is prepared by extracting sweet wormwood in 65% ethanol, extracting volatile oil from elsholtzia and patchouli by a water vapor extraction method, clathrating the extracted volatile oil with beta-cyclodextrin, and finally mixing the sweet wormwood ethanol extract, the volatile oil from elsholtzia and patchouli with extractum obtained from water extracts of forsythia, honeysuckle stem, wild chrysanthemum, bitter trifoliate and scutellaria baicalensis, drying and crushing. It is apparent from table 1 that the lung index inhibition ratio of the extraction method of comparative example 4 is lower than that of example 3, which proves that inclusion of volatile oil components by cyclodextrin or cyclodextrin derivatives can better exert the drug properties of elsholtzia and pogostemon cablin, and further improve the drug effect of the composition.
It will be appreciated by those skilled in the art that the above embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.

Claims (7)

1. The compound traditional Chinese medicine composition for treating cold is characterized by comprising the following raw materials in parts by weight: 350-600 parts of scutellaria baicalensis, 400-600 parts of fructus forsythiae, 400-650 parts of elsholtzia, 400-600 parts of pogostemon cablin, 700-900 parts of honeysuckle stem, 400-650 parts of wild chrysanthemum flower, 300-600 parts of sweet wormwood and 400-600 parts of trifurcate bitter;
the extraction method of the compound cold traditional Chinese medicine composition comprises the following steps:
s1: adding water, and extracting herba Moslae and herba Agastaches by steam distillation to obtain volatile oil;
s2: clathrating the volatile oil obtained in the step S1 with cyclodextrin or cyclodextrin derivative, drying, and pulverizing to obtain volatile oil clathrate;
s3: decocting fructus forsythiae, honeysuckle stem, wild chrysanthemum, sweet wormwood, thin evodia leaf and scutellaria baicalensis in water to obtain decoction, filtering the decoction, and concentrating the decoction to obtain an extract with the relative density of 1.10-1.14 at 50 ℃;
s4: adding ethanol into the extract obtained in the step S3, standing, filtering, concentrating to obtain a thick paste with the relative density of 1.25-1.30 at 50 ℃, vacuum-drying at 75 ℃, and crushing to obtain concentrated powder;
s5: mixing the volatile oil clathrate compound obtained in the step S2 and the concentrated powder obtained in the step S4 to obtain the volatile oil clathrate compound;
in the step S3, the number of times of water adding and decocting is 2, 6-10 times of water is added in the first time of decoction for 1-3 hours, 5-8 times of water is added in the second time of decoction for 1-3 hours, the decoctions are combined, the decoction is filtered and concentrated to an extract with the relative density of 1.10-1.14 at 50 ℃; in step S3, the charging sequence of the traditional Chinese medicines is as follows: decocting fructus forsythiae, honeysuckle stem, wild chrysanthemum flower, sweet wormwood herb and thin evodia leaf in water until the temperature of a water extracting solution reaches 85-95 ℃, and then adding scutellaria baicalensis.
2. The compound cold traditional Chinese medicine composition according to claim 1, which is characterized by comprising the following raw materials in parts by weight: 400-500 parts of scutellaria baicalensis, 450-550 parts of fructus forsythiae, 450-550 parts of elsholtzia, 450-550 parts of pogostemon cablin, 750-850 parts of honeysuckle stem, 500-550 parts of wild chrysanthemum flower, 450-520 parts of sweet wormwood herb and 450-550 parts of evodia lepta.
3. The compound cold traditional Chinese medicine composition of claim 1, wherein in step S1, the weight of the water is 5-8 times of the total weight of the elsholtzia and the pogostemon cablin.
4. The compound cold traditional Chinese medicine composition according to claim 1, wherein in step S1, the extraction time is 3-5 h.
5. The compound traditional Chinese medicine composition for treating cold as claimed in claim 1, wherein in step S2, the weight ratio of the volatile oil to the cyclodextrin or the cyclodextrin derivative is 1: 10-20.
6. The compound traditional Chinese medicine composition for treating cold according to claim 1, wherein in step S2, the inclusion method is one of a water-saturated solution method, a colloid milling method and a grinding method.
7. The compound cold traditional Chinese medicine composition according to claim 1, wherein the volume ratio of the ethanol to the extract is 6-10: 3.
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