CN109820826B - Anti-inflammatory traditional Chinese medicine granules and preparation method thereof - Google Patents

Anti-inflammatory traditional Chinese medicine granules and preparation method thereof Download PDF

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CN109820826B
CN109820826B CN201910222666.4A CN201910222666A CN109820826B CN 109820826 B CN109820826 B CN 109820826B CN 201910222666 A CN201910222666 A CN 201910222666A CN 109820826 B CN109820826 B CN 109820826B
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CN109820826A (en
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范惠君
陈邦辉
孙新平
谢明艳
杨华
许焰辉
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JIANGXI JIUHUA PHARMACEUTICAL CO Ltd
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Abstract

The invention belongs to the field of pharmacy, relates to a traditional Chinese medicine composition and a preparation method thereof, and particularly relates to a traditional Chinese medicine composition with an anti-inflammatory effect and a preparation method thereof. The traditional Chinese medicine composition provided by the invention comprises the following components in percentage by weight: 20-30% of picria felterrae lour, 15-25% of glabrous sarcandra herb, 10-20% of heartleaf houttuynia herb, 10-20% of pubescent holly root, 5-15% of baical skullcap root, 2-5% of liquoric root and 20-25% of flavoring agent.

Description

Anti-inflammatory traditional Chinese medicine granules and preparation method thereof
Technical Field
The invention belongs to the field of pharmacy, relates to a traditional Chinese medicine composition and a preparation method thereof, and particularly relates to a traditional Chinese medicine composition with an anti-inflammatory effect and a preparation method thereof.
Technical Field
The upper respiratory tract infection belongs to common diseases in the world, frequently occurs and has great harm to human health. Modern medical research suggests that upper respiratory tract infection is mainly caused by bacteria, viruses or bacteria and viruses, about 70% -80% of which are caused by bacteria and viruses, and inflammation is caused by invasion of pathogens such as bacteria or influenza viruses to the nose, pharynx, tonsil and throat.
In the prior art, many researches on anti-inflammatory preparations, such as tablets, capsules, oral liquid preparations and the like, have been carried out, and related standards are promulgated at national level, for example, anti-inflammatory preparations are recorded in eighth volume of drug standard Chinese medicinal prescription preparations of ministry of health, and the spelling name is as follows: xiaoyanlingpia; standard numbering: WS 3-B-1613-9; [ PREPARATION METHOD ] providing radix Picriae Felterrae 550g, herba Pileae Scriptae 350g, herba Senecionis Scandentis 225g, radix Ilicis Pubescentis 225g, and radix Glycyrrhizae over 50g, pulverizing radix Picriae Felterrae 100g into fine powder, decocting the rest radix Picriae Felterrae and the rest herba Pileae Scriptae in water twice, 2 hr for the first time and 1 hr for the second time, mixing decoctions, filtering, concentrating the filtrate to obtain soft extract, adding ethanol to reach ethanol content of 70%, standing for 24 hr, filtering, concentrating the filtrate to obtain soft extract, adding the above powder, mixing, oven drying, pulverizing into fine powder, adding adjuvant, mixing, granulating, pressing into 1000 tablets, and coating with sugar.
In the actual production process, the problems of large solvent loss, complicated purification process, low extraction rate of active components and the like in the extraction process are caused due to more medicinal ingredients and complex impurity components, and the effective utilization amount of the extracted active components is far lower than the actual content of the raw material dry product. With the reduction of the defense function of human bodies and the aggravation of environmental pollution, more and more published reports on the research of upper respiratory tract infectious diseases are provided. Most of them are children, the elderly, pregnant women, etc., and the oral administration compliance of tablets and capsules is poor, especially the administration of young children is difficult. No study related to granules is found at present.
In order to solve the problems and improve the treatment effect of the medicine, the invention provides the traditional Chinese medicine granule with the anti-inflammatory effect.
Disclosure of Invention
The invention aims to provide a traditional Chinese medicine granule with an anti-inflammatory effect.
The traditional Chinese medicine granule provided by the invention comprises the following components in percentage by weight:
20 to 30 percent of picria fel-terrae lour,
15 to 25 percent of glabrous sarcandra herb,
10 to 20 percent of heartleaf houttuynia herb,
10 to 20 percent of pubescent holly root,
5 to 15 percent of scutellaria baicalensis,
2 to 5 percent of liquorice,
20 to 25 percent of flavoring agent.
Wherein, the flavoring agent is selected from: one or more of glucose, fructose, sucrose, maltose, starch sugar or lactose, preferably sucrose.
Preferably, the traditional Chinese medicine granule of the invention consists of the following components:
900g of picria felterrae lour, 700g of glabrous sarcandra herb, 450g of houttuynia cordata, 450g of pubescent holly root, 250g of baical skullcap root, 100g of liquorice and 850g of cane sugar.
The traditional Chinese medicine used in the invention has the pharmacological and medicinal properties:
[ glabrous sarcandra ] nature flavor: slightly warm in nature, bitter and pungent in flavor.
The efficacy is as follows: resisting bacteria, relieving inflammation, dispelling pathogenic wind, dredging collaterals, promoting blood circulation, and resolving hard mass.
The main treatment is as follows: can be used for treating pneumonia, appendicitis, cellulitis, rheumatalgia, traumatic injury, and tumor.
[ KU-SHEN-XIANG ] has the following properties: bitter taste and cold nature.
Meridian tropism: it enters lung, stomach and liver meridians.
The efficacy is as follows: clear heat and remove toxicity, relieve swelling and alleviate pain.
The main treatment is as follows: wind-heat type common cold, sore throat, mumps, abdominal pain, dysentery, traumatic injury, furuncle, and venomous snake bite.
[ hairy holly ] has the following characteristics and tastes: slightly bitter and sweet in taste, mild in nature and non-toxic.
Has the effects of clearing away heat and toxic materials, promoting blood circulation and dredging collaterals.
The main treatment is as follows: it can be used for treating wind-heat type common cold, lung heat cough and asthma, larynx edema, tonsillitis, dysentery, coronary atherosclerotic heart disease, hemiplegia due to cerebrovascular accident, thromboangiitis obliterans, erysipelas, scald, central retinitis, uveitis, and acute suppurative inflammation of skin.
[ houttuynia cordata ] has a characteristic flavor: pungent and slightly cold.
Meridian tropism: it enters lung meridian.
The efficacy is as follows: clearing away heat and toxic material, curing abscess and discharging pus, inducing diuresis and treating stranguria.
The main treatment is as follows: can be used for treating pneumonia, lung abscess, urinary system infection, dysentery, mastitis, nephritis, cellulitis, otitis media, snake bite, furuncle, and carbuncle. It has effects in inhibiting influenza virus, relieving pain, stopping bleeding, relieving cough, and promoting urination.
[ Scutellariae ] nature and flavor: bitter taste and cold nature.
Meridian tropism: it enters lung, gallbladder, spleen, large intestine and small intestine meridians.
The efficacy is as follows: clear heat and dry dampness, purge fire and remove toxicity, stop bleeding, prevent abortion.
The main treatment is as follows: epidemic febrile disease, upper respiratory infection, cough due to lung heat, yellow gallbladder due to damp-heat, pneumonia, dysentery, hemoptysis, conjunctival congestion, threatened abortion, hypertension, carbuncle, furuncle, sore, etc.
[ CALORIC ACID ] nature and flavor: sweet in flavor and neutral in nature.
Meridian tropism: it enters heart, lung, spleen and stomach meridians.
The efficacy is as follows: invigorating spleen and replenishing qi, clearing away heat and toxic material, eliminating phlegm and relieving cough, relieving spasm and pain, and harmonizing the drugs.
The main treatment is as follows: can be used for treating weakness of spleen and stomach, asthenia, palpitation, short breath, cough, excessive phlegm, abdominal and limb spasm, pain, carbuncle, swelling, sore, and drug toxicity and strong nature.
The invention has good synergistic effect among various medicines, the glabrous sarcandra herb and the heartleaf houttuynia herb have the effects of bacteriostasis and antivirus, and the radix scutellariae has the functions of clearing heat, drying dampness, purging fire and detoxifying: the picria felterrae lour has the effects of clearing away heat and toxic materials, relieving swelling and pain, the pubescent holly root has the functions of promoting blood circulation and dredging collaterals, and the hay has the functions of tonifying spleen and qi, clearing away heat and toxic materials, and plays a very remarkable synergistic effect under the combined action. Especially has good curative effect on treating upper respiratory tract inflammation, bronchitis, rhinitis, pharyngolaryngitis, tonsillitis, bacillary dysentery and chronic cholecystitis.
The invention also aims to provide a preparation method of the traditional Chinese medicine granules.
The preparation method comprises the following steps:
(1) the preparation method of the sucrose powder comprises the following steps: pulverizing sucrose into superfine powder by micronizing technology;
(2) extracting the traditional Chinese medicine raw materials: coarse pulverizing radix Picriae Felterrae, herba Pileae Scriptae, herba Houttuyniae, radix Ilicis Pubescentis, Scutellariae radix, and Glycyrrhrizae radix, wherein radix Picriae Felterrae, herba Pileae Scriptae, herba Houttuyniae, radix Ilicis Pubescentis, and Glycyrrhrizae radix, placing into a pot-group countercurrent extraction unit, adding 6-12 times of water, and soaking for 15-60 min; decocting under heating, adding Scutellariae radix after boiling, extracting for 1-3 times (each time for 1-3 hr), mixing extractive solutions, filtering, transferring to double-effect concentrating tank, vacuum concentrating under reduced pressure to obtain extract, adding ethanol, standing, filtering to obtain filtrate, concentrating to obtain extract,
(3) adding appropriate amount of sucrose powder into the above extract, granulating, and drying.
Wherein, the extraction of the traditional Chinese medicine raw materials in the step (2) comprises the following steps:
taking radix Picriae Felterrae, herba Pileae Scriptae, herba Houttuyniae, radix Ilicis Pubescentis, Scutellariae radix, and Glycyrrhrizae radix, coarsely pulverizing, wherein the five medicines of radix Picriae Felterrae, herba Pileae Scriptae, herba Houttuyniae, radix Ilicis Pubescentis, and Glycyrrhrizae radix are put into a pot-group type countercurrent extraction machine set, adding 9 times of water of the total weight of the traditional Chinese medicinal materials, soaking for 30 minutes, heating, decocting, boiling, adding Scutellariae radix, extracting for 2 times, extracting for 2 hours for the first time, adding 6 times of water of the total weight of the traditional Chinese medicinal materials for the second time, extracting for 1 hour, mixing the extractive solutions, filtering with 1.5 μm filter membrane, transferring the filtrate into a double-effect concentration paste-collecting tank, vacuum concentrating to obtain an extract with a relative density of 1.15-1.20 (60 ℃), adding ethanol to make the ethanol content 70%, standing for 24 hours, filtering with 1.5 μm filter membrane, transferring the filtrate into a double-effect concentration paste-collecting tank, recovering ethanol, and vacuum concentrating at low temperature to obtain an extract with a relative density of 1.28-1.32 (60 ℃).
Most preferably, the preparation method comprises the following steps:
(1) the preparation method of the sucrose powder comprises the following steps: pulverizing sucrose into superfine powder by micronizing technology;
(2) taking radix Picriae Felterrae, herba Pileae Scriptae, herba Houttuyniae, radix Ilicis Pubescentis, Scutellariae radix, and Glycyrrhrizae radix, coarsely pulverizing, wherein radix Picriae Felterrae, herba Pileae Scriptae, herba Houttuyniae, radix Ilicis Pubescentis, and Glycyrrhrizae radix, putting into a pot-group countercurrent extraction unit, adding 9 times of water, soaking for 30 min, heating, decocting, boiling, adding Scutellariae radix, extracting for 2 times, extracting for 2h, adding 6 times of water, extracting for 1h, mixing extractive solutions, filtering with 1.5 μm filter membrane, transferring the filtrate into a double-effect concentration paste-collecting pot, vacuum concentrating under reduced pressure to obtain extract with relative density of 1.15-1.20 (60 deg.C), adding ethanol to make ethanol content 70%, standing for 24 hr, filtering with 1.5 μm filter membrane, transferring the filtrate into a double-effect concentration paste-collecting pot, recovering ethanol, vacuum concentrating under reduced pressure at low temperature to relative density of 1.28-1.32 (60 deg.C),
(3) adding appropriate amount of sucrose powder, granulating, drying, and making into 1000 g; and (5) obtaining the product.
The pharmaceutical dosage form prepared by the method of the invention is a sterile and non-sterile preparation referred to in pharmaceutics.
It is another object of the present invention to provide pharmaceutical uses of the pharmaceutical compositions of the present invention.
The traditional Chinese medicine composition disclosed by the invention is applied to preparation of medicines with the effects of treating upper respiratory tract infection, sterilizing and resisting viruses, eliminating inflammation, improving the functions of internal organs of a body and enhancing the resistance of a human body.
The traditional Chinese medicine composition disclosed by the invention is applied to preparation of medicines with anti-inflammatory effects.
Compared with the existing medicine formula and preparation process, the invention is greatly improved and optimized.
The preparation method can improve the extraction amount and purity of the effective components of the raw materials, fully utilize the raw materials and reduce the consumption of the solvent.
The invention adopts a tank-group type countercurrent extraction unit for extraction, and adopts a double-effect concentration paste-collecting tank for concentration, thereby improving the extraction amount and purity of effective components of raw materials, fully utilizing the raw materials and simultaneously reducing the consumption of solvent.
The traditional Chinese medicine composition has the combined effects of antibacterial and antiviral traditional Chinese medicines, such as glabrous sarcandra herb, heartleaf houttuynia herb and the like, and the radix scutellariae is used for clearing heat and drying dampness, purging fire and detoxifying, the picria felterrae lour is used for clearing heat and detoxifying, relieving swelling and pain, and the pubescent holly root is used for activating blood and dredging collaterals, so that the traditional Chinese medicine composition has an obvious curative effect on treating the upper respiratory tract infection.
The preparation method of the anti-inflammatory granules adopts a pot-group countercurrent extraction unit for extraction, can improve the concentration difference between a solvent and medicinal materials, extracts the effective components in the medicinal materials to the maximum extent, has high extraction rate, accelerates the diffusion of the effective components by using forced circulation measures, has small solvent consumption, greatly reduces the energy consumption of subsequent processes, and reduces the production cost.
The preparation method of the anti-inflammatory granules adopts a double-effect concentration paste collection tank for concentration, has low evaporation temperature and high speed, effectively ensures that thermosensitive substances are not damaged in the evaporation process, and effectively saves energy.
The anti-inflammatory granules have good oral compliance, simple preparation operation and easy realization of industrialization.
The invention is based on exogenous fever, wherein six exogenous pathogens invade the body surface, the pathogens compete with each other in defense, and nutrient-defense is disharmony, while wind-heat pathogenic toxin causes diseases by taking advantage of deficiency; or the lung and stomach two channels accumulate heat, the exogenous pathogenic factor is recovered, the wind-heat is mutually conflicted, the qi-blood stagnation and the depression are used for transforming toxin, the pathogenesis of the disease is the excess syndrome of the exogenous wind-heat, the invention is modified according to the symptoms in the prescription of the anti-inflammatory tablet, the essence part of the anti-inflammatory tablet is reserved, and the method takes the heat clearing, the detoxification, the detumescence and the pain relieving as the prescription according to the basic principle of 'monarch, minister, assistant and guide' formed by the compatibility of the prescription. In the formula, picria felterrae lour is bitter and cold in nature, has the function of clearing heat and removing toxicity, and is a monarch drug in the formula; the glabrous sarcandra herb is bitter and pungent in flavor and mild in property, has the effects of resisting bacteria and diminishing inflammation, dispelling wind and removing dampness, and promoting blood circulation to remove meridian obstruction, and is a Chinese and ministerial medicine; the pubescent holly root is slightly bitter and sweet in taste and neutral in nature, has the functions of clearing heat and removing toxicity, promoting blood circulation and removing meridian obstruction, the houttuynia cordata is pungent and slightly cold in taste and has the functions of clearing heat and removing toxicity, eliminating carbuncle and discharging pus, and inducing diuresis for treating stranguria, and the scutellaria baicalensis is bitter and cold in taste and has the functions of clearing heat and drying dampness, purging pathogenic fire and removing toxicity, and the pubescent holly root, the pubescent holly root and the scutellaria baicalensis are adjuvant drugs in the formula; licorice root, radix Glycyrrhizae, as a guiding drug in the recipe, has the effects of clearing away heat and toxic materials, and relieving spasm and pain to harmonize the effects of the other drugs in the recipe. In the formula, the five traditional Chinese medicines such as picria felterrae lour and the like have the functions of clearing heat and removing toxicity, so that the curative effect is obviously enhanced; the compatibility of glabrous sarcandra herb and pubescent holly root enhances the efficacy of promoting blood circulation and removing obstruction in channels; the combination of Yu xing Cao and Huang Qin can strengthen the actions of clearing heat and removing toxicity, relieving swelling and discharging pus, clearing lung-heat and relieving cough.
The medicines are combined to play the effects of clearing away heat and toxic materials and relieving swelling and pain. Compared with the existing anti-inflammatory tablets, anti-inflammatory capsules and the like, the anti-inflammatory granules prepared by the prescription are used for enhancing the curative effect of upper respiratory tract inflammation, bronchitis, rhinitis, sphagitis, tonsillitis, bacillary dysentery and chronic cholecystitis.
Compared with the existing method, the preparation method of the invention is improved in multiple places, and comprises the following steps:
the preparation method of the invention is that after boiling, the scutellaria baicalensis is added. Its advantage is no influence to content detection.
1) The invention carries out countercurrent extraction for 2 times, 9 times of water is added for the first time, and 6 times of water is added for the second time. The method has the advantages of improving the concentration difference between the solvent and the medicinal materials, extracting the effective components in the medicinal materials to the maximum extent, reducing the dosage of the solvent and lowering the production cost.
2) The countercurrent extraction is carried out for 2 times, the first extraction time is 2 hours, and the second extraction time is 1 hour. Has the advantages of fully extracting effective components in the shortest time and reducing energy consumption.
3) The concentration equipment used by the invention is a double-effect concentration paste collecting tank. The evaporation device has the advantages of accelerating evaporation speed, effectively ensuring that the thermosensitive substance is not damaged in the evaporation process and effectively saving energy.
4) The concentration is carried out in the invention, the concentration is carried out for the first time until the relative density is 1.15-1.20 (60 ℃), and the concentration is carried out for the second time until the relative density is 1.28-1.32 (60 ℃). The method has the advantages that impurities can be removed to a certain degree, and the ethanol dosage in the alcohol precipitation process can be reduced.
5) The alcohol precipitation of the invention is carried out by adding ethanol to ensure that the alcohol content is 70 percent and standing for 24 hours. The method has the advantages of removing impurities to the maximum extent, retaining effective components and improving purity.
Detailed Description
The present invention is further illustrated by the following specific examples, which are not to be construed as limiting the invention thereto. Embodiment 1
The formula is as follows: picria fel-terrae lour 900g sarcandra glabra 700g cordate houttuynia 450g
Hairy holly root 450g baikal skullcap root 250g licorice root 100g
Auxiliary materials: 850g of sucrose
The preparation method comprises the following steps: the six medicines are taken and coarsely crushed, the five medicines such as picria felterrae lour and the like except the baical skullcap root are firstly put into a pot-group type countercurrent extraction machine set, 9 times of total weight of the materials are firstly added into water for soaking for 30 minutes (after the materials are boiled, the baical skullcap root is added), 2 times of extraction is carried out, 2 hours of first extraction is carried out, 6 times of total weight of the materials are secondly added into water for extraction for 1 hour, the extracting solution is combined and filtered by a 1.5 mu m filter membrane, the filtrate is transferred into a double-effect concentration paste collection pot, vacuum decompression concentration is carried out under vacuum until the relative density is 1.18(60 ℃), ethanol is added until the ethanol content is 70%, standing is carried out for 24 hours, the filtrate is filtered by a 1.5 mu m filter membrane, the filtrate is transferred into the double-effect concentration paste collection pot, the ethanol is recovered, vacuum decompression concentration is carried out under low temperature until the relative density is 1.30(60 ℃), a proper amount of sucrose powder is added, the sucrose powder is prepared into particles, and the particles are dried, and the particles are prepared into 1000 g; and (5) obtaining the product.
Example II
The formula is as follows: picria fel-terrae lour 900g sarcandra glabra 700g cordate houttuynia 450g
Hairy holly root 450g baikal skullcap root 250g licorice root 100g
Auxiliary materials: 850g of sucrose
The preparation method comprises the following steps: the six medicines are taken and coarsely crushed, the five medicines such as picria felterrae lour and the like except the baical skullcap root are firstly put into a pot-group type countercurrent extraction machine set, 9 times of total weight of the materials are firstly added to soak for 30 minutes (after the materials are boiled, the baical skullcap root is added), 2 times of extraction is carried out, 2 hours of first extraction is carried out, 6 times of total weight of the materials are secondly added to extract for 1 hour, the extract is combined and filtered by a 1 mu m filter membrane, the filtrate is transferred into a double-effect concentration paste collecting pot, vacuum reduced pressure concentration is carried out under vacuum until the relative density is 1.18(60 ℃), ethanol is added until the ethanol content is 70%, standing is carried out for 24 hours, the filtrate is filtered by a 1 mu m filter membrane, the filtrate is transferred into a double-effect concentration paste collecting pot, the ethanol is recovered, vacuum reduced pressure reduced at low temperature until the relative density is 1.30(60 ℃), a proper amount of sucrose powder is added, granules are prepared, and dried to prepare 1000 g; and (5) obtaining the product.
Example three
The formula is as follows: picria fel-terrae lour 900g sarcandra glabra 750g cordate houttuynia 400g
Hairy holly root 400g baikal skullcap root 300g licorice root 100g
Auxiliary materials: 850g of sucrose
The preparation method comprises the following steps: the six medicines are taken and coarsely crushed, the five medicines such as picria felterrae lour and the like except the baical skullcap root are firstly put into a pot-group type countercurrent extraction machine set, 9 times of total weight of the materials are firstly added into water for soaking for 30 minutes (after the materials are boiled, the baical skullcap root is added), 2 times of extraction is carried out, 2 hours of first extraction is carried out, 6 times of total weight of the materials are secondly added into water for extraction for 1 hour, the extracting solution is combined and filtered by a 1.5 mu m filter membrane, the filtrate is transferred into a double-effect concentration paste collection pot, vacuum decompression concentration is carried out under vacuum until the relative density is 1.18(60 ℃), ethanol is added until the ethanol content is 70%, standing is carried out for 24 hours, the filtrate is filtered by a 1.5 mu m filter membrane, the filtrate is transferred into the double-effect concentration paste collection pot, the ethanol is recovered, vacuum decompression concentration is carried out under low temperature until the relative density is 1.30(60 ℃), a proper amount of sucrose powder is added, the sucrose powder is prepared into particles, and the particles are dried, and the particles are prepared into 1000 g; and (5) obtaining the product.
Example four
The formula is as follows: picria fel-terrae lour 950g sarcandra herb 750g cordate houttuynia 450g
Hairy holly root 450g baikal skullcap root 250g licorice root 100g
Auxiliary materials: 850g of sucrose
The preparation method comprises the following steps: the six medicines are taken and coarsely crushed, the five medicines such as picria felterrae lour and the like except the baical skullcap root are firstly put into a pot-group type countercurrent extraction machine set, 9 times of total weight of the materials are firstly added into water for soaking for 30 minutes (after the materials are boiled, the baical skullcap root is added), 2 times of extraction is carried out, 2 hours of first extraction is carried out, 6 times of total weight of the materials are secondly added into water for extraction for 1 hour, the extracting solution is combined and filtered by a 1.5 mu m filter membrane, the filtrate is transferred into a double-effect concentration paste collection pot, vacuum decompression concentration is carried out under vacuum until the relative density is 1.18(60 ℃), ethanol is added until the ethanol content is 70%, standing is carried out for 24 hours, the filtrate is filtered by a 1.5 mu m filter membrane, the filtrate is transferred into the double-effect concentration paste collection pot, the ethanol is recovered, vacuum decompression concentration is carried out under low temperature until the relative density is 1.30(60 ℃), a proper amount of sucrose powder is added, the sucrose powder is prepared into particles, and the particles are dried, and the particles are prepared into 1000 g; and (5) obtaining the product.
Example five
The formula is as follows: picria fel-terrae lour 900g sarcandra herb 750g cordate houttuynia 450g
Hairy holly root 450g baikal skullcap root 300g licorice root 100g
Auxiliary materials: 850g of sucrose
The preparation method comprises the following steps: the six medicines are taken and coarsely crushed, the five medicines such as picria felterrae lour and the like except the baical skullcap root are firstly put into a pot-group type countercurrent extraction machine set, 9 times of total weight of the materials are firstly added into water for soaking for 30 minutes (after the materials are boiled, the baical skullcap root is added), 2 times of extraction is carried out, 2 hours of first extraction is carried out, 6 times of total weight of the materials are secondly added into water for extraction for 1 hour, the extracting solution is combined and filtered by a 1.5 mu m filter membrane, the filtrate is transferred into a double-effect concentration paste collection pot, vacuum decompression concentration is carried out under vacuum until the relative density is 1.18(60 ℃), ethanol is added until the ethanol content is 70%, standing is carried out for 24 hours, the filtrate is filtered by a 1.5 mu m filter membrane, the filtrate is transferred into the double-effect concentration paste collection pot, the ethanol is recovered, vacuum decompression concentration is carried out under low temperature until the relative density is 1.30(60 ℃), a proper amount of sucrose powder is added, the sucrose powder is prepared into particles, and the particles are dried, and the particles are prepared into 1000 g; and (5) obtaining the product.
Example six
The formula is as follows: picria fel-terrae lour 900g sarcandra glabra 700g cordate houttuynia 450g
Hairy holly root 450g baikal skullcap root 250g licorice root 100g
Auxiliary materials: 850g of sucrose
The preparation method comprises the following steps: the six medicines are taken and coarsely crushed, the five medicines such as picria felterrae lour and the like except the baical skullcap root are firstly put into a pot-group type countercurrent extraction machine set, 9 times of total weight of the materials are firstly added into water for soaking for 30 minutes (after the materials are boiled, the baical skullcap root is added), 2 times of extraction is carried out, 2 hours of first extraction is carried out, 6 times of total weight of the materials are secondly added into water for extraction for 1 hour, the extracting solution is combined and filtered by a 1.5 mu m filter membrane, the filtrate is transferred into a double-effect concentration paste collection pot, vacuum decompression concentration is carried out under vacuum until the relative density is 1.20(60 ℃), ethanol is added until the ethanol content is 70%, standing is carried out for 24 hours, the filtrate is filtered by a 1.5 mu m filter membrane, the filtrate is transferred into the double-effect concentration paste collection pot, the ethanol is recovered, vacuum decompression concentration is carried out under low temperature until the relative density is 1.32(60 ℃), a proper amount of sucrose powder is added, the sucrose powder is prepared into particles, and the particles are dried, and the 1000g is prepared; and (5) obtaining the product.
Example seven
The formula is as follows: picria fel-terrae lour 900g sarcandra glabra 700g cordate houttuynia 450g
Hairy holly root 450g baikal skullcap root 250g licorice root 100g
Auxiliary materials: 850g of sucrose
The preparation method comprises the following steps: the six medicines are taken and coarsely crushed, the five medicines such as picria felterrae lour and the like except the baical skullcap root are firstly put into a pot-group type countercurrent extraction machine set, 9 times of total weight of the materials are firstly added into water for soaking for 30 minutes (after the materials are boiled, the baical skullcap root is added), 2 times of extraction is carried out, 2 hours of first extraction is carried out, 6 times of total weight of the materials are secondly added into water for extraction for 1 hour, the extracting solution is combined, the filtering solution is filtered by a 1 mu m filtering film, the filtering solution is transferred into a double-effect concentration paste collecting pot, vacuum concentration is carried out under vacuum at low temperature until the relative density is 1.20(60 ℃), the ethanol content is 70 percent, standing is carried out for 24 hours, the filtering solution is carried out by a 1 mu m filtering film, the filtering solution is transferred into a double-effect concentration paste collecting pot, the ethanol is recycled, vacuum concentration is carried out at low temperature until the relative density is 1.32(60 ℃), a proper amount of sucrose powder is added, the sucrose powder is prepared into particles, and the particles are dried, and the particles are prepared into 1000 g; and (5) obtaining the product.
Eight implementation cases
The formula is as follows: picria fel-terrae lour 900g sarcandra glabra 700g cordate houttuynia 450g
Hairy holly root 450g baikal skullcap root 250g licorice root 100g
Auxiliary materials: 850g of sucrose
The preparation method comprises the following steps: the six medicines are taken and coarsely crushed, the five medicines such as picria felterrae lour and the like except the baical skullcap root are firstly put into a pot-group type countercurrent extraction machine set, 9 times of total weight of the materials are firstly added into water for soaking for 30 minutes (after the materials are boiled, the baical skullcap root is added), 2 times of extraction is carried out, 2 hours of first extraction is carried out, 6 times of total weight of the materials are secondly added into water for extraction for 1 hour, the extracting solution is combined and filtered by a 1.5 mu m filter membrane, the filtrate is transferred into a double-effect concentration paste collection pot, vacuum decompression concentration is carried out under vacuum until the relative density is 1.15(60 ℃), ethanol is added until the ethanol content is 70%, standing is carried out for 24 hours, the filtrate is filtered by a 1.5 mu m filter membrane, the filtrate is transferred into the double-effect concentration paste collection pot, the ethanol is recovered, vacuum decompression concentration is carried out under low temperature until the relative density is 1.28(60 ℃), a proper amount of sucrose powder is added, the sucrose powder is prepared into particles, and the particles are dried, and the particles are prepared into 1000 g; and (5) obtaining the product.
Example nine
The formula is as follows: picria fel-terrae lour 900g sarcandra glabra 700g cordate houttuynia 450g
Hairy holly root 450g baikal skullcap root 250g licorice root 100g
Auxiliary materials: 850g of sucrose
The preparation method comprises the following steps: the six medicines are taken and coarsely crushed, the five medicines such as picria felterrae lour and the like except the baical skullcap root are firstly put into a pot-group type countercurrent extraction machine set, 9 times of total weight of the materials are firstly added into water for soaking for 30 minutes (after the materials are boiled, the baical skullcap root is added), 2 times of extraction is carried out, 2 hours of first extraction is carried out, 6 times of total weight of the materials are secondly added into water for extraction for 1 hour, the extracting solution is combined, the filtering solution is filtered by a 1 mu m filtering film, the filtering solution is transferred into a double-effect concentration paste collecting pot, vacuum concentration is carried out under vacuum at low temperature until the relative density is 1.15(60 ℃), the ethanol content is 70 percent, standing is carried out for 24 hours, the filtering solution is carried out by a 1 mu m filtering film, the filtering solution is transferred into a double-effect concentration paste collecting pot, the ethanol is recycled, vacuum concentration is carried out at low temperature until the relative density is 1.28(60 ℃), a proper amount of sucrose powder is added, the sucrose powder is prepared into particles, and the particles are dried, and the particles are prepared into 1000 g; and (5) obtaining the product.
Ten implementation cases
The formula is as follows: picria fel-terrae lour 900g sarcandra glabra 750g cordate houttuynia 400g
Hairy holly root 400g baikal skullcap root 300g licorice root 100g
Auxiliary materials: 850g of sucrose
The preparation method comprises the following steps: the six medicines are taken and coarsely crushed, the five medicines such as picria felterrae lour and the like except the baical skullcap root are firstly put into a pot-group type countercurrent extraction machine set, 9 times of total weight of the materials are firstly added to soak for 30 minutes (after the materials are boiled, the baical skullcap root is added), 2 times of extraction is carried out, 2 hours of first extraction is carried out, 6 times of total weight of the materials are secondly added to extract for 1 hour, the extract is combined and filtered by a 1 mu m filter membrane, the filtrate is transferred into a double-effect concentration paste collecting pot, vacuum reduced pressure concentration is carried out under vacuum until the relative density is 1.18(60 ℃), ethanol is added until the ethanol content is 70%, standing is carried out for 24 hours, the filtrate is filtered by a 1 mu m filter membrane, the filtrate is transferred into a double-effect concentration paste collecting pot, the ethanol is recovered, vacuum reduced pressure reduced at low temperature until the relative density is 1.30(60 ℃), a proper amount of sucrose powder is added, granules are prepared, and dried to prepare 1000 g; and (5) obtaining the product.
The above experiments all meet the quality standard through QC inspection.
Test example 1
Clinical curative effect test.
First, criteria for selecting case
Rhinitis, pharyngolaryngitis, tonsillitis, and upper respiratory infection such as acute tonsillitis, acute bronchitis, acute viral pharyngitis or laryngitis caused by common cold. The common clinical features are hoarseness, difficulty speaking, pain at cough, often fever, sore throat or cough. The body examination shows laryngeal edema, congestion, mild swelling and tenderness of local lymph nodes, swollen tonsils, and audible wheezing sound of the throat.
Second, treatment scheme
Patients diagnosed with upper respiratory tract infection are treated by taking the traditional Chinese medicine provided by the invention, the traditional Chinese medicine is taken once in the morning, at noon and at night every day, 1 bag (10 g/bag) is used each time, 7 days is a treatment course, and the treatment effect is counted after one treatment course.
Thirdly, evaluation standard of curative effect
And (3) curing: the symptoms in the diagnostic criteria are completely disappeared, and the normal work, life, study and labor can be realized.
The method has the following advantages: symptoms referred to in the diagnostic criteria are improved and markedly improved, requiring continued treatment.
And (4) invalidation: the symptoms referred to in the diagnostic criteria are not improved and tend to be even more severe, and other medications are required to be selected for treatment.
Fourthly, statistical treatment
The patients with upper respiratory tract infection disease 110 were treated by taking medicine according to the criteria of selected cases and after the diagnosis, wherein 64 men and 46 women are aged at 5-45 years, and the specific statistical data are as follows:
Figure BDA0002004124810000101
Figure BDA0002004124810000111
wherein, the comparative example 1 refers to a compound traditional Chinese medicine preparation for treating upper respiratory tract infection prepared in the example 2 of Chinese patent (application number: 200910114230. X).
Preliminary clinical tests show that the medicine has obvious effects of clearing away heat and toxic materials and relieving swelling and pain, avoids the defects of long onset time, temporary solution, pain, difficult administration and the like compared with other tablets, capsules and injections, and has the characteristics of convenient use, quick response, easy acceptance by patients and the like.
Test example 2 screening test of the production Process of the present invention
The invention screens preparation process parameters, and mainly comprises the following steps: the four parts of the decocting times, the extraction time, the water adding amount and the alcohol precipitation concentration are optimized in experiments, the transfer rate of the isofraxidin is used as an evaluation index, and the optimal preparation process is preferably obtained by the following steps:
(1) the preparation method of the sucrose powder comprises the following steps: pulverizing sucrose into superfine powder by micronizing technology;
(2) taking six medicines of picria felterrae lour, glabrous sarcandra herb, heartleaf houttuynia herb, pubescent holly root, baical skullcap root and liquoric root, roughly crushing, putting the picria felterrae lour, the glabrous sarcandra herb, the heartleaf houttuynia herb, the pubescent holly root and the liquoric root into a pot-group type countercurrent extraction machine set, and adding water with the weight being 9 times of the total weight of the materials for soaking for 30 minutes for the first time. Heating and decocting, adding scutellaria baicalensis after boiling, extracting for 2 times, extracting for 2 hours for the first time, adding water with the weight of 6 times of the total weight of the materials for the second time, extracting for 1 hour, combining the extracting solutions, filtering by a 1.5 mu m filter membrane, transferring the filtrate into a double-effect concentration paste-collecting tank, concentrating under vacuum until the relative density is 1.15-1.20 (60 ℃), adding ethanol until the alcohol content is 70%, standing for 24 hours, filtering by a 1.5 mu m filter membrane, transferring the filtrate into a double-effect concentration paste-collecting tank, recovering the ethanol, concentrating under vacuum at low temperature until the relative density is 1.28-1.32 (60 ℃),
(3) adding appropriate amount of sucrose powder, granulating, drying, and making into 1000 g; and (5) obtaining the product.
Experimental procedure
1. Screening of the number of times of decoction
The preparation method comprises the following steps of roughly crushing 3 parts of medicinal materials (900 g of picria felterrae lour, 700g of glabrous sarcandra herb, 450g of heartleaf houttuynia herb, 450g of pubescent holly root, 250g of baical skullcap root and 100g of liquoric root) according to the prescription amount, putting the picria felterrae lour, the glabrous sarcandra herb, the heartleaf houttuynia herb, the pubescent holly root and the liquoric root into a pot-type countercurrent extraction unit, and adding water with the weight being 9 times of the total weight of the materials for soaking for 30 minutes. Decocting under heating, adding Scutellariae radix after boiling, decocting for 1 time, 2 times, and 3 times respectively, and collecting three groups. Adding 9 times of water each time, decocting for 2 hours each time, mixing the extractive solutions, detecting the extractive solution, and calculating the transfer rate of isofraxidin. See table 1.
TABLE 1
Number of times of decoction Isofraxidin transfer ratio (%)
1 62
2 99.6
3 99.4
And (4) conclusion: the medicinal materials are not completely extracted after being decocted for 1 time, and the transfer rate of isofraxidin is not improved after being decocted for 3 times, so that the optimal time of decocting is 2 times.
2. Screening of extraction time
The preparation method comprises the following steps of roughly crushing the medicinal materials (900 g of picria felterrae lour, 700g of glabrous sarcandra herb, 450g of heartleaf houttuynia herb, 450g of pubescent holly root, 250g of baical skullcap root and 100g of liquoric root) according to the prescription amount, putting the picria felterrae lour, the glabrous sarcandra herb, the heartleaf houttuynia herb, the pubescent holly root and the liquoric root into a pot-type countercurrent extraction unit, and adding water with the weight being 9 times of the total weight of the materials for soaking for 30 minutes. Heating and decocting, adding Scutellariae radix after boiling, extracting for 2 times, adding 9 times of water each time, extracting for 2h for the first time, extracting for 0.5h, 1h, 1.5h and 2h for the second time respectively, combining the extractive solutions, taking the extractive solution, detecting, and calculating the transfer rate of isofraxidin. See table 2.
TABLE 2
Extraction time Isofraxidin transfer ratio (%)
0.5h 78
1h 99.5
1.5h 99.6
2h 98.9
And (4) conclusion: decocting the medicinal materials twice, extracting for 2h for the first time, and extracting for 1h for the second time optimally.
3. Screening of the amount of water added
3.1 first Water addition screening
The method comprises the following steps of roughly crushing 3 parts of medicinal materials (900 g of picria felterrae lour, 700g of glabrous sarcandra herb, 450g of houttuynia cordata, 450g of pubescent holly root, 250g of scutellaria baicalensis and 100g of liquorice) according to the prescription amount, putting the picria felterrae lour, the glabrous sarcandra herb, the houttuynia cordata, the pubescent holly root and the liquorice into a pot-type countercurrent extraction unit, adding water which is 8 times, 9 times and 10 times of the total weight of the medicinal materials respectively for soaking for 30 minutes for the first time, paralleling three groups, and observing the condition that the medicinal materials are immersed in the liquid surface. Heating and decocting, adding Scutellariae radix after boiling, extracting for 2 times for 2h for the first time, adding water 6 times the total weight of the materials for the second time, extracting for 1h, mixing extractive solutions, detecting the extractive solution, and calculating the transfer rate of isofraxidin. See table 3.
TABLE 3
Amount of added water Isofraxidin transfer ratio (%) The situation of medicinal materials immersed in liquid level
8 times of the total amount of the raw materials 82 Is not completely immersed
9 times of the total amount of the raw materials 99.5 Is completely immersed
10 times of the total amount of the raw materials 99 Is completely immersed
And (4) conclusion: the medicinal materials are not completely immersed by adding 8 times of water, the extraction is incomplete, and the transfer rate of isofraxidin is not improved by adding 10 times of water, so that the optimal water amount is 9 times of the first time.
3.2 second Water addition screening
The preparation method comprises the following steps of roughly crushing 3 parts of medicinal materials (900 g of picria felterrae lour, 700g of glabrous sarcandra herb, 450g of heartleaf houttuynia herb, 450g of pubescent holly root, 250g of baical skullcap root and 100g of liquoric root) according to the prescription amount, putting the picria felterrae lour, the glabrous sarcandra herb, the heartleaf houttuynia herb, the pubescent holly root and the liquoric root into a pot-type countercurrent extraction machine set, and adding 9 times of water in the total weight of the materials for soaking for 30 minutes for the first time. Heating and decocting, adding Scutellariae radix after boiling, extracting for 2 times for the first time for 2h, adding water 5 times, 6 times and 7 times of the total weight of the materials for the second time, extracting for 1h in parallel, mixing the extractive solutions, detecting the extractive solution, and calculating the transfer rate of isofraxidin. See table 4.
TABLE 4
Amount of added water Isofraxidin transfer ratio (%)
5 times of the total amount of the raw materials 83
6 times of the total amount of the raw materials 99.5
7 times of the total amount of the raw materials 98.9
And (4) conclusion: the medicinal materials are not completely extracted by adding 5 times of water, and the transfer rate of isofraxidin is not improved by adding 7 times of water, so that the optimal water adding amount for the second time is 6 times.
4. Screening of alcohol precipitation concentration
The method comprises the following steps of roughly crushing the medicinal materials (900 g of picria felterrae lour, 700g of glabrous sarcandra herb, 450g of houttuynia cordata, 450g of pubescent holly root, 250g of scutellaria baicalensis and 100g of liquorice) according to the prescription amount, putting the picria felterrae lour, the glabrous sarcandra herb, the houttuynia cordata, the pubescent holly root and the liquorice into a pot-type countercurrent extraction unit, and adding water with the weight being 9 times of the total weight of the materials for soaking for 30 minutes for the first time. Heating and decocting, adding scutellaria baicalensis after boiling, extracting for 2 times, extracting for 2 hours for the first time, adding water with the weight 6 times of the total weight of the materials for the second time, extracting for 1 hour, combining extracting solutions, filtering by using a 1.5 mu m filter membrane, transferring the filtrate into a double-effect concentration paste-collecting tank, concentrating under vacuum and reduced pressure to obtain an extract with the relative density of 1.15-1.20 (60 ℃), respectively adding ethanol to ensure that the alcohol content is 50%, 60%, 70%, 80% and 85%, standing for 24 hours, filtering by using a 1.5 mu m filter membrane, taking the supernatant, and detecting to calculate the transfer rate of isofraxidin. See table 5.
TABLE 5
Alcohol precipitation concentration Isofraxidin transfer ratio (%)
50% 83
60% 82
70% 87
80% 60
85% 52
And (4) conclusion: the purity is reduced because impurities are not sufficiently removed due to too low alcohol precipitation concentration, and effective components with too high concentration are wrapped by the impurities and lost, so the alcohol precipitation concentration is 70% optimal.
5. Three batches of verifications
The preparation method comprises the following steps of roughly crushing 3 parts of medicinal materials (900 g of picria felterrae lour, 700g of glabrous sarcandra herb, 450g of heartleaf houttuynia herb, 450g of pubescent holly root, 250g of baical skullcap root and 100g of liquoric root) according to the prescription amount, putting the picria felterrae lour, the glabrous sarcandra herb, the heartleaf houttuynia herb, the pubescent holly root and the liquoric root into a pot-type countercurrent extraction machine set, and adding 9 times of water in the total weight of the materials for soaking for 30 minutes for the first time. Heating and decocting, adding scutellaria baicalensis after boiling, extracting for 2 times, extracting for 2 hours for the first time, adding water with the weight 6 times of the total weight of the materials for the second time, extracting for 1 hour, combining extracting solutions, filtering by using a 1.5 mu m filter membrane, transferring the filtrate into a double-effect concentration paste-collecting tank, concentrating under vacuum and reduced pressure to obtain an extract with the relative density of 1.15-1.20 (60 ℃), respectively adding ethanol to ensure that the alcohol content is 70%, standing for 24 hours, filtering by using a 1.5 mu m filter membrane, taking the supernatant, detecting, and calculating the transfer rate of isofraxidin. The results are shown in table 6, and the average transfer rate of isofraxidin is 86%, which shows that the process can effectively improve the extraction rate of isofraxidin and has strong stability.
TABLE 6
Batches of Isofraxidin transfer ratio (%)
1 85
2 87
3 86

Claims (5)

1. A traditional Chinese medicine granule with anti-inflammatory effect is prepared from the following components in percentage by weight:
20 to 30 percent of picria fel-terrae lour,
15 to 25 percent of glabrous sarcandra herb,
10 to 20 percent of heartleaf houttuynia herb,
10 to 20 percent of pubescent holly root,
5 to 15 percent of scutellaria baicalensis,
2 to 5 percent of liquorice,
20 to 25 percent of cane sugar,
the preparation method comprises the following steps:
(1) the preparation method of the sucrose powder comprises the following steps: pulverizing sucrose into superfine powder by micronizing technology;
(2) extracting the traditional Chinese medicine raw materials: coarse pulverizing radix Picriae Felterrae, herba Pileae Scriptae, herba Houttuyniae, radix Ilicis Pubescentis, Scutellariae radix, and Glycyrrhrizae radix, wherein radix Picriae Felterrae, herba Pileae Scriptae, herba Houttuyniae, radix Ilicis Pubescentis, and Glycyrrhrizae radix, placing into a pot-group countercurrent extraction unit, adding 6-12 times of water, and soaking for 15-60 min; decocting under heating, adding Scutellariae radix after boiling, extracting for 2 times (each time for 1-3 hr), mixing extractive solutions, filtering, transferring filtrate to double-effect concentrating tank, vacuum concentrating under reduced pressure to obtain extract, adding ethanol to ethanol content of 50%, 60% or 70%, standing, filtering, concentrating filtrate to obtain extract,
(3) adding appropriate amount of sucrose powder into the above extract, granulating, and drying.
2. The traditional Chinese medicine granule as claimed in claim 1, which is prepared from the following components in proportion:
900g of picria felterrae lour, 700g of glabrous sarcandra herb, 450g of houttuynia cordata, 450g of pubescent holly root, 250g of baical skullcap root, 100g of liquorice and 850g of cane sugar.
3. The preparation method of the traditional Chinese medicine granules of claim 1, which is characterized by comprising the following steps:
(1) the preparation method of the sucrose powder comprises the following steps: pulverizing sucrose into superfine powder by micronizing technology;
(2) extracting the traditional Chinese medicine raw materials: taking radix Picriae Felterrae, herba Pileae Scriptae, herba Houttuyniae, radix Ilicis Pubescentis, Scutellariae radix, and Glycyrrhrizae radix, coarsely pulverizing, wherein the five medicines of radix Picriae Felterrae, herba Pileae Scriptae, herba Houttuyniae, radix Ilicis Pubescentis, and Glycyrrhrizae radix are firstly put into a pot-group type countercurrent extraction machine set, adding 9 times of water of the total weight of the traditional Chinese medicinal materials, soaking for 30 minutes, heating, decocting, boiling, adding Scutellariae radix, extracting for 2 times, extracting for 2 hours for the first time, adding 6 times of water of the total weight of the traditional Chinese medicinal materials for the second time, extracting for 1 hour, mixing the extractive solutions, filtering with a 1.5 μm filter membrane, transferring the filtrate into a double-effect concentration paste-collecting tank, vacuum concentrating to obtain an extract with a relative density of 1.15-1.20 at 60 ℃, adding ethanol to make the ethanol content 70%, standing for 24 hours, filtering with a 1.5 μm filter membrane, transferring the filtrate into a double-effect concentration paste-collecting tank, recovering ethanol, and vacuum concentrating at low temperature to obtain an extract with a relative density of 1.28-1.32 at 60 ℃;
(3) adding appropriate amount of sucrose powder into the above extract, granulating, and drying.
4. The use of the Chinese medicinal granule of claim 1 in the preparation of medicaments for treating upper respiratory tract infection, sterilizing and resisting virus, eliminating inflammation, improving the functions of internal organs of a body and enhancing the resistance of the body.
5. The use of the Chinese medicinal granule of claim 1 in the preparation of a medicament having anti-inflammatory effects.
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