CN116603042A - Traditional Chinese medicine preparation for treating initial stage of viral influenza and preparation method and application thereof - Google Patents

Abstract

The invention discloses a traditional Chinese medicine preparation for treating an initial stage of viral influenza, which comprises the following raw material medicines in parts by weight: 15 parts of honeysuckle, 15 parts of weeping forsythiae capsule, 10 parts of radix bupleuri, 10 parts of baical skullcap root, 12 parts of rhizoma atractylodis, 10 parts of wrinkled gianthyssop herb, 8 parts of great burdock achene, 15 parts of Indian buead, 8 parts of caulis perllae, 6 parts of almond, 10 parts of turmeric, and 10 parts of incised notopterygium rhizome. The traditional Chinese medicine preparation has obvious improvement effects on fever, muscle pain, pharyngalgia and cough caused by the initial stage of the viral influenza, and is obviously superior to the traditional Chinese medicine in antipyretic speed compared with the traditional Chinese medicine.

Description

Traditional Chinese medicine preparation for treating initial stage of viral influenza and preparation method and application thereof

Technical Field

The invention relates to the technical field of traditional Chinese medicines. More specifically, the invention relates to a traditional Chinese medicine preparation for treating the initial stage of viral influenza, a preparation method and application thereof.

Background

Influenza is an acute respiratory infectious disease caused by viruses and is transmitted through the nasal cavity mainly by exposure to airborne or object surface pathogens. Viruses are present in the respiratory tract of a patient and spread by droplets produced when the patient sneezes or coughs. The influenza has strong infectivity, high transmission speed, difficult control of transmission paths and great difficulty in prevention and control. Clinical symptoms are usually fever, headache, cough, pharyngalgia, muscular soreness, hypodynamia, severe symptoms such as pneumonia and respiratory failure can appear in severe cases. Influenza is urgent in onset, severe in symptoms, seriously affects the daily life of patients, and can be developed into a social large-scale cold. Therefore, it is particularly important to control the progression of influenza in its early stages.

Disclosure of Invention

The invention aims to provide a traditional Chinese medicine preparation for treating an initial stage of viral influenza, and a preparation method and application thereof.

To achieve these objects and other advantages and in accordance with the purpose of the invention, there is provided a Chinese medicinal preparation for treating an early stage of viral influenza, comprising the following raw materials in parts by weight: 15 parts of honeysuckle, 15 parts of weeping forsythiae capsule, 10 parts of radix bupleuri, 10 parts of baical skullcap root, 12 parts of rhizoma atractylodis, 10 parts of wrinkled gianthyssop herb, 8 parts of great burdock achene, 15 parts of Indian buead, 8 parts of caulis perllae, 6 parts of almond, 10 parts of turmeric, and 10 parts of incised notopterygium rhizome.

The invention also provides a preparation method of the traditional Chinese medicine preparation, which comprises the following steps:

taking the honeysuckle decoction pieces, fructus forsythiae decoction pieces, radix bupleuri decoction pieces, radix scutellariae decoction pieces, rhizoma atractylodis decoction pieces, wrinkled gianthyssop decoction pieces, burdock decoction pieces, poria cocos decoction pieces, caulis perllae decoction pieces, almond decoction pieces, rhizoma curcumae longae decoction pieces and notopterygium root decoction pieces, respectively granulating, and uniformly mixing.

Preferably, the method for granulating a crude drug decoction piece comprises the following steps: taking the above raw material decoction pieces in parts by weight, adding 8-12 times of water, decocting for 30 minutes to 2 hours, filtering, reserving the raw material decoction pieces, adding 6-8 times of water again, decocting for 20 minutes to 2 hours, filtering, combining the two filtrates, vacuum drying and concentrating at 60-80 ℃ to obtain extract, enabling the density of the extract to be 1.00-1.23 at 70+/-5 ℃, sieving the extract through a 80-150 mesh sieve after spray drying to obtain extract powder, adding silicon dioxide with the particle size of 0.3%, magnesium stearate with the particle size of 0.1% and maltodextrin with the particle size of the complement, uniformly mixing, granulating, and obtaining the raw material granules.

It is preferred that the composition of the present invention,

each 1g of honeysuckle particles contains 23.0 to 55.0mg of chlorogenic acid, and phenolic acid-containing substances account for 35.0 to 81.0mg of the total amount of chlorogenic acid, 3, 5-di-O-caffeoylquinic acid and 4, 5-di-O-caffeoylquinic acid;

each 1g of fructus forsythiae granule contains 10.0 mg-30.0 mg of forsythin;

each 1g of the bupleurum particles contains 10.0 to 30.0mg of saikosaponin a;

each 1g of baicalin particles contains 148.0 mg-274.0 mg of baicalin;

each 1g of rhizoma atractylodis granule contains 0.086 mg-0.650 mg of chlorogenic acid;

each 1g of the agastache particles contains 0.7 mg-3.0 mg of pogostemon ketone;

each 1g of burdock granules contains 110.70 mg-230.0 mg of arctiin;

each 1g of poria cocos granule contains 0.10 mg-0.40 mg of poria cocos acid B and 0.08 mg-0.30 mg of poria cocos acid A;

1.2mg to 4.0mg of rosmarinic acid is contained in each 1g of caulis perllae granule;

each 1g of almond particles contains 60.0 mg-120.0 mg of amygdalin;

the curcuma zedoary glycol is contained in each 1g of curcuma zedoary particle by 0.5 mg-2.5 mg;

each 1g of the notopterygium root particles contains 1.5mg to 8.0mg of ferulic acid and 0.5mg to 4.0mg of total content of notopterygium root alcohol and isoimperatorin.

The invention also provides application of the traditional Chinese medicine preparation in preparation of the traditional Chinese medicine preparation for treating the initial stage of viral influenza.

Preferably, the traditional Chinese medicine preparation is in the form of granules.

The invention at least comprises the following beneficial effects:

At the beginning of the viral cold, pathogenic wind-heat with damp-toxin invades the lung and defensive qi, and is in the defensive qi system, and the pathogenic wind-heat stagnates in the stomach and spleen, and the pathogenic wind-heat stagnates in the muscle striae, which causes fever and body pain. Pathogenic factors entering from the mouth and nose can attack the lung and cough can be seen if lung qi is not dispersed; wind-heat accumulation, damp-heat accumulation and toxic formation, and invasion of heat toxin into the lung system portal, manifested as red, swollen and painful throat. The disorder of qi movement can cause nausea and anorexia. A red tongue with yellow coating and rapid pulse, a pale tongue with dark coating and a slippery pulse due to excessive damp-toxin.

The honeysuckle and the weeping forsythia have aromatic smell, so that the honeysuckle and weeping forsythia not only can disperse wind and heat, clear heat and detoxify, but also can remove dirt and turbid qi, and can remove Wei Fenbiao evil thoroughly, and meanwhile, the characteristics of toxin accumulation and turbid qi inclusion are taken into consideration, so the honeysuckle and weeping forsythia are reused as monarch drugs;

bupleurum root, radix bupleuri, with pungent and cold nature, is the key herb for relieving muscles and has the effect of soothing the vital energy; notopterygium root, rhizoma Et radix Notopterygium, helps bupleuri radix, pungent and dispel the exterior, has the effect of dispelling pathogenic wind and removing dampness. Wenyujin, rhizoma Wenyujin Concisa, has the actions of activating qi-flowing and resolving stagnation, and also can be used with Qiang Huo to relieve pain. Radix Scutellariae helps radix bupleuri to dispel pathogenic heat of shaoyang;

wrinkled giant hyssop, herba Pogostemonis, relieving exterior syndrome and resolving dampness, and taking the fragrant qi to resolve the turbid dampness; poria is matched for strengthening spleen and promoting diuresis, and promoting wrinkled giant hyssop for eliminating turbid dampness;

rhizoma atractylodis, capable of dispelling wind, strengthening spleen and eliminating dampness. Fructus Arctii, having effects of dispelling wind and heat, dispersing lung qi, removing toxic substances, relieving swelling and relieving sore throat. Caulis Perillae, with effects of regulating qi and relieving middle energizer, can be used in combination with semen Armeniacae amarum for lowering and promoting lung qi to relieve asthma and cough;

The whole recipe aims at the pathogenesis of the disease, adopts the treatment rules of dispelling wind, clearing heat, resolving dampness, removing toxicity and regulating qi movement, so that the heat accumulated on the surface of the muscle is accumulated on the heat of damp evil, and the heat of qi movement stagnation is dispersed and removed.

Compared with the traditional Chinese medicine powder for treating cough, the traditional Chinese medicine powder is prepared by combining chest and hypochondrium bitter taste and no desire to eat and adding two traditional Chinese medicines of radix bupleuri and radix scutellariae on the basis of treating exogenous wind-heat and dry mouth cough, and aims at focusing on resolving heat stagnation. Radix bupleuri is taken to enter liver, gall bladder and lung meridians, dispel pathogenic factors and dispel heat, radix scutellariae is taken to enter lung, gall bladder meridians, spleen, large intestine and small intestine meridians due to bitter and cold, and is good at clearing heat of upper-jiao, and the two herbs are combined to clear heat of half exterior and half interior, clear heat and resolve depression, and assist the whole formula in bringing down fever. Rhizoma Wenyujin Concisa is added to the recipe to assist bupleuri radix and Scutellariae radix in harmonizing ying and wei. Semen Armeniacae amarum can be added to treat lung qi depression and cough and asthma. Added into Yinqiao powder mainly for dispersing, lifting and floating, so that the Chinese medicinal materials can be reduced, and the qi movement can be regulated, so that the lung qi can be regulated, and the cough relieving effect of the whole formula can be achieved.

The actual treatment proves that the traditional Chinese medicine preparation has obvious improvement effects on fever, muscle pain, pharyngalgia and cough caused by the initial stage of the viral influenza, and compared with the traditional Chinese medicine, the traditional Chinese medicine preparation is obviously superior to the traditional Chinese medicine in antipyretic speed.

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

Detailed Description

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

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

< example >

A traditional Chinese medicine preparation for treating the initial stage of viral influenza comprises the following raw materials in parts by weight: 15 parts of honeysuckle, 15 parts of weeping forsythiae capsule, 10 parts of radix bupleuri, 10 parts of baical skullcap root, 12 parts of rhizoma atractylodis, 10 parts of wrinkled gianthyssop herb, 8 parts of great burdock achene, 15 parts of Indian buead, 8 parts of caulis perllae, 6 parts of almond, 10 parts of turmeric, and 10 parts of incised notopterygium rhizome.

The preparation method of the traditional Chinese medicine preparation comprises the following steps:

taking the honeysuckle decoction pieces, fructus forsythiae decoction pieces, radix bupleuri decoction pieces, radix scutellariae decoction pieces, rhizoma atractylodis decoction pieces, wrinkled gianthyssop decoction pieces, burdock decoction pieces, poria cocos decoction pieces, caulis perllae decoction pieces, almond decoction pieces, rhizoma curcumae longae decoction pieces and notopterygium root decoction pieces, respectively granulating, and uniformly mixing.

Specifically, the method for preparing the honeysuckle decoction pieces into particles comprises the following steps: decocting the honeysuckle decoction pieces in 10-12 times of water for 30 minutes, filtering, reserving the honeysuckle decoction pieces, adding 6-8 times of water again, decocting for 20 minutes, filtering, combining the two filtrates, vacuum drying and concentrating at 60-80 ℃ to obtain extract, enabling the density of the extract to be 1.02-1.15 at 70+/-5 ℃, sieving the extract by 80-150 meshes to obtain extract powder, adding silicon dioxide with the grain size of 0.3%, magnesium stearate with the grain size of 0.1% and maltodextrin with the grain size of the complement, uniformly mixing, granulating, and obtaining honeysuckle grains.

Specifically, the method for preparing the fructus forsythiae decoction pieces into granules comprises the following steps: decocting fructus forsythiae decoction pieces in 8-10 times of water for 1-2 hr, filtering, retaining fructus forsythiae decoction pieces, adding 6-8 times of water again, decocting for 1-2 hr, filtering, mixing the two filtrates, vacuum drying at 60-80deg.C to obtain extract with paste density of 1.02-1.15 at 70+ -5deg.C, spray drying the extract, sieving with 80-150 mesh sieve to obtain extract powder, adding 0.3% silicon dioxide, 0.1% magnesium stearate and maltodextrin, mixing, and granulating to obtain fructus forsythiae granule.

Specifically, the method for preparing the bupleurum chinense decoction pieces into granules comprises the following steps: decocting the prepared radix bupleuri decoction pieces in 8-10 times of water for 1-2 hours, filtering, reserving the radix bupleuri decoction pieces, adding 6-8 times of water again, decocting for 1-2 hours, filtering, combining the two filtrates, vacuum drying and concentrating at 60-80 ℃ to obtain extract, enabling the density of the extract to be 1.18-1.23 at 70+/-5 ℃, sieving the extract through a 80-mesh sieve after spray drying to obtain extract powder, adding silicon dioxide with the particle preparation amount of 0.3%, magnesium stearate with the particle preparation amount of maltodextrin, uniformly mixing, granulating, and obtaining the radix bupleuri particles.

Specifically, the method for preparing the baical skullcap root decoction pieces into granules comprises the following steps: decocting the above radix Scutellariae decoction pieces with 8-10 times of water for 1-2 hr, filtering, retaining radix Scutellariae decoction pieces, adding 6-8 times of water again, decocting for 1-2 hr, filtering, mixing the two filtrates, vacuum drying at 60-80deg.C to obtain extract with paste density of 1.00-1.10 at 70+ -5deg.C, spray drying the extract, sieving with 80-150 mesh sieve to obtain extract powder, adding 0.3% silicon dioxide, 0.1% magnesium stearate and maltodextrin, mixing, and granulating to obtain radix Scutellariae granule.

Specifically, the method for preparing the rhizoma atractylodis decoction pieces into granules comprises the following steps: decocting rhizoma Atractylodis decoction pieces with 8-10 times of water for 1-2 hr, filtering, retaining rhizoma Atractylodis decoction pieces, adding 6-8 times of water again, decocting for 1-2 hr, filtering, mixing the two filtrates, vacuum drying at 60-80deg.C to obtain extract with paste density of 1.03-1.10 at 70+ -5deg.C, spray drying the extract, sieving with 80-150 mesh sieve to obtain extract powder, adding 0.3% silicon dioxide, 0.1% magnesium stearate and maltodextrin, mixing, and granulating to obtain rhizoma Atractylodis granule.

Specifically, the method for preparing the wrinkled giant hyssop decoction pieces into particles comprises the following steps: decocting herba Agastaches decoction pieces in 8-10 times of water for 1-2 hr, filtering, retaining herba Agastaches decoction pieces, adding 6-8 times of water again, decocting for 1-2 hr, filtering, mixing the two filtrates, vacuum drying at 60-80deg.C to obtain extract with paste density of 1.00-1.10 at 70+ -5deg.C, spray drying the extract, sieving with 80-150 mesh sieve to obtain extract powder, adding 0.3% silicon dioxide, 0.1% magnesium stearate and maltodextrin, mixing, and granulating to obtain herba Agastaches granule.

Specifically, the method for preparing the burdock decoction pieces into granules comprises the following steps: decocting fructus Arctii decoction pieces with 8-10 times of water for 1-2 hr, filtering, retaining fructus Arctii decoction pieces, adding 6-8 times of water again, decocting for 1-2 hr, filtering, mixing the two filtrates, vacuum drying at 60-80deg.C, concentrating to obtain extract with paste density of 1.02-1.10 at 70+ -5deg.C, spray drying the extract, sieving with 80-150 mesh sieve to obtain extract powder, adding 0.3% silicon dioxide, 0.1% magnesium stearate and maltodextrin, mixing, and granulating to obtain fructus Arctii granule.

Specifically, the method for preparing the poria cocos decoction pieces into granules comprises the following steps: decocting Poria decoction pieces with 8-10 times of water for 1-2 hr, filtering, retaining Poria decoction pieces, adding 6-8 times of water again, decocting for 1-2 hr, filtering, mixing the two filtrates, vacuum drying at 60-80deg.C to obtain extract with paste density of 1.00-1.10 at 70+ -5deg.C, spray drying the extract, sieving with 80-150 mesh sieve to obtain extract powder, adding 0.3% silicon dioxide, 0.1% magnesium stearate and maltodextrin, mixing, and granulating to obtain Poria granule.

Specifically, the method for preparing the caulis perllae decoction pieces into granules comprises the following steps: decocting the caulis perllae decoction pieces in 8 times of water for 1.5 hours, filtering, reserving the caulis perllae decoction pieces, adding 6 times of water again, decocting for 1 hour, filtering, combining the two filtrates, vacuum drying and concentrating at 60-80 ℃ to obtain extract, enabling the density of the extract to be 1.05-1.08 at 70+/-5 ℃, sieving the extract through a 80-150 mesh sieve to obtain extract powder, adding silicon dioxide with the grain size of 0.3%, magnesium stearate with the grain size of 0.1% and maltodextrin with the grain size of the complement, uniformly mixing, granulating, and obtaining the caulis perllae granules.

Specifically, the method for preparing the almond decoction pieces into granules comprises the following steps: taking the almond decoction pieces in parts by weight, adding 8-10 times of water, decocting for 1-2 hours, filtering, reserving the almond decoction pieces, adding 6-8 times of water again, decocting for 1-2 hours, filtering, combining the two filtrates, vacuum drying and concentrating at 60-80 ℃ to obtain extract, enabling the density of the extract to be 1.04-1.07 at 70+/-5 ℃, sieving the extract through a 80-150 mesh sieve after spray drying to obtain extract powder, adding silicon dioxide with the particle preparation amount of 0.3%, magnesium stearate with the particle preparation amount of 0.1% and maltodextrin with the particle preparation amount of the supplement, uniformly mixing, granulating, and obtaining the almond particles.

Specifically, the method for preparing the curcuma longa decoction pieces into particles comprises the following steps: decocting rhizoma Wenyujin Concisa decoction pieces in 8-10 times of water for 1-2 hours, filtering, reserving rhizoma Wenyujin Concisa decoction pieces, adding 6-8 times of water again, decocting for 1-2 hours, filtering, combining the two filtrates, vacuum drying and concentrating at 60-80 ℃ to obtain extract, spraying and drying the extract with density of 1.00-1.10 at 70+ -5 ℃, sieving the extract with 80-150 meshes to obtain extract powder, adding silicon dioxide with particle content of 0.3%, magnesium stearate with particle content of 0.1% and maltodextrin with particle content, uniformly mixing, granulating to obtain rhizoma Wenyujin Concisa granule.

Specifically, the method for preparing the notopterygium root decoction pieces into granules comprises the following steps: decocting the notopterygium root decoction pieces in 8-10 times of water for 1-2 hours, filtering, reserving the notopterygium root decoction pieces, adding 6-8 times of water again, decocting for 1-2 hours, filtering, combining the two filtrates, vacuum drying and concentrating at 60-80 ℃ to obtain extract, enabling the density of the extract to be 1.00-1.10 at 70+/-5 ℃, sieving the extract through a 80-150 mesh sieve after spray drying to obtain extract powder, adding silicon dioxide with the particle preparation amount of 0.3%, magnesium stearate with the particle preparation amount of 0.1% and maltodextrin with the particle preparation amount of the supplement, uniformly mixing, granulating, and obtaining notopterygium root particles.

< quality control of formulation >

1. And (3) quality control of honeysuckle particles:

the identification method comprises the following steps: taking 1g of the product, grinding, adding 10ml of methanol, carrying out ultrasonic treatment for 20 minutes, cooling, filtering, and taking filtrate as a test solution. And (3) taking 2g of honeysuckle flower reference medicine, adding 50ml of water, boiling for 30 minutes, filtering, evaporating filtrate to dryness, and preparing the reference medicine solution by the same method from the step of adding 10ml of methanol into residues. And adding methanol into chlorogenic acid reference substance to obtain 1mg solution per 1ml, and taking the chlorogenic acid reference substance solution as reference substance solution. According to thin layer chromatography (0502 of Chinese pharmacopoeia 2020 edition), 5 μl of each of the test solution and the reference solution is absorbed, 10 μl of the reference solution is respectively spotted on the same silica gel G thin layer plate, and the supernatant of butyl acetate-formic acid-water (7:2.5:2.5) is used as developing agent, and then developed, taken out, dried, and inspected under ultraviolet lamp (365 nm). In the sample chromatogram, fluorescent spots with the same color appear at the positions corresponding to the control chromatogram and the control chromatogram.

And (3) measuring the content of active ingredients:

1) Preparation of a control solution: taking chlorogenic acid reference substance, 3, 5-di-O-caffeoylquinic acid reference substance and 4, 5-di-O-caffeoylquinic acid reference substance, precisely weighing, placing into brown measuring flask, and adding 75% methanol to obtain solution containing 0.28mg, 0.15mg and 44 μg per 1 ml.

2) Preparation of test solution: taking a proper amount of the product, grinding, taking about 0.2g, precisely weighing, placing into a conical flask with a plug, precisely adding 50ml of 75% methanol, weighing, performing ultrasonic treatment (power 500W, frequency 40 kHz) for 30 minutes, cooling, weighing again, supplementing the lost weight with 75% methanol, shaking uniformly, filtering, and taking a subsequent filtrate.

3) And (3) measuring: respectively precisely sucking 10 μl of each of the control solution and the sample solution, and injecting into a liquid chromatograph for measurement. Octadecylsilane chemically bonded silica is used as a filler in a liquid chromatograph; acetonitrile as mobile phase A and 0.1% phosphoric acid solution as mobile phase B, and performing gradient elution according to the following specification in Table 1; the column temperature is not higher than 25 ℃; the flow rate was 0.7ml per minute and the detection wavelength was 327nm. The theoretical plate number is not less than 10000 calculated according to chlorogenic acid peak.

TABLE 1

The product contains chlorogenic acid (C) per 1g ₁₆ H ₁₈ O ₉ ) 23.0 mg-55.0 mg of chlorogenic acid (C) per 1g of phenolic acid ₁₆ H ₁₈ O ₉ ) 3, 5-di-O-caffeoylquinic acid (C) ₂₅ H ₂₄ O ₁₂ ) And 4, 5-di-O-caffeoylquinic acid (C) ₂₅ H ₂₄ O ₁₂ ) The total amount of (2) should be 35.0mg to 81.0mg.

2. And (3) controlling the quality of fructus forsythiae particles:

the identification method comprises the following steps: taking 1g of the product, grinding, adding 25ml of methanol, carrying out ultrasonic treatment for 20 minutes, filtering, and taking the subsequent filtrate as a test solution. Taking 1g of fructus forsythiae reference medicine, adding 20ml of petroleum ether (30-60 ℃) into the medicine, sealing the medicine, carrying out ultrasonic treatment for 15 minutes, filtering, discarding petroleum ether liquid, volatilizing petroleum ether from residues, adding 20ml of methanol into the medicine, carrying out ultrasonic treatment for 20 minutes, filtering, evaporating filtrate into dryness, and adding 5ml of methanol into residues to dissolve the residues to obtain the reference medicine solution. And adding methanol into the forsythin reference substance to prepare a solution containing 0.25mg per 1ml, wherein the solution is used as a reference substance solution. According to thin layer chromatography (rule 0502 of Chinese pharmacopoeia 2020 edition), sucking 3 μl of each of the above three solutions, respectively spotting on the same silica gel G thin layer plate, spreading with chloroform-methanol (8:1) as developing agent, taking out, air drying, spraying 10% sulfuric acid ethanol solution, heating at 105deg.C until the color of the spots is clear, and inspecting in sunlight. In the sample chromatogram, spots with the same color appear at the positions corresponding to the control chromatogram and the control chromatogram.

And (3) measuring the content of active ingredients:

1) Preparation of a control solution: taking a proper amount of forsythin reference substance, precisely weighing, adding 50% methanol to prepare a solution containing 0.05mg per 1 ml.

2) Preparation of test solution: grinding the product, taking about 0.2g, precisely weighing, placing into a conical flask with a plug, precisely adding 25ml of 50% methanol, sealing, weighing, performing ultrasonic treatment (power 250W, frequency 40 kHz) for 40 minutes, cooling, weighing again, supplementing the lost weight with 50% methanol, shaking, filtering, and collecting the subsequent filtrate.

3) And (3) measuring: 2 μl of each of the control solution and the sample solution was precisely sucked, and the mixture was injected into a liquid chromatograph to be measured. Octadecylsilane chemically bonded silica is used as filler in a liquid chromatograph (column length is 100mm, inner diameter is 2.1mm, and particle diameter is 1.8 μm); acetonitrile as mobile phase a and 0.1% phosphoric acid solution as mobile phase B, and gradient elution was performed as specified in table 2 below; the flow rate is 0.2ml per minute; the column temperature is 25 ℃; the detection wavelength was 235nm. The theoretical plate number is not less than 10000 calculated according to the forsythin peak.

TABLE 2

The product contains forsythin (C) per 1g ₂₇ H ₃₄ O ₁₁ ) 10.0mg to 30.0mg.

3. The quality control of the bupleurum particles:

The identification method comprises the following steps: taking 0.5g of the product, grinding, adding 20ml of methanol, carrying out ultrasonic treatment for 10 minutes, filtering, and concentrating the filtrate to 2ml to obtain a sample solution. 1g of radix bupleuri reference medicine is added with 50ml of water, decocted for 30 minutes, filtered, the filtrate is evaporated to dryness, and the residue is added with 20ml of methanol, so as to prepare reference medicine solution. And adding methanol into the control of saikosaponin a to prepare a solution containing 0.5mg per 1ml as the control solution. According to thin layer chromatography (rule 0502 of Chinese pharmacopoeia 2020 edition), sucking 3 μl of each of the test solution and the control solution, and 6 μl of the control solution, respectively spotting on the same silica gel G thin layer plate, pre-saturating with ethyl acetate-ethanol-water (8:2:1) as developing agent for 30 min, developing, taking out, air drying, spraying 40% sulfuric acid solution of 2% p-dimethylaminobenzaldehyde, heating at 60deg.C until the spot color is clear, and respectively inspecting under sunlight and ultraviolet light (365 nm). In the chromatogram of the test sample, spots or fluorescent spots with the same color are respectively displayed at the corresponding positions of the chromatogram of the control medicinal material and the chromatogram of the control sample.

And (3) measuring the content of active ingredients:

1) Preparation of a control solution: taking a proper amount of saikosaponin a reference substance, precisely weighing, adding methanol to prepare a solution containing 75 mug per 1 ml.

2) Preparation of test solution: grinding the product, taking about 1.0g, precisely weighing, placing into a conical flask with a plug, precisely adding 25ml of 50% ethanol solution containing 5% concentrated ammonia test solution, sealing, weighing, performing ultrasonic treatment (power 250W, frequency 40 kHz) for 30 minutes, cooling, weighing again, supplementing the lost weight with 50% ethanol solution of 5% concentrated ammonia test solution, shaking, filtering, and collecting the subsequent filtrate.

3) And (3) measuring: 3 μl of each of the control solution and the sample solution was precisely sucked, and the mixture was injected into a liquid chromatograph to measure the volume of the sample solution. Octadecylsilane chemically bonded silica is used as filler in a liquid chromatograph (column length is 100mm, inner diameter is 2.1mm, and particle diameter is 1.7 μm); acetonitrile as mobile phase A and water as mobile phase B, and performing gradient elution according to the following specification in Table 3; the detection wavelength is 211nm and 250nm; the column temperature is 35 ℃; the flow rate was 0.4ml per minute. The number of theoretical plates is not less than 10000 according to the peak of saikosaponin a.

TABLE 3 Table 3

The product contains saikosaponin a (C) per 1g ₄₂ H ₆₈ O ₁₃ ) Should be 1.60mg to 5.00mg.

4. Quality control of the baikal skullcap root particles:

the identification method comprises the following steps: taking 0.5g of the product, grinding, adding 20ml of methanol, carrying out ultrasonic treatment for 30 minutes, filtering, evaporating the filtrate to dryness, and adding 2ml of methanol into residues to dissolve the residues to obtain a sample solution. And 1g of radix scutellariae reference medicine is prepared into a reference medicine solution by the same method. And adding methanol into baicalin reference substance, baicalein reference substance and wogonin reference substance to obtain solutions containing 1mg, 0.5mg and 0.5mg of each 1ml of the solutions as reference substance solutions. According to thin layer chromatography (rule 0502 of Chinese pharmacopoeia 2020 edition), sucking 2 μl of each of the sample solution and the control medicinal solution and 1 μl of each of the three control solutions, respectively spotting on the same polyamide film, pre-saturating with toluene-ethyl acetate-methanol-formic acid (10:3:1:2) as developing agent for 30 min, developing, taking out, air drying, and inspecting under ultraviolet lamp (365 nm). In the chromatogram of the sample, main spots with the same color appear at the positions corresponding to the chromatogram of the reference medicinal material; three identical dark spots were developed at the positions corresponding to the control chromatogram.

And (3) measuring the content of active ingredients:

1) Preparation of a control solution: taking appropriate amount of baicalin reference substance, precisely weighing, and adding methanol to obtain solution containing 25 μg per 1 ml.

2) Preparation of test solution: taking a proper amount of the product, grinding, taking about 0.1g, precisely weighing, placing into a 100ml measuring flask, adding a proper amount of water to dissolve, adding water to the scale, and shaking uniformly. Precisely measuring 1ml, placing into a 10ml measuring flask, adding methanol to scale, and shaking.

3) And (3) measuring: precisely sucking 1 μl of each of the control solution and the sample solution, and injecting into a liquid chromatograph for measurement. Octadecylsilane chemically bonded silica is used as filler in a liquid chromatograph (column length is 100mm, inner diameter is 2.1mm, and particle diameter is 1.8 μm); gradient elution was performed using methanol-water (47:53) as mobile phase (methanol as mobile phase A, water (0.05% phosphoric acid) as mobile phase B) as specified in Table 4; the flow rate is 0.35ml per minute; the column temperature is 30 ℃; the detection wavelength was 280nm. The theoretical plate number is not lower than 2500 calculated according to baicalin peak.

TABLE 4 Table 4

The product contains baicalin (C) per 1g ₂₁ H ₁₈ O ₁₁ ) 148.0mg to 274.0mg.

5. Controlling the quality of rhizoma atractylodis particles:

the identification method comprises the following steps: taking 1g of the product, grinding, adding 30ml of water to dissolve, shaking and extracting with ethyl acetate three times, 20ml each time, combining ethyl acetate solutions, evaporating to dryness, and adding 1.5ml of ethyl acetate into residues to dissolve to obtain a test solution. And (3) adding 50ml of water into 0.5g of rhizoma atractylodis reference medicine, boiling for 30 minutes, filtering, taking filtrate, and extracting three times by shaking with ethyl acetate to prepare reference medicine solution. According to thin layer chromatography (rule 0502 of Chinese pharmacopoeia 2020 edition), sucking 10 μl of each of the sample solution and the control medicinal solution, respectively spotting on the same silica gel G thin layer plate, pre-saturating with n-hexane-ethyl acetate-glacial acetic acid (4:3:0.1) as developing agent for 30 min, developing, taking out, air drying, and inspecting under ultraviolet lamp (365 nm). In the chromatogram of the test sample, fluorescent spots with the same color appear at the positions corresponding to the chromatogram of the control medicinal material.

And (3) measuring the content of active ingredients:

1) Preparation of a control solution: taking a proper amount of chlorogenic acid reference substance, precisely weighing, adding 10% methanol to prepare a solution containing 20 mug of chlorogenic acid per 1ml, and filtering to obtain reference substance solution.

2) Preparation of test solution: taking a proper amount of the product, grinding, taking about 0.5g, precisely weighing, placing into a conical flask with a plug, precisely adding 20ml of 10% methanol, sealing, weighing, performing ultrasonic treatment (power is 250W and frequency is 40 kHz) for 40 minutes, taking out, cooling, weighing again, supplementing the lost weight with 10% methanol, shaking uniformly, filtering, and taking the subsequent filtrate.

3) And (3) measuring: precisely sucking 5 μl of each of the control solution and the sample solution, and injecting into a liquid chromatograph for measurement. In the liquid chromatograph, octadecylsilane chemically bonded silica is used as a filler (column length is 100mm, inner diameter is 2.1mm, and particle diameter is 1.8 μm); gradient elution was performed using acetonitrile as mobile phase a and 0.1% formic acid as mobile phase B, as specified in table 5 below; the detection wavelength is 284nm for 0-8.5 min, 336nm for 8.5-45 min, and the flow rate is 0.4ml per minute; the column temperature is 30 ℃; the theoretical plate number should be not less than 5000 as calculated by chlorogenic acid peak.

TABLE 5

The product contains chlorogenic acid (C) per 1g ₁₆ H ₁₈ O ₉ ) Should be 0.086mg to 0.650mg.

6. Quality control of wrinkled giant hyssop particles:

the identification method comprises the following steps: taking 2g of the product, grinding, shaking for 10 minutes with 20ml of heated water, and cooling. Extracting with petroleum ether (30-60deg.C) for 3 times under shaking, mixing petroleum ether solutions 25ml each time, volatilizing, and dissolving residue with ethyl acetate 1ml to obtain test solution. And adding ethyl acetate into patchouli alcohol reference substance to prepare a solution containing 2mg per 1ml, wherein the solution is used as reference substance solution. According to thin layer chromatography (rule 0502 of Chinese pharmacopoeia 2020 edition), sucking 10 μl of the sample solution and 1 μl of the control solution, respectively spotting on the same silica gel G thin layer plate, pre-saturating with petroleum ether-ethyl acetate-formic acid (10:1:0.05) as developing agent for 30 min, developing, taking out, air drying, spraying 5% vanillin sulfuric acid ethanol solution, heating at 105deg.C until spots are clear, and inspecting in sunlight. The sample chromatogram has the same purple red spot at the corresponding position with the control chromatogram.

And (3) measuring the content of active ingredients:

1) Preparation of a control solution: taking appropriate amount of patchoulenone reference substance, precisely weighing, adding methanol to obtain solution containing 40 μg per 1ml, and taking as reference substance solution.

2) Preparation of test solution: taking a proper amount of the product, grinding, taking about 0.2g, precisely weighing, placing into a conical flask with a plug, precisely adding 20ml of methanol, weighing, performing ultrasonic treatment (power is 250W and frequency is 40 kHz) for 30 minutes, taking out, cooling, weighing again, supplementing the lost weight with methanol, shaking uniformly, filtering, and taking the subsequent filtrate.

3) And (3) measuring: 2 μl of each of the control solution and the sample solution was precisely sucked, and the mixture was injected into a liquid chromatograph to be measured. In the liquid chromatograph, octadecylsilane chemically bonded silica is used as a filler (column length is 100mm, inner diameter is 2.1mm, and particle diameter is 1.7 μm); gradient elution was performed using methanol as mobile phase a and 0.1% formic acid solution as mobile phase B, as specified in table 6 below; the flow rate is 0.3ml per minute; column temperature is 40 ℃; the detection wavelength is 310nm, and the theoretical plate number is not less than 3000 calculated according to the peak of patchoulenone.

TABLE 6

It was found that the product contains patchoulenone (C) per 1g ₁₂ H ₁₆ O ₄ ) Should be 0.7mg to 3.0mg.

7. And (3) controlling the quality of burdock granules:

the identification method comprises the following steps: taking 0.1g of the product, grinding, adding 20ml of ethanol, carrying out ultrasonic treatment for 30 minutes, filtering, evaporating the filtrate to dryness, and adding 1ml of ethanol into residues to dissolve the residues to obtain a sample solution. And 1g of burdock fruit reference medicine, 50ml of water is added, the mixture is decocted for 30 minutes, filtered, the filtrate is evaporated to dryness, and 20ml of ethanol is added into residues, so that a reference medicine solution is prepared. And adding ethanol into the arctiin reference substance to prepare a solution containing 5mg per 1ml of arctiin reference substance as a reference substance solution. According to thin layer chromatography (rule 0502 of Chinese pharmacopoeia 2020 edition), sucking 5 μl of each of the above three solutions, respectively spotting on the same silica gel G thin layer plate, spreading with chloroform-methanol-water (40:8:1) as developing agent, taking out, air drying, spraying 10% sulfuric acid ethanol solution, and heating at 105deg.C until the spot color is clear. In the sample chromatogram, spots with the same color appear at the positions corresponding to the control chromatogram and the control chromatogram.

And (3) measuring the content of active ingredients:

1) Preparation of a control solution: taking appropriate amount of arctiin reference substance, precisely weighing, and adding methanol to obtain solution containing 0.5mg per 1 ml.

2) Preparation of test solution: taking a proper amount of the product, grinding, taking about 0.1g, precisely weighing, placing into a conical flask with a plug, precisely adding 50ml of 70% methanol, sealing, weighing, performing ultrasonic treatment (power 250W, frequency 40 kHz) for 30 minutes, cooling, weighing again, supplementing the lost weight with 70% methanol, shaking uniformly, filtering, and taking the subsequent filtrate.

3) And (3) measuring: precisely sucking 1 μl of each of the control solution and the sample solution, and injecting into a liquid chromatograph for measurement. Octadecylsilane chemically bonded silica is used as filler in a liquid chromatograph (column length is 100mm, inner diameter is 2.1mm, and particle diameter is 1.8 μm); gradient elution was performed with methanol-water (43:57) as mobile phase (methanol as mobile phase a and water as mobile phase B) as specified in table 7 below; the flow rate is 0.3ml per minute; the theoretical plate number with the detection wavelength of 280nm is calculated according to arctiin peak and is not lower than 1500.

TABLE 7

The product contains arctiin (C) per 1g ₂₇ H ₃₄ O ₁₁ ) 110.0mg to 230.0mg.

8. Poria cocos granule quality control:

the identification method comprises the following steps: taking 3g of the product, grinding, adding 50ml of diethyl ether, carrying out ultrasonic treatment for 30 minutes, filtering, evaporating the filtrate to dryness, and adding 1ml of methanol into the residue to dissolve the residue to obtain a test sample solution. And 1g of poria cocos reference medicine is prepared into a reference medicine solution in the same way. According to thin layer chromatography (rule 0502 of Chinese pharmacopoeia 2020 edition), sucking 8 μl of sample solution and 12 μl of control medicinal solution, respectively spotting on the same silica gel G thin layer plate, spreading with toluene-ethyl acetate-formic acid (20:5:0.5) as developing agent, taking out, air drying, spraying 5% vanillin sulfuric acid solution, and heating at 105deg.C until the spots are clear. Spots of the same color appear on the chromatogram of the test sample at positions corresponding to those of the chromatogram of the control drug.

And (3) measuring the content of active ingredients:

1) Preparation of a control solution: taking appropriate amounts of pachymic acid B reference substance and pachymic acid A reference substance, precisely weighing, and adding methanol to obtain mixed solution containing 20 μg per 1 ml.

2) Preparation of test solution: taking a proper amount of the product, grinding, taking about 0.24g, precisely weighing, placing into a conical flask with a plug, precisely adding 10ml of 50% methanol, sealing, weighing, performing ultrasonic treatment (power is 250W, frequency is 40 kHz) for 30 minutes, cooling, weighing again, supplementing the lost weight with 50% methanol, shaking uniformly, centrifuging, taking supernatant, filtering, and taking subsequent filtrate.

3) And (3) measuring: 2 μl of each of the control solution and the sample solution is precisely sucked, and injected into an ultra-high performance liquid chromatograph for measurement. Octadecylsilane chemically bonded silica is used as filler in an ultra-high performance liquid chromatograph (column length is 150mm, inner diameter is 2.1mm, and particle diameter is 1.6 μm); gradient elution was performed using acetonitrile as mobile phase a and 0.1% formic acid solution as mobile phase B, as specified in table 8 below; the flow rate is 0.2ml per minute; the column temperature is 30 ℃; the detection wavelength was 252nm. The theoretical plate number is not less than 5000 calculated according to the pachymic acid B peak.

TABLE 8

It was found that the product contains pachymic acid B (C) per 1g ₃₀ H ₄₄ O ₅ ) 0.10mg to 0.40mg; pachymic acid A (C) ₃₁ H ₄₆ O ₅ ) Should be 0.08mg to 0.30mg.

9. Quality control of caulis Perillae granule:

the identification method comprises the following steps: taking 2g of the product, grinding, adding 25ml of methanol, carrying out ultrasonic treatment for 30 minutes, filtering, evaporating filtrate to dryness, and adding 1ml of methanol into residues to dissolve the residues to obtain a test sample solution. And adding 50ml of water into 1g of perilla stem control medicinal material, decocting for 30 minutes, filtering, evaporating filtrate to dryness, adding 25ml of methanol into residues, and preparing a control medicinal material solution by the same method. And adding methanol into rosmarinic acid reference substance to obtain solution containing 0.5mg per 1ml as reference substance solution. According to a thin layer chromatography (China Pharmacopeia 2020 edition rule 0502), sucking 1-4 μl of each of the above three solutions, respectively spotting on the same silica gel G thin layer plate, spreading with n-hexane-ethyl acetate-formic acid (3:3:0.2) as developing agent, taking out, air drying, and inspecting under ultraviolet lamp (365 nm). In the sample chromatogram, fluorescent spots with the same color appear at the positions corresponding to the control chromatogram and the control chromatogram.

And (3) measuring the content of active ingredients:

1) Preparation of a control solution: taking a proper amount of rosmarinic acid reference substance, precisely weighing, and adding 60% acetone to prepare a solution containing 40 μg per 1 ml.

2) Preparation of test solution: grinding the product, taking about 0.5g, precisely weighing, placing into a conical flask with a plug, precisely adding 25ml of 60% acetone, sealing, weighing, performing ultrasonic treatment (power 500W, frequency 40 kHz) for 30 minutes, cooling, weighing again, supplementing the lost weight with 60% acetone, shaking, filtering, and collecting the subsequent filtrate.

3) And (3) measuring: precisely sucking 5-20 μl of each of the reference solution and the sample solution, and injecting into a liquid chromatograph for measurement. Octadecylsilane chemically bonded silica is used as a filler in a liquid chromatograph; gradient elution was performed with methanol-0.1% formic acid solution (38:62) as mobile phase (methanol as mobile phase a,0.1% formic acid solution as mobile phase B) as specified in table 9 below; the column temperature is 30 ℃, the flow rate is 0.3mL/min, and the detection wavelength is 330nm. The number of theoretical plates should be not less than 3000 calculated as rosmarinic acid peak.

TABLE 9

The product contains rosmarinic acid (C) per 1g ₁₈ H ₁₆ O ₈ ) Should be 1.2mg to 4.0mg.

10. And (3) controlling the quality of almond particles:

the identification method comprises the following steps: grinding the materials into fine powder, grinding 0.1g, adding 10ml of methanol, performing ultrasonic treatment for 30 min, and filtering to obtain filtrate as sample solution. And (3) adding 0.3g of bitter apricot kernel reference medicine into 30ml of boiling water, keeping micro boiling for 30 minutes, filtering, evaporating filtrate to dryness, adding 10ml of methanol into residues, and preparing the reference medicine solution by the same method. And adding methanol into amygdalin reference substance to obtain 1mg solution per 1ml, and taking as reference substance solution. According to thin layer chromatography (rule 0502 of Chinese pharmacopoeia 2020 edition), sucking 3 μl of each of the test solution and the reference solution, respectively, and placing 5 μl of the reference solution on the same silica gel G thin layer plate, spreading with chloroform-ethyl acetate-methanol-water (15:40:22:10) as developing agent for 12 hr under 5-10deg.C, taking out, spraying 0.8% phosphomolybdic acid 15% sulfuric acid ethanol solution, and heating at 105deg.C until spot color development is clear. Spots of the same color appear on the sample chromatogram at the positions corresponding to the control material chromatogram and the control material chromatogram.

And (3) measuring the content of active ingredients:

1) Preparation of a control solution: taking appropriate amount of amygdalin reference substance, precisely weighing, and adding 50% methanol to obtain solution containing 50 μg per 1 ml.

2) Preparation of test solution: taking a proper amount of the product, grinding, taking about 0.2g, precisely weighing, placing into a conical flask with a plug, precisely adding 25ml of 50% methanol, weighing, performing ultrasonic treatment (power is 250W and frequency is 40 kHz) for 30 minutes, taking out, cooling, weighing again, supplementing the lost weight with 50% methanol, shaking uniformly, centrifuging (rotating at the speed of more than 4000 revolutions per minute) for 10 minutes, precisely weighing 2ml of supernatant, placing into a measuring flask with 25ml, diluting to a scale with 50% methanol, shaking uniformly, filtering, and taking subsequent filtrate.

3) And (3) measuring: precisely sucking 10 μl of each of the control solution and the sample solution, injecting into a liquid chromatograph, and measuring. Octadecylsilane chemically bonded silica is used as filler in liquid chromatograph (column length of 250mm, inner diameter of 4.6mm, particle diameter of 5 μm); acetonitrile-0.1% phosphoric acid solution (6:94) was used as mobile phase (isocratic elution); the flow rate is 0.3mL/min, and the column temperature is 20-25 ℃; the detection wavelength was 207nm. The theoretical plate number should be not less than 7000 calculated as amygdalin peak.

As measured, the product contains amygdalin (C) per 1g ₂₀ H ₂₇ NO ₁₁ ) 60.0mg to 120.0mg.

11. Quality control of curcuma longa particles:

the identification method comprises the following steps: taking 0.5g of the product, grinding, adding 20ml of methanol, carrying out ultrasonic treatment for 20 minutes, filtering, evaporating the filtrate at low temperature, and adding 1ml of methanol into the residue to dissolve the residue to obtain a sample solution. And (3) taking 0.5g of curcuma longa control medicinal material, adding 5ml of petroleum ether (30-60 ℃) and shaking for 30 minutes at any time, and filtering to obtain a filtrate serving as a control medicinal material solution. And adding methanol into the curcumenol reference substance to prepare a solution containing 1mg per 1ml of the curcumenol reference substance as a reference substance solution. According to thin layer chromatography (rule 0502 of Chinese pharmacopoeia 2020 edition), sucking 5 μl of each of the test solution and the control solution, and 2 μl of the control solution, respectively spotting on the same silica gel G thin layer plate, spreading with petroleum ether-ethyl acetate (22:1) as developing agent, taking out, air drying, spraying 1% vanillin sulfuric acid solution, and heating at 100deg.C until the color of spots is clear. In the sample chromatogram, spots with the same color appear at the positions corresponding to the control chromatogram and the control chromatogram.

And (3) measuring the content of active ingredients:

1) Preparation of a control solution: taking a proper amount of curcumenol reference substance, precisely weighing, adding 70% methanol to prepare a solution containing 25 mug per 1 ml.

2) Preparation of test solution: taking a proper amount of the product, grinding, taking about 0.5g, precisely weighing, placing into a conical flask with a plug, precisely adding 20ml of 70% methanol, sealing, weighing, performing ultrasonic treatment (power 250W, frequency 40 kHz) for 30 minutes, cooling, weighing again, supplementing the lost weight with 70% methanol, shaking uniformly, filtering, and taking the subsequent filtrate.

3) And (3) measuring: precisely sucking 1 μl of each of the control solution and the sample solution, and injecting into an ultra-high performance liquid chromatograph for measurement. Octadecylsilane chemically bonded silica is used as filler in an ultra-high performance liquid chromatograph (column length is 100mm, inner diameter is 2.1mm, and particle diameter is 1.8 μm); gradient elution was performed with acetonitrile-0.1% phosphoric acid solution (20:80) as mobile phase (acetonitrile as mobile phase a,0.1% phosphoric acid solution as mobile phase B) as specified in table 10 below; the flow rate was 0.3mL/min, the column temperature was 30deg.C, and the detection wavelength was 254nm. The theoretical plate number is not less than 5000 calculated according to the curcumenol peak.

Table 10

The product contains curcumenol (C) per 1g ₁₅ H ₂₂ O ₃ ) Should be 0.5mg to 2.5mg.

12. Controlling the quality of notopterygium root particles:

the identification method comprises the following steps: taking 1g of the product, grinding, adding 5ml of methanol, carrying out ultrasonic treatment for 20 minutes, standing, and taking supernatant as a test solution. 1g of notopterygium root reference medicine is prepared to obtain a reference medicine solution. Then taking the decursin reference substance, adding methanol to prepare a solution containing 0.5mg per 1ml, and taking the solution as the reference substance solution. According to thin layer chromatography (0502 of Chinese pharmacopoeia 2020 edition), sucking 10 μl of the sample solution, 4 μl of the control medicinal material solution and 4 μl of the control medicinal material solution, respectively spotting on the same silica gel G thin layer plate, spreading with chloroform-methanol (8:2) as developing agent, taking out, air drying, and inspecting under ultraviolet lamp (365 nm). In the sample chromatogram, fluorescent spots with the same color appear at the positions corresponding to the control chromatogram and the control chromatogram.

And (3) measuring the content of active ingredients:

1) Preparation of a control solution: taking appropriate amounts of ferulic acid reference substance, notopterol reference substance and isoimperatorin reference substance, precisely determining, and adding methanol to obtain mixed solution containing ferulic acid 25 μg, notopterol 8 μg and isoimperatorin 2 μg per 1 ml.

2) Preparation of test solution: the product is prepared by grinding proper amount, taking about 0.1g, precisely weighing, placing into conical flask with plug, precisely adding 25ml of 50% methanol, sealing, weighing, ultrasonic treating (power 250W, frequency 40 kHz) for 30 min, cooling, weighing again, supplementing the lost weight with 50% methanol, shaking, filtering, and collecting filtrate.

3) And (3) measuring: precisely sucking 2 μl of each of the control solution and the sample solution, and injecting into an ultra-high performance liquid chromatograph for measurement. Octadecylsilane chemically bonded silica is used as filler in an ultra-high performance liquid chromatograph (column length is 150mm, inner diameter is 2.1mm, particle diameter is 1.8 μm); gradient elution was performed using methanol as mobile phase a and 0.2% phosphoric acid solution as mobile phase B, as specified in table 11 below; the flow rate is 0.25ml per minute; the column temperature is 30 ℃; the detection wavelength was 316nm. The theoretical plate number is not less than 10000 calculated according to the alcohol peak of Notopterygii rhizoma.

TABLE 11

It was found that the product contains ferulic acid (C) per 1g ₁₀ H ₁₀ O ₄ ) 1.5mg to 8.0mg; notopterygium alcohol (C) ₂₁ H ₂₂ O ₅ ) And isoimperatorin (C) ₁₆ H ₁₄ O ₄ ) The total amount of (2) should be 0.5mg to 4.0mg.

< clinical test >

The study paper is used for carrying out follow-up medication on patients taking the traditional Chinese medicine preparation, the traditional Chinese medicine and the western medicine antipyretic.

1. The questionnaire content settings are shown in tables 12 and 13.

Table 12 patient basic information collection table

Table 13 statistics of efficacy of patients after taking the drugs

2. Investigation of group patient basic information condition statistics

The investigation is carried out to collect 97 cases of feedback, wherein 30 cases of traditional Chinese medicines (comprising 30 cases of traditional Chinese medicine classical prescription Yinqiao powder, xiaochaihu decoction, huoxiang Zhengqi powder and Shengshao powder) are applied, 30 cases of traditional Chinese medicine preparation are applied, 37 cases of western medicine antipyretics are combined by the traditional Chinese medicine preparation, and the statistics and grouping information of the basic conditions of patients are shown in Table 14. The basic conditions of patients of the traditional Chinese medicine group, the traditional Chinese medicine preparation group and the western medicine preparation combined antipyretic group have no significant difference (P is more than 0.05).

TABLE 14

3. Observation of drug efficacy

By arranging the questionnaires, the traditional Chinese medicine preparation and the western medicine antipyretic are combined to count the improvement effects of fever, muscle pain, pharyngalgia and cough and the occurrence of adverse reactions. The result adopts a cross-table chi-square test to calculate the significance difference, and takes 95% as a confidence interval, and the significance difference is found when P is less than 0.05. The results are shown in tables 15 to 17.

TABLE 15

Table 16

Note that: ^** compared with the traditional Chinese medicine group, the time for taking the traditional Chinese medicine preparation to restore the normal body temperature is obviously reduced (P is less than 0.05);

^*** compared with the traditional Chinese medicine group, the time for recovering the body temperature to be normal is obviously reduced (P is less than 0.05) by taking the traditional Chinese medicine preparation and combining western medicines;

TABLE 17

The result shows that the total effective rate of the antipyretic effect of the traditional Chinese medicine preparation is 96.70%, and the antipyretic effect of the traditional Chinese medicine preparation has no obvious difference (P is more than 0.05) with the antipyretic group of the traditional Chinese medicine preparation combined with western medicines; the total effective rate of the traditional Chinese medicine preparation for improving muscle pain is 91.30%, and the traditional Chinese medicine preparation has no obvious difference (P is more than 0.05) with a traditional Chinese medicine group and a western medicine antipyretic group combined with the traditional Chinese medicine preparation; the total effective rate of the Chinese medicinal preparation for improving the pharyngeal pain is 81.00%, and the Chinese medicinal preparation has no obvious difference (P is more than 0.05) with the traditional Chinese medicinal composition and the Chinese medicinal preparation combined western medicine antipyretic composition; the total effective rate of the traditional Chinese medicine preparation for improving cough is 70.80%, and the traditional Chinese medicine preparation has no obvious difference (P is more than 0.05) with the traditional Chinese medicine group and the western medicine antipyretic group combined with the traditional Chinese medicine preparation (Table 15); the average antipyretic time of the patients in the traditional Chinese medicine preparation group is 24.62+/-25.64 hours, and compared with the traditional Chinese medicine group, the patient has obvious difference (P is less than 0.05) (Table 5); the occurrence rate of adverse reaction of the traditional Chinese medicine preparation group and the traditional Chinese medicine group and the western medicine antipyretic group combined by the traditional Chinese medicine preparation is not significantly different (P is more than 0.05) (Table 6).

According to the analysis of the results, the traditional Chinese medicine preparation and the combined antipyretic have the effect of improving fever, muscle pain, pharyngalgia and cough caused by the initial stage of the viral influenza. Compared with the traditional Chinese medicine treatment, the traditional Chinese medicine preparation provided by the invention is obviously superior to the traditional Chinese medicine in terms of antipyretic speed, the effect is equivalent to that of the combined application of western medicines, and the occurrence rate of adverse reactions is not significant.

Although embodiments of the present invention have been disclosed above, it is not limited to the details and embodiments shown, it is well suited to various fields of use for which the invention is suited, and further modifications may be readily made by one skilled in the art, and the invention is therefore not to be limited to the particular details and examples shown and described herein, without departing from the general concepts defined by the claims and the equivalents thereof.

Claims (6)

1. The traditional Chinese medicine preparation for treating the initial stage of the viral influenza is characterized by comprising the following raw material medicines in parts by weight: 15 parts of honeysuckle, 15 parts of weeping forsythiae capsule, 10 parts of radix bupleuri, 10 parts of baical skullcap root, 12 parts of rhizoma atractylodis, 10 parts of wrinkled gianthyssop herb, 8 parts of great burdock achene, 15 parts of Indian buead, 8 parts of caulis perllae, 6 parts of almond, 10 parts of turmeric, and 10 parts of incised notopterygium rhizome.

2. The method for preparing a Chinese medicinal preparation according to claim 1, comprising:

taking the honeysuckle decoction pieces, fructus forsythiae decoction pieces, radix bupleuri decoction pieces, radix scutellariae decoction pieces, rhizoma atractylodis decoction pieces, wrinkled gianthyssop decoction pieces, burdock decoction pieces, poria cocos decoction pieces, caulis perllae decoction pieces, almond decoction pieces, rhizoma curcumae longae decoction pieces and notopterygium root decoction pieces, respectively granulating, and uniformly mixing.

3. The method for preparing a Chinese medicinal preparation according to claim 2, wherein the method for granulating a crude drug decoction piece comprises: taking the above raw material decoction pieces in parts by weight, adding 8-12 times of water, decocting for 30 minutes to 2 hours, filtering, reserving the raw material decoction pieces, adding 6-8 times of water again, decocting for 20 minutes to 2 hours, filtering, combining the two filtrates, vacuum drying and concentrating at 60-80 ℃ to obtain extract, enabling the density of the extract to be 1.00-1.23 at 70+/-5 ℃, sieving the extract through a 80-150 mesh sieve after spray drying to obtain extract powder, adding silicon dioxide with the particle size of 0.3%, magnesium stearate with the particle size of 0.1% and maltodextrin with the particle size of the complement, uniformly mixing, granulating, and obtaining the raw material granules.

4. The method for preparing the Chinese medicinal preparation according to claim 2,

Each 1g of honeysuckle particles contains 23.0 to 55.0mg of chlorogenic acid, and phenolic acid-containing substances account for 35.0 to 81.0mg of the total amount of chlorogenic acid, 3, 5-di-O-caffeoylquinic acid and 4, 5-di-O-caffeoylquinic acid;

each 1g of fructus forsythiae granule contains 10.0 mg-30.0 mg of forsythin;

each 1g of the bupleurum particles contains 10.0 to 30.0mg of saikosaponin a;

each 1g of baicalin particles contains 148.0 mg-274.0 mg of baicalin;

each 1g of rhizoma atractylodis granule contains 0.086 mg-0.650 mg of chlorogenic acid;

each 1g of the agastache particles contains 0.7 mg-3.0 mg of pogostemon ketone;

each 1g of burdock granules contains 110.70 mg-230.0 mg of arctiin;

each 1g of tuckahoe granule contains 0.10mg to 0.40mg of tuckahoe acid B and 0.08mg to 0.30mg of tuckahoe acid A;

1.2mg to 4.0mg of rosmarinic acid is contained in each 1g of caulis perllae granule;

each 1g of almond particles contains 60.0 mg-120.0 mg of amygdalin;

the curcuma zedoary glycol is contained in each 1g of curcuma zedoary particle by 0.5 mg-2.5 mg;

each 1g of the notopterygium root particles contains 1.5mg to 8.0mg of ferulic acid and 0.5mg to 4.0mg of total content of notopterygium root alcohol and isoimperatorin.

5. The use of a Chinese medicinal preparation as claimed in claim 1 for the preparation of a medicament for the treatment of an initial stage of viral influenza.

6. The use of a Chinese medicinal preparation according to claim 5, wherein the Chinese medicinal preparation is in the form of granules.