CN104922564B

CN104922564B - A kind of preparation method for treating medicine pill lungy

Info

Publication number: CN104922564B
Application number: CN201510259867.3A
Authority: CN
Inventors: 杨劝生; 杨岩; 胥顺堂
Original assignee: GANSU TIANSHUI QIHUANG PHARMACEUTICAL Co Ltd
Current assignee: GANSU TIANSHUI QIHUANG PHARMACEUTICAL Co Ltd
Priority date: 2015-05-20
Filing date: 2015-05-20
Publication date: 2019-03-22
Anticipated expiration: 2035-05-20
Also published as: CN104922564A

Abstract

The invention discloses a kind of preparation methods for treating medicine pill lungy, the multifunctional extracting pot that glutinous rehmannia, Rehmannia glutinosa, asparagus fern, the sweet tuber of stemona, Radix Ophiopogonis, prepared RADIX ET RHIZOMA RHEI, bletilla, eight taste medicine materical crude slice of Radix Glehniae are put into built-in ultrasonic generator is decocted and is extracted three times, filtrate is concentrated to get thick paste A；By vinegar tortoise plastron, oyster, vinegar turtle shell, keel, amethyst, bulbus fritillariae cirrhosae Six-element coarse crushing are forged into particle, then by high speed stagewise pulverizing grading machine, to crushing material at 45um fine powder below；Donkey-hide gelatin, beeswax are utilized respectively liquid nitrogen frozen pulverizer to crushing material into 45um particle below, obtained fine powder and particle are mixed to get medicinal powder B；Medicinal powder B is mixed with thick paste A 3.5:1 in mass ratio, and softwood is made in addition auxiliary material, with active carbon coating, polishing up to pill.The method of the present invention, which can shorten, leaches time limit, the release conducive to effective component, and product quality can be improved, and reduces production cost, shortens the production cycle, reduces energy consumption.

Description

A kind of preparation method for treating medicine pill lungy

Technical field

The invention belongs to pharmaceutical technology fields, and in particular to a kind of preparation method for treating medicine pill lungy.

Background technique

Tuberculosis is modern medicine title, and motherland's medicine has accumulated clinical experience abundant to this disease, is existed for tubercle bacillus A kind of chronic infectious disease caused by intrapulmonary belongs to a kind of special inflammation, there is the tubercle bacillus affection of various approach: including Air flue, blood, lymphatic system and directly erosion.Since the fifties, though China's fashion trend lungy has decline, each department The control of epidemic situation is still uneven, is still when previous public health problem outstanding, is one of national ten big Death causes.

Effectively treat phthisical drug, mainly Western medicine；Such as streptomysin, rimifon, rifampin, ethambutol, different cigarette Hydrazine etc., the successive synthesis of these drugs more enable the number of global lunger be greatly decreased, but Western medicine generally have it is biggish Toxic side effect.Chinese medicine then thinks that the disease of tuberculosis the five internal organs is visible, but is easy to invade with the internal organs of lesion mainly in lung, therefore claims It is tuberculosis；And the tuberculosis in bone occurs, it is called bone tuberculosis.Tuberculosis primary symptom is cough, hemoptysis, hectic fever, night sweat, body It is gradually thin.Clinic with damage and exhaustion of lung-YIN be it is common, even also showing fire excess from yin deficiency, deficiency of both qi and yin, yin-yang deficiency, treatment should be trained with qi-restoratives Member and treating tuberculosis and killing worm are principle, treat big method based on enriching yin, and qi-restoratives is with emphasis on lung, while tonifying spleen and kidney tonifying, hyperactivity of fire it is simultaneous clear Fire, deficiency of vital energy person's tonifying Qi simultaneously, yin-yang deficiency then nourishment for vitality, and also tcm methods treatment has treating both manifestation and root cause of disease, Small side effects Effect, thus urgently research and develop the treating tuberculosis class Chinese medicine of good effect Small side effects.

Currently, the tuberculous bolus sold in the market mainly uses traditional condensed pill production technology, have in production to the kind It is lower to imitate ingredient release rate, it is longer to leach the time limit, containing animal drugs such as tortoiseshell, turtle shells in prescription, in process of production to micro- life The control higher cost of object limit index.So being badly in need of a kind of raising product inherent quality, reducing production cost, energy consumption is reduced, Reduce the production technology of environmental pollution.

Summary of the invention

The present invention is longer for the time limit there are effective component release rate is lower, is leached in the production of existing tuberculous bolus, because containing The animal pharmaceuticals such as tortoiseshell, turtle shell, in process of production to the control higher cost of microbial limit index the problems such as, it is therefore intended that A kind of preparation method for treating medicine pill lungy is provided.

The present invention is realized especially by following scheme:

A kind of preparation method for treating medicine pill lungy, including following preparation method:

1) pharmaceutical formulation is weighed by weight:

Active component: 150 parts of vinegar tortoise plastron, sweet 150 parts of the tuber of stemona, 100 parts of vinegar turtle shell, forge 50 parts of amethyst, 100 parts of glutinous rehmannia, 100 parts of Rehmannia glutinosa, 50 parts of asparagus fern, 100 parts of Radix Glehniae, 100 parts of oyster, 100 parts of donkey-hide gelatin, 50 parts of keel, 50 parts of Radix Ophiopogonis, beeswax 100 parts, 25 parts of prepared RADIX ET RHIZOMA RHEI, 100 parts of bletilla, 100 parts of bulbus fritillariae cirrhosae；

Auxiliary material: 10 parts of active carbon, 0.84 part of river wax, 10 parts of sucrose, 20 parts of talcum powder；

2) medicinal material processing:

A. tortoise plastron and turtle shell: sand is set in pot, is heated to the sliding benefit of sand, when being easy to stir, investment size stepping with high heat Only tortoise plastron or turtle shell are fried to matter shortcake, and surface weeds out sand in faint yellow taking-up, and slightly leaching picks up in investment vinegar liquid while hot, drying for standby；

B. the tuber of stemona: weighing refined honey, and after adding a small amount of boiled water to dilute, leaching is mixed thoroughly in the net tuber of stemona, slightly bored, non-sticky with being fried with slow fire When hand, taking-up is cooled；

C. amethyst；Amethyst is put to be fired in pot and is popular in, is put into vinegar while hot, cooling is allowed to crispy suddenly.

3) glutinous rehmannia, Rehmannia glutinosa, asparagus fern, the sweet tuber of stemona, Radix Ophiopogonis, prepared RADIX ET RHIZOMA RHEI, bletilla, eight taste medicine materical crude slice of Radix Glehniae are put into built-in super The multifunctional extracting pot of acoustic generator, which decocts, to be extracted three times, and it is 1.30~1.35 that filtrate, which is concentrated into relative density, obtains thick paste A；

4) by vinegar tortoise plastron, oyster, vinegar turtle shell, keel, forge amethyst, the coarse crushing of bulbus fritillariae cirrhosae Six-element at < 15mm particle, then By high speed stagewise pulverizing grading machine, to crushing material at 45um fine powder below；By donkey-hide gelatin, that beeswax is utilized respectively liquid nitrogen is cold Freeze pulverizer to crushing material into 45um particle below, obtained fine powder and particle are mixed to get medicinal powder B；

5) medicinal powder B is mixed with thick paste A 3.5:1 in mass ratio, mixing temperature is controlled at 20~30 DEG C, is refined into suitable system The softwood of ball, pill, 70~80 DEG C of drying are made coating slurry with active carbon, sucrose and 20 parts of purified waters, dry ball are set coating In pot, coating pan is opened, coating slurry is added by several times, is sprinkled into talcum powder for the side Bian Xuanzhuan, drying of drying, repeatedly repeatedly, packet Clothing is finished slurry, dries layer by layer to 10 to 16 layers, spreads people's river wax, bottling sealing, packaging.

The Rehmannia glutinosa is produced by the following method: taking clean radix rehmanniae recen that yellow rice wine is added to mix thoroughly, every 100 kilograms of radix rehmanniae recens With 30 kilograms of yellow rice wine, set closed in tank, it is in corvinus gloss, taste turns sweet tea, takes out drying for standby that water proof is ignorant to be exhausted to wine.

The prepared RADIX ET RHIZOMA RHEI is produced by the following method: taking rheum officinale block to be mixed thoroughly with yellow rice wine, every 100kg rheum officinale yellow rice wine 30kg, until closed in tank, water proof is ignorant to taking out drying when being in dark brown inside and outside rheum officinale.

Every 100kg tortoise plastron or turtle shell vinegar 20kg in step (2)；Every 100kg tuber of stemona refined honey 12.5kg；Every 100kg is purple Quartz vinegar 20-30kg.

Extraction described in step (3) is specially to add 60 DEG C of the water ultrasonic extractions 60 minutes of 10 times of medicine materical crude slice amounts for the first time three times, The another device storage of extracting solution is collected, second of dregs of a decoction adds 65 DEG C of the water ultrasonic extraction 45 minutes of 8 times of medicine materical crude slice amounts, collects extracting solution, the The dregs of a decoction add 70 DEG C of the water ultrasonic extraction 30 minutes of 6 times of medicine materical crude slice amounts three times, collect extracting solution, will extracting solution filtering mixing three times.

The invention has the benefit that ultrasonic wave extraction, traditional Chinese medicine fine powder micronization technology to be used for the production work of tuberculous bolus Skill substitutes original decocting method technique by ultrasonic wave extraction, traditional Chinese medicine fine powder is micronized production technology and substitutes common traditional Chinese medicine Powder production technology is beaten, can shorten and leach time limit, the release conducive to effective component, product quality can be improved, reduces production cost, contracting Short production cycle reduces energy consumption.

Specific embodiment

The present invention will be further explained with reference to the examples below, as described below, is only to preferable implementation of the invention Example, not limits the present invention, any person skilled in the art is possibly also with the disclosure above Technology contents be changed to the equivalent embodiment changed on an equal basis.Without departing from the concept of the present invention, according to the present invention Technical spirit any simple modification or equivalent variations that following embodiment is made, fall within the scope of protection of the present invention.

Embodiment 1

A kind of preparation method for treating medicine pill lungy, is completed especially by following procedure:

1) tuberculous bolus prescription:

Vinegar tortoise plastron 150g, sweet tuber of stemona 150g, vinegar turtle shell 100g, amethyst 50g, glutinous rehmannia 100g, Rehmannia glutinosa 100g, asparagus fern are forged 50g, Radix Glehniae 100g, oyster 100g, donkey-hide gelatin 100g, keel 50g, Radix Ophiopogonis 50g, beeswax 100g, prepared RADIX ET RHIZOMA RHEI 25g, bletilla 100g, Bulbus fritillariae cirrhosae 100g.Auxiliary material: active carbon 10g, river wax 0.84g, sucrose 10g, talcum powder 20g.

2) medicinal material processing:

Tortoise plastron: sand is set in pot, is heated to the sliding benefit of sand with high heat, when being easy to stir, is put into the net tortoise plastron of size stepping, fry To matter shortcake, surface weeds out sand in faint yellow taking-up, and slightly leaching picks up (every 100kg tortoise plastron vinegar 20kg) in investment vinegar liquid while hot, does It is dry.

Turtle shell: sand is set in pot, is heated to the sliding benefit of sand with high heat, when being easy to stir, is put into the net turtle shell of size stepping, fry To matter shortcake, appearance weeds out sand in buff taking-up, and slightly leaching picks up (every 100kg turtle shell vinegar 20kg) in investment vinegar liquid while hot, does It is dry.

Rehmannia glutinosa: taking clean radix rehmanniae recen that yellow rice wine is added to mix thoroughly, and (every 100 kilograms of radix rehmanniae recens with yellow rice wine 30 kilograms) is set close in tank It closes, it is in corvinus gloss that water proof is ignorant to be exhausted to wine, and taste turns sweet tea, takes out drying.

The tuber of stemona: every 100kg tuber of stemona weighs refined honey 12.5kg, and after adding a small amount of boiled water to dilute, leaching is mixed thoroughly in the net tuber of stemona, slightly It is bored, be fried with slow fire do not touch with one's hand when, taking-up cools.

Amethyst；Amethyst is put to be fired in pot and is popular in, puts into (every 100kg amethyst vinegar 20- in vinegar while hot 30kg), cooling is allowed to crispy suddenly.

Prepared RADIX ET RHIZOMA RHEI: rheum officinale block is taken to mix (every 100kg rheum officinale yellow rice wine 30kg) thoroughly with yellow rice wine, until closed in tank, water proof is ignorant extremely Drying is taken out when inside and outside rheum officinale being in dark brown.

3) production technology:

Glutinous rehmannia is weighed by recipe quantity, Rehmannia glutinosa, asparagus fern, the sweet tuber of stemona, Radix Ophiopogonis, prepared RADIX ET RHIZOMA RHEI, bletilla, eight taste medicine materical crude slice of Radix Glehniae are set Multifunctional extracting pot (built-in ultrasonic generator), which decocts, to be extracted three times.For the first time plus 60 DEG C of ultrasonic extractions 60 of water of 10 times of medicine materical crude slice amounts are divided Clock collects the another device storage of extracting solution, and second of dregs of a decoction adds 65 DEG C of the water ultrasonic extraction 45 minutes of 8 times of medicine materical crude slice amounts, collect extracting solution, The third time dregs of a decoction add 70 DEG C of the water ultrasonic extraction 30 minutes of 6 times of medicine materical crude slice amounts, collect extracting solution.It extracting solution filtering will mix three times, Filtrate is concentrated into the thick paste of relative density 1.30~1.35, and paste-forming rate is 35% or more.

Vinegar tortoise plastron is weighed by recipe quantity, oyster, vinegar turtle shell, keel, forges amethyst, bulbus fritillariae cirrhosae, donkey-hide gelatin, eight taste of beeswax drink Piece by vinegar tortoise plastron, oyster, vinegar turtle shell, keel, is forged amethyst, the coarse crushing of bulbus fritillariae cirrhosae Six-element into the fine powder (particle) of < 15mm, then is led to High speed stagewise pulverizing grading machine is crossed, using motor high speed rotation, generates centrifugal force, is made between material, impact hammer head and liner plate Between gap location impacted, rubbed, collided, sheared, to crushing material at 45um fine powder below (particle)；By donkey-hide gelatin, Beeswax is utilized respectively liquid nitrogen frozen pulverizer to crushing material into 45um particle below.

Medicinal powder made of above-mentioned steps and thick paste (ratio is about 3.5:1) are mixed, mixing temperature is controlled at 18~25 DEG C, Add appropriate auxiliary material, mix, softwood of the refining at suitable pill, pill controls ball and weighs about as 1.85g/10 ball (1.75~1.95g/ 10 balls), 70~80 DEG C of drying, with active carbon coating, polishing, bottling sealing, packaging.It sets at shady and cool, dry, it is moisture-proof.

Medicinal powder and thick paste mixing temperature are higher, product to leach the time limit longer because containing donkey-hide gelatin, beeswax etc. in medicinal powder Colloidality ingredient is easily gelatinized if temperature is higher, is increased medicament viscosity, is influenced the time limit that leaches of product, therefore mixing temperature should be controlled System also complies with D grades of clean area production control temperature requirement conditions, at 18~25 DEG C to guarantee product quality.

Below by way of the beneficial effect of the experiment selected drug that comes that the present invention is further explained, test includes drug one of the present invention The pharmacodynamic experiment of kind tuberculous bolus.

2 Tuberculosis in vitro nuclear tests of embodiment

1) experimental material:

1. drug: experimental group: embodiment 1 prepares tuberculous bolus；Control group: tuberculous bolus (honeyed bolus) 0.56/g containing crude drug, by sweet Respectful sky and water qi xanthate industry limited liability company system is standby, and rifampin leads to pharmaceuticals's (Shanghai Xinyi everything medicine company purchased from Lanzhou nine divisions of China in remote antiquity Limited liability company's production).

2. animal: Kun Ming mice 210~220, half male and half female is provided by pharmaceutical college, Lanzhou University.

3. bacterial strain: mycobacterium tuberculosis H37RV (Yycobaclercum tuberc-ulosis~H37RV) and human-like point Branch bacillus is introduced by tuberculosis prevention and treatment research institute, Gansu Province, passes on Roche ovum gallinaceum inclined-plane, and 37 DEG C are cultivated two weeks for test With.

2) test method:

1. minimum inhibitory concentration (MIC): experimental group and control group are soaked in distilled water respectively, set in 60 DEG C of water-baths, Heat preservation 8 hours, cooling, centrifugation, separates supernatant, and high pressure sterilization is spare.

Rifampin is dissolved through a small amount of dimethylformamide (DMP), and for constant volume in volumetric flask, high pressure sterilization is spare.

Referring to " antituberculotic experimental method " in vitro test, above-mentioned solution and Roche basal liquid are mixed, 2 times of series are made into Each liquor strength is diluted, 85 DEG C of discontinuous sterilizations are twice.In inclined plane inoculating 1X10^-3The uniform bacterium of mg/ml hangs 0.1ml, final to be inoculated with Amount is 10³Viable bacteria unit (CFU), 37 DEG C are cultivated two weeks, have no the minimum concentration (MIC, mg/ml) of mycobacterium tuberculosis, Li Fu Flat minimum concentration is consistent with reported in literature.

2. mouse half animal survival time (ST₅₀)

It is treated referring to " antituberculotic experimental method " animality, selects Kunming hybrid small white mouse, each batch of the weight of animals difference is not More than ± 2g, general weight is 16~18g, and half male and half female is random to be grouped, every group 10, by experimental group and control group administration group It is respectively 3 groups, dosage are as follows: 2.116g/kg weight, 1.732g/kg weight, 1.384g/kg weight；Through caudal vein infection one Strain M. tuberculosis mycobacteria H37RV virulent experimental strain 0.5mg (weight in wet base, containing about viable bacteria unit 10⁶).After infection from the 4th day Gastric infusion is administered by 0.4ml/20g weight, twice a day, successive administration 3 days, groups of animals death toll is recorded, by Litch- Each group half animal survival time and its 95% fiducial limit are asked in the mapping of fieldShi method.

3. half animal effective dose (ED₅₀G/kg weight)

Animal selects same ST₅₀Experiment, animal is grouped at random, every group 10, and experimental group and control group are respectively 5 groups, administration Dosage are as follows: 2.703g/kg weight, 2.116g/kg weight, 1.732g/kg weight, 1.384g/kg weight, 1.215g/kg weight, It separately sets and does not treat control group and rifampin control group, rifampicin treatment control group dosage is 10 × 10^-3.Through caudal vein infection one Strain M. tuberculosis mycobacteria H₃₇The virulent experimental strain 0.5mg of RV, gastric infusion, records mouse survival situation, meter once a day Each administration group mouse survival percentage when all animals death of non-administration control group is calculated, is asked by probability unit method (Bliss) Half animal effective dose and 95% fiducial limit.

4. animal and test method ST₅₀, each dosage experiments group half animal survival time is calculated, acquires each dose as the following formula Amount group ST₅₀Percentage extends:

With the ST of each dosage group₅₀Percentage is extended for ordinate, and the logarithm of dosage is abscissa, does regression straight line side Journey obtains ST₅₀%, 100%, 200% extends required dosage, acquires ST via following formula₅₀Percentage prolonged dose coefficient:

5. result is as follows:

1 experimental group of table and control group are to M. tuberculosis mycobacteria and Bacillus tuberculosis in Roche ovum gallinaceum culture medium The minimum concentration of H37RV compares (MIC, mg/ml)

	Experimental group	Control group
			M. tuberculosis mycobacteria	35.24±1.66	40.23±1.98
Bacillus tuberculosis H₃₇R_V	0.48±0.04	0.71±0.05

2 experimental group of table and control group anti-mouse acute experiment expression activitiy

3 experimental group of table and control group ED₅₀Expression activitiy

4 experimental group of table and control group extend active ratio to infectivity experiment tuberculosis mouse half animal survival time percentage Compared with

The results showed that two kinds of dosage forms in vitro with stronger anti-tubercular, experimental group are shown in Mice Body It is substantially better than control group, through statistical test, difference is statistically significant (P < 0.05).And experimental group have it is easy to carry, It is ideal drug that convenient to take, the advantages that stability is preferable, which is a kind of,.

3 animal acute toxicity test of embodiment

1) experimental material:

1. drug and reagent: the preparation gained tuberculous bolus of embodiment 1 is mentioned by Gansu Tianshui Qihuang Pharmaceutical Co., Ltd. For after grinding drug plus distilled water is made into 40% suspension, for zoopery.

2. animal: Kunming mouse, male and female have concurrently, 20 ± 2g, and by Lanzhou, medical college is provided.

2) method:

Acute toxicity testing: 20 ± 2g Kun Ming mice 30, half male and half female, after being deprived of food but not water 12 hours, Ig40% tuberculous bolus suspension 35ml/kg (maximum concentration, maximum capacity) the upper and lower noon is each primary, is observed continuously 7 days.

3) result:

Mouse be administered in one day it is secondary, total dosage be 35g crude drug/kg.d.Observation 7 days, behavior without exception occur, do not go out What incumbent poisoning symptom；Mouse feed, excrement, fur are normal, and vegetative activity is good, none dead mouse.Gross necropsy master Want internal organs no abnormality seen.Obtaining the maximum day dosis tolerata of mouse ig is 35g crude drug/kg, and the clinic for being equivalent to recommendation appoints the 186 of dose Times；Show that LD50 > 35g crude drug/kg, i.e. tuberculous bolus acute toxicity are small.

4 long term toxicity test of embodiment

1) experimental material:

1. drug and reagent: 1 method of embodiment preparation gained tuberculous bolus, every gram of 1.25g containing crude drug are yellow by Tianshui city qi Medicine company Co., Ltd provides；After grinding plus distilled water is made into 40% suspension, for zoopery.DL- alanine, sulphur Acid every, 2,4- dinitrophenylhydrazine be Beijing Chemical Plant's product；Other reagents are that commercially available analysis is pure.

2. animal: Wistar big white mouse, 5~6 week old, half male and half female are provided by Beijing Experimental Animal Center.

3. instrument: 721 type spectrophotometers (manufacture of Shanghai third analysis instrument factory).

2) method:

Wistar big white mouse, 80~100g of weight are adapted to after a week in laboratory, and tail point takes hematometry SGPT, selects just Healthy white rat 120 of normal range, are divided into 3 groups, every group 40, male and female each 20 by gender, weight and SGPT value equilibrium.By Acute experiment can not measure LD the result shows that the medicine toxicity is lower₅₀.According to " drug registration management method " (office enables No. 28) and Pertinent regulations in " Chinese medicine, natural medicinal formulations long term toxicity investigative technique guideline ", if high and low dose group and control group.

1. high dose experimental group: being administered as 4.0g crude drug/kg, which is that (2.116g is raw for the high dose of pharmacodynamics test Medicine/kg) 2 times, be the 1/8.41 of the maximum day dosis tolerata of intragastric administration on mice, be equivalent to and recommend clinical day for human beings dosage (9.0g/ days) 27.2 times.

2. low dosage experimental group: being administered as 1.5g crude drug/kg, which is slightly above the low dosage of pharmacodynamics test (1.384g crude drug/kg) is the 1/21.6 of the maximum day dosis tolerata of intragastric administration on mice, is equivalent to recommendation clinical day for human beings dosage (9.0g/ Day) 10 times.

3. control group: giving 5ml/kg physiological saline.

4. operation: every morning, ig was primary, 6 days weekly, continuous 180 days；Growth of animal situation, general behavior are observed, often Week weighing is primary；Tail point is adopted standby when before administration and 60 days, 120 days, 180 days after administration, checks blood picture and hepatic and renal function.180 days When sacrificed by decapitation half animal, remaining half puts to death after stopping administration observation 2 weeks.The animal progress gross necropsy of execution, coring, Liver, lung, spleen, kidney, small intestine, testis or uterus are fixed with 10% formalin, carry out pathological examination after HF dyeing.Such as high dose Group has obvious poisoning symptom or damage, and drug withdrawal carries out every measurement again after two weeks and checks, to observe the invertibity of damage.

3) conclusion:

1. the long-time service of this medicine has no significant effect the growth and development of rat, to immune organ (thymus gland, spleen) weight without aobvious Writing influences.

2. the long-time service of this medicine has no significant effect Rat Erythrocytes, leucocyte, platelet counts, content of hemoglobin It has no significant effect.

3. the long-time service of this medicine does not damage rat Liver and kidney function.

4. long-term administration is to rat important organ such as stomach, small intestine, the heart, liver,spleen,kidney, testis, uterus etc. without obvious shadow It rings.

5. prompting the safe range of the medicine larger according to Mouse Acute Toxicity and results of pharmacodynamic test.Therapeutic index LD50/ED50 > 24.4 (ig).

Described in summary, this medicine is curative for effect, is a kind of safely and effectively drug without apparent toxic side effect.

5 clinical test of embodiment

Clinical data: 150 typical patients of symptom for suffering from tuberculosis illness, this 150 trouble are collected throughout the country 107 people of person male, 43 people of women is oldest 68 years old, 18 years old the smallest, and average age 46 years old.Patient is randomly divided into two Group, experimental group carry out clinical trial with Chinese medicine prepared by the present invention.

Treatment method: preparing gained pill using embodiment 1 and treated, taken orally 20 tablets each time, two times a day, warm water It takes；Bone tuberculosis patient per is taken medicine with deer horn glue 15g decoction.Control group is set up, control group is referred to using national tuberculosis prevention and treatment Therapeutic scheme as defined in south carries out clinical trial.

The course for the treatment of: treatment group 2 months is as a treatment course, generally needs 3 courses for the treatment of or more；Control group is treated according to as defined in " guide " Cheng Jinhang.

Criterion of therapeutical effect: it is classified according to the symptom situation of change and cardinal symptom of patient.

Recovery from illness: symptom eliminates, sputum bacteria is more than continuous half a year negative, x-ray rabat lesion hypersorption, and erythrocyte sedimentation rate is normal.

Effective: symptom substantially eliminates, sputum conversion, and x-ray rabat lesion absorbs 1/3 or more, and cavity is closed, and erythrocyte sedimentation rate is normal.

Effective: symptom improves, and sputum conversion or reduction, x-ray rabat lesion are slightly shown in absorption or stable earlier above, and erythrocyte sedimentation rate slows down.

Invalid: rabat, sputum bacteria, erythrocyte sedimentation rate, symptom are without improvement, or only certain symptoms slightly improver.

Treatment results statistics such as table 5, for two groups of validity through Chi-square Test, difference is not statistically significant, prompts the present invention Prepared Chinese medicine has certain therapeutic effect to tuberculosis.

The comparison of table 5 experimental group and control group clinical test

Group	n	Recovery from illness	It is effective	Effectively	In vain
						Control group	75	21	48	5	1
Experimental group	75	56	17	2	0

Embodiment 6

1) 1 sample of Example, finely ground, set microscopically observation: light yellow irregular fragment is clear to, and surface has superfine Texture (vinegar tortoise plastron, vinegar turtle shell).There are minimum black hole, microbend (oyster) in the translucent fragment of colourless or yellowish-brown, surface.Shallowly The translucent tablet of yellow is clear to, and surface has micro-texture (donkey-hide gelatin).Colourless or brown ambiguity fragment, surface have irregularly And have granular substance (keel).

2) 1 sample 10g of Example, it is finely ground, add methanol 40ml, be ultrasonically treated 20 minutes, filtration, filtrate is evaporated, residue Add water 10ml just to dissolve, then plus hydrochloric acid 1ml, set in water-bath and heat 30 minutes, cool down immediately, with ether shaking extract 2 times, every time 20ml merges ether solution, is evaporated, residue adds chloroform 1ml to make to dissolve, as test solution.Separately take rheum officinale control medicinal material 0.1g is made in the same way of control medicinal material solution.Rhein reference substance is taken again, adds methanol that solution of every 1ml containing 1mg is made, as right It according to product solution, is tested according to thin-layered chromatography (one annex VI B of Chinese Pharmacopoeia version in 2010), it is each to draw above-mentioned three kinds of solution 5ul is put respectively on the silica gel H lamellae in same using sodium carboxymethylcellulose as binder, with petroleum ether (30~60 DEG C)- The upper solution of acetic ether-methanoic acid (15:5:1) is solvent, is unfolded, and takes out, dries.In sample chromatogram, with compare On medicinal material and the corresponding position of reference substance chromatography, the spot of same color is shown；It sets after being smoked in ammonia steam, spot becomes red.

3) 1 sample 20g of Example, finely ground, family 90% ethyl alcohol 50ml and 2% hydrochloric acid solution 2ml are heated to reflux and keep It slightly boiled 40 minutes, places 4 hours, filtration, filtrate is concentrated to dryness, and residue adds water 5ml to make to dissolve, then enriching ammonia solution adjusts pH value To 10 or more, is extracted 2 times, each 10ml with chloroform shaking, merge chloroform liquid, be concentrated to dryness, residue adds methanol 2ml Make to dissolve, as test liquid solution, separately take tuber of stemona control medicinal material 2g, be made in the same way of control medicinal material solution, according to thin-layered chromatography (in One annex VI B of state's pharmacopeia version in 2010) test, each 10ul of above two solution is drawn, is put respectively in same silica G thin layer On plate, with chloroform-acetate-methanol (10:2:1) for solvent, it is unfolded, takes out, dry, spray is tried with bismuth potassium iodide Liquid.In sample chromatogram, on position corresponding with reference medicine chromatography, the spot of same color is shown.

4) 1 sample 10g of Example, it is finely ground, add methanol 10ml, be ultrasonically treated 30 minutes, filtration, filtrate is as test sample Solution.Bletilla striata control medicinal material 1g separately is taken, is made in the same way of control medicinal material solution, according to thin-layered chromatography (Chinese Pharmacopoeia version one in 2010 Portion annex VI B) test, each 15ul of above two solution is drawn, is put respectively on same silica gel g thin-layer plate, with petroleum ether (30 ~60 DEG C) upper solution of-acetic ether-methanoic acid (15:5:1) is solvent, it is unfolded, takes out, dry, sprays with 5% vanillic aldehyde Sulfuric acid solution heats about 5 minutes at 100 DEG C.In sample chromatogram, on position corresponding with reference medicine chromatography, show identical The spot of color.

5) 1 sample of Example is appropriate, finely ground, takes powder about 1g, accurately weighed, sets in crucible, slowly blazing to complete Carbonization, lets cool, nitric acid about 1ml is added to make to moisten, low-temperature heat to nitrogen eliminates, and gradually rises temperature to 700-800 DEG C, makes complete ash Change, let cool, add dilute hydrochloric acid 5ml, stir, make to dissolve, filters into 50ml measuring bottle, container is washed with water, and washing lotion is filtered into same amount In bottle, scale is added water to, is shaken up.Precision measures 10ml, and Calcium Disodium Versenate titrating solution (0.05mol/L) is added in precision 25ml ammoniates test solution 8ml, and the black T indicator of network is a small amount of, and being titrated to zinc titrating solution (0.05mol/L) from blue becomes aubergine, To obtain the final product.The Calcium Disodium Versenate titrating solution (0.05mol/L) of every 1ml is equivalent to the calcium of 2.004mg.The every 1g calcic of this product is not It obtains and is less than 88mg.

Claims

1. a kind of preparation method for treating medicine pill lungy, it is characterised in that the following steps are included:

1) weigh pharmaceutical formulation by weight: active component: 150 parts of vinegar tortoise plastron, 100 parts of vinegar turtle shell, forges purple at sweet 150 parts of the tuber of stemona Quartzy 50 parts, 100 parts of glutinous rehmannia, 100 parts of Rehmannia glutinosa, 50 parts of asparagus fern, 100 parts of Radix Glehniae, 100 parts of oyster, 100 parts of donkey-hide gelatin, keel 50 parts, 50 parts of Radix Ophiopogonis, 100 parts of beeswax, 25 parts of prepared RADIX ET RHIZOMA RHEI, 100 parts of bletilla, 100 parts of bulbus fritillariae cirrhosae；Auxiliary material: 10 parts of active carbon, river wax 0.84 part, 10 parts of sucrose, 20 parts of talcum powder；

2) medicinal material processing:

A. tortoise plastron and turtle shell: sand is set in pot, is heated to the sliding benefit of sand with high heat, when being easy to stir, is put into the net tortoise of size stepping First or turtle shell are fried to matter shortcake, and surface weeds out sand in faint yellow taking-up, and slightly leaching picks up in investment vinegar liquid while hot, drying for standby；

B. the tuber of stemona: weighing refined honey, and after adding a small amount of boiled water to dilute, leaching is mixed thoroughly in the net tuber of stemona, slightly bored, is not touched with one's hand with being fried with slow fire When, taking-up cools；

C. amethyst；Amethyst is put to be fired in pot and is popular in, is put into vinegar while hot, cooling is allowed to crispy suddenly；

3) glutinous rehmannia, Rehmannia glutinosa, asparagus fern, the sweet tuber of stemona, Radix Ophiopogonis, prepared RADIX ET RHIZOMA RHEI, bletilla, eight taste medicine materical crude slice of Radix Glehniae are put into built-in ultrasound hair The multifunctional extracting pot of raw device, which decocts, to be extracted three times, and it is 1.30~1.35 that filtrate, which is concentrated into relative density, obtains thick paste A；

4) by vinegar tortoise plastron, oyster, vinegar turtle shell, keel, forge amethyst, the coarse crushing of bulbus fritillariae cirrhosae Six-element into the particle of < 15mm, then pass through High speed stagewise pulverizing grading machine, to crushing material at 45um fine powder below；Donkey-hide gelatin, beeswax are utilized respectively liquid nitrogen frozen powder Obtained fine powder and particle, at 45um particle below, are mixed to get medicinal powder B to crushing material by broken machine；

5) medicinal powder B is mixed with thick paste A 3.5:1 in mass ratio, mixing temperature control is 18~25, and DEG C refining is at suitable pill Softwood, pill, 70~80 DEG C of drying are made coating slurry with active carbon, sucrose and 20 parts of purified waters, dry ball are set coating pan It is interior, coating pan is opened, coating slurry is added by several times, is sprinkled into talcum powder for the side Bian Xuanzhuan, drying of drying, repeatedly repeatedly, coating To 10 to 16 layers, it is finished slurry, is dried layer by layer, spreads people's river wax, active carbon coating, polishing, bottling sealing, packaging.

2. a kind of preparation method for treating medicine pill lungy according to claim 1, it is characterised in that: described Rehmannia glutinosa is produced by the following method: take clean radix rehmanniae recen that yellow rice wine is added to mix thoroughly, every 100 kilograms of radix rehmanniae recens with 30 kilograms of yellow rice wine, Set closed in tank, it is in corvinus gloss, taste turns sweet tea, takes out drying for standby that water proof is ignorant to be exhausted to wine.

3. a kind of preparation method for treating medicine pill lungy according to claim 1, it is characterised in that: described Prepared RADIX ET RHIZOMA RHEI is produced by the following method: take rheum officinale block to be mixed thoroughly with yellow rice wine, every 100kg rheum officinale yellow rice wine 30kg, until it is closed in tank, every Water is ignorant to taking out drying when inside and outside rheum officinale being in dark brown.

4. a kind of preparation method for treating medicine pill lungy according to claim 1, it is characterised in that: step (2) every 100kg tortoise plastron or turtle shell vinegar 20kg in；Every 100kg tuber of stemona refined honey 12.5kg；Every 100kg amethyst vinegar 20- 30kg。

5. a kind of preparation method for treating medicine pill lungy according to claim 1, it is characterised in that: step (3) extracting described in is specially 60 DEG C of the water ultrasonic extractions 60 minutes for adding 10 times of medicine materical crude slice amounts for the first time three times, and it is another to collect extracting solution Device storage, second of dregs of a decoction add 65 DEG C of the water ultrasonic extraction 45 minutes of 8 times of medicine materical crude slice amounts, collect extracting solution, and the third time dregs of a decoction add drink 70 DEG C of the water ultrasonic extraction 30 minutes of 6 times of piece amounts collects extracting solution, will extracting solution filtering mixing three times.