Traditional Chinese medicine preparation for treating early stage of viral cold and its preparation method and use

Abstract

The invention discloses a Chinese medicine preparation for treating the early stage of viral cold, comprising the following raw materials in parts by weight: 15 parts of honeysuckle, 15 parts of forsythia, 10 parts of bupleurum, 10 parts of scutellaria, 12 parts of atractylodes, 10 parts of patchouli, 8 parts of arctium, 15 parts of tuckahoe, 8 parts of sophora flavescens, 6 parts of apricot kernel, 10 parts of turmeric slices, and 10 parts of notopterygium. The Chinese medicine preparation of the invention has a significant improvement effect on fever, muscle pain, sore throat, and cough caused by the early stage of viral cold, and is significantly superior to traditional Chinese medicine in terms of fever-reducing speed compared with traditional Chinese medicine.

Description

Technical Field

[0001] The present invention relates to the technical field of traditional Chinese medicine, and more specifically, to a traditional Chinese medicine preparation for treating the early stage of viral cold, and a preparation method and use thereof. Background Art

[0002] Influenza is an acute respiratory infectious disease caused by a virus, which is mainly transmitted through the nasal cavity through contact with pathogens in the air or on the surface of objects. The virus exists in the patient's respiratory tract and is transmitted through droplets produced when the patient sneezes or coughs. Influenza is highly contagious, spreads quickly, and the transmission route is difficult to control, which makes prevention and control very difficult. Clinical symptoms usually manifest as fever, headache, cough, sore throat, muscle aches, and fatigue. In severe cases, severe symptoms such as pneumonia and respiratory failure may occur. Influenza has an acute onset and severe symptoms, which seriously affects the patient's daily life and can even develop into a large-scale social cold. Therefore, it is particularly important to control the course of influenza in the early stages of the disease. Summary of the invention

[0003] The purpose of the present invention is to provide a Chinese medicine preparation for treating the early stage of viral cold and its preparation method and use.

[0004] In order to achieve these purposes and other advantages according to the present invention, a traditional Chinese medicine preparation for treating the early stage of viral cold is provided, comprising the following raw materials in parts by weight: 15 parts of honeysuckle, 15 parts of forsythia, 10 parts of bupleurum, 10 parts of scutellaria, 12 parts of atractylodes, 10 parts of patches of patches, 8 parts of arctium, 15 parts of tuckahoe, 8 parts of perilla stem, 6 parts of apricot kernel, 10 parts of turmeric slices, and 10 parts of notopterygium.

[0005] The present invention also provides a method for preparing the above-mentioned Chinese medicine preparation, comprising:

[0006] Take the above-mentioned weight portions of honeysuckle slices, forsythia slices, northern bupleurum slices, scutellaria slices, atractylodes slices, patchouli slices, burdock fruit slices, Poria slices, perilla stem slices, almond slices, turmeric slices, and notopterygium wilfordii slices, make them into granules respectively, and then mix them evenly.

[0007] Preferably, the method for preparing a raw material medicine slice into granules comprises: taking a raw material medicine slice of the above weight portion, adding 8-12 times the amount of water and boiling for 30 minutes to 2 hours, filtering, retaining the raw material medicine slice and adding 6-8 times the amount of water again, boiling for 20 minutes to 2 hours, filtering, combining the two filtrates, vacuum drying and concentrating at 60-80°C to obtain an extract, the density of the paste is 1.00-1.23 at 70±5°C, spray drying the extract and sieving it through 80-150 mesh to obtain extract powder, adding 0.3% of silicon dioxide and 0.1% of magnesium stearate in the amount of granules to the extract powder and maltodextrin to make up the amount of granules, mixing evenly, and granulating to obtain raw material medicine granules.

[0008] Preferably,

[0009] Each 1g of honeysuckle granules contains 23.0mg-55.0mg of chlorogenic acid, and the total amount of phenolic acid substances, including chlorogenic acid, 3,5-di-O-caffeoylquinic acid and 4,5-di-O-caffeoylquinic acid, is 35.0mg-81.0mg;

[0010] Each 1g of Forsythia suspensa granules contains 10.0mg to 30.0mg of forsythiaside;

[0011] Each 1g of Bupleurum chinense granules contains 10.0mg to 30.0mg of saikosaponin a;

[0012] Each 1g of Huangqin granules contains 148.0mg to 274.0mg of baicalin;

[0013] Each 1g of Atractylodes lancea granules contains 0.086mg to 0.650mg of chlorogenic acid;

[0014] Each 1g of Patchouli Granules contains 0.7mg to 3.0mg of patchouli ketone;

[0015] Each 1g of burdock granules contains 110.70mg to 230.0mg of arctiin;

[0016] Each 1g of Poria granules contains 0.10mg-0.40mg of Pachymic Acid B and 0.08mg-0.30mg of Pachymic Acid A.

[0017] Each 1g of Sugeng granules contains 1.2mg~4.0mg of rosmarinic acid;

[0018] Each 1g of almond granules contains 60.0mg to 120.0mg of amygdalin;

[0019] Each 1g piece of turmeric granules contains 0.5mg to 2.5mg of curcuma diol;

[0020] Each 1g of Notopterygium wilfordii granules contains 1.5mg to 8.0mg of ferulic acid, and a total amount of notopterygium wilfordii alcohol and isoimperatorin of 0.5mg to 4.0mg.

[0021] The present invention also provides the use of the above-mentioned traditional Chinese medicine preparation in preparing the initial stage of treating viral cold.

[0022] Preferably, the dosage form of the traditional Chinese medicine preparation is granules.

[0023] The present invention has at least the following beneficial effects:

[0024] In the early stage of a viral cold, the evil of wind, heat and dampness and toxicity invade the lungs. The evil is in the Wei division, the Wei Yang is depressed, and the heat is gathered in the skin, which causes fever and body pain. The evil enters from the mouth and nose, and then it invades the lungs. The lung qi fails to be released, which causes coughing. The wind and heat are combined, the dampness accumulates and becomes toxic. The heat and toxicity invade the portal of the lung system, which causes redness, swelling and pain in the throat. The evil gradually enters the interior, and the qi movement is abnormal, which causes nausea and poor appetite. If the heat is strong, the tongue will be red, the coating will be yellow, and the pulse will be rapid. If the dampness and toxicity are strong, the tongue will be pale, the coating will be greasy, and the pulse will be slippery.

[0025] The honeysuckle and forsythia in this prescription have a fragrant smell, which can dispel wind-heat, clear away heat and detoxify, and eliminate filth and turbidity. While dispersing the external evil of the Wei division, they also take into account the characteristics of the evil qi accumulating into poison and mixed with filth and turbidity, so they are used as the main medicine.

[0026] Bupleurum is pungent in taste and cold in nature. It is a "muscle-relieving medicine" and has the function of relaxing the qi. Notopterygium root helps Bupleurum to disperse the exterior and has the effect of dispelling wind and dampness. Turmeric can promote qi and relieve depression, and can relieve pain together with Notopterygium root. Scutellaria root helps Bupleurum to penetrate and relieve the evil heat of Shaoyang.

[0027] Patchouli can dispel dampness from the exterior, and its aromatic aroma can dissolve dampness and turbidity inside the body; it is combined with Poria cocos to strengthen the spleen and move dampness, and help Patchouli dissolve dampness and turbidity inside the body;

[0028] Atractylodes lancea dispels wind, strengthens the spleen and dries dampness. Burdock seeds disperse wind and heat, clear the lungs and detoxify, reduce swelling and relieve sore throat. Sophora japonica root regulates qi and relieves fullness, and combined with apricot kernel, it lowers lung qi and relieves asthma and cough.

[0029] The whole prescription targets the pathogenesis of the disease, and adopts the treatment principles of dispersing wind and heat, resolving dampness and detoxifying, and regulating Qi, so that the heat accumulated on the skin surface, the heat hidden in dampness, and the heat caused by stagnant Qi can be dispersed and resolved.

[0030] Compared with the classic traditional cough treatment Yinqiao Powder, the whole prescription is based on the treatment of exogenous wind-heat and dry mouth cough, combined with the clinical patients' chest and flank bitterness and loss of appetite, and adds two Chinese medicines, Bupleurum and Scutellaria, to focus on clearing heat and relieving depression. Bupleurum is taken from the liver, gallbladder, and lung meridians, which means it can dispel evil qi and relieve fever. Scutellaria is taken from the bitter and cold lung, gallbladder, spleen, large intestine, and small intestine meridians, which means it can clear the heat of the upper jiao. The two medicines are used together to clear the heat of the half surface and half interior, clear heat and relieve depression, and help the whole prescription to reduce fever. Turmeric is added to the prescription to help Bupleurum and Scutellaria harmonize the Ying and Wei. Apricot kernel is added to reduce lung qi and relieve cough and asthma. Adding it to Yinqiao Powder, which is mainly used for dispersion and ascent, can make it descend while dispersing, one dispersing and one descending, regulate the qi mechanism, regulate the lung qi, and help the whole prescription to relieve cough.

[0031] The actual treatment verification shows that the Chinese medicine preparation of the present invention has a significant improvement effect on fever, muscle pain, sore throat and cough caused by the early stage of viral cold, and is significantly superior to traditional Chinese medicine in terms of fever-reducing speed.

[0032] Other advantages, objectives and features of the present invention will be embodied in part through the following description, and in part will be understood by those skilled in the art through study and practice of the present invention. DETAILED DESCRIPTION

[0033] The present invention is further described in detail below in conjunction with embodiments so that those skilled in the art can implement the invention with reference to the description.

[0034] It should be noted that the experimental methods described in the following embodiments are conventional methods unless otherwise specified, and the reagents and materials can be obtained from commercial channels unless otherwise specified.

[0035] <Example>

[0036] A traditional Chinese medicine preparation for treating the early stage of viral cold, comprising the following raw materials in parts by weight: 15 parts of honeysuckle, 15 parts of forsythia, 10 parts of bupleurum, 10 parts of scutellaria, 12 parts of atractylodes, 10 parts of patches of patches, 8 parts of burdock seeds, 15 parts of tuckahoe, 8 parts of perilla stem, 6 parts of apricot kernel, 10 parts of turmeric slices, and 10 parts of notopterygium wilfordii.

[0037] The preparation method of the above-mentioned Chinese medicine preparation comprises:

[0038] Take the above-mentioned weight portions of honeysuckle slices, forsythia slices, northern bupleurum slices, scutellaria slices, atractylodes slices, patchouli slices, burdock fruit slices, Poria slices, perilla stem slices, almond slices, turmeric slices, and notopterygium wilfordii slices, make them into granules respectively, and then mix them evenly.

[0039] Specifically, the method for making honeysuckle slices into granules includes: taking the above-mentioned weight portion of honeysuckle slices, adding 10-12 times the amount of water, boiling for 30 minutes, filtering, retaining the honeysuckle slices and adding 6-8 times the amount of water again, boiling for 20 minutes, filtering, combining the two filtrates, vacuum drying and concentrating at 60-80°C to obtain an extract, the density of the paste is 1.02-1.15 at 70±5°C, spray-drying the extract and sieving it through 80-150 mesh to obtain extract powder, adding 0.3% of silicon dioxide and 0.1% of magnesium stearate in a granule preparation amount and maltodextrin to make up the granule preparation amount to the extract powder, mixing evenly, and granulating to obtain honeysuckle granules.

[0040] Specifically, the method for making granules from the Forsythia slices includes: taking the Forsythia slices in the above-mentioned weight portion, adding 8-10 times the amount of water, decocting for 1-2 hours, filtering, retaining the Forsythia slices and adding 6-8 times the amount of water again, decocting for 1-2 hours, filtering, combining the two filtrates, vacuum drying and concentrating at 60-80°C to obtain an extract, the density of the paste is 1.02-1.15 at 70±5°C, spray-drying the extract and sieving it through 80-150 mesh to obtain extract powder, adding 0.3% of silicon dioxide and 0.1% of magnesium stearate in the amount of granules and maltodextrin to make up the amount of granules to the extract powder, mixing evenly, and granulating to obtain Forsythia suspensa granules.

[0041] Specifically, the method for making granules from the Northern Bupleurum slices includes: taking the Northern Bupleurum slices in the above-mentioned weight portion, adding 8-10 times the amount of water, decocting for 1-2 hours, filtering, retaining the Northern Bupleurum slices and adding 6-8 times the amount of water again, decocting for 1-2 hours, filtering, combining the two filtrates, vacuum drying and concentrating at 60-80°C to obtain an extract, the density of the paste is 1.18-1.23 at 70±5°C, spray-drying the extract and sieving it through 80 mesh to obtain extract powder, adding 0.3% of silicon dioxide and 0.1% of magnesium stearate in the amount of granules and maltodextrin to make up the amount of granules to the extract powder, mixing evenly, and granulating to obtain Northern Bupleurum granules.

[0042] Specifically, the method for preparing granules from the decoction pieces of Scutellaria baicalensis comprises: taking the decoction pieces of Scutellaria baicalensis in the above-mentioned weight proportion, adding 8-10 times the amount of water, decocting for 1-2 hours, filtering, retaining the decoction pieces of Scutellaria baicalensis and adding 6-8 times the amount of water again, decocting for 1-2 hours, filtering, combining the two filtrates, vacuum drying and concentrating at 60-80° C. to obtain an extract, wherein the density of the extract is 1.00-1.10 at 70±5° C., spray drying the extract and sieving it through 80-150 mesh to obtain an extract powder, adding 0.3% of silicon dioxide and 0.1% of magnesium stearate in a granule preparation amount and maltodextrin in a granule preparation amount to the extract powder, uniformly mixing, and granulating to obtain Scutellaria baicalensis granules.

[0043] Specifically, the method for making granules from Atractylodes macrocephala slices includes: taking the above-mentioned weight portion of Atractylodes macrocephala slices, adding 8-10 times the amount of water, decocting for 1-2 hours, filtering, retaining the Atractylodes macrocephala slices and adding 6-8 times the amount of water again, decocting for 1-2 hours, filtering, combining the two filtrates, vacuum drying and concentrating at 60-80°C to obtain an extract, the density of the paste is 1.03-1.10 at 70±5°C, spray-drying the extract and sieving it through 80-150 mesh to obtain extract powder, adding 0.3% of silicon dioxide and 0.1% of magnesium stearate in the amount of granules and maltodextrin to make up the amount of granules to the extract powder, mixing evenly, and granulating to obtain Atractylodes macrocephala granules.

[0044] Specifically, the method for making granules from Patchouli slices includes: taking the above-mentioned weight portion of Patchouli slices, adding 8-10 times the amount of water, decocting for 1-2 hours, filtering, retaining the Patchouli slices and adding 6-8 times the amount of water again, decocting for 1-2 hours, filtering, combining the two filtrates, vacuum drying and concentrating at 60-80°C to obtain an extract, the density of the paste is 1.00-1.10 at 70±5°C, spray-drying the extract and sieving it through 80-150 mesh to obtain extract powder, adding 0.3% of silicon dioxide and 0.1% of magnesium stearate in the amount of granules and maltodextrin to make up the amount of granules to the extract powder, mixing evenly, and granulating to obtain Patchouli granules.

[0045] Specifically, the method for preparing burdock fruit slices into granules comprises: taking the burdock fruit slices in the above-mentioned weight portion, adding 8-10 times the amount of water, boiling for 1-2 hours, filtering, retaining the burdock fruit slices and adding 6-8 times the amount of water again, boiling for 1-2 hours, filtering, combining the two filtrates, vacuum drying and concentrating at 60-80° C. to obtain an extract, wherein the density of the extract is 1.02-1.10 at 70±5° C., spray drying the extract and sieving it through 80-150 mesh to obtain an extract powder, adding 0.3% of silicon dioxide in the amount of granules, 0.1% of magnesium stearate and maltodextrin in the amount of granules to the extract powder, uniformly mixing, and granulating to obtain burdock fruit granules.

[0046] Specifically, the method for making granules from Poria cocos slices includes: taking the above-mentioned weight portion of Poria cocos slices, adding 8-10 times the amount of water, decocting for 1-2 hours, filtering, retaining the Poria cocos slices and adding 6-8 times the amount of water again, decocting for 1-2 hours, filtering, combining the two filtrates, vacuum drying and concentrating at 60-80°C to obtain an extract, the density of the paste is 1.00-1.10 at 70±5°C, spray-drying the extract and sieving it through 80-150 mesh to obtain extract powder, adding 0.3% of silicon dioxide and 0.1% of magnesium stearate in a granule preparation amount and maltodextrin to make up the granule preparation amount to the extract powder, mixing evenly, and granulating to obtain Poria cocos granules.

[0047] Specifically, the method for making Sugeng slices into granules includes: taking the above-mentioned Sugeng slices by weight, adding 8 times the amount of water and boiling for 1.5 hours, filtering, retaining the Sugeng slices and adding 6 times the amount of water again, boiling for 1 hour, filtering, combining the two filtrates, vacuum drying and concentrating at 60-80°C to obtain an extract, the density of the paste is 1.05-1.08 at 70±5°C, spray-drying the extract and sieving it through 80-150 mesh to obtain extract powder, adding 0.3% of silicon dioxide and 0.1% of magnesium stearate in the amount of granules and maltodextrin to make up the amount of granules to the extract powder, mixing evenly, and granulating to obtain Sugeng granules.

[0048] Specifically, the method for making almond slices into granules includes: taking the above-mentioned almond slices by weight, adding 8-10 times the amount of water, boiling for 1-2 hours, filtering, retaining the almond slices and adding 6-8 times the amount of water again, boiling for 1-2 hours, filtering, combining the two filtrates, vacuum drying and concentrating at 60-80°C to obtain an extract, the density of the paste is 1.04-1.07 at 70±5°C, spray drying the extract and sieving it through 80-150 mesh to obtain extract powder, adding 0.3% of silicon dioxide and 0.1% of magnesium stearate in the amount of granules and maltodextrin to make up the amount of granules to the extract powder, mixing evenly, and granulating to obtain almond granules.

[0049] Specifically, the method for preparing turmeric slices into granules comprises: taking the turmeric slices in the above-mentioned weight portion, adding 8-10 times the amount of water, decocting for 1-2 hours, filtering, retaining the turmeric slices and adding 6-8 times the amount of water again, decocting for 1-2 hours, filtering, combining the two filtrates, vacuum drying and concentrating at 60-80° C. to obtain an extract, wherein the density of the paste is 1.00-1.10 at 70±5° C., spray drying the extract and sieving it through 80-150 mesh to obtain an extract powder, adding 0.3% of silicon dioxide and 0.1% of magnesium stearate in a granule preparation amount and maltodextrin in a granule preparation amount to the extract powder, uniformly mixing, and granulating to obtain turmeric slice granules.

[0050] Specifically, the method for making granules from Notopterygium wilfordii slices includes: taking the Notopterygium wilfordii slices in the above-mentioned weight portion, adding 8-10 times the amount of water, decocting for 1-2 hours, filtering, retaining the Notopterygium wilfordii slices and adding 6-8 times the amount of water again, decocting for 1-2 hours, filtering, combining the two filtrates, vacuum drying and concentrating at 60-80°C to obtain an extract, the density of the paste being 1.00-1.10 at 70±5°C, spray-drying the extract and sieving it through 80-150 mesh to obtain an extract powder, adding 0.3% of silicon dioxide and 0.1% of magnesium stearate in a granule preparation amount and maltodextrin to make up the granule preparation amount to the extract powder, mixing evenly, and granulating to obtain Notopterygium wilfordii granules.

[0051] <Quality Control of Preparations>

[0052] 1. Quality control of honeysuckle granules:

[0053] Identification method: Take 1g of this product, grind it, add 10ml of methanol, ultrasonically treat it for 20 minutes, cool it, filter it, and take the filtrate as the test solution. Take another 2g of honeysuckle reference medicinal material, add 50ml of water, boil it for 30 minutes, filter it, evaporate the filtrate, and make the reference medicinal material solution in the same way as the residue from "add 10ml of methanol". Take the chlorogenic acid reference substance again, add methanol to make a solution containing 1mg per 1ml, as the reference substance solution. According to the thin layer chromatography method (General Rules 0502 of the 2020 Edition of the Chinese Pharmacopoeia), take 5μl of the test solution and the reference solution, and 10μl of the reference medicinal material solution, and spot them on the same silica gel G thin layer plate, use the upper layer of butyl acetate-formic acid-water (7:2.5:2.5) as the developing agent, develop, take out, dry, and inspect under ultraviolet light (365nm). In the test sample chromatogram, fluorescent spots of the same color appear at the corresponding positions in the control medicinal material chromatogram and the control sample chromatogram.

[0054] Determination of active ingredient content:

[0055] 1) Preparation of reference solution: Take appropriate amount of chlorogenic acid reference substance, 3,5-di-O-caffeoylquinic acid reference substance and 4,5-di-O-caffeoylquinic acid reference substance, accurately weigh them, place them in a brown volumetric flask, add 75% methanol to make solutions containing 0.28 mg, 0.15 mg and 44 μg per 1 ml.

[0056] 2) Preparation of test solution: Take an appropriate amount of the product, grind it into powder, take about 0.2g, weigh it accurately, put it in a stoppered conical flask, accurately add 50ml of 75% methanol, weigh it, treat it with ultrasound (power 500W, frequency 40kHz) for 30 minutes, let it cool, weigh it again, make up the lost weight with 75% methanol, shake it well, filter it, and take the filtrate to obtain it.

[0057] 3) Determination: Accurately pipette 10 μl of reference solution and test solution respectively, inject into liquid chromatograph for determination. The liquid chromatograph uses octadecylsilane bonded silica gel as filler; acetonitrile as mobile phase A, 0.1% phosphoric acid solution as mobile phase B, and gradient elution is performed according to the provisions in Table 1 below; the column temperature is not higher than 25°C; the flow rate is 0.7 ml per minute, and the detection wavelength is 327 nm. The theoretical plate number calculated based on the chlorogenic acid peak should be no less than 10,000.

[0058] Table 1

[0059]

[0060] It has been found that each 1g of this product contains chlorogenic acid (C 16 H 18 O9) should be 23.0mg~55.0mg, and each 1g contains phenolic acids, mainly chlorogenic acid (C 16 H 18O9), 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 ) should be 35.0mg~81.0mg.

[0061] 2. Quality control of Lianqiao granules:

[0062] Identification method: Take 1g of this product, grind it, add 25ml of methanol, ultrasonically treat it for 20 minutes, filter it, and take the filtrate as the test solution. Take another 1g of Forsythia suspensa reference medicinal material, add 20ml of petroleum ether (30-60℃), plug it, ultrasonically treat it for 15 minutes, filter it, discard the petroleum ether liquid, evaporate the petroleum ether from the residue, add 20ml of methanol, ultrasonically treat it for 20 minutes, filter it, evaporate the filtrate to dryness, add 5ml of methanol to dissolve the residue, and use it as the reference medicinal material solution. Take the Forsythia suspensa reference substance again, add methanol to make a solution containing 0.25mg per 1ml, and use it as the reference substance solution. According to the thin layer chromatography method (Chinese Pharmacopoeia 2020 General Rules 0502), 3 μl of each of the three solutions were taken and spotted on the same silica gel G thin layer plate, and chloroform-methanol (8:1) was used as the developing solvent. After development, the plate was taken out, dried, sprayed with 10% sulfuric acid ethanol solution, heated at 105°C until the spots were clearly colored, and then inspected under sunlight. In the chromatogram of the test sample, spots of the same color appeared at the corresponding positions of the chromatogram of the reference medicinal material and the chromatogram of the reference sample.

[0063] Determination of active ingredient content:

[0064] 1) Preparation of reference solution: Take an appropriate amount of forsythiaside reference substance, accurately weigh it, and add 50% methanol to make a solution containing 0.05 mg per 1 ml.

[0065] 2) Preparation of test solution: Take an appropriate amount of the product, grind it into powder, take about 0.2g, weigh it accurately, put it in a stoppered conical flask, accurately add 25ml of 50% methanol, stopper it, weigh it, ultrasonically treat it (power 250W, frequency 40kHz) for 40 minutes, cool it, weigh it again, make up the lost weight with 50% methanol, shake it well, filter it, and take the filtrate to obtain the solution.

[0066] 3) Determination: Accurately pipette 2 μl of reference solution and test solution respectively, inject into liquid chromatograph for determination. The liquid chromatograph uses octadecylsilane bonded silica gel as filler (column length is 100 mm, inner diameter is 2.1 mm, particle size is 1.8 μm); acetonitrile is used as mobile phase A, 0.1% phosphoric acid solution is used as mobile phase B, and gradient elution is performed according to the provisions in Table 2 below; the flow rate is 0.2 ml per minute; the column temperature is 25°C; the detection wavelength is 235 nm. The theoretical plate number calculated based on the forsythiaside peak should not be less than 10,000.

[0067] Table 2

[0068]

[0069] It has been found that each 1g of this product contains forsythiaside (C 27 H 34 O 11 ) should be 10.0mg~30.0mg.

[0070] 3. Quality control of Bupleurum chinense granules:

[0071] Identification method: Take 0.5g of this product, grind it into powder, add 20ml of methanol, ultrasonically treat it for 10 minutes, filter it, and concentrate the filtrate to 2ml as the test solution. Take 1g of the reference medicinal material of Bupleurum chinense, add 50ml of water, decoct it for 30 minutes, filter it, evaporate the filtrate, add 20ml of methanol to the residue, and prepare the reference medicinal material solution in the same way. Take the reference material of Bupleurum chinense a, add methanol to make a solution containing 0.5mg per 1ml, and use it as the reference solution. According to the thin layer chromatography method (General Rules 0502 of the 2020 edition of the Chinese Pharmacopoeia), 3 μl of the above-mentioned test solution and reference solution and 6 μl of the reference medicinal material solution were taken and spotted on the same silica gel G thin layer plate, ethyl acetate-ethanol-water (8:2:1) was used as the developing solvent, pre-saturated for 30 minutes, developed, taken out, dried, sprayed with 2% p-dimethylaminobenzaldehyde in 40% sulfuric acid solution, heated at 60°C until the spots were clearly colored, and examined under sunlight and ultraviolet light (365nm). In the chromatogram of the test sample, spots of the same color or fluorescent spots appeared at the corresponding positions of the chromatograms of the reference medicinal material and the reference substance, respectively.

[0072] Determination of active ingredient content:

[0073] 1) Preparation of reference solution: Take an appropriate amount of saikosaponin a reference substance, weigh it accurately, and add methanol to make a solution containing 75 μg per 1 ml.

[0074] 2) Preparation of test solution: Take an appropriate amount of the product, grind it into powder, take about 1.0 g, weigh it accurately, put it in a stoppered conical flask, accurately add 25 ml of 5% 5% ethanol solution containing 5% concentrated ammonia test solution, stopper it tightly, weigh it, ultrasonically treat it (power 250 W, frequency 40 kHz) for 30 minutes, cool it, weigh it again, make up the lost weight with 5% 5% ethanol solution containing 5% concentrated ammonia test solution, shake it well, filter it, and take the filtrate to obtain it.

[0075] 3) Determination: Accurately pipette 3 μl of reference solution and test solution respectively, inject into liquid chromatograph for determination. The liquid chromatograph uses octadecylsilane bonded silica gel as filler (column length is 100 mm, inner diameter is 2.1 mm, particle size is 1.7 μm); acetonitrile is used as mobile phase A, water is used as mobile phase B, and gradient elution is performed according to the provisions in Table 3 below; detection wavelength is 211 nm, 250 nm; column temperature is 35°C; flow rate is 0.4 ml per minute. The number of theoretical plates calculated based on the saikosaponin a peak should not be less than 10,000.

[0076] Table 3

[0077]

[0078] It has been found that each 1g of this product contains saikosaponin a (C 42 H 68 O 13 ) should be 1.60mg~5.00mg.

[0079] 4. Quality Control of Huangqin Granules:

[0080] Identification method: Take 0.5g of this product, grind it, add 20ml of methanol, ultrasonically treat it for 30 minutes, filter it, evaporate the filtrate, and add 2ml of methanol to dissolve the residue as the test solution. Take another 1g of Scutellaria baicalensis reference medicinal material and prepare the reference medicinal material solution in the same way. Then take baicalin reference substance, baicalein reference substance, and wogonin reference substance, add methanol to prepare solutions containing 1mg, 0.5mg, and 0.5mg per 1ml respectively as the reference solution. According to the thin layer chromatography method (General Rules 0502 of the 2020 Edition of the Chinese Pharmacopoeia), 2μl of the test solution, the reference medicinal material solution, and 1μl of the above three reference solutions are taken and spotted on the same polyamide film, respectively, with toluene-ethyl acetate-methanol-formic acid (10:3:1:2) as the developing agent, pre-saturated for 30 minutes, developed, taken out, dried, and inspected under ultraviolet light (365nm). In the chromatogram of the test sample, a main spot of the same color appears at the corresponding position in the chromatogram of the reference medicinal material; and three identical dark spots appear at the corresponding position in the chromatogram of the reference sample.

[0081] Determination of active ingredient content:

[0082] 1) Preparation of reference solution: Take an appropriate amount of baicalin reference substance, weigh accurately, and add methanol to make a solution containing 25 μg per 1 ml.

[0083] 2) Preparation of test solution: Take an appropriate amount of the product, grind it into powder, take about 0.1g, weigh it accurately, put it in a 100ml volumetric flask, add an appropriate amount of water to dissolve it, add water to the scale, shake it well. Accurately measure 1ml, put it in a 10ml volumetric flask, add methanol to the scale, shake it well, and you have it.

[0084] 3) Determination: Accurately pipette 1 μl of reference solution and test solution respectively, inject into liquid chromatograph for determination. The liquid chromatograph uses octadecylsilane bonded silica gel as filler (column length is 100 mm, inner diameter is 2.1 mm, particle size is 1.8 μm); methanol-water (47:53) is used as mobile phase (methanol is mobile phase A, water (containing 0.05% phosphoric acid) is mobile phase B), and gradient elution is performed according to the provisions in Table 4 below; the flow rate is 0.35 ml per minute; the column temperature is 30°C; the detection wavelength is 280 nm. The theoretical plate number calculated based on the baicalin peak should not be less than 2500.

[0085] Table 4

[0086]

[0087] It has been found that each 1g of this product contains baicalin (C 21 H 18 O 11 ) should be 148.0mg~274.0mg.

[0088] 5. Quality control of Atractylodes lancea granules:

[0089] Identification method: Take 1g of this product, grind it, add 30ml of water to dissolve it, shake and extract it with ethyl acetate three times, 20ml each time, combine the ethyl acetate solution, evaporate to dryness, add 1.5ml of ethyl acetate to dissolve the residue, and use it as the test solution. Take 0.5g of the reference medicinal material of Atractylodes lancea, add 50ml of water, boil for 30 minutes, filter, take the filtrate, shake and extract it with ethyl acetate three times, and prepare the reference medicinal material solution in the same way. According to the thin layer chromatography method (General Rules 0502 of the 2020 Edition of the Chinese Pharmacopoeia), take 10μl of the above test solution and reference medicinal material solution, respectively, and spot them on the same silica gel G thin layer plate, use n-hexane-ethyl acetate-glacial acetic acid (4:3:0.1) as the developing agent, pre-saturate for 30 minutes, develop, take out, dry, and examine under ultraviolet light (365nm). In the chromatogram of the test product, fluorescent spots of the same color appear at the corresponding position of the chromatogram of the reference medicinal material.

[0090] Determination of active ingredient content:

[0091] 1) Preparation of reference solution: Take an appropriate amount of chlorogenic acid reference substance, accurately weigh it, add 10% methanol to make a solution containing 20 μg of chlorogenic acid per 1 ml, filter it, and use it as the reference solution.

[0092] 2) Preparation of test solution: Take an appropriate amount of the product, grind it into powder, take about 0.5g, weigh it accurately, put it in a stoppered conical flask, accurately add 20ml of 10% methanol, stopper it tightly, weigh it, and treat it with ultrasound (power 250W, frequency 40kHz) for 40 minutes. Take it out, cool it, weigh it again, make up the lost weight with 10% methanol, shake it well, filter it, and take the filtrate to obtain it.

[0093] 3) Determination: Accurately pipette 5 μl of the reference solution and the test solution respectively, inject into the liquid chromatograph for determination. The liquid chromatograph uses octadecylsilane bonded silica gel as the filler (column length is 100 mm, inner diameter is 2.1 mm, particle size is 1.8 μm) chromatographic column; acetonitrile is used as mobile phase A, 0.1% formic acid is used as mobile phase B, and gradient elution is performed according to the provisions in Table 5 below; the detection wavelength is 284 nm from 0 to 8.5 minutes, 336 nm from 8.5 to 45 minutes, and the flow rate is 0.4 ml per minute; the column temperature is 30°C; the theoretical plate number calculated based on the chlorogenic acid peak should be no less than 5000.

[0094] Table 5

[0095]

[0096] It has been found that each 1g of this product contains chlorogenic acid (C 16 H 18 O9) should be 0.086mg~0.650mg.

[0097] 6. Quality control of Huoxiang granules:

[0098] Identification method: Take 2g of this product, grind it, add 20ml of hot water and shake it for 10 minutes, and let it cool. Add petroleum ether (30-60℃) and shake to extract 3 times, 25ml each time, combine the petroleum ether solution, evaporate it, and add 1ml of ethyl acetate to the residue to dissolve it as the test solution. Take another reference substance of Patchouli alcohol, add ethyl acetate to make a solution containing 2mg per 1ml as the reference solution. According to the thin layer chromatography method (General Rules 0502 of the 2020 Edition of the Chinese Pharmacopoeia), take 10μl of the above test solution and 1μl of the reference solution, and spot them on the same silica gel G thin layer plate, use petroleum ether-ethyl acetate-formic acid (10:1:0.05) as the developing agent, pre-saturate for 30 minutes, develop, take out, dry, spray with 5% vanillin sulfuric acid ethanol solution, heat at 105℃ until the spots are clear, and inspect under sunlight. In the chromatogram of the test product, the same purple-red spots appear at the corresponding position of the chromatogram of the reference medicinal material.

[0099] Determination of active ingredient content:

[0100] 1) Preparation of reference solution: Take an appropriate amount of patchouli ketone reference substance, weigh it accurately, and add methanol to make a solution containing 40 μg per 1 ml as the reference solution.

[0101] 2) Preparation of test solution: Take an appropriate amount of the product, grind it into powder, take about 0.2g, weigh it accurately, put it in a stoppered conical flask, add 20ml of methanol and weigh it accurately, treat it with ultrasound (power 250W, frequency 40kHz) for 30 minutes, take it out, cool it, weigh it again, make up the lost weight with methanol, shake it well, filter it, and take the filtrate to obtain it.

[0102] 3) Determination: Accurately pipette 2 μl of reference solution and test solution respectively, inject into liquid chromatograph for determination. The liquid chromatograph uses octadecylsilane bonded silica gel as filler (column length 100 mm, inner diameter 2.1 mm, particle size 1.7 μm) chromatographic column; methanol as mobile phase A, 0.1% formic acid solution as mobile phase B, gradient elution according to the provisions in Table 6 below; flow rate 0.3 ml per minute; column temperature 40°C; detection wavelength 310 nm, theoretical plate number calculated based on patchouli ketone peak should not be less than 3000.

[0103] Table 6

[0104]

[0105] It has been found that each 1g of this product contains patchouli ketone (C 12 H 16 O4) should be 0.7mg~3.0mg.

[0106] 7. Burdock granules quality control:

[0107] Identification method: Take 0.1g of this product, grind it, add 20ml of ethanol, ultrasonically treat for 30 minutes, filter, evaporate the filtrate, and add 1ml of ethanol to the residue to dissolve it as the test solution. Take another 1g of burdock seed reference medicinal material, add 50ml of water, decoct for 30 minutes, filter, evaporate the filtrate, add 20ml of ethanol to the residue, and prepare the reference medicinal material solution in the same way. Take the arctiin reference substance again, add ethanol to make a solution containing 5mg per 1ml, as the reference substance solution. According to the thin layer chromatography method (General Rules 0502 of the 2020 Edition of the Chinese Pharmacopoeia), take 5μl of each of the above three solutions, spot them on the same silica gel G thin layer plate, use chloroform-methanol-water (40:8:1) as the developing solvent, develop, take out, dry, spray with 10% sulfuric acid ethanol solution, and heat at 105°C until the spots are clearly colored. In the test sample chromatogram, spots of the same color appear at corresponding positions in the control medicinal material chromatogram and the control sample chromatogram.

[0108] Determination of active ingredient content:

[0109] 1) Preparation of reference solution: Take an appropriate amount of arctiin reference substance, accurately weigh it, and add methanol to make a solution containing 0.5 mg per 1 ml.

[0110] 2) Preparation of test solution: Take an appropriate amount of the product, grind it into powder, take about 0.1g, weigh it accurately, put it in a stoppered conical flask, accurately add 50ml of 70% methanol, stopper it tightly, weigh it, ultrasonically treat it (power 250W, frequency 40kHz) for 30 minutes, cool it, weigh it again, make up the lost weight with 70% methanol, shake it well, filter it, and take the filtrate to obtain the solution.

[0111] 3) Determination: Accurately pipette 1 μl of reference solution and test solution respectively, inject into liquid chromatograph for determination. The liquid chromatograph uses octadecylsilane bonded silica gel as filler (column length is 100 mm, inner diameter is 2.1 mm, particle size is 1.8 μm); methanol-water (43:57) is used as mobile phase (methanol is mobile phase A, water is mobile phase B), and gradient elution is performed according to the provisions in Table 7 below; the flow rate is 0.3 ml per minute; the detection wavelength is 280 nm, and the theoretical plate number calculated based on the arctiin peak should be no less than 1500.

[0112] Table 7

[0113]

[0114] It has been found that each 1g of this product contains arctiin (C 27 H 34 O 11 ) should be 110.0mg~230.0mg.

[0115] 8. Quality Control of Fuling Granules:

[0116] Identification method: Take 3g of this product, grind it, add 50ml of ether, ultrasonically treat it for 30 minutes, filter it, evaporate the filtrate, and add 1ml of methanol to the residue to dissolve it as the test solution. Take another 1g of Poria cocos control medicinal material and prepare the control medicinal material solution in the same way. According to the thin layer chromatography method (General Rules 0502 of the 2020 Edition of the Chinese Pharmacopoeia), take 8μl of the test solution and 12μl of the control medicinal material solution, and spot them on the same silica gel G thin layer plate, respectively, with toluene-ethyl acetate-formic acid (20:5:0.5) as the developing agent, develop it, take it out, dry it, spray it with 5% vanillin sulfuric acid solution, and heat it at 105°C until the spots are clearly colored. In the chromatogram of the test sample, spots of the same color appear at the corresponding position of the chromatogram of the control medicinal material.

[0117] Determination of active ingredient content:

[0118] 1) Preparation of reference solution: Take appropriate amount of Pachymaranth acid B reference substance and Pachymaranth acid A reference substance, weigh accurately, add methanol to make a mixed solution containing 20 μg of each per 1 ml.

[0119] 2) Preparation of test solution: Take an appropriate amount of the product, grind it into powder, take about 0.24g, weigh it accurately, put it in a stoppered conical flask, accurately add 10ml of 50% methanol, stopper it tightly, weigh it, ultrasonically treat it (power 250W, frequency 40kHz) for 30 minutes, cool it, weigh it again, make up the lost weight with 50% methanol, shake it well, centrifuge it, take the supernatant, filter it, and take the filtrate to obtain the solution.

[0120] 3) Determination: Accurately pipette 2 μl of reference solution and test solution respectively, inject into ultra-high performance liquid chromatography, and determine. The ultra-high performance liquid chromatography uses octadecylsilane bonded silica gel as filler (column length is 150 mm, inner diameter is 2.1 mm, particle size is 1.6 μm); acetonitrile is used as mobile phase A, 0.1% formic acid solution is used as mobile phase B, and gradient elution is performed according to the provisions in Table 8 below; the flow rate is 0.2 ml per minute; the column temperature is 30°C; the detection wavelength is 252 nm. The number of theoretical plates calculated based on the Pachycolic acid B peak should not be less than 5000.

[0121] Table 8

[0122]

[0123] It has been found that each 1g of this product contains Pachycolic acid B (C 30 H 44 O5) should be 0.10mg~0.40mg; Pachycolic acid A (C 31 H 46 O5) should be 0.08mg~0.30mg.

[0124] 9. Quality control of Sugeng granules:

[0125] Identification method: Take 2g of this product, grind it, add 25ml of methanol, ultrasonically treat it for 30 minutes, filter, evaporate the filtrate, and add 1ml of methanol to the residue to dissolve it as the test solution. Take another 1g of the perilla stem reference medicinal material, add 50ml of water, decoct for 30 minutes, filter, evaporate the filtrate, add 25ml of methanol to the residue, and make a reference medicinal material solution in the same way. Take the rosmarinic acid reference substance again, add methanol to make a solution containing 0.5mg per 1ml as the reference substance solution. According to the thin layer chromatography method (General Rules 0502 of the 2020 Edition of the Chinese Pharmacopoeia), take 1 to 4μl of each of the above three solutions, and spot them on the same silica gel G thin layer plate, use n-hexane-ethyl acetate-formic acid (3:3:0.2) as the developing agent, develop, take out, dry, and examine under ultraviolet light (365nm). In the test sample chromatogram, fluorescent spots of the same color appear at the corresponding positions of the reference medicinal material chromatogram and the reference substance chromatogram.

[0126] Determination of active ingredient content:

[0127] 1) Preparation of reference solution: Take an appropriate amount of rosmarinic acid reference substance, accurately weigh it, and add 60% acetone to make a solution containing 40 μg per 1 ml.

[0128] 2) Preparation of test solution: Take an appropriate amount of the product, grind it into powder, take about 0.5g, weigh it accurately, put it in a stoppered conical flask, accurately add 25ml of 60% acetone, stopper it tightly, weigh it, ultrasonically treat it (power 500W, frequency 40kHz) for 30 minutes, cool it, weigh it again, make up the lost weight with 60% acetone, shake it well, filter it, and take the filtrate to obtain it.

[0129] 3) Determination: Accurately pipette 5-20 μl of reference solution and test solution respectively, inject into liquid chromatograph for determination. The liquid chromatograph uses octadecylsilane bonded silica gel as filler; 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), and gradient elution is performed according to the provisions in Table 9 below; column temperature is 30°C, flow rate is 0.3 mL / min, and detection wavelength is 330 nm. The theoretical plate number calculated based on the rosmarinic acid peak should be no less than 3000.

[0130] Table 9

[0131]

[0132] It has been found that each 1g of this product contains rosmarinic acid (C 18 H 16 O8) should be 1.2mg~4.0mg.

[0133] 10. Quality control of almond particles:

[0134] Identification method: Take an appropriate amount of this product, grind it into powder, take 0.1g, grind it into powder, add 10ml of methanol, ultrasonically treat it for 30 minutes, filter it, and use the filtrate as the test solution. Take another 0.3g of bitter almond reference medicinal material, add it to 30ml of boiling water, keep it slightly boiling for 30 minutes, filter it, evaporate the filtrate to dryness, add 10ml of methanol to the residue, and prepare the reference medicinal material solution in the same way. Take the amygdalin reference substance again, add methanol to make a solution containing 1mg per 1ml, as the reference substance solution. According to the thin layer chromatography method (General Rules 0502 of the 2020 edition of the Chinese Pharmacopoeia), 3 μl of the test solution and the reference solution, and 5 μl of the reference medicinal material solution were taken and spotted on the same silica gel G thin layer plate, respectively, and the lower layer solution of chloroform-ethyl acetate-methanol-water (15:40:22:10) placed at 5-10°C for 12 hours was used as the developing agent, developed, taken out, sprayed with 0.8% phosphomolybdic acid in 15% sulfuric acid ethanol solution, and heated at 105°C until the spots were clearly colored. In the chromatogram of the test sample, spots of the same color appeared at the corresponding positions of the chromatograms of the reference medicinal material and the reference substance.

[0135] Determination of active ingredient content:

[0136] 1) Preparation of reference solution: Take an appropriate amount of amygdalin reference substance, weigh accurately, and add 50% methanol to make a solution containing 50 μg per 1 ml.

[0137] 2) Preparation of test solution: Take an appropriate amount of the product, grind it into powder, take about 0.2g, weigh it accurately, put it in a stoppered conical flask, accurately add 25ml of 50% methanol, weigh it, ultrasonically treat it (power 250W, frequency 40kHz) for 30 minutes, take it out, cool it, weigh it again, make up the lost weight with 50% methanol, shake it well, centrifuge it (speed is more than 4000 revolutions per minute) for 10 minutes, accurately measure 2ml of supernatant, put it in a 25ml volumetric flask, add 50% methanol to dilute to the scale, shake it well, filter it, and take the filtrate.

[0138] 3) Determination: Accurately pipette 10μl of reference solution and test solution respectively, inject into liquid chromatograph for determination. The liquid chromatograph uses octadecylsilane bonded silica gel as filler (column length 250mm, inner diameter 4.6mm, particle size 5μm); acetonitrile-0.1% phosphoric acid solution (6:94) as mobile phase (isocratic elution); flow rate 0.3mL / min, column temperature 20-25℃; detection wavelength 207nm. The theoretical plate number calculated based on the amygdalin peak should be no less than 7000.

[0139] It has been found that each 1g of this product contains amygdalin (C 20 H 27 NO 11 ) should be 60.0mg~120.0mg.

[0140] 11. Quality control of turmeric granules:

[0141] Identification method: Take 0.5g of this product, grind it, add 20ml of methanol, ultrasonically treat it for 20 minutes, filter it, evaporate the filtrate at low temperature, and add 1ml of methanol to dissolve the residue as the test solution. Take another 0.5g of the turmeric reference medicinal material, add 5ml of petroleum ether (30-60℃), shake it from time to time for 30 minutes, filter it, and use the filtrate as the reference medicinal material solution. Take the zedoary diol reference material again, add methanol to make a solution containing 1mg per 1ml, as the reference material solution. According to the thin layer chromatography method (General Rules 0502 of the 2020 Edition of the Chinese Pharmacopoeia), take 5μl of the test solution and the reference medicinal material solution, and 2μl of the reference solution, and spot them on the same silica gel G thin layer plate, use petroleum ether-ethyl acetate (22:1) as the developing solvent, develop, take out, dry, spray with 1% vanillin sulfuric acid solution, and heat at 100℃ until the spots are clearly colored. In the test sample chromatogram, spots of the same color appear at corresponding positions in the control medicinal material chromatogram and the control sample chromatogram.

[0142] Determination of active ingredient content:

[0143] 1) Preparation of reference solution: Take an appropriate amount of Curcuma diol reference substance, accurately weigh it, and add 70% methanol to make a solution containing 25 μg per 1 ml.

[0144] 2) Preparation of test solution: Take an appropriate amount of the product, grind it into powder, take about 0.5g, weigh it accurately, put it in a stoppered conical flask, accurately add 20ml of 70% methanol, stopper it tightly, weigh it, ultrasonically treat it (power 250W, frequency 40kHz) for 30 minutes, cool it, weigh it again, make up the lost weight with 70% methanol, shake it well, filter it, and take the filtrate to obtain the solution.

[0145] 3) Determination: Accurately pipette 1 μl of the reference solution and the test solution respectively, inject into the ultra-high performance liquid chromatograph for determination. The ultra-high performance liquid chromatograph uses octadecylsilane bonded silica gel as the filler (column length is 100 mm, inner diameter is 2.1 mm, particle size is 1.8 μm); acetonitrile-0.1% phosphoric acid solution (20:80) is used as the mobile phase (acetonitrile is mobile phase A, 0.1% phosphoric acid solution is mobile phase B) and gradient elution is performed according to the provisions in Table 10 below; flow rate is 0.3 mL / min, column temperature is 30°C, and detection wavelength is 254 nm. The number of theoretical plates calculated based on the peak of Curcuma zedoariae diol should not be less than 5000.

[0146] Table 10

[0147]

[0148] It has been found that each 1g of this product contains curcuma diol (C 15 H 22 O3) should be 0.5mg~2.5mg.

[0149] 12. Qianghuo Granules Quality Control:

[0150] Identification method: Take 1g of this product, grind it, add 5ml of methanol, ultrasonically treat it for 20 minutes, let it stand, and take the supernatant as the test solution. Take another 1g of Notopterygium root control medicinal material and make a control medicinal material solution in the same way. Take the purple flower chaerucoside reference substance and add methanol to make a solution containing 0.5mg per 1ml as the reference solution. According to the thin layer chromatography method (General Rules 0502 of the 2020 Edition of the Chinese Pharmacopoeia), take 10μl of the test solution, 4μl of the control medicinal material solution and the reference solution, and spot them on the same silica gel G thin layer plate, use chloroform-methanol (8:2) as the developing agent, develop, take out, dry, and examine under ultraviolet light (365nm). In the test sample chromatogram, fluorescent spots of the same color appear at the corresponding positions of the control medicinal material chromatogram and the reference substance chromatogram.

[0151] Determination of active ingredient content:

[0152] 1) Preparation of reference solution: Take appropriate amount of ferulic acid reference, notopterygium alcohol reference and isoimperatorin reference, accurately determine the concentration, and add methanol to prepare a mixed solution containing 25 μg of ferulic acid, 8 μg of notopterygium alcohol and 2 μg of isoimperatorin per 1 ml.

[0153] 2) Preparation of test solution: Grind an appropriate amount of the product, take about 0.1 g, weigh accurately, place in a stoppered conical flask, accurately add 25 ml of 50% methanol, stopper, weigh, ultrasonically treat (power 250 W, frequency 40 kHz) for 30 minutes, cool, weigh again, make up the lost weight with 50% methanol, shake well, filter, and take the filtrate.

[0154] 3) Determination: Accurately pipette 2μl of reference solution and test solution respectively, inject into ultra-high performance liquid chromatography, and determine. The ultra-high performance liquid chromatography uses octadecylsilane bonded silica gel as filler (column length is 150mm, inner diameter is 2.1mm, particle size is 1.8μm); methanol is used as mobile phase A, 0.2% phosphoric acid solution is used as mobile phase B, and gradient elution is performed according to the provisions in Table 11 below; the flow rate is 0.25ml per minute; the column temperature is 30℃; the detection wavelength is 316nm. The theoretical plate number calculated based on the Qianghuo alcohol peak should not be less than 10,000.

[0155] Table 11

[0156]

[0157] It has been found that each 1g of this product contains ferulic acid (C 10 H 10 O4) should be 1.5mg~8.0mg; Qianghuo alcohol (C 21 H 22 O5) and isoimperatorin (C 16 H 14 O4) should be 0.5mg~4.0mg.

[0158] <Clinical Trials>

[0159] The patients who took the Chinese medicine preparation of the present invention, traditional Chinese medicine, and the Chinese medicine preparation of the present invention combined with Western medicine antipyretic drugs were followed up with questionnaires.

[0160] 1. The contents of the survey questionnaire are set as shown in Tables 12 and 13.

[0161] Table 12 Patient basic information collection form

[0162]

[0163] Table 13 Statistical table of efficacy of patients after taking medicine

[0164]

[0165]

[0166] 2. Statistics of basic information of patients enrolled in the survey

[0167] A total of 97 case feedbacks were collected in the survey, of which 30 cases used traditional Chinese medicine (including the classic Chinese medicine prescriptions Yinqiao Powder, Xiao Chaihu Decoction, Huoxiang Zhengqi Powder and Shengjiang Powder, a total of 30 cases of classic Chinese medicine prescriptions), 30 cases used the Chinese medicine preparations described in the present invention, and 37 cases used the Chinese medicine preparations described in the present invention combined with Western medicine antipyretics. The basic information and grouping information of the patients are shown in Table 14. There was no significant difference in the basic information of the patients in the traditional Chinese medicine group, the Chinese medicine preparation group, and the Chinese medicine preparation combined with Western medicine antipyretics group (P>0.05).

[0168] Table 14

[0169]

[0170] 3. Observation of drug efficacy

[0171] Through the arrangement of the questionnaire, the improvement effects of traditional Chinese medicine, the Chinese medicine preparation of the present invention, and the Chinese medicine preparation of the present invention combined with Western medicine antipyretic drugs on fever, muscle pain, sore throat, and cough, as well as the occurrence of adverse reactions were statistically analyzed. The results were calculated using a cross-tabulation chi-square test, with a confidence interval of 95%, and P < 0.05 was considered to be significantly different. The results are shown in Tables 15 to 17.

[0172] Table 15

[0173]

[0174] Table 16

[0175]

[0176]

[0177] Note: ** Compared with the traditional Chinese medicine group, the time it took for the body temperature to return to normal after taking the Chinese medicine preparation was significantly reduced (P<0.05);

[0178] *** Compared with the traditional Chinese medicine group, the time taken for the body temperature to return to normal after taking Chinese medicine preparations combined with Western antipyretics was significantly reduced (P < 0.05);

[0179] Table 17

[0180]

[0181] The results showed that the total effective rate of the antipyretic effect of the Chinese medicine preparation of the present invention was 96.70%, which was not significantly different from the traditional Chinese medicine group and the Chinese medicine preparation combined with Western medicine antipyretic group (P>0.05); the total effective rate of the Chinese medicine preparation of the present invention in improving muscle pain was 91.30%, which was not significantly different from the traditional Chinese medicine group and the Chinese medicine preparation combined with Western medicine antipyretic group (P>0.05); the total effective rate of the Chinese medicine preparation of the present invention in improving pharyngeal pain was 81.00%, which was not significantly different from the traditional Chinese medicine group and the Chinese medicine preparation combined with Western medicine antipyretic group (P>0. 05); the total effective rate of the Chinese medicine preparation of the present invention in improving cough was 70.80%, which was not significantly different from the traditional Chinese medicine group and the Chinese medicine preparation combined with Western medicine antipyretic group (P>0.05) (Table 15); the average time required for fever reduction in the Chinese medicine preparation group was 24.62±25.64 hours, which was significantly different from the traditional Chinese medicine group (P<0.05) (Table 5); the incidence of adverse reactions between the Chinese medicine preparation group of the present invention and the traditional Chinese medicine group and the Chinese medicine preparation combined with Western medicine antipyretic group was not significantly different (P>0.05) (Table 6).

[0182] The above results were analyzed and found that the Chinese medicine preparation of the present invention, traditional Chinese medicine, and Chinese medicine preparation combined with antipyretic drugs all have an improvement effect on fever, muscle pain, sore throat, and cough caused by the initial stage of viral cold. However, compared with traditional Chinese medicine treatment, the Chinese medicine preparation of the present invention is significantly better than traditional Chinese medicine in terms of antipyretic speed, and the effect is equivalent to the combined use of Western medicine, and the incidence of adverse reactions is not significant.

[0183] Although the embodiments of the present invention have been disclosed as above, they are not limited to the applications listed in the specification and the implementation modes. They can be fully applied to various fields suitable for the present invention. For those familiar with the art, additional modifications can be easily implemented. Therefore, without departing from the general concept defined by the claims and the scope of equivalents, the present invention is not limited to the specific details and the embodiments shown and described herein.

Claims

1. A Chinese medicine preparation for treating the early stage of viral cold, characterized in that: The drug is composed of the following raw materials in parts by weight: 15 parts of honeysuckle, 15 parts of forsythia, 10 parts of bupleurum, 10 parts of scutellaria, 12 parts of atractylodes, 10 parts of patches of patches, 8 parts of burdock seeds, 15 parts of poria, 8 parts of perilla stem, 6 parts of apricot kernel, 10 parts of turmeric slices, and 10 parts of notopterygium.

2. The method for preparing the Chinese medicine preparation as claimed in claim 1, characterized in that: include: Take the above-mentioned weight portions of honeysuckle slices, forsythia slices, northern bupleurum slices, scutellaria slices, atractylodes slices, patchouli slices, burdock fruit slices, Poria slices, perilla stem slices, almond slices, turmeric slices, and notopterygium wilfordii slices, make them into granules respectively, and then mix them evenly.

3. The method for preparing the Chinese medicine preparation as claimed in claim 2, characterized in that: The method for preparing a raw material medicine slice into granules comprises: taking a raw material medicine slice as mentioned above in weight, adding 8-12 times of water and boiling for 30 minutes to 2 hours, filtering, retaining the raw material medicine slice and adding 6-8 times of water again, boiling for 20 minutes to 2 hours, filtering, combining the two filtrates, vacuum drying and concentrating at 60-80°C to obtain an extract, wherein the density of the extract is 1.00-1.23 at 70±5°C, spray drying the extract and sieving it through 80-150 mesh to obtain an extract powder, adding 0.3% of silicon dioxide in the amount of granules, 0.1% of magnesium stearate and maltodextrin in the amount of granules to the extract powder, uniformly mixing, granulating, and obtaining raw material medicine granules.

4. The method for preparing the Chinese medicine preparation as claimed in claim 2, characterized in that: Each gram of honeysuckle granules contains 23.0 mg to 55.0 mg of chlorogenic acid, and the total amount of phenolic acid substances, including chlorogenic acid, 3,5-di-O-caffeoylquinic acid and 4,5-di-O-caffeoylquinic acid, is 35.0 mg to 81.0 mg; Each 1g of Forsythia suspensa granules contains 10.0 mg to 30.0 mg of forsythiaside; Each 1g of Bupleurum chinense granules contains 10.0 mg to 30.0 mg of saikosaponin a; Each 1g of Huangqin granules contains 148.0mg~274.0mg of baicalin; Each 1g of Atractylodes lancea granules contains 0.086 mg~0.650 mg of chlorogenic acid; Each 1g of Patchouli Granules contains 0.7mg~3.0mg of Patchouli Ketone; Each 1g of burdock granules contains 110.70mg~230.0mg of arctiin; Each 1g of Poria granules contains 0.10mg~0.40mg of Pachymic acid B and 0.08mg~0.30mg of Pachymic acid A; Each 1g of Sugeng granules contains 1.2mg~4.0mg of rosmarinic acid; Each 1g of almond granules contains 60.0mg~120.0mg of amygdalin; Each 1g piece of turmeric granules contains 0.5mg~2.5mg of curcuma diol; Each 1g of Notopterygium wilfordii granules contains 1.5mg~8.0mg of ferulic acid, and a total amount of notopterygium wilfordii alcohol and isoimperatorin of 0.5mg~4.0mg.

5. Use of the Chinese medicine preparation as claimed in claim 1 in preparing medicine for treating the early stage of viral cold.

6. The use of the Chinese medicine preparation as claimed in claim 5, characterized in that: The dosage form of the traditional Chinese medicine preparation is granules.

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