CN102188600B - Chinese medicinal preparation for treating tracheitis and preparation method thereof - Google Patents

Abstract

The invention relates to a Chinese medicinal granule preparation for treating tracheitis, which is prepared from the following raw materials in part by weight: 4.5 parts of ephedra, 5.5 parts of red tangerine peel, 5.0 parts of szechuan tangshen root, 2.0 parts of bulbus fritilariae, 2.5 parts of almond, 1.8 parts of honey-fried coltsfoot, 1.8 parts of aristolochia, 1.8 parts of whiteflower hogfennel root, 2.0 parts of polygalae and 1.8 parts of Chinese magnoliavine fruit. A preparation method comprises the following steps of: performing water extraction and alcohol precipitation on the medicinal materials to prepare thick paste, adding 1 part of dextrin and 4 parts of cane sugar into 1 part of thick paste, and mixing and granulating. The Chinese medicinal granule preparation is mainly used for treating cough and dyspnea with lung heat, polypnea asthma, accumulation of phlegm-savliva and stuffy septum pectoral which are caused by exogenous wind-cold, and has the excellent effects of relieving cough and asthma, clearing heat and eliminating phlegm. Clinical observation indicates that the Chinese medicinal granule preparation has the good clinical effect, can improve the symptoms such as cough, phlegm, asthma and the like of acute and chronic bronchitis effectively, does not have toxic or side effect, and is used conveniently and safely.

Description

A kind of Chinese medicine preparation that is used to treat tracheitis and preparation method thereof

Technical field

The present invention relates to treat the Chinese medicine preparation of respiratory tract disease, is a kind of Chinese medicine preparation that is used to treat tracheitis specifically, and the present invention also comprises method of making preparation.

Background technology

Acute and chronic bronchitis is meant the chronic nonspecific inflammation of trachea, bronchial mucosa and surrounding tissue thereof, clinical with the cough, expectoration be cardinal symptom or with pant and repeatedly the outbreak chronic process be characteristic.The state of an illness is if slowly make progress Chang Bingfa obstructive emphysema, even lung dynamic high-pressure, chronic pulmonary heart disease.Domestic survey data shows that prevalence is 3%., chronic bronchitis is as a kind of commonly encountered diseases, the serious harm people's health.Be higher than south in China prevalence north, this disease in Lanzhou area sickness rate higher, had a strong impact on people health, clinical manifestation is cough, asthma, abundant expectoration, uncomfortable in chest and dyspnea during this seizure of disease, even death by suffocation.Because doctor trained in Western medicine adopts hormone spasmolytic and antibiotic etc., cure the symptoms, not the disease, and side effect is big.At present, the Western medicine kind of diseases such as disease such as treat acute and chronic bronchitis and pant is more, has like cough medicine: carbetapentane citrate, codeine, dextromethorphan etc.; Expectorant has: ammonia chloride, bromhexine hydrochloride etc.; Anti-asthmatic has: albuterol, aminophylline etc., Western medicine are because curative effect is clear and definite, and advantage such as produce effects is fast has occupied antitussive, most of market of the disease medication of relievining asthma, eliminate the phlegm.Modern medicine is unclear fully as yet about the chronic bronchitis definite cause of disease and pathogenesis.It is generally acknowledged, when the human body resistance goes down, exist at air flue on the basis of sensitivity in various degree, have one or more exopathogenic factors to exist, comprise factors such as infection, physics and chemistry allergy, weather, smoking, prolonged and repeated effect can develop into chronic bronchitis.What environment in recent years was polluted in addition increases the weight of and antibiotic abuse, and it is little that the infection of doctor trained in Western medicine and symptomatic treatment measure more show the power single-action.Chinese medicine is from integral body, and determination of cause of disease according to differentiation of symptoms and signs is examined because of discussing and controlled curative effect Chang Xianzhu.

Summary of the invention

Technical problem to be solved by this invention provides a kind of according to theory of Chinese medical science; Catch the basic cause of disease prescription of tracheitis, use Chinese medicines such as Herba Ephedrae, dried tangerine peel, Bulbus Fritillariae Cirrhosae, depressed lung-energy dispersing; Nourishing YIN and clearing away lung-heat, relieving cough and resolving phlegm; The convergence lung qi, various acute and chronic tracheitiies are had good result, effectively antitussive, eliminate the phlegm and lax tracheal smooth muscle effect; And a kind of Chinese medicinal granule preparation that is used to treat tracheitis of the smooth muscle contraction that can cause antihistaminic, another object of the present invention provides the method for preparing of this pure Chinese medicinal preparation.

The technical solution adopted for the present invention to solve the technical problems is:

A kind of Chinese medicinal granule preparation that is used to treat tracheitis is prepared from following raw material and weight portion proportioning:

4.5 parts in Herba Ephedrae, 5.5 parts of dried tangerine peels, 5.0 parts of Radix Codonopsis, 2.0 parts of Bulbus Fritillariae Cirrhosae, 2.5 parts in Semen Armeniacae Amarum, 1.8 parts of honey-fried FLOS FARFARAEs, 1.8 parts of Fructus Aristolochiaes, 1.8 parts of Radix Peucedanis, 2.0 parts of Radix Polygalaes, Fructus Schisandrae Chinensis 1.8;

Above-mentioned medical material is processed thick paste behind water extract-alcohol precipitation, 1 part of thick paste adds 1 part in dextrin, 4 parts of sucrose.

Prepare by following processing step:

1) get above-mentioned ten flavor raw medicinal materials, oven dry is weighed by proportioning, mixes;

2) decocte with water is three times, and for the first time amount of water is 11 times of medical material weight, decocts 2 hours; For the second time amount of water is 8 times of medical material weight, decocts 1 hour; Amount of water is 8 times of medical material weight for the third time, decocts 1 hour;

3) collecting decoction filters, and it is 1.08～1.10 that filtrating is concentrated into relative density, add ethanol make filtrating to contain the alcohol amount be 60%, left standstill 24 hours, get supernatant liquid filtering, reclaim ethanol, filtrating is concentrated into the thick paste of relative density 1.38～1.41;

4) in the ratio of 4:1:1 with sucrose, dextrin and thick paste mixing granulation, 50～60 ℃ of dryings, granulate, packing.

Character: these article are the brown granule.

Function cures mainly: nourishing YIN and clearing away lung-heat, relieving cough and resolving phlegm are used for exogenous cough, tracheitis.

Usage and dosage: boiled water is taken after mixing it with water, every day 3 times, each 10g.Or follow the doctor's advice.

Untoward reaction: do not find adverse effect.

Contraindication: ephedrine autopath forbidding, hyperpietic, the careful usefulness of anemia of pregnant woman.

Points for attention: these article should be positioned over the place that the child is difficult for obtaining, and wrongly take avoiding.

The present invention is according to Chinese medical theory, adopt use more than 30 year carry out systematic research through proved recipe, for extensive patients provides a kind of good medicine of treating acute and chronic tracheitis and bronchitis disease.

Gansu is the abundant big province of China's Chinese material medicine resource; Herba Ephedrae, Radix Codonopsis, Semen Armeniacae Amarum etc. are the genuine medical material of this province; Plantation output is big; The particulate development of tracheitis has made full use of the abundant advantage of this province herb resource, and be primarily aimed at present China development of Chinese herb products and exist starting early, but problems such as starting point is low, slower development; Be prerequisite to improve clinical efficacy, keep the Chinese medicine characteristics, the technology content that improves development of Chinese herb products is standard; Effectively solve similar herbal species disintegration time length, absorption difference, problems such as bioavailability is low, supplementary product consumption is big, taking dose height, through the investigation of extraction process, it is completely vexed to be mainly used in lung-heat cough with asthma, tachypnea asthma, accumulation and obstruction of sputum, septum pectorale that affection of exogenous wind-cold causes through clinical observation tracheitis granule.Show to have clinical efficacy preferably through clinical observation, can effectively improve and acute and chronicly bronchiticly cough, expectorant, symptom such as breathe heavily, and not have obvious toxic-side effects, safety easy to use.Prescription is rigorous rationally, carries, taking convenience, and applying of it will be filled up the blank that this area chronic bronchitis is treated local medication, produce good economic benefit and social benefit.

These article are pure Chinese medicinal preparation, and according to theory of Chinese medical science, the cause of disease of tracheitis is six climate exopathogens exopathogen invasion and attack lung system or visceral dysfunction, and the dried lung of interior heresy causes that impaired depurative descending of lung QI, abnormal rising of lung-QI cough.Treatment is main with nourishing YIN and clearing away lung-heat, relieving cough and resolving phlegm.According to theory of Chinese medical science, catch the basic cause of disease prescription of tracheitis, use Chinese medicines such as Herba Ephedrae, dried tangerine peel, Bulbus Fritillariae Cirrhosae, depressed lung-energy dispersing, nourishing YIN and clearing away lung-heat, relieving cough and resolving phlegm, the convergence lung qi has good result to various acute and chronic tracheitiies.These article of pharmacological evaluation proof effectively antitussive, eliminate the phlegm and lax tracheal smooth muscle effect and the smooth muscle contraction that can cause antihistaminic.Nearly 30 years of clinical use amounts to and observes 10000 routine many cases, and total effective rate is 96%.These article are pure Chinese medicinal preparation, and are safe in utilization, and acute toxicity testing shows that mice is to these article water extract maximum tolerated dose>140g/kg, 1166.67 times of the consumption that is equivalent to be grown up, adverse effect is rare.

Tracheitis granule of the present invention is to be made up of kinds of traditional Chinese medicines such as Semen Armeniacae Amarum, Herba Ephedrae, Bulbus Fritillariae Uninbracteataes; Be pure Chinese medicinal preparation; It is full vexed to be mainly used in lung-heat cough with asthma, tachypnea asthma, accumulation and obstruction of sputum, chest and diaphragm that affection of exogenous wind-cold causes, has good relieving cough and asthma, the removing heat-phlegm effect.Show to have clinical efficacy preferably through clinical observation, can effectively improve and acute and chronicly bronchiticly cough, expectorant, symptom such as breathe heavily, and not have obvious toxic-side effects, safety easy to use.

The bronchitic clinical observation on the therapeutic effect of tracheitis granule therapy

1 clinical data

1.1 case history is selected

Select bronochitic's 240 examples, the case of including in all meets acute and chronic bronchitis diagnostic criteria, Chinese medical discrimination syndrome of wind-cold attacking lung person, and the age is between 18～65 years old.Get rid of scenario simultaneously: the age is under-18s or over-65s person, confirms on inspection by the patient that pants of the cough due to pulmonary tuberculosis, fungus, tumor, the irritative gas allergy; The concurrent severe cardiac of chronic bronchitis functional defect person; Be associated with serious primary disease such as cardiovascular, kidney, liver and hemopoietic system, the psychotic; Gestation or women breast-feeding their children are to this medicine allergy sufferers; All standards of including in that do not meet by the regulation medication, can't not judged curative effect, or safety judgement person.All patients are divided into treatment group 120 example and matched group 120 examples at random, and 120 examples are organized in treatment, male 62 examples, women 58 examples; 65 examples of the course of disease＜3 d, 37 examples of 4～5 d, 18 examples of 6～7 d, average course of disease 3.7 d; Year mean age (42.5 ± 3.2).Matched group 120 examples, male 56 examples, women 64 examples; 62 examples of the course of disease course of disease＜3 d, 35 examples of 4～5 d, 23 examples of 6～7 d, average course of disease 3.5 d; Year mean age (43.6 ± 3.2).Data differences such as two groups of patient ages, the course of disease, the state of an illness do not have significance (P>0.05), have comparability.

1.2 diagnostic criteria is according to " traditional Chinese medical science disease diagnosis criterion of therapeutical effect " [2], " practical internal medicine " [3] and " new Chinese medicine clinical research guideline " formulations such as [4].

2 Therapeutic Method

2.1 oral tracheitis granule (10g/ bag) is organized in the Therapeutic Method treatment, each 10g, every day 3 times; The oral Chinese ephedra and almond containing cough stopping capsule of matched group (the refreshing army in Gansu Province, Gansu are sent out pharmaceutical Co. Ltd, 12/box), each 2, every day 3 times; All took medicine 14 days observation periods, other relevant medicines of forbidding in the therapeutic process continuously 7～14 days.

2.2 observation index biological indicator: observe patient's sex, age, body constitution amount, body temperature, heart rate, blood pressure.Diagnostic index: observe the symptoms, the course of disease, severity extent, tongue fur, pulse condition.Health giving quality index: observe and to change before and after primary symptom (cough, expectorant, the breathe heavily) treatment and pulmonary's sign changes.Safety indexes: observe routine blood test, routine urinalysis, electrocardiogram, liver function, renal function and untoward reaction.

Observation of symptoms: the patient is from medication the 0th day to the 7th day and the 14th day each observed and recorded 1 time.Safety indexes: the patient finishes respectively to check 1 time from the 0th day with the course of treatment.

3 results

3.1 criterion of therapeutical effect clinical recovery: treat cough in 14 days, expectorant, the control of asthma shape or basic controlling.Produce effects: treat cough in 14 days, expectorant, asthma shape and be clearly better.Effectively: treat cough in 14 days, expectorant, asthma shape and all take a favorable turn.Invalid: treating cough in 14 days, expectorant, asthma shape does not have obvious improvement, even increases the weight of.

3.2 1 grade of safety evaluatio standard: safety, there is not any untoward reaction.The safety indexes inspection is no abnormal.2 grades: compare safety,, need not do any processing and can continue administration if any untoward reaction.The safety indexes inspection is no abnormal.3 grades: safety issue is arranged, moderate untoward reaction is arranged, can continue administration after processing, the safety indexes inspection has mile abnormality.4 grades; Because of untoward reaction stops research, or the safety indexes inspection has obviously unusual.

3.3 therapeutic outcome

3.3.1 the two groups of total effectses in treatment back are seen table 1.

Table 1 treatment group and matched group curative effect be (example) relatively

Group	The example number	Clinical recovery	Produce effects	Effectively	Invalid	Total obvious effective rate (%)	Total effective rate (%)
								The treatment group	120	51	47	15	7	81.67	94.17
Matched group	120	39	44	28	9	69.17	92.50

Through statistical analysis, total effective rate does not have significance (P>0.05) between two groups, and total obvious effective rate difference has significance (P < 0.05) between two groups.

3.3.2 cough between two groups, expectorant, breathe heavily situation, see table 2.

Table 2 treatment group and matched group are coughed, expectorant, breathe heavily curative effect relatively

Symptom	Group	The example number	Clinical recovery	Produce effects	Effectively	Invalid	Total effective rate (%)
								Cough	The treatment group	120	41	47	26	6	95.00
?	Matched group	120	35	49	27	9	92.50
								Expectorant	The treatment group	105	31	29	35	10	90.48
?	Matched group	108	28	35	33	12	88.89
								Breathe heavily	The treatment group	44	9	20	11	4	90.91
?	Matched group	52	12	23	9	8	84.62

Through the Ridit check analysis: two groups of coughs relatively, U=0.5207, P>0.05; Comparison: the U=0.3012 that coughs up phlegm, P>0.05; Comparison: the U=0.1672 that pants, P>0.05; Above individual event symptom is coughed, expectorant, breathe heavily the treatment group and the matched group curative effect does not relatively have significant difference.

3.3.3 the treatment group is to body temperature and leukocytic influence

Treatment group patient temperature by treatment before (38.32 ± 0.87) ℃ reduce to (36.18 ± 0.73); Leukocyte is reduced to (7.327 ± 1.176) * 109/L by preceding (12.97 ± the 2.986) * 109/L of treatment; Significant difference (all P < 0.01) is all arranged before and after the treatment, explain that the tracheitis granule has the antipyretic and anti-inflammatory effect.

3.3.4 safety evaluatio

Treatment group and matched group have all carried out the just inspection of projects such as routine, hepatic and renal function and electrocardiogram of hematuria before and after test, do not see obvious toxic-side effects; Laboratory indexes is abnormal before seeing test, and test back laboratory indexes is unusual.Tracheitis granule drug safety is described.

4 conclusions

Tracheitis is that mucous secretion increases owing to infect or trachea, bronchial mucosa inflammatory that non-infective agent causes change, clinically with cough, cough up phlegm or be principal character with panting.The primary disease early symptom is lighter, and how in the winter time outbreak alleviate after the spring is warm, and the course of disease is slow, so do not note for people.Late period lesion growth, during concurrent obstructive emphysema, the pulmonary function sustain damage, unhealthful and the labour force is very big.Primary disease is one of China's common frdquently encountered disease, and regular incidence is in the middle-aged and elderly people more than 40 years old, and the smoking patient is higher than south apparently higher than the non-smoking patient in China prevalence north, and the rural area is high slightly than the city sickness rate.Chinese medicine has certain curative effect and remarkable advantages at the treatment primary disease, and the acute and chronic bronchitic special effect Chinese preparation of exploitation treatment is significant, and the treatment of China aspect Chinese medicine antitussive, the disease of relievining asthma, eliminate the phlegm obtained certain achievement.

The specific embodiment

Embodiment 1

1, gets Herba Ephedrae 4.5g, tangerine 5.5g, Radix Codonopsis 5.0g, Bulbus Fritillariae Cirrhosae 2.0g, Semen Armeniacae Amarum 2.5g, honey-fried FLOS FARFARAE 1.8 g, Fructus Aristolochiae 1.8 g, Radix Peucedani 1.8 g, Radix Polygalae 2.0g, Fructus Schisandrae Chinensis 1.8g;

2, each medical material is cleaned, dries, weighed by proportioning, mix;

3, decocte with water is 3 times, adds water 426ml for the first time, decocts 2 hours; For the second time add water 310ml, decocted 1 hour; Add water 310ml for the third time, decocted 1 hour, filter, it is 1.08 that filtrating is concentrated into relative density; Add precipitant ethanol, make the alcohol amount that contains of filtrating reach 60%, static 24 hours, get supernatant; It is 1.38 thick paste that filtrating is concentrated into relative density, with 38.8g sucrose, 9.7g dextrin and 9.7g thick paste mixing granulation, 50 ℃ of dryings; Granulate, packing, every bag 10 gram.

Embodiment 2

1, gets Herba Ephedrae 45g, tangerine 55g, Radix Codonopsis 50g, Bulbus Fritillariae Cirrhosae 20g, Semen Armeniacae Amarum 25g, honey-fried FLOS FARFARAE 18 g, Fructus Aristolochiae 18 g, Radix Peucedani 18 g, Radix Polygalae 20g, Fructus Schisandrae Chinensis 18g;

2, each medical material is cleaned, dries, weighed by proportioning, mix;

3, decocte with water is 3 times, adds 4260ml for the first time, decocts 2 hours; For the second time add water 3100ml, decocted 1 hour; Add water 3100ml for the third time, decocted 1 hour, filter, it is 1.10 that filtrating is concentrated into relative density; Add precipitant ethanol, make filtrating to contain the alcohol amount be 60%, static 24 hours, get supernatant; Filtrating is concentrated into the thick paste of relative density 1.41, with 388g sucrose, 97g dextrin and 97g thick paste mixing granulation, 50 ℃ of dryings; Granulate, packing, every bag 10 gram.

The detection test of tracheitis granular mass standard

The tracheitis granule is made up of kinds of traditional Chinese medicines such as Herba Ephedrae, Semen Armeniacae Amarum, Radix Peucedani, Flos Farfaraes, is the cipher prescription of my institute, has good relieving cough and asthma, the removing heat-phlegm effect.Effect with nourishing YIN and moistening the lung, relieving cough and resolving phlegm, it is full vexed to be used for lung-heat cough with asthma, tachypnea asthma, accumulation and obstruction of sputum, septum pectorale that affection of exogenous wind-cold causes clinically.Herba Ephedrae is these article monarch drug, and the content Chang Zuowei of ephedrine estimates medical material quanlity, guarantees the leading indicator of drug safety and preparation quality standard.In order better to control and improve the quality standard of said preparation, this paper adopts thin layer chromatography (TLC) discriminating side's epheday intermedia and Fructus Pruni effective ingredient earnestly, has set up Determination of Ephedrine Hydrochloride assay method in Herba Ephedrae medical material and the tracheitis granule after deliberation.

One, instrument and reagent

Waters 600 high performance liquid chromatographs; 486 detectors; PC 800 chromatographic work stations; AS3120A supersound extraction device; Cross 0.45ul mocromembrane filter; Ephedrine hydrochloride, amygdaloside (Nat'l Pharmaceutical & Biological Products Control Institute); Tracheitis granule (certain hospital, lot number); Methanol is chromatographically pure, and water is the redistillation deionized water, and other reagent are analytical pure.　

Two, TLC differentiates

1. the discriminating of Herba Ephedrae

1.1 TLC formulations prepared from solutions: get tracheitis granule 1.0g, add strong ammonia solution number droplet, add chloroform 10ml again, heating in water bath refluxed 1 hour, filters, and the filtrating evaporate to dryness, residue adds methanol 2ml shake well, filters, and filtrating is as tracheitis granule need testing solution.Take by weighing each medical material in the prescription ratio, by production technology preparation self-control tracheitis granule extractum, take by weighing extractum 0.65g, the tracheitis of preparation self-control by the same method granule need testing solution.Other gets the ephedrine hydrochloride reference substance, adds methanol and processes the solution that every 1ml contains 1mg, as reference substance solution.Get scarce Herba Ephedrae negative sample 2.0 g, process negative control solution with method.According to the thin layer chromatography test, draw above 3 kinds of each 5ul of solution respectively, put on same silica gel thin-layer plate; With chloroform one methanol, one strong ammonia solution (20:5:0.5) is developing solvent; Launch, take out, dry; Spray is with 0.2% ninhydrin solution, and it is clear to develop the color to speckle in about 5 minutes 105 ℃ of bakings.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the punctation of same color, negative control is noiseless on the relevant position.

1.2 TLC condition: silica gel G-CMC lamellae; Developing solvent: chloroform-methanol-liquor ammoniae fortis (20: 5: 0.5); Point sample amount: test liquid 5～10 μ L, contrast liquid 5 μ L; Colour developing: ninhydrin solution, 105 ℃ of about 5 min of baking.Results sample, control medicinal material, reference substance speckle unanimity, negative no ephedrine speckle

2. amygdalate discriminating

2.1 TLC formulations prepared from solutions: get these article powder 1.0 g, add petroleum ether 30 mL and make dissolving, heating in water bath refluxed 1 hour, discarded petroleum ether liquid; Residue volatilizes after washing with petroleum ether 25mL, adds methanol 30 mL, heating extraction 0.5 hour; Be placed to room temperature, filter, filtrating is as need testing solution.Other gets Herba Ephedrae control medicinal material 2 g, gets the amygdaloside reference substance in addition according to medical material solution in pairs with legal system, adds methanol and processes 2.0 mg/mL, as reference substance solution.Get scarce Semen Armeniacae Amarum negative sample 2.0g, get negative control solution with legal system.According to thin layer chromatography test, draw respectively need testing solution and negative control solution each 5, reference substance solution 2 L; Point is developing solvent with 5-10 ℃ of lower floor's solution of placing 12 h of chloroform one ethyl acetate one methanol, one water (15:40:22:10) on the lamellae of same silica gel G, launches; Take out, spray immediately that (phosphomolybdic acid 2 g add water 20 mL and make dissolving with the phosphomolybdic acid sulfuric acid solution; Slowly add sulphuric acid 30 mL again, mixing), it is clear to be heated to speckle colour developing at 105 ℃.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color, negative control is noiseless on the relevant position.

2.2 TLC condition: silica gel G-CMC lamellae; Developing solvent: chloroform one ethyl acetate one methanol, one water (15:40:22:10); Point sample amount: test liquid 5～10 μ L, contrast liquid 5 μ L; Colour developing: phosphomolybdic acid sulfuric acid solution, 105 ℃ of about 5 min of baking.Results sample, control medicinal material, reference substance speckle unanimity, blank no amygdaloside speckle.

Three, HPLC differentiates

1. the preparation of chromatographic condition and test liquid

1.1 chromatographic condition

Chromatographic column: the SpherisorbC18 post (5 μ m, 4.6mm * 250mm); Mobile phase: 0.01mol.L-1 potassium dihydrogen phosphate-methanol-triethylamine (95: 5: 0.02), it is 2.5 that phosphoric acid is transferred pH; Detect wavelength: 210nm; Sample size 10ul; Flow velocity: 1.0mL.min-1; Column temperature: 30 ℃.

The preparation of need testing solution

Get the tracheitis granule and take by weighing weight 0.63g, put in the 25ml volumetric flask, add mobile phase to scale, supersound process 40min (power 200W, frequency 50HZ) is put coldly, supplies weightlessness with above-mentioned mobile phase, is settled to the scale scale, promptly gets tracheitis granule need testing solution.

Take by weighing each medical material in the prescription ratio,, take by weighing extractum 0.65g, the preparation of the tracheitis of preparation self-control by the same method granule need testing solution 1.3 reference substance solution by production technology preparation self-control tracheitis granule extractum

Precision takes by weighing ephedrine hydrochloride reference substance 3.4mg, puts in the 25mL volumetric flask, adds the mutual-assistance dissolving of flowing, and supersound process (24 ℃, frequency 50HZ) 30min gets hydrochloric ephedrine 0.136mgmL ^-1Solution promptly gets.

1.4 the preparation of negative control solution

Remove the tracheitis granule Herba Ephedrae negative sample of Herba Ephedrae by tracheitis granule prescription and process preparation, process negative control solution according to the need testing solution method for preparing.

2. selectivity test

Draw each 10 μ L of reference substance solution, need testing solution and negative control solution, injecting chromatograph respectively, chromatograph result show the negative control solution chromatograph with reference substance chromatographic peak relevant position on do not disturb.

3. the investigation of linear relationship

Respectively accurately draw 0.5,1,1.5,2.0,3.0,5.0mL puts in the 25mL measuring bottle, is diluted to scale with mobile phase, makes that hydrochloric ephedrine is 2.72,5.44,8.16,10.88 among every 1mL, the reference substance solution of 16.32,27.20 μ g.The accurate reference substance solution 10 μ L that draw variable concentrations inject high performance liquid chromatograph; Record peak area, (μ g) is abscissa with the ephedrine hydrochloride sample size, and peak area is a vertical coordinate drawing standard curve; Getting regression equation is Y=18488X+13980; R=0.9995, result show ephedrine hydrochloride in the scope of sample size 0.027～0.27 μ g, and linear relationship is good.

4. precision and replica test

The accurate reference substance solution 10 μ L that draw repeat sample introduction 5 times, and recording the average peak area integrated value is 20 571, and RSD is 0.65% (n=5); Same lot sample article are carried out 5 times measure, trying to achieve RSD is 1.41%.

5. assay

Accurate self-control tracheitis granule need testing solution, tracheitis granule need testing solution and each 10ul of ephedrine hydrochloride reference substance solution (0.136 mgmL) of drawing measures by above-mentioned chromatographic condition, calculates.The result makes that ephedrine hydrochloride content (mgg) is respectively 1.49,1.52,1.29 (n=3) in the sample by oneself, and ephedrine hydrochloride content (mgg) is respectively 0.157,0.159,0.176 (n=3) in the tracheitis granule.

6. discuss

Through TLC method qualitative identification tracheitis granule epheday intermedia, Semen Armeniacae Amarum effectively, blank noiseless, specificity is strong, and favorable reproducibility overcomes the shortcoming that alkaloid test-tube reaction in the ministry standard, amygdaloside are differentiated the specificity difference.

Herba Ephedrae has the effect of relieving cough and asthma, and is identical with our medical knowledge, therefore chooses the contained ephedrine of Herba Ephedrae as the assay index.

Compared in the water-bath and refluxed and ultrasonic two kinds of method for distilling, the gained result proves that supersound extraction is complete, and easy and simple to handle, and fluid infusion is few, so adopt ultrasonic extraction.Adopt the content of high effective liquid chromatography for measuring ephedrine, operate comparatively simple, accuracy, favorable reproducibility.

Claims (2)

1. Chinese medicine preparation that is used to treat tracheitis is characterized in that being prepared from following raw material and weight portion proportioning:

4.5 parts in Herba Ephedrae, 5.5 parts of dried tangerine peels, 5.0 parts of Radix Codonopsis, 2.0 parts of Bulbus Fritillariae Cirrhosae, 2.5 parts in Semen Armeniacae Amarum, 1.8 parts of honey-fried FLOS FARFARAEs, 1.8 parts of Fructus Aristolochiaes, 1.8 parts of Radix Peucedanis, 2.0 parts of Radix Polygalaes, 1.8 parts of Fructus Schisandrae Chinensis;

Above-mentioned medical material is processed thick paste behind water extract-alcohol precipitation, 1 part of thick paste adds 1 part in dextrin, 4 parts of sucrose.

2. method for preparing the Chinese medicine preparation that is used to treat tracheitis according to claim 1, by following processing step preparation:

1) get above-mentioned ten flavor raw medicinal materials, oven dry is weighed by proportioning, mixes;

2) decocte with water is three times, and for the first time amount of water is 11 times of medical material weight, decocts 2 hours; For the second time amount of water is 8 times of medical material weight, decocts 1 hour; Amount of water is 8 times of medical material weight for the third time, decocts 1 hour;

3) collecting decoction filters, and it is 1.08～1.10 that filtrating is concentrated into relative density, add ethanol make filtrating to contain the alcohol amount be 60%, left standstill 24 hours, get supernatant liquid filtering, reclaim ethanol, filtrating is concentrated into the thick paste of relative density 1.38～1.41;

4) in the ratio of 4:1:1 with sucrose, dextrin and thick paste mixing granulation, 50～60 ℃ of dryings, granulate, packing.